CA2115360A1

CA2115360A1 - Heating/cooling apparatus made of ceramics

Info

Publication number: CA2115360A1
Application number: CA002115360A
Authority: CA
Inventors: Keiichi Katoh; Syuzi Ueda
Original assignee: Individual
Current assignee: Individual
Priority date: 1992-07-01
Filing date: 1993-06-28
Publication date: 1994-01-20
Also published as: KR100346861B1; EP0603411B1; DE69320449D1; EP0603411A4; EP0603411A1; DE69320449T2; WO1994001529A1

Abstract

ABSTRACT OF THE DISCLOSURE
The present invention relates to a heating/cooling apparatus made of a ceramics, which permits a precise temperature control of an object to be heated or cooled, i.e., a sample, in accordance with a predetermined temperature pattern, and which is useful for the temperature control of a sample in such fields as biotechnology, chemistry, medicine and bioengineering.
The heating/cooling apparatus made of a ceramics of the present invention comprises: a sintered body comprising an electrically insulating ceramics and having any one of a face, at least one hole, at least one recess and at least one groove, each for receiving a sample; and a resistance-heating element as a heating means, which is buried into the sintered body. The whole of the 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 has furthermore a cooling means. According to the heating/cooling apparatus of the present invention, heat transfer from the sintered body to the sample is accomplished efficiently because of a large contact area with the sample, whereby it is possible to precisely heat and cool the sample in accordance with a predetermined temperature program, while keeping a uniform temperature distribution in the sample.

Description

J J ~

IlEA'r l NC/C()()l. I:N(G /~'I'AI~\'I'U.S MAI)I~ ' C~ AM I ('';

FIl~,r,D_OF_TIIE, _T.NVI~'.N'rION

The present invention relates to a hcating/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.

B~CKGROUND OE THE INVENTION

Various types of heating/cooling apparatus have conventionally been employed in the above-men-tioned 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 separa-te 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 dificult to achieve a desired heating pattern. The ~ ' ~ ' ' ',:' ~.' '' ~: , available cooling means or the s.~m~lc inclu~le, on ~he other hand, a spontaneous cooling, a rorced cooling wilh the use oE a coolant such as a gas or a li-~uid, and a combinat.ion thereof. It is however di.fficult to preci.sely control a cooli.ng rate by such a cooli.ng means alone. It is thus conceivable to control the cooling rate by usiny 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 eff.iciently 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 ~i 25 sample.

i~ DISCLOSURE OF THE INVENTION

. ~-- - . . . .

~7 ' , "~, ' , . . ~, .,, , ,~ ~ ' , . ~ ' ~: ~ "~.~' ~', ' ' ' ' ' ,,. ,~, . ' ' . ', ~' "' ' " '' ',, ' '' ' ~" ~ " , " ~ ", ' In the hcating/cool i.ng apparal ~Ir m~lde Or a ceram.ics Or thc present i.nvent.;.oll, at lellsl: on-~ Or a face, at least one hole, at least one rcc.ss and al lerlst.
one groove, the shape Or whi.ch co;.nc;des wi.Lh that Or an object to be heatcd or cooled, i.e., a sample, rOr receiving the sample, to increase a contact area wi.th 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 conducti.ve resistance-heat.ing 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 ¦ 20 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 ~ins, Jt~b1) provided on Lhc sintered bo(ly, and a heal-r;ldi~ll.in~J pl~lo havi.ng a honeycomb structure, provided on the sintere~
body, each for ef.r~ctin9 a heat exctlange, on th~ o~her hand. The heat-radiati.ng plate comprises any one of a metal and a cerami.cs.

According to the heating/cooli.ng 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.

BRIEF DESCRIPTION OF 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.
.

Fig. 2 is a schematic sectional view of Fig. 1 cut along the line A-A'.

; ~ ...... ' - ' '. ' . "~

b l~

Fig. 3 is a schematic cxplode~i pers~)e(tivc view il]ustratillg a manu[actur;ng process or the he.ltin-J/
cooling apparatus made of a ceramicr. o~ the rirst embodiment oF the presenL invent-ion shown in r~'ig. 1.

