EP0603411B1 - Ceramic heating/cooling device - Google Patents
Ceramic heating/cooling device Download PDFInfo
- Publication number
- EP0603411B1 EP0603411B1 EP93913596A EP93913596A EP0603411B1 EP 0603411 B1 EP0603411 B1 EP 0603411B1 EP 93913596 A EP93913596 A EP 93913596A EP 93913596 A EP93913596 A EP 93913596A EP 0603411 B1 EP0603411 B1 EP 0603411B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- heating
- sintered body
- ceramics
- cooling apparatus
- cooling
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000001816 cooling Methods 0.000 title claims abstract description 165
- 238000010438 heat treatment Methods 0.000 title claims description 149
- 239000000919 ceramic Substances 0.000 title claims description 96
- 239000002826 coolant Substances 0.000 claims description 21
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 21
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 11
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 239000011733 molybdenum Substances 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 239000010937 tungsten Substances 0.000 claims description 5
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 4
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 4
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 claims description 4
- 229910021344 molybdenum silicide Inorganic materials 0.000 claims description 4
- 229910052702 rhenium Inorganic materials 0.000 claims description 4
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 4
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 229910003468 tantalcarbide Inorganic materials 0.000 claims description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 4
- 239000003814 drug Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000011056 performance test Methods 0.000 description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 238000012360 testing method Methods 0.000 description 16
- 239000000112 cooling gas Substances 0.000 description 5
- 239000010410 layer Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/22—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible
- H05B3/28—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor embedded in insulating material
- H05B3/283—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor embedded in insulating material the insulating material being an inorganic material, e.g. ceramic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L7/00—Heating or cooling apparatus; Heat insulating devices
- B01L7/52—Heating or cooling apparatus; Heat insulating devices with provision for submitting samples to a predetermined sequence of different temperatures, e.g. for treating nucleic acid samples
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F21/00—Constructions of heat-exchange apparatus characterised by the selection of particular materials
- F28F21/04—Constructions of heat-exchange apparatus characterised by the selection of particular materials of ceramic; of concrete; of natural stone
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
Definitions
- the present invention relates to a heating/cooling apparatus made of a ceramics, which permits a rapid heating and a rapid cooling of various samples in such fields as biotechnology, chemistry, medicine and bioengineering, and achievement of a precise temperature control of the sample and a uniform temperature distribution in the sample.
- a heating/cooling apparatus of any of these types, a receptacle made of a metal such as aluminum or the like for receiving an object to be heated or cooled, i.e., a sample, and a heating means are configured as two separate components. This results in a poorer heat transfer coefficiency from the heating means to the receptacle for the sample, makes it difficult to rapidly heat the sample, and furthermore, leads to a non-uniform temperature distribution in the sample. It is therefore difficult to achieve a desired heating pattern.
- the available cooling means of the sample include, on the other hand, a spontaneous cooling, a forced cooling with the use of a coolant such as a gas or a liquid, and a combination thereof. It is however difficult to precisely control a cooling rate by such a cooling means alone. It is thus conceivable to control the cooling rate by using any of the above-mentioned cooling means while supplying a prescribed heat quantity from the heating means to the sample. In this manner of cooling, however, the heat supplied by the heating means cannot be efficiently transferred to the receptacle for the sample. It is therefore difficult to rapidly decrease the sample temperature to a desired temperature, and moreover, the temperature distribution in the sample is non-uniform, resulting in difficulty in achieving a desired cooling pattern.
- An object of the present invention is therefore to provide a heating/cooling apparatus made of a ceramics, which solves the above-mentioned problems, and permits a rapid heating and a rapid cooling of various samples, allows a precise temperature control of the sample, thereby enabling a temperature control of the sample in accordance with a predetermined temperature pattern, and achieving a uniform temperature distribution in the sample.
- At least one of a face, at least one hole, at least one recess and at least one groove, the shape of which coincides with that of an object to be heated or cooled, i.e., a sample, for receiving the sample, to increase a contact area with the sample, is formed at an arbitrary position on a sintered body comprising an electrically insulating ceramics having a thermal conductivity of at least 10 W/(m ⁇ k).
- An electrically conductive resistance-heating element comprising a metal, an electrically conductive ceramics or carbon is buried into the sintered body.
- the whole of the above-mentioned sintered body may comprise an electrically conductive ceramics, thereby the sintered body itself forming a resistance-heating element as a heating means.
- the heating/cooling apparatus made of a ceramics of the present invention further comprises a cooling means.
- the cooling means comprises a coolant feeder, provided outside the sintered body, for feeding a coolant such as a gas or a liquid to the sintered body, on the one hand, and at least one of part of a surface of the sintered body, a rugged portion formed on part of a surface of the sintered body, at least one cooling through-hole, through which the coolant passes, formed in the sintered body, a heat-radiating plate having fins, provided on the sintered body, and a heat-radiating plate having a honeycomb structure, provided on the sintered body, each for effecting a heat exchange, on the other hand.
- the heat-radiating plate comprises any one of a metal and a ceramics.
- the sample is in contact with the face, at least one hole, at least one recess or at least one groove, each for receiving the sample, provided on the sintered body having a satisfactory thermal conductivity, so that the temperature of the sample rapidly becomes equal to the temperature of the sintered body, thus permitting a precise temperature control during the heating and the cooling of the sample.
- Fig. 1 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a first embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride.
- Fig. 2 is a schematic sectional view of Fig. 1 cut along the line A-A'.
- Fig. 3 is a schematic exploded perspective view illustrating a manufacturing process of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention shown in Fig. 1.
- Fig. 4 is a schematic descriptive view illustrating a combination of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention shown in Fig. 1, and a coolant feeder.
- Fig. 5 is a graph illustrating a predetermined temperature pattern in a performance test of a heating/cooling apparatus made of a ceramics.
- Fig. 6 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a second embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride.
- Fig. 7 is a schematic sectional view of Fig. 6 cut along the line A-A'.
- Fig. 8 is a schematic perspective view illustrating two green blocks for the heating/cooling apparatus made of a ceramics of the second embodiment of the present invention shown in Fig. 6.
- Fig. 9 is a schematic perspective view illustrating the state in which a resistance-heating element is attached onto one of the two green blocks shown in Fig. 8.
- Fig. 10 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a third embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, and a heat-radiating plate having fins, as a cooling means.
- Fig. 11 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a fourth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, and at least one cooling through-hole as a cooling means, formed in the sintered body.
- Fig. 12 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a fifth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising silicon carbide.
- Fig. 13 is a schematic perspective view illustrating a green block for the heating/cooling apparatus made of a ceramics of the fifth embodiment of the present invention shown in Fig. 12.
- Fig. 14 is a schematic perspective view illustrating a green block having holes formed therein for receiving objects to be heated or cooled, i.e., samples, for the heating/cooling apparatus made of a ceramics of the fifth embodiment of the present invention shown in Fig. 12.
- Fig. 15 is a schematic descriptive view illustrating a combination of the heating/cooling apparatus made of a ceramics of the fifth embodiment of the present invention shown in Fig. 12, and a coolant feeder.
- Fig. 16 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a sixth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, provided with at least one peephole.
- Fig. 17 is a schematic sectional view of Fig. 16 cut along the line A-A'.
- Fig. 18 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a seventh embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride.
- Fig. 19 is a schematic sectional view of Fig. 18 cut along the line A-A'.
- Fig. 20 is a schematic sectional view of Fig. 18 cut along the line B-B', illustrating the heating/cooling apparatus made of a ceramics of the seventh embodiment of the present invention shown in Fig. 18, which is attached with a sample receptacle.
- Fig. 1 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a first embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride
- Fig. 2 is a schematic sectional view of Fig. 1 cut along the line A-A'.
- the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention is manufactured as follows. As shown in Fig. 3, holes 2 and 3 for receiving samples are formed in each of green sheets 7, 8 and 10 made of a ceramics comprising aluminum nitride.