S Fig. ~ is a schematic descriptive view ustrating a combination of the heating/cooling ~ apparatus made oE a ceramics of the first embodiment o~
`~ the present invention shown in Fig. 1, and a coolant Eeeder.

.
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.

2 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 inven-tion shown in Fig. 6.

i . r) _ . , -b L .
~' , , '' , ~ "j"

Fi(l. ~ is 1 sc~l~nk~tic pC! rsp~cl,iv(~ Vi~!w illustrati,ng the state in which a resist<lnce-ll(;ll,in-l element is attached onto one Or Lhe two green blockf; shown in F'i 9. 8.

Fig. 10 is a schematic perspective view il]ustra-ting a heating/cooling apparatus made of a ceramics of a third embodiment ol the present invention, whi,ch comprises a sintered body made of a ceramics comprising aluminum nitride, and a heat-radiatinq plate having fins, as a cooling means.

Fig. 11 is a schematic perspective view illustrating a heating/coolinq 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 ~ ' ~ , , ' ' ' ' ' ' ~'' .. . . -.., 1 1. ) ~1 I) l~

r.~us m~d(~ c)r .~ c~ mic~ c~r l.h~ ri rt~. ~mt)-~clim-!n~ ~r ~he present i.nvention shown in Fig. I.~.

Fig. 14 is a schemat;.c perspective view illustrati.ng a green block hav;.ny holes rormed therei.n 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 inventi,on shown in Fig. 12.

Fig. 15 is a schematic descriptive view il].ustrating 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 perspec-tive 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 i.s a schematic sectional view oE Fig. 16 cut along the line A-A'.

Fig. 18 is a schematic perspective view illustrating a heating/cooling apparatus made of a ~" ' ''''"'~' ' '' '`'' -''' ' ~ , .~ J ~ i 1) U

c~r~ lics Or a s~v~llL~l c~mboc~:im~ l. Or ~ r)r~C;r~rl~
; invention, wh:ich compr i ses a si ntered body madc Or a ceramics comprising aluminum ni.l,rid(!.

Fig. 19 is a schema~ic secLional view Or Fig. 18 cut along the line A-A'.

Fig. 20 is a schematic sectional view of Fig. 18 cut along the line s-B', illustrating the heatingtcooling apparatus made of a ceramics of the seventh embodiment of the present invention shown in Fig. 18, which is attached with a sample receptacle.

DESCRIPTION OF THE PREFERRED EMBODIMENTS
"
Now, the heating/cooling apparatus made of a '' ceramics of the presen-t invention is described further in ~ detail with reference to the drawings.
., ' 15 Fig. 1 is a schematic perspective view illustrating a heating/cooling apparatus made of a ceramics of a first embodiment of the present invention, iil which comprises a sintered body made of a ceramics 3 comprising aluminum nitride, and Fig. 2 is a schematic ! 20 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 i,nvention is manufactured as follows. ~s shown in Fig. 3, holes 2 and 3 for receiving . .
/

: s sumples arc! rc)rmed in each Or yreen shec!L~; /, K ~In~l In made Or a cerami.cs comprising aluminum nitridr!. With the use o.[ a paste preparcd by kneading at le.lsl one ~owdery raw materi.al ~elected from the group cons.i.sLing or tungsten, mo]ybdenum and rhenium, a resis~ance-heatin-l element 5 i.s ormed on the sur.face of the green sh~et 8 by a method such as a screen printi.ng. Then, the green sheets 7, 8 and 10 are pi.led 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 appara~us by means of a blower 11 as a 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 .' ., .;
'', ..,' ' ~ '''"' ' ' : ... ..
, ~ i I ., c) l) lJ

to ~1 PlD (abbrevi.l~ion or proportion;ll-p]u~:-int,e-Jr;~l-.l plus-derivative) control on ~he basis Or Lhe temp(lr;l--,re measured by the thermocouple, so ~haL Lhe Lempera~llre of the test tub~ coincide w;th a taryet temperaLurc.
Electric power Or the resistance-hcating c]ement 5 was con-trolled with -the use o~ a thyristor.