- a resistance-heating element 5 is formed on the surface of the green sheet 8 by a method such as a screen printing. Then, the green sheets 7, 8 and 10 are piled one upon another, and a sintered body 1 is formed by sintering these green sheets 7, 8 and 10 thus piled up.
- the sintered body 1 thus formed has a shape as shown in Fig. 1, and the side surfaces opposite to each other have electrodes 4 and 4', respectively, connected to the resistance-heating element 5.
- FIG. 4 is a schematic descriptive view illustrating a combination of the above-mentioned heating/cooling apparatus of the first embodiment of the present invention, and a coolant feeder.
- a cooling gas was supplied to the heating/cooling apparatus by means of a blower 11 as the coolant feeder.
- test tubes having a thermocouple received therein was inserted into each of the holes 2 and 3 to investigate the performance of the heating/cooling apparatus.
- Temperature of each test tube was subjected to a PID (abbreviation of proportional-plus-integral-plus-derivative) control on the basis of the temperature measured by the thermocouple, so that the temperature of the test tube coincided with a target temperature.
- Electric power of the resistance-heating element 5 was controlled with the use of a thyristor.
- the performance test was carried out as follows. Two test tubes filled with objects to be heated or cooled, i.e., samples, were inserted respectively into the holes 2 and 3 for receiving samples of the heating/cooling apparatus, and the samples were heated or cooled with the use of the above-mentioned heating/cooling apparatus in accordance with a predetermined temperature pattern as shown in Fig. 5, thereby precisely controlling the temperature of the samples. More specifically, the test tubes each receiving 1.5 ml of pure water were inserted respectively into the holes 2 and 3, each having an inside diameter agreeing with the outside diameter of the test tubes, of the heating/cooling apparatus shown in Fig. 1. A thermocouple for measuring temperature was immersed into the middle of pure water received in each of the test tubes. Pure water in each of the two test tubes showed an initial temperature of 17 °C, as measured by the thermocouple.
- a program regarding set temperatures and set periods for heating and cooling pure water was input into a controller for controlling the operation of the heating/cooling apparatus.
- the above-mentioned program comprised, as shown in Fig. 5: increasing the temperature of pure water to 95°C (hereinafter referred to as the "first set temperature”), then keeping this temperature for ten minutes (hereinafter referred to as the "first set period”), then decreasing the temperature of pure water to 4°C (hereinafter referred to as the "second set temperature”), then keeping this temperature for 60 minutes (hereinafter referred to as the "second set period”), then increasing again the temperature of pure water to 25°C (hereinafter referred to as the "third set temperature”), then keeping this temperature for 20 minutes (hereinafter referred to as the "third set period” ), and then discontinuing the operation of the heating/cooling apparatus.
- the heating/cooling apparatus was operated under the control by means of the controller, and actual changes in temperature with time of pure water received in each of the two test tubes, were measured by the thermocouple.
- the results of measurement were as follows. Upon the lapse of eight seconds after the start of operation of the heating/cooling apparatus, the temperature of pure water in each of the test tubes increased to 95 °C which was the first set temperature. Thereafter, during ten minutes which were the first set period, the temperature of pure water in each of the test tubes was kept at a temperature of 95 ⁇ 0.1°C. Then, upon the lapse of 20 seconds after the first set period, the temperature of pure water in each of the test tubes decreased to 4°C which was the second set temperature.
- the temperature of pure water in each of the test tubes was kept at a temperature of 4 ⁇ 0.1°C. Subsequently, upon the lapse of two seconds after the second set period, the temperature of pure water in each of the test tubes increased to 25°C which was the third set temperature. Then, during 20 minutes which were the third set period, the temperature of pure water in each of the test tubes was kept at a temperature of 25 ⁇ 0.1°C, and thereafter, the operation of the heating/cooling apparatus was discontinued.
- the sintered body 1 of the heating/cooling apparatus made of a ceramics of the above-mentioned first embodiment of the present invention has been described above as comprising an electrically insulating ceramics comprising aluminum nitride.
- the sintered body 1 may however comprise an electrically insulating ceramics comprising at least one of silicon carbide, silicon nitride, aluminum oxide and beryllium oxide, other than aluminum nitride.
- the material for forming the resistance-heating element 5 is not limited to at least one metal selected from the group consisting of tungsten, molybdenum and rhenium, but may be carbon, and furthermore, may be at least one electrically conductive ceramics selected from the group consisting of silicon carbide, titanium nitride, molybdenum silicide, zirconium boride, tungsten carbide and tantalum carbide.
- the resistance-heating element 5 is buried in the form of a single layer into the sintered body 1.
- a resistance-heating element comprising a plurality of layers may be buried into the sintered body 1.
- the holes 2 and 3 for receiving the samples may have any shape in any number.
- Fig. 6 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a second embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride
- Fig. 7 is a schematic sectional view of Fig. 6 cut along the line A-A'.
- the heating-cooling apparatus made of a ceramics of the second embodiment of the present invention is manufactured as follows. A powdery raw material comprising aluminum nitride is charged into a metallic mold not shown to form two green blocks 21 and 22 as shown in Fig. 8.
- resistance-heating elements 19 and 20 each comprising a coiled wire made of at least one metal selected from the group consisting of tungsten, molybdenum and rhenium, are arranged on the surface of the green block 22 as shown in Fig. 9.
- the other green block 21 is placed upon the green block 22, and as shown in Figs. 6 and 7, holes 13, 14, 15 and 16 for receiving samples are formed by means of a cutting.
- the two green blocks thus provided with the holes are sintered by a hot press method, thereby preparing a sintered body 12 made of a ceramics comprising aluminum nitride having the resistance-heating elements 19 and 20 buried therein.
- the side surfaces of the sintered body 12 are ground to expose ends of the coiled wires as the resistance-heating elements 19 and 20.
- electrodes 17 and 18 are brazed onto the ends of the coiled wires thus exposed.
- a performance test of the heating/cooling apparatus made of a ceramics of the above-mentioned second embodiment of the present invention was carried out in the same manner as in that of the heating/cooling apparatus made of the ceramics of the first embodiment of the present invention.
- a blower as a coolant feeder was arranged below the heating/cooling apparatus, thereby blowing a cooling gas toward the heating-cooling apparatus to cool same.
- the temperature of the sample was controlled also in the same manner as in the performance test of the heating/cooling apparatus of the first embodiment of the present invention.
- the heating/cooling apparatus of the second embodiment of the present invention there were obtained excellent results of the performance test as in the heating/cooling apparatus of the first embodiment of the present invention. Furthermore, the heating/cooling apparatus of the second embodiment of the present invention was improved by providing a rugged portion or fins by means of a grinding on part of the surface of the sintered body 12, and the same performance test as described above was carried out for each of such improvements. There were obtained excellent results of the performance test as in the heating/cooling apparatus of the second embodiment of the present invention. Particularly within a range of temperature of from 100 to 600°C, there was available a cooling rate higher than that in the heating/cooling apparatus of the first embodiment of the present invention.
- the holes 13, 14, 15 and 16 for receiving samples may be of any shape in any number, and the resistance-heating elements 19 and 20 may be in any number.
- Fig. 10 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a third embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, and a heat-radiating plate having fins, as a cooling means.
- the heating/cooling apparatus of the third embodiment of the present invention is configured by forming a metallic layer comprising at least one metal of copper, nickel, molybdenum and manganese on the lower surface of the heating/cooling apparatus of the above-mentioned second embodiment of the present invention, and then brazing a metallic heat-radiating plate 30 having fins, as a cooling means, onto the metallic layer.
- 23 is a sintered body; 24, 25, 26 and 27 are holes for receiving samples; and 28 and 29 are electrodes.