The performance test was carried out as follows.
Two -test tubes filled with objec-ts 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-men-tioned 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 m~ 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 ;j 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.
.
- 25 Subsequently, a program regarding set temperatures and set periods for heating and cooling pure water, was O

j~
. . ~
. , .':, ,. .,,. '' .' - : ' , ~, ~

, . ,~ .

inpu~ ial~o c~ con~roller ror controlling ~he oper;llion Or the heating/cooli.ng apparalus. The above-mentioned program compri.sed, as shown in Fig. S: i.ncreasi.n-l the temperature of pure water to 95"C ~hereinafter rererred -to as the ".Eirst set temperature"), then keepi.ng this temperature for ten minutes (hereinafter re~erred to as the "first set period"), then decreasing the temperature of pure water to 4C (llereinafter 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 25C (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 discon-tinuing the operation of the heating/cooling apparatus.

Then, the heating/cooling apparatus was opera-ted 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 ---Il-. .

~JI,~c)~

~lh~ was k~ <1 ~c~m~c!r~ lr~ Or '~5 1 0.l"('. ~ n, upon ~he lapsc Or 20 seconds ar~er ~he fi rs~, s(~t r~erio(i, the temperature Or pure water in each Or Ihe teF.L t-lbc!s decreased ~o 4"C which was the second 5et LenlpCraLUr-`.
Then, during 60 minutes which were the second set perio(l, the temperature or pure water in each of the test tubes was kept at a temperature of 4 ~ o.l"C. Subsequently, upon the lapse Or two seconds after the second set period, the temperature of pure water in each of the test tubes increased to 25C 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 a-t a temperature of 25 ~ 0-1C, and thereafter, the operation of the heating/cooling apparatus was discontinued.

The sin-tered 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 1 20 comprising aluminum nitride. The sintered body 1 may however comprise an electrically insulating ceramics ¦ comprising at least one of silicon carbide, silicon ni-tride, 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 I ~." . ,.,,~ :.. -, :,-~, . . : .: , .
~, ' ''~ ''' ., '' .
. ~ ~' ''' ~'""'~,' ' " , '. EurL11ermore, m(ly bc aL ]easL one e1ccLr.ic.l11y cc)n~uc~ive : ceram.ics selected rrom the group consisti,n-J of si1i.con carbide, titanium ni,tride, mo1ybdcnum 5ili.cide, %irCOlliUm bori.de, ~ungsten carb.i.de and tanta1um carbi.de. In addi.tion, in the heati.ng/cool;.ng apparatus mada o~ the ceramics of the above-mentioned r;.rst embodi,ment of the : present invention, the resistance-heating element 5 is buri,ed in the form of a single layer into the sintered body 1. However, a resistance-heating element comprising ' lO a p~urality 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 illus-trating a heating/cooling appara-tus 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 lin~ 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 l9 and 20 each comprising a coiled wire made of at least one _~ .J ~ V

me~.ll selec~c!d rrorn l,bc (lroup consis,~in-l Or ~nln~ls~,erl~
~olybdenum and rhenium, are arranged on ~h(` surr.lcc Or th-`
green block 22 as shown in ~ig. 9. Then, I.he ol her rJreer block 21 is placed upon the green block 22, and as shown in Figs. 6 and 7, holes 13, 1~, 15 and 16 for receiving samples are formed by mcans 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 yas toward the heating-cooling apparatus to cool same. The temperature of the sa~ple was controlled also in the same manner as in the performance ,, : ` .

lesL Or llle heaLilul/coolinl3 ap~ara~us Or Ihe rirr;t embodiment Or the prcsent invcnl:ion. Also in the performance test Or ~he hea~ing/cooling appar;ltuf; or t~e second embodiment of the present invention, ~herc werc!
obtained excellen~ results Or the performance test as in the heatlng/cooling apparatus of the first embodiment of the present inventlon. 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 600C , 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, - l 5 -,~' ' . .. .

whic~ comprisc!s a sin~ered body madc! Or a c~r.1n1i(!~
comprisi.ng alumi.num nitride, and ~ hecl~-r~di.llin~3 p1;1te having fins, a~ a cool;ng m~ns. ~rh~ he~Lin~1/coo1in apparatus o.[ ~he ~hird cmbodiment Or the prcsent 5 invention is confi.gured by .rorming 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-menti.oned 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/coolinq apparatus made of a ceramics of the above-mentioned third embodiment of the presen-t invention was carried out in the ~ same manner as in that of the heatinq/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 ~,',' ' '' ' "'~ ' :6j :