- a performance test of the heating/cooling apparatus made of a ceramics of the above-mentioned third embodiment of the present invention was carried out in the same manner as in that of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention. Also in the performance test of the heating/cooling apparatus of the third embodiment of the present invention, there were obtained excellent results of the performance test as in the heating/cooling apparatus of the first embodiment of the present invention. Particularly within a range of temperature of from 100 to 600°C, there was available a cooling rate higher than that of the heating/cooling apparatus of the first embodiment of the present invention.
- the metallic heat-radiating plate 30 having fins, as a cooling means has been described as being provided on the lower surface of the sintered body 23.
- the above-mentioned heat-radiating plate 30 may be provided on a surface other than the lower surface of the sintered body 23, for example, on a side surface thereof.
- the above-mentioned heat-radiating plate 30 may have a honeycomb structure in place of the fins.
- Fig. 11 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a fourth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, and at least one cooling through-hole as a cooling means, formed in the sintered body.
- the heating/cooling apparatus of the fourth embodiment of the present invention is configured by forming cooling through-holes 38 and 39 as cooling means, as shown in Fig. 11, by means of an ultrasonic working, a diamond grinding or the like, in the sintered body of the heating/cooling apparatus of the second embodiment of the present invention.
- 31 is a sintered body; 32, 33, 34 and 35 are holes for receiving samples; and 36 and 37 are electrodes.
- a cooling gas is supplied into the cooling through-holes 38 and 39.
- a performance test of the heating/cooling apparatus made of a ceramics of the above-mentioned fourth embodiment of the present invention was carried out in the same manner as in that of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention. Also in the performance test of the heating/cooling apparatus of the fourth embodiment of the present invention, there were obtained excellent results of the performance test as in the heating/cooling apparatus of the first embodiment of the present invention. Particularly within a range of temperature of from 100 to 600 °C, there was available a cooling rate higher than that of the heating/cooling apparatus of the first embodiment of the present invention.
- a cooling gas has been described as being supplied into the cooling through-holes 38 and 39 as the cooling means.
- a liquid coolant may be supplied into the cooling through-holes 38 and 39.
- a partition having a honeycomb structure may be provided as required in each of the cooling through-holes 38 and 39.
- Fig. 12 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a fifth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising silicon carbide.
- 40 is a sintered body made of an electrically conductive ceramics comprising silicon carbide; and 41 and 42 are holes for receiving samples.
- the heating/cooling apparatus made of a ceramics of the fifth embodiment of the present invention is manufactured as follows. A powdery raw material comprising an electrically conductive ceramics comprising silicon carbide is charged into a metallic mold not shown to form a green block 45 as shown in Fig. 13. Then, as shown in Fig. 14, holes 41 and 42 for receiving samples are formed in the green block 45 by means of a cutting.
- the green block 45 thus provided with the holes 41 and 42 is sintered under the known sintering conditions.
- metallic layers as electrodes 43 and 44 are attached, as shown in Fig. 12, onto the opposing side surfaces of the resultant sintered body 40, respectively.
- the sintered body 40 itself forms a resistance-heating element serving as a heating means. There is no need therefore to specifically provide resistance-heating element in the sintered body 40.
- a performance test of the heating/cooling apparatus made of a ceramics of the above-mentioned fifth embodiment of the present invention was carried out in the same manner as in that of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention.
- a blower 50 as a coolant feeder was arranged, as shown in Fig. 15, below the heating/cooling apparatus, thereby blowing a cooling gas toward the heating/cooling apparatus to cooling same.
- the sintered body 40 of the heating/cooling apparatus of the fifth embodiment of the present invention has been described above as comprising an electrically conductive ceramics comprising silicon carbide, but the sintered body 40 may comprise any one electrically conductive ceramics selected from the group consisting of titanium nitride, a mixture of aluminum nitride and carbon and a mixture of silicon nitride and molybdenum silicide, other than silicon carbide.
- the heating/cooling apparatus of the fifth embodiment of the present invention has been described above as having the two holes 41 and 42 for receiving samples. It is not however limited to this structure, but the holes may be of any shape in any number. It is also possible, as required, to provide the sintered body 40 with a heat-radiating plate having fins, a heat-radiating plate having a honeycomb structure, or at least one cooling through-hole, as a cooling means.
- Fig. 16 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a sixth embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride, provided with at least one peephole.
- 51 is a sintered body
- 52 and 53 are holes for receiving samples
- 54 is an electrode
- 55 and 56 are peepholes for visually or optically observing samples in test tubes, for example
- 57, 58 and 59 are cooling through-holes, as cooling means, through which a coolant passes.
- Fig. 17 is a schematic sectional view of Fig. 16 cut along the line A-A'.
- Fig. 17, 63 is a resistance-heating element.
- the heating/cooling apparatus of the sixth embodiment of the present invention it is possible to observe, through the peepholes 55 and 56, the state of samples while appropriately controlling the temperature of the samples.
- the peepholes 55 and 56 may be of any shape in any number. It is possible to form optical paths for observation by filling the peepholes 55 and 56 with any one of an optically permeable ceramics, an optically permeable glass and an optically permeable resin.
- the heating/cooling apparatus of the sixth embodiment of the present invention there is used a combination of: (1) any one of the several kinds of the chemical composition of the sintered body, and (2) any one of the several kinds of the chemical composition of the resistance-heating element, as described above in relation to the above-mentioned first to fifth embodiments of the present invention.
- the holes 52 and 53 for receiving samples may be of any shape in any number.
- Fig. 18 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramic of a seventh embodiment of the present invention, which comprises a sintered body made of a ceramics comprising aluminum nitride.
- 60 is a sintered body made of a ceramics comprising aluminum nitride;
- 61 is an electrode;
- 62 are a plurality of cooling through-holes as cooling means, through which a coolant passes.
- Fig. 19 is a schematic sectional view of Fig. 18 cut along the line A-A'.
- 66 is a resistance-heating element comprising tungsten, connected to the electrode 61.
- Fig. 20 is a schematic sectional view of Fig.
- FIG. 18 cut along the line B-B', illustrating the heating/cooling apparatus of the seventh embodiment of the present invention shown in Fig. 18, which is attached with a sample receptacle 64.
- Fig. 20 65 are a plurality of recesses for samples; and 62 is a cooling through-hole as a cooling means.
- a performance test of the heating/cooling apparatus made of a ceramics of the above-mentioned seventh embodiment of the present invention was carried out in the same manner as in that of the heating/cooling apparatus made of a ceramics of the first embodiment of the present invention. Pure water identical with that in the performance test of the heating/cooling apparatus of the first embodiment of the present invention, was poured into each of the recesses for samples 65. Also in the performance test of the heating/cooling apparatus of the seventh embodiment of the present invention, there was employed the same temperature controlling method as that in the performance test of the heating/cooling apparatus of the first embodiment of the present invention.
- control of temperature was effected on the basis of the temperatures of pure water measured by means of the thermocouple immersed into pure water received in each of the recesses for samples 65. Satisfactory results of the performance test were obtained in the performance test of the heating/cooling apparatus of the seventh embodiment of the present invention. An error between the temperature of pure water in each of the recesses for samples 65 and the target temperature was within ⁇ 1°C.
- heating/cooling apparatus of the seventh embodiment of the present invention there may be used a combination of: (1) any one of the several kinds of the chemical composition of the sintered body, (2) any one of the several kinds of the chemical composition of the resistance-heating element, and (3) any one of the several kinds of the cooling means, as described above in relation to the above-mentioned first to fifth embodiments of the present invention.
- the heating/cooling apparatus made of a ceramics of the present invention it is possible to rapidly heat and cool various samples, to precisely control the temperature of the sample, to keep a uniform temperature distribution in the sample, and to conduct a precise temperature control in accordance with a predetermined complicated temperature program, which was impossible by any of the conventional technologies, thus providing useful effects in such fields as biotechnology, chemistry, medicine and bioengineering, and providing industrially useful effects.
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Abstract
The invention aims at enabling various precise temperature control and programmed temperature management and control, which have been impossible by the prior art technology, thereby developing an epoch-making scientific technique and new uses and applications thereof in the field of biotechnology and the fields relating to chemistry, medicine and engineering. The device of the invention is made from a sinter with good heat conductivity, which sinter has holes or grooves for supporting an object on an arbitrary face thereof, a heat-generating resistor buried therein, and a cooling surface. This device has such a wide area of contact with the object as to permit efficient heat conduction from the device to the object. Therefore it is possible to effect rapid temperature rise and fall toward a predetermined temperature and secure a high accuracy of temperature distribution, thus realizing precise temperature control.
Description
The present invention relates to a heating/cooling
apparatus made of a ceramics, which permits a rapid
heating and a rapid cooling of various samples in such
fields as biotechnology, chemistry, medicine and
bioengineering, and achievement of a precise temperature
control of the sample and a uniform temperature
distribution in the sample.
Various types of heating/cooling apparatus have
conventionally been employed in the above-mentioned fields
for the purpose of rapidly and accurately heating and
cooling various samples under a precise temperature
control. In a heating/cooling apparatus of any of these
types, a receptacle made of a metal such as aluminum or
the like for receiving an object to be heated or cooled,
i.e., a sample, and a heating means are configured as two
separate components. This results in a poorer heat
transfer coefficiency from the heating means to the
receptacle for the sample, makes it difficult to rapidly
heat the sample, and furthermore, leads to a non-uniform
temperature distribution in the sample. It is therefore
difficult to achieve a desired heating pattern. The
available cooling means of the sample include, on the
other hand, a spontaneous cooling, a forced cooling with
the use of a coolant such as a gas or a liquid, and a
combination thereof. It is however difficult to precisely
control a cooling rate by such a cooling means alone. It
is thus conceivable to control the cooling rate by using
any of the above-mentioned cooling means while supplying a
prescribed heat quantity from the heating means to the
sample. In this manner of cooling, however, the heat
supplied by the heating means cannot be efficiently
transferred to the receptacle for the sample. It is
therefore difficult to rapidly decrease the sample
temperature to a desired temperature, and moreover, the
temperature distribution in the sample is non-uniform,
resulting in difficulty in achieving a desired cooling
pattern.
An object of the present invention is therefore to
provide a heating/cooling apparatus made of a ceramics,
which solves the above-mentioned problems, and permits a
rapid heating and a rapid cooling of various samples,
allows a precise temperature control of the sample,
thereby enabling a temperature control of the sample in
accordance with a predetermined temperature pattern, and
achieving a uniform temperature distribution in the
sample.
According to the present invention there is provided
a heating/cooling apparatus made of ceramics as defined in claims 1 and 6.
In the heating/cooling apparatus made of a
ceramics of the present invention, at least one of a
face, at least one hole, at least one recess and at least
one groove, the shape of which coincides with that of an
object to be heated or cooled, i.e., a sample, for
receiving the sample, to increase a contact area with the
sample, is formed at an arbitrary position on a sintered
body comprising an electrically insulating ceramics
having a thermal conductivity of at least 10 W/(m · k).
An electrically conductive resistance-heating element
comprising a metal, an electrically conductive ceramics
or carbon is buried into the sintered body. In the
heating/cooling apparatus made of a ceramics of the
present invention, the whole of the above-mentioned
sintered body may comprise an electrically conductive
ceramics, thereby the sintered body itself forming a
resistance-heating element as a heating means.
The heating/cooling apparatus made of a ceramics
of the present invention further comprises a cooling
means. The cooling means comprises a coolant feeder,
provided outside the sintered body, for feeding a coolant
such as a gas or a liquid to the sintered body, on the one
hand, and at least one of part of a surface of the
sintered body, a rugged portion formed on part of a
surface of the sintered body, at least one cooling
through-hole, through which the coolant passes, formed in
the sintered body, a heat-radiating plate having fins,
provided on the sintered body, and a heat-radiating plate
having a honeycomb structure, provided on the sintered
body, each for effecting a heat exchange, on the other
hand. The heat-radiating plate comprises any one of a
metal and a ceramics.
According to the heating/cooling apparatus made of
a ceramics having the construction as described above,
the sample is in contact with the face, at least one hole,
at least one recess or at least one groove, each for
receiving the sample, provided on the sintered body having
a satisfactory thermal conductivity, so that the
temperature of the sample rapidly becomes equal to the
temperature of the sintered body, thus permitting a
precise temperature control during the heating and the
cooling of the sample.
Fig. 1 is a schematic perspective view
illustrating a heating/cooling apparatus made of a
ceramics of a first embodiment of the present invention,
which comprises a sintered body made of a ceramics
comprising aluminum nitride.
Fig. 2 is a schematic sectional view of Fig. 1 cut
along the line A-A'.
Fig. 3 is a schematic exploded perspective view
illustrating a manufacturing process of the
heating/cooling apparatus made of a ceramics of the first
embodiment of the present invention shown in Fig. 1.
Fig. 4 is a schematic descriptive view
illustrating a combination of the heating/cooling
apparatus made of a ceramics of the first embodiment of
the present invention shown in Fig. 1, and a coolant
feeder.
Fig. 5 is a graph illustrating a predetermined
temperature pattern in a performance test of a
heating/cooling apparatus made of a ceramics.
Fig. 6 is a schematic perspective view
illustrating a heating/cooling apparatus made of a
ceramics of a second embodiment of the present invention,
which comprises a sintered body made of a ceramics
comprising aluminum nitride.
Fig. 7 is a schematic sectional view of Fig. 6 cut
along the line A-A'.
Fig. 8 is a schematic perspective view
illustrating two green blocks for the heating/cooling
apparatus made of a ceramics of the second embodiment of
the present invention shown in Fig. 6.
Fig. 9 is a schematic perspective view
illustrating the state in which a resistance-heating
element is attached onto one of the two green blocks shown
in Fig. 8.
Fig. 10 is a schematic perspective view
illustrating a heating/cooling apparatus made of a
ceramics of a third embodiment of the present invention,
which comprises a sintered body made of a ceramics
comprising aluminum nitride, and a heat-radiating plate
having fins, as a cooling means.
Fig. 11 is a schematic perspective view
illustrating a heating/cooling apparatus made of a
ceramics of a fourth embodiment of the present invention,
which comprises a sintered body made of a ceramics
comprising aluminum nitride, and at least one cooling
through-hole as a cooling means, formed in the sintered
body.
Fig. 12 is a schematic perspective view
illustrating a heating/cooling apparatus made of a
ceramics of a fifth embodiment of the present invention,
which comprises a sintered body made of a ceramics
comprising silicon carbide.
Fig. 13 is a schematic perspective view
illustrating a green block for the heating/cooling
apparatus made of a ceramics of the fifth embodiment of
the present invention shown in Fig. 12.
Fig. 14 is a schematic perspective view
illustrating a green block having holes formed therein for
receiving objects to be heated or cooled, i.e., samples,
for the heating/cooling apparatus made of a ceramics of
the fifth embodiment of the present invention shown in
Fig. 12.
Fig. 15 is a schematic descriptive view
illustrating a combination of the heating/cooling
apparatus made of a ceramics of the fifth embodiment of
the present invention shown in Fig. 12, and a coolant
feeder.
Fig. 16 is a schematic perspective view
illustrating a heating/cooling apparatus made of a
ceramics of a sixth embodiment of the present invention,
which comprises a sintered body made of a ceramics
comprising aluminum nitride, provided with at least one
peephole.
Fig. 17 is a schematic sectional view of Fig. 16
cut along the line A-A'.
Fig. 18 is a schematic perspective view
illustrating a heating/cooling apparatus made of a
ceramics of a seventh embodiment of the present
invention, which comprises a sintered body made of a
ceramics comprising aluminum nitride.
Fig. 19 is a schematic sectional view of Fig. 18
cut along the line A-A'.
Fig. 20 is a schematic sectional view of Fig. 18
cut along the line B-B', illustrating the heating/cooling
apparatus made of a ceramics of the seventh embodiment of
the present invention shown in Fig. 18, which is attached
with a sample receptacle.