... i 1. ~) .i 1) ll llc~l~L;I.9/cc,o~ r~ r~l~us Or thc~ ir(l ~mbc)(lim~n~ c,r ~h~
present invention, the met.lllic ~lc~t-r~di.lting pl,lte 30 having rins~ as a coolLng mcalls, llas becn descrit)c!cl a~
being provided on the lowcr surrace Or the s;nterc~ body 23. Ilowever, ~he above-mcn~ioned heat-radiating plat~ 30 may be provid~d on a sur~ace o~her 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 . - ~' ' ' ,. ~, ; . .

~' ' ~, '- ". ,., ~''' ., I i ~l)U

cool ing through-holes 38 and 39.

A perrormance test of thc heatin~/-oolin-J
apparatus made of a ceram;.cs o:f Lh~ above-menl.ion~d rourlh embodimen-t 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 o~
the present inventlon. Also in the performance tcst 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 !I from 100 to 600 C , there was available a cooling rate ; higher than tha-t of the heating/cooling apparatus of the ~i 15 first embodiment of the present invention. In the performance tes-t 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 liguid 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, ., ~ ' ' .
. - , ,,, ' ',, ` ""' ,. ~ , .
' ".

'' . , 1 1 ,, .) I) l) which comprises a s:in~ered body made Or a crr~1mi(s compri.sing silicon carbidc. rn Fig. 1.2, 40 i5 a 5intert!d body made of an e:lectrical1y conducti.vc cer.lmics comprising silicon carbidc; and 4l and 42 are ho1cs ror receiving samples. The hea~i.ng/coo1;.ng apparatus made Or a ceramics of the fi.fth embodiment of th~ 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 4Z 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 elec-trodes 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 serv.ing 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 Ei~th embodiment of the present invention was carried out in the same manner as in that of the heating/cooling appara~us made o[ a ceramics or Lhe rirst embodim~n~ Or Lh~ prcsent invention. As in the per~ormance test o~ ~he heating/cooling apparatus o r the rirst embodiment o r Lhe present invention, a blower 50 as a coolant ~eeder 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. ~lso 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 qO of the heating/cooling apparatus of the fifth embodiment of the present invention has been described above as comprising an electrically conduc-tive 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 $ --) c~ tj ~) .
; having r ins, a hea~radic~ g pla~e tlavi.ll-J cl hOllC!yCC~mt) structure, or at ]east one cooling through-hole~ a~ a ` cooling means.

;~ Fig~ 16 is a schematic perspective view illustra-ting a heating/cooling apparatus made of a ceramics of a sixth embodiment of the present invention, il wllich comprises a sintered body made of a ceramics comprising aluminum nitride, provided with at least one j peephole. In Fig. 16, 51 is a sintered body; 52 and 53 u 10 are holes for receiving samples; 5~ is an electrode; 55 and 56 are peepholes for visually and optically observing samples in test tubes, for example; and 57, 58 and 59 are coollng through-holes, as cooling means, through which a -~ coolant passes. Fig. 17 is a schematic sectional view of ¦ 15 Fig. 16 cut along the line A-A'. In Fig. 17, 63 is a resist~nce-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 , ,, , ~.. .

4;~ "';" , Y

, ~ : .. . " ~ ' " . ~, ~ ," , ~ ' .. , . i v,l L~

onc Or the s~veral kinds Or Lhc chemic.ll corn~or;ilion Or the sinter(.d body, and (2) any onc or the sevc!r.ll kin~s of the chemi.cal composi.tion Or ~he res.i.sLance-hea~ing element, as descri.bed above .in relation to ~he above-menLioned :[irst to .[ifth 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 il].ustratinq a heating/cooling apparatus made of a ceramic Or 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-ho].es 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 e].ectrode 61. Fig. 20 is a schematic sectional view of Fig. 18 cut along the line B-B', illustratinq the heating/coo].ing 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 -- 2 ~ -~ , ' ,, :' ' '.