Now, the heating/cooling apparatus made of a
ceramics of the present invention is described further in
detail with reference to the drawings.
Fig. 1 is a schematic perspective view
illustrating a heating/cooling apparatus made of a
ceramics of a first embodiment of the present invention,
which comprises a sintered body made of a ceramics
comprising aluminum nitride, and Fig. 2 is a schematic
sectional view of Fig. 1 cut along the line A-A'. The
heating/cooling apparatus made of a ceramics of the first
embodiment of the present invention is manufactured as
follows. As shown in Fig. 3, holes 2 and 3 for receiving
samples are formed in each of green sheets 7, 8 and 10
made of a ceramics comprising aluminum nitride. With the
use of a paste prepared by kneading at least one powdery
raw material selected from the group consisting of
tungsten, molybdenum and rhenium, a resistance-heating
element 5 is formed on the surface of the green sheet 8
by a method such as a screen printing. Then, the green
sheets 7, 8 and 10 are piled one upon another, and a
sintered body 1 is formed by sintering these green sheets
7, 8 and 10 thus piled up. The sintered body 1 thus
formed has a shape as shown in Fig. 1, and the side
surfaces opposite to each other have electrodes 4 and 4',
respectively, connected to the resistance-heating element
5.
Then, a performance test was carried out by using
the heating/cooling apparatus made of a ceramics prepared
as described above. Fig. 4 is a schematic descriptive
view illustrating a combination of the above-mentioned
heating/cooling apparatus of the first embodiment of the
present invention, and a coolant feeder. When heating a
sample, voltage was impressed on the electrodes 4 and 4'.
When cooling the sample, a cooling gas was supplied to the
heating/cooling apparatus by means of a blower 11 as the
coolant feeder. Each of test tubes having a thermocouple
received therein was inserted into each of the holes 2 and
3 to investigate the performance of the heating/cooling
apparatus. Temperature of each test tube was subjected
to a PID (abbreviation of proportional-plus-integral-plus-derivative)
control on the basis of the temperature
measured by the thermocouple, so that the temperature of
the test tube coincided with a target temperature.
Electric power of the resistance-heating element 5 was
controlled with the use of a thyristor.
The performance test was carried out as follows.
Two test tubes filled with objects to be heated or cooled,
i.e., samples, were inserted respectively into the holes
2 and 3 for receiving samples of the heating/cooling
apparatus, and the samples were heated or cooled with the
use of the above-mentioned heating/cooling apparatus in
accordance with a predetermined temperature pattern as
shown in Fig. 5, thereby precisely controlling the
temperature of the samples. More specifically, the test
tubes each receiving 1.5 mℓ of pure water were inserted
respectively into the holes 2 and 3, each having an
inside diameter agreeing with the outside diameter of the
test tubes, of the heating/cooling apparatus shown in
Fig. 1. A thermocouple for measuring temperature was
immersed into the middle of pure water received in each
of the test tubes. Pure water in each of the two test
tubes showed an initial temperature of 17 °C, as measured
by the thermocouple.
Subsequently, a program regarding set temperatures
and set periods for heating and cooling pure water, was
input into a controller for controlling the operation of
the heating/cooling apparatus. The above-mentioned
program comprised, as shown in Fig. 5: increasing the
temperature of pure water to 95°C (hereinafter referred
to as the "first set temperature"), then keeping this
temperature for ten minutes (hereinafter referred to as
the "first set period"), then decreasing the temperature
of pure water to 4°C (hereinafter referred to as the
"second set temperature"), then keeping this temperature
for 60 minutes (hereinafter referred to as the "second set
period"), then increasing again the temperature of pure
water to 25°C (hereinafter referred to as the "third set
temperature"), then keeping this temperature for 20
minutes (hereinafter referred to as the "third set period"
), and then discontinuing the operation of the
heating/cooling apparatus.
Then, the heating/cooling apparatus was operated
under the control by means of the controller, and actual
changes in temperature with time of pure water received in
each of the two test tubes, were measured by the
thermocouple. The results of measurement were as follows.
Upon the lapse of eight seconds after the start of
operation of the heating/cooling apparatus, the
temperature of pure water in each of the test tubes
increased to 95 °C which was the first set temperature.
Thereafter, during ten minutes which were the first set
period, the temperature of pure water in each of the test
tubes was kept at a temperature of 95 ± 0.1°C. Then,
upon the lapse of 20 seconds after the first set period,
the temperature of pure water in each of the test tubes
decreased to 4°C which was the second set temperature.
Then, during 60 minutes which were the second set period,
the temperature of pure water in each of the test tubes
was kept at a temperature of 4 ± 0.1°C. Subsequently,
upon the lapse of two seconds after the second set
period, the temperature of pure water in each of the test
tubes increased to 25°C which was the third set
temperature. Then, during 20 minutes which were the
third set period, the temperature of pure water in each of
the test tubes was kept at a temperature of 25 ± 0.1°C,
and thereafter, the operation of the heating/cooling
apparatus was discontinued.
The sintered body 1 of the heating/cooling
apparatus made of a ceramics of the above-mentioned first
embodiment of the present invention, has been described
above as comprising an electrically insulating ceramics
comprising aluminum nitride. The sintered body 1 may
however comprise an electrically insulating ceramics
comprising at least one of silicon carbide, silicon
nitride, aluminum oxide and beryllium oxide, other than
aluminum nitride. The material for forming the
resistance-heating element 5 is not limited to at least
one metal selected from the group consisting of tungsten,
molybdenum and rhenium, but may be carbon, and
furthermore, may be at least one electrically conductive
ceramics selected from the group consisting of silicon
carbide, titanium nitride, molybdenum silicide, zirconium
boride, tungsten carbide and tantalum carbide. In
addition, in the heating/cooling apparatus made of the
ceramics of the above-mentioned first embodiment of the
present invention, the resistance-heating element 5 is
buried in the form of a single layer into the sintered
body 1. However, a resistance-heating element comprising
a plurality of layers may be buried into the sintered
body 1. In the heating/cooling apparatus of the above-mentioned
first embodiment of the present invention, the
holes 2 and 3 for receiving the samples may have any
shape in any number.
Fig. 6 is a schematic perspective view
illustrating a heating/cooling apparatus made of a
ceramics of a second embodiment of the present invention,
which comprises a sintered body made of a ceramics
comprising aluminum nitride, and Fig. 7 is a schematic
sectional view of Fig. 6 cut along the line A-A'. The
heating-cooling apparatus made of a ceramics of the
second embodiment of the present invention is
manufactured as follows. A powdery raw material
comprising aluminum nitride is charged into a metallic
mold not shown to form two green blocks 21 and 22 as
shown in Fig. 8. Then, resistance- heating elements 19 and
20 each comprising a coiled wire made of at least one
metal selected from the group consisting of tungsten,
molybdenum and rhenium, are arranged on the surface of the
green block 22 as shown in Fig. 9. Then, the other green
block 21 is placed upon the green block 22, and as shown
in Figs. 6 and 7, holes 13, 14, 15 and 16 for receiving
samples are formed by means of a cutting. Thereafter, the
two green blocks thus provided with the holes are
sintered by a hot press method, thereby preparing a
sintered body 12 made of a ceramics comprising aluminum
nitride having the resistance- heating elements 19 and 20
buried therein. Then, the side surfaces of the sintered
body 12 are ground to expose ends of the coiled wires as
the resistance- heating elements 19 and 20. Then,
electrodes 17 and 18 are brazed onto the ends of the
coiled wires thus exposed.
A performance test of the heating/cooling
apparatus made of a ceramics of the above-mentioned second
embodiment of the present invention was carried out in
the same manner as in that of the heating/cooling
apparatus made of the ceramics of the first embodiment of
the present invention. As in the performance test of the
heating/cooling apparatus of the first embodiment of the
present invention, a blower as a coolant feeder was
arranged below the heating/cooling apparatus, thereby
blowing a cooling gas toward the heating-cooling
apparatus to cool same. The temperature of the sample was
controlled also in the same manner as in the performance
test of the heating/cooling apparatus of the first
embodiment of the present invention. Also in the
performance test of the heating/cooling apparatus of the
second embodiment of the present invention, there were
obtained excellent results of the performance test as in
the heating/cooling apparatus of the first embodiment of
the present invention. Furthermore, the heating/cooling
apparatus of the second embodiment of the present
invention was improved by providing a rugged portion or
fins by means of a grinding on part of the surface of the
sintered body 12, and the same performance test as
described above was carried out for each of such
improvements. There were obtained excellent results of
the performance test as in the heating/cooling apparatus
of the second embodiment of the present invention.
Particularly within a range of temperature of from 100 to
600°C, there was available a cooling rate higher than
that in the heating/cooling apparatus of the first
embodiment of the present invention. In the
heating/cooling apparatus of the second embodiment of the
present invention, the holes 13, 14, 15 and 16 for
receiving samples may be of any shape in any number, and
the resistance- heating elements 19 and 20 may be in any
number.
Fig. 10 is a schematic perspective view
illustrating a heating/cooling apparatus made of a
ceramics of a third embodiment of the present invention,
which comprises a sintered body made of a ceramics
comprising aluminum nitride, and a heat-radiating plate
having fins, as a cooling means. The heating/cooling
apparatus of the third embodiment of the present
invention is configured by forming a metallic layer
comprising at least one metal of copper, nickel,
molybdenum and manganese on the lower surface of the
heating/cooling apparatus of the above-mentioned second
embodiment of the present invention, and then brazing a
metallic heat-radiating plate 30 having fins, as a cooling
means, onto the metallic layer. In Fig. 10, 23 is a
sintered body; 24, 25, 26 and 27 are holes for receiving
samples; and 28 and 29 are electrodes.
A performance test of the heating/cooling
apparatus made of a ceramics of the above-mentioned third
embodiment of the present invention was carried out in the
same manner as in that of the heating/cooling apparatus
made of a ceramics of the first embodiment of the present
invention. Also in the performance test of the
heating/cooling apparatus of the third embodiment of the
present invention, there were obtained excellent results
of the performance test as in the heating/cooling
apparatus of the first embodiment of the present
invention. Particularly within a range of temperature of
from 100 to 600°C, there was available a cooling rate
higher than that of the heating/cooling apparatus of the
first embodiment of the present invention. In the
heating/cooling apparatus of the third embodiment of the
present invention, the metallic heat-radiating plate 30
having fins, as a cooling means, has been described as
being provided on the lower surface of the sintered body
23. However, the above-mentioned heat-radiating plate 30
may be provided on a surface other than the lower surface
of the sintered body 23, for example, on a side surface
thereof. Furthermore, the above-mentioned heat-radiating
plate 30 may have a honeycomb structure in place of the
fins.
Fig. 11 is a schematic perspective view
illustrating a heating/cooling apparatus made of a
ceramics of a fourth embodiment of the present invention,
which comprises a sintered body made of a ceramics
comprising aluminum nitride, and at least one cooling
through-hole as a cooling means, formed in the sintered
body. The heating/cooling apparatus of the fourth
embodiment of the present invention is configured by
forming cooling through- holes 38 and 39 as cooling means,
as shown in Fig. 11, by means of an ultrasonic working, a
diamond grinding or the like, in the sintered body of the
heating/cooling apparatus of the second embodiment of the
present invention. In Fig. 11, 31 is a sintered body; 32,
33, 34 and 35 are holes for receiving samples; and 36 and
37 are electrodes. When cooling samples with the use of
the heating/cooling apparatus of the fourth embodiment of
the present invention, a cooling gas is supplied into the
cooling through- holes 38 and 39.
A performance test of the heating/cooling
apparatus made of a ceramics of the above-mentioned fourth
embodiment of the present invention was carried out in
the same manner as in that of the heating/cooling
apparatus made of a ceramics of the first embodiment of
the present invention. Also in the performance test of
the heating/cooling apparatus of the fourth embodiment of
the present invention, there were obtained excellent
results of the performance test as in the heating/cooling
apparatus of the first embodiment of the present
invention. Particularly within a range of temperature of
from 100 to 600 °C, there was available a cooling rate
higher than that of the heating/cooling apparatus of the
first embodiment of the present invention. In the
performance test of the heating/cooling apparatus of the
fourth embodiment of the present invention, a cooling gas
has been described as being supplied into the cooling
through- holes 38 and 39 as the cooling means. However, a
liquid coolant may be supplied into the cooling through- holes
38 and 39. A partition having a honeycomb structure
may be provided as required in each of the cooling
through- holes 38 and 39.
Fig. 12 is a schematic perspective view
illustrating a heating/cooling apparatus made of a
ceramics of a fifth embodiment of the present invention,
which comprises a sintered body made of a ceramics
comprising silicon carbide. In Fig. 12, 40 is a sintered
body made of an electrically conductive ceramics
comprising silicon carbide; and 41 and 42 are holes for
receiving samples. The heating/cooling apparatus made of
a ceramics of the fifth embodiment of the present
invention is manufactured as follows. A powdery raw
material comprising an electrically conductive ceramics
comprising silicon carbide is charged into a metallic
mold not shown to form a green block 45 as shown in Fig.
13. Then, as shown in Fig. 14, holes 41 and 42 for
receiving samples are formed in the green block 45 by
means of a cutting. Subsequently, the green block 45 thus
provided with the holes 41 and 42 is sintered under the
known sintering conditions. Then, metallic layers as
electrodes 43 and 44 are attached, as shown in Fig. 12,
onto the opposing side surfaces of the resultant sintered
body 40, respectively. In the heating/cooling apparatus
of the fifth embodiment of the present invention, the
sintered body 40 itself forms a resistance-heating element
serving as a heating means. There is no need therefore
to specifically provide resistance-heating element in the
sintered body 40.
A performance test of the heating/cooling
apparatus made of a ceramics of the above-mentioned fifth
embodiment of the present invention was carried out in the
same manner as in that of the heating/cooling apparatus
made of a ceramics of the first embodiment of the present
invention. As in the performance test of the
heating/cooling apparatus of the first embodiment of the
present invention, a blower 50 as a coolant feeder was
arranged, as shown in Fig. 15, below the heating/cooling
apparatus, thereby blowing a cooling gas toward the
heating/cooling apparatus to cooling same. Also in the
performance test of the heating/cooling apparatus of the
fifth embodiment of the present invention, there were
obtained excellent results of the performance test as in
the heating/cooling apparatus of the first embodiment of
the present invention.
The sintered body 40 of the heating/cooling
apparatus of the fifth embodiment of the present invention
has been described above as comprising an electrically
conductive ceramics comprising silicon carbide, but the
sintered body 40 may comprise any one electrically
conductive ceramics selected from the group consisting of
titanium nitride, a mixture of aluminum nitride and
carbon and a mixture of silicon nitride and molybdenum
silicide, other than silicon carbide. The heating/cooling
apparatus of the fifth embodiment of the present
invention has been described above as having the two holes
41 and 42 for receiving samples. It is not however
limited to this structure, but the holes may be of any
shape in any number. It is also possible, as required, to
provide the sintered body 40 with a heat-radiating plate
having fins, a heat-radiating plate having a honeycomb
structure, or at least one cooling through-hole, as a
cooling means.
Fig. 16 is a schematic perspective view
illustrating a heating/cooling apparatus made of a
ceramics of a sixth embodiment of the present invention,
which comprises a sintered body made of a ceramics
comprising aluminum nitride, provided with at least one
peephole. In Fig. 16, 51 is a sintered body; 52 and 53
are holes for receiving samples; 54 is an electrode; 55
and 56 are peepholes for visually or optically observing
samples in test tubes, for example; and 57, 58 and 59 are
cooling through-holes, as cooling means, through which a
coolant passes. Fig. 17 is a schematic sectional view of
Fig. 16 cut along the line A-A'. In Fig. 17, 63 is a
resistance-heating element. According to the
heating/cooling apparatus of the sixth embodiment of the
present invention, it is possible to observe, through the
peepholes 55 and 56, the state of samples while
appropriately controlling the temperature of the samples.