.,~ ~b~

apF)arcllus made of a ccran1ic; or ~hc! ahc)v(!-mc!rltic)ncd seventh embodi.men~ of ~he presen~ inventi.on W.l; CclrrieCI
out in the same manner as ln Lhat of the hcati.n-l/cool:ing appara~us made of a cerami.cs of ~he fi.rst embodiment of the present inventi.on. Pure water identical wi.th that in the performance test of the heat:Lng/cooling apparatus of the firs-t embodiment of the present invention, was poured into each of the recesses for samples 65. Also in the performance test of the heati.ng/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, 1C. In the heating/cooling apparatus of the seventh embodiment of the present invention, there is used a combination of: (1) any one of the several kinds of the chemical composition o~ the sintered body, (2) any one of the several kinds of the chemical composition Or the resistance-heating element, - 2 :3 -i ~ 3~

a~ld (3) any one Or lhc several kinds o~ coolin~l means, as describcd ab~vc in rclaLion ~o tllc ~IbcJvc-menti.oned Llrst to ri ~Lh embod.i.mcnLs Or t.he pre";en~
invention.

INDUSTRIAL AppLIcAsILITy According to the heating/cooling apparatus made of a ceramics of -the presen-t invention, as described above in detail, it is possible to rapidly heat and cool various samples, to precisely control the temperature of 10 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 effec-ts in such fields 15 as biotechnology, chemistry, medicine and bioengineering, and providing industrially useful effec-ts.

'.'Y "~
: ,:, '. ' ~, ' ' ~ ' ' ' ' ' ''- -:.

Claims

Amendment of Claims According to PCT 19(1) (Rule 46) WHAT IS CLAIMED IS:

1. A heating/cooling apparatus made of a ceramics, which comprises:

a sintered body having at least one of a face, at least one hole, at least one recess and at least one groove, each for receiving an object to be heated or cooled, said sintered body comprising an electrically insulating ceramics having a thermal conductivity of at least 10 W/(m ? k); and at least one resistance-heating element serving as a heating means, which is buried into said sintered body.

2. A heating/cooling apparatus made of a ceramics, which comprises:

a sintered body having at least one of a face, at least one hole, 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 comprising any one of an electrically conductive ceramics, a metal and carbon, thereby said sintered body itself forming a resistance-heating clement serving as a heating means.

3. A heating/cooling apparatus made of a ceramics as claimed in Claim 1 or 2, wherein:

said sintered body has a cooling means.

4. A heating/cooling apparatus made of a ceramics as claimed in Claim 3, wherein:

said cooling means comprises a coolant feeder, provided outside said sintered body, for feeding a coolant to said sintered body, on the one hand, 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, through which said coolant passes, formed in said sintered body, a heat-radiating plate 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, on the other hand.

5. A heating/cooling apparatus made of a ceramics as claimed in Claim 4, wherein:

said heat-radiating plate comprises any one of a metal and a ceramics.

6. A heating/cooling apparatus made of a ceramics as claimed in Claim 4, wherein:

said at least one cooling through-hole comprises a plurality of through-holes, and each of said plurality of through-holes has a honeycomb structure.

7. A heating/cooling apparatus made of a ceramics as claimed in Claim 1 or 2, wherein:

at least one peephole 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, for receiving said object to be heated or cooled, is formed in said sintered body.

8. A heating/cooling apparatus made of a ceramics as claimed in Claim 7, wherein:

said at least one peephole is filled with any one of an optically permeable ceramics, an optically permeable glass and an optically permeable resin.

9. A heating/cooling apparatus made of a ceramics as claimed in Claim 1, wherein:

said sintered body comprises an electrically insulating ceramics comprising at least one selected from the group consisting of aluminum nitride, silicon carbide, silicon nitride, aluminum oxide and beryllium oxide.

10. A heating/cooling apparatus made of a ceramics as claimed in Claim 2, wherein:

said sintered body 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.

11. A heating/cooling apparatus made of a ceramics as claimed in Claim 1, wherein:

said resistance-heating element comprises any one of a metal, an electrically conductive ceramics and carbon.

12. A heating/cooling apparatus made of a ceramics as claimed in Claim 11, wherein:

said resistance-heating element comprises at least one metal selected from the group consisting of tungsten, molybdenum and rhenium.

13. A heating/cooling apparatus made of a ceramics as claimed in Claim 11, 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.