The peepholes 55 and 56 may be of any shape in any
number. It is possible to form optical paths for
observation by filling the peepholes 55 and 56 with any
one of an optically permeable ceramics, an optically
permeable glass and an optically permeable resin. In the
heating/cooling apparatus of the sixth embodiment of the
present invention, there is used a combination of: (1) any
one of the several kinds of the chemical composition of
the sintered body, and (2) any one of the several kinds
of the chemical composition of the resistance-heating
element, as described above in relation to the above-mentioned
first to fifth embodiments of the present
invention. The holes 52 and 53 for receiving samples may
be of any shape in any number.
Fig. 18 is a schematic perspective view
illustrating a heating/cooling apparatus made of a ceramic
of a seventh embodiment of the present invention, which
comprises a sintered body made of a ceramics comprising
aluminum nitride. In Fig. 18, 60 is a sintered body made
of a ceramics comprising aluminum nitride; 61 is an
electrode; and 62 are a plurality of cooling through-holes
as cooling means, through which a coolant passes.
Fig. 19 is a schematic sectional view of Fig. 18 cut
along the line A-A'. In Fig. 19, 66 is a resistance-heating
element comprising tungsten, connected to the
electrode 61. Fig. 20 is a schematic sectional view of
Fig. 18 cut along the line B-B', illustrating the
heating/cooling apparatus of the seventh embodiment of
the present invention shown in Fig. 18, which is attached
with a sample receptacle 64. In Fig. 20, 65 are a
plurality of recesses for samples; and 62 is a cooling
through-hole as a cooling means.
A performance test of the heating/cooling
apparatus made of a ceramics of the above-mentioned
seventh embodiment of the present invention was carried
out in the same manner as in that of the heating/cooling
apparatus made of a ceramics of the first embodiment of
the present invention. Pure water identical with that in
the performance test of the heating/cooling apparatus of
the first embodiment of the present invention, was poured
into each of the recesses for samples 65. Also in the
performance test of the heating/cooling apparatus of the
seventh embodiment of the present invention, there was
employed the same temperature controlling method as that
in the performance test of the heating/cooling apparatus
of the first embodiment of the present invention. More
specifically, the control of temperature was effected on
the basis of the temperatures of pure water measured by
means of the thermocouple immersed into pure water
received in each of the recesses for samples 65.
Satisfactory results of the performance test were
obtained in the performance test of the heating/cooling
apparatus of the seventh embodiment of the present
invention. An error between the temperature of pure water
in each of the recesses for samples 65 and the target
temperature was within ± 1°C. In the heating/cooling
apparatus of the seventh embodiment of the present
invention, there may be used a combination of: (1) any one of
the several kinds of the chemical composition of the
sintered body, (2) any one of the several kinds of the
chemical composition of the resistance-heating element,
and (3) any one of the several kinds of the cooling
means, as described above in relation to the above-mentioned
first to fifth embodiments of the present
invention.
According to the heating/cooling apparatus made of
a ceramics of the present invention, as described above
in detail, it is possible to rapidly heat and cool
various samples, to precisely control the temperature of
the sample, to keep a uniform temperature distribution in
the sample, and to conduct a precise temperature control
in accordance with a predetermined complicated temperature
program, which was impossible by any of the conventional
technologies, thus providing useful effects in such fields
as biotechnology, chemistry, medicine and bioengineering,
and providing industrially useful effects.
Claims (11)
- A heating/cooling apparatus made of a ceramics, which comprises:
a sintered body (1;12;23;31;51;60) having at least one of :a face, at least one hole (2,3;13-16;24-27;32-35;52,53), at least one recess (65) and at least one groove, each for receiving an object to be heated or cooled, said sintered body (1;12;23;31;51;60) comprising an electrically insulating ceramics having a thermal conductivity of at least 10 W/(m•k) ;at least one resistance-heating element (5;19,20;63) serving as a heating means, which is buried into said sintered body (1;12;23;31;51;60); anda cooling means comprising a coolant feeder (11;50), provided outside said sintered body (1;12;23;31;51;60), for feeding a coolant to said sintered body, and at least one of: part of a surface of said sintered body, a rugged portion formed on part of a surface of said sintered body, at least one cooling through-hole (38,39;57-59;62), through which said coolant passes, formed in said sintered body, a heat-radiating plate (30) having fins, provided on said sintered body, and a heat-radiating plate having a honeycomb structure, provided on said sintered body, each for effecting a heat exchange with said fed coolant. - A heating/cooling apparatus made of a ceramics as claimed in claim 1, wherein:said sintered body (1;12;23;31;51;60) comprises said electrically insulating ceramics comprising at least one selected from the group consisting of aluminum nitride, silicon carbide, silicon nitride, aluminum oxide and beryllium oxide.
- A heating/cooling apparatus made of a ceramics as claimed in claim 1 or 2, wherein:said resistance-heating element (5;19,20;63) comprises any one of a metal, an electrically conductive ceramics and carbon.
- A heating/cooling apparatus made of a ceramics as claimed in claim 3, wherein:said resistance-heating element comprises at least one metal selected from the group consisting of tungsten, molybdenum and rhenium.
- A heating/cooling apparatus made of a ceramics as claimed in claim 3, wherein:said resistance-heating element comprises at least one electrically conductive ceramics selected from the group consisting of silicon carbide, titanium nitride, molybdenum silicide, zirconium boride, tungsten carbide and tantalum carbide.
- A heating/cooling apparatus made of a ceramics, which comprises:
a sintered body (40) having at least one of :a face, at least one hole (41,42), at least one recess and at least one groove, each for receiving an object to be heated or cooled, the whole of said sintered body (40) comprising an electrically conductive ceramics, thereby said sintered body (40) itself forming a resistance-heating element serving as a heating means; anda cooling means comprising a coolant feeder (11;50) provided outside said sintered body (40), for feeding a coolant to said sintered body, and at least one of : part of a surface of said sintered body, a rugged portion formed on part of a surface of said sintered body, at least one cooling through-hole (38,39;57-59;62), through which said coolant passes, formed in said sintered body, a heat-radiating plate (30) having fins, provided on said sintered body, and a heat-radiating plate having a honeycomb structure, provided on said sintered body, each for effecting a heat exchange with the fed coolant. - A heating/cooling apparatus made of a ceramics as claimed in claim 6, wherein:said sintered body (40) comprises any one electrically conductive ceramics selected from the group consisting of silicon carbide, titanium nitride, a mixture of aluminum nitride and carbon and a mixture of silicon nitride and molybdenum silicide.
- A heating/cooling apparatus made of a ceramics as claimed in any one of the claims 1 to 7, wherein:said heat-radiating plate comprises any one of a metal and a ceramics.
- A heating/cooling apparatus made of a ceramics as claimed in any one of claims 1 to 7, wherein:said at least one cooling through-hole comprises a plurality of through-holes (57,58,59), and each of said plurality of through-holes has a honeycomb structure.
- A heating/cooling apparatus made of a ceramics as claimed in any one of the preceding claims, wherein:at least one peephole (55,56) for observing said object to be heated or cooled, which communicates with said at least one hole, said at least one recess or said at least one groove of said sintered body (1;12;23;31;40;51;60), for receiving said object to be heated or cooled, is formed in said sinted body (1;12;23;31;40;51;60).
- A heating/cooling apparatus made of a ceramics as claimed in claim 10, wherein:said at least one peephole (55,56) is filled with any one of an optically permeable ceramics, an optically permeable glass and an optically permeable resin.
Applications Claiming Priority (9)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP211937/92 | 1992-07-01 | ||
| JP21193792 | 1992-07-01 | ||
| JP21314492 | 1992-07-02 | ||
| JP213144/92 | 1992-07-02 | ||
| JP213145/92 | 1992-07-02 | ||
| JP21314592 | 1992-07-02 | ||
| JP19155393A JPH0699085A (en) | 1992-07-01 | 1993-06-23 | Ceramic heater/cooler |
| JP191553/93 | 1993-06-23 | ||
| PCT/JP1993/000881 WO1994001529A1 (en) | 1992-07-01 | 1993-06-28 | Ceramic heating/cooling device |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| EP0603411A1 EP0603411A1 (en) | 1994-06-29 |
| EP0603411A4 EP0603411A4 (en) | 1995-02-22 |
| EP0603411B1 true EP0603411B1 (en) | 1998-08-19 |
Family
ID=27475544
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP93913596A Expired - Lifetime EP0603411B1 (en) | 1992-07-01 | 1993-06-28 | Ceramic heating/cooling device |
Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP0603411B1 (en) |
| KR (1) | KR100346861B1 (en) |
| CA (1) | CA2115360A1 (en) |
| DE (1) | DE69320449T2 (en) |
| WO (1) | WO1994001529A1 (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5958349A (en) * | 1997-02-28 | 1999-09-28 | Cepheid | Reaction vessel for heat-exchanging chemical processes |
| US6074868A (en) * | 1997-03-03 | 2000-06-13 | Regents Of The University Of Minnesota | Alumina plate method and device for controlling temperature |
| US6300124B1 (en) | 1999-11-02 | 2001-10-09 | Regents Of The University Of Minnesota | Device and method to directly control the temperature of microscope slides |
| US6307186B1 (en) | 1997-04-24 | 2001-10-23 | Jean-Luc Jouvin | Hydrocolloid processing module |
| EP1279973A2 (en) * | 2001-07-21 | 2003-01-29 | Samsung Electronics Co., Ltd. | Integrated heat transfer device for planar light-wave circuit module |
| US6565815B1 (en) | 1997-02-28 | 2003-05-20 | Cepheid | Heat exchanging, optically interrogated chemical reaction assembly |
| US6602473B1 (en) | 1995-06-20 | 2003-08-05 | The Regents Of The University Of California | Temperature control apparatus |
| US6618539B2 (en) | 2000-09-25 | 2003-09-09 | Sumitomo Electric Industries, Ltd. | Heater module and optical waveguide module |
| US6635492B2 (en) | 1996-01-25 | 2003-10-21 | Bjs Company Ltd. | Heating specimen carriers |
| US6660228B1 (en) | 1998-03-02 | 2003-12-09 | Cepheid | Apparatus for performing heat-exchanging, chemical reactions |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4409436A1 (en) * | 1994-03-19 | 1995-09-21 | Boehringer Mannheim Gmbh | Process for processing nucleic acids |
| ES2151241T3 (en) * | 1996-01-25 | 2000-12-16 | Bjs Company Ltd | WARMING UP OF A SAMPLE STAND. |
| GB9616540D0 (en) * | 1996-08-06 | 1996-09-25 | Cavendish Kinetics Ltd | Integrated circuit device manufacture |
| JPH10117765A (en) * | 1996-10-18 | 1998-05-12 | Ngk Insulators Ltd | Specimen holder and its production |
| GB9712439D0 (en) * | 1997-06-17 | 1997-08-13 | Delta Theta Ltd | Heating elements |
| US7255833B2 (en) | 2000-07-25 | 2007-08-14 | Cepheid | Apparatus and reaction vessel for controlling the temperature of a sample |
| JP2018503217A (en) * | 2014-11-24 | 2018-02-01 | セラムテック ゲゼルシャフト ミット ベシュレンクテル ハフツングＣｅｒａｍＴｅｃ ＧｍｂＨ | Thermal management in the field of e-mobility |
| CN105536903A (en) * | 2015-12-24 | 2016-05-04 | 青岛顺昕电子科技有限公司 | Method for extending application range of heating device |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60256375A (en) * | 1984-05-31 | 1985-12-18 | Shimadzu Corp | Bioreactor |
| JPS6418974A (en) * | 1987-07-13 | 1989-01-23 | Ibiden Co Ltd | Production of heat-exchanger made of sintered silicon carbide |
| JPH0193472A (en) * | 1987-09-30 | 1989-04-12 | Toshiba Corp | Heat-exchanger |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4865986A (en) * | 1988-10-06 | 1989-09-12 | Coy Corporation | Temperature control apparatus |
| US4950608A (en) * | 1989-04-25 | 1990-08-21 | Scinics Co., Ltd. | Temperature regulating container |
| JPH033436U (en) * | 1989-05-30 | 1991-01-14 |
-
1993
- 1993-06-28 KR KR1019940700539A patent/KR100346861B1/en not_active IP Right Cessation
- 1993-06-28 WO PCT/JP1993/000881 patent/WO1994001529A1/en active IP Right Grant
- 1993-06-28 CA CA002115360A patent/CA2115360A1/en not_active Abandoned
- 1993-06-28 EP EP93913596A patent/EP0603411B1/en not_active Expired - Lifetime
- 1993-06-28 DE DE69320449T patent/DE69320449T2/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60256375A (en) * | 1984-05-31 | 1985-12-18 | Shimadzu Corp | Bioreactor |
| JPS6418974A (en) * | 1987-07-13 | 1989-01-23 | Ibiden Co Ltd | Production of heat-exchanger made of sintered silicon carbide |
| JPH0193472A (en) * | 1987-09-30 | 1989-04-12 | Toshiba Corp | Heat-exchanger |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6602473B1 (en) | 1995-06-20 | 2003-08-05 | The Regents Of The University Of California | Temperature control apparatus |
| US6635492B2 (en) | 1996-01-25 | 2003-10-21 | Bjs Company Ltd. | Heating specimen carriers |
| US5958349A (en) * | 1997-02-28 | 1999-09-28 | Cepheid | Reaction vessel for heat-exchanging chemical processes |
| US6565815B1 (en) | 1997-02-28 | 2003-05-20 | Cepheid | Heat exchanging, optically interrogated chemical reaction assembly |
| US6074868A (en) * | 1997-03-03 | 2000-06-13 | Regents Of The University Of Minnesota | Alumina plate method and device for controlling temperature |
| US6228634B1 (en) | 1997-03-03 | 2001-05-08 | Regents Of The University Of Minnesota | Thermal cycling or temperature control device and method using alumina plate |
| US6307186B1 (en) | 1997-04-24 | 2001-10-23 | Jean-Luc Jouvin | Hydrocolloid processing module |
| US6660228B1 (en) | 1998-03-02 | 2003-12-09 | Cepheid | Apparatus for performing heat-exchanging, chemical reactions |
| US6300124B1 (en) | 1999-11-02 | 2001-10-09 | Regents Of The University Of Minnesota | Device and method to directly control the temperature of microscope slides |
| US6618539B2 (en) | 2000-09-25 | 2003-09-09 | Sumitomo Electric Industries, Ltd. | Heater module and optical waveguide module |
| EP1279973A2 (en) * | 2001-07-21 | 2003-01-29 | Samsung Electronics Co., Ltd. | Integrated heat transfer device for planar light-wave circuit module |
| US6757452B2 (en) | 2001-07-21 | 2004-06-29 | Samsung Electronics Co., Ltd. | Integrated heat transfer device for PLC module |
Also Published As
| Publication number | Publication date |
|---|---|
| KR100346861B1 (en) | 2003-01-08 |
| DE69320449D1 (en) | 1998-09-24 |
| EP0603411A4 (en) | 1995-02-22 |
| EP0603411A1 (en) | 1994-06-29 |
| CA2115360A1 (en) | 1994-01-20 |
| DE69320449T2 (en) | 1999-02-18 |
| WO1994001529A1 (en) | 1994-01-20 |
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