CN102340900A - Electric heating element of rare earth thick film circuit based on IR-LED (Infrared Light Emitting Diode) ceramic substrate and preparation method thereof - Google Patents
Electric heating element of rare earth thick film circuit based on IR-LED (Infrared Light Emitting Diode) ceramic substrate and preparation method thereof Download PDFInfo
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- CN102340900A CN102340900A CN2011102047742A CN201110204774A CN102340900A CN 102340900 A CN102340900 A CN 102340900A CN 2011102047742 A CN2011102047742 A CN 2011102047742A CN 201110204774 A CN201110204774 A CN 201110204774A CN 102340900 A CN102340900 A CN 102340900A
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Abstract
The invention discloses an electric heating element of a rare earth thick film circuit based on an IR-LED (Infrared Light Emitting Diode) ceramic substrate and a preparation method thereof. The electric heating element is characterized by comprising a quartz ceramic substrate and serial rare earth electronic slurry. The serial rare earth electronic slurry is prepared on the quartz ceramic substrate in a form of a thick film circuit; and the thick film circuit is provided with an electrode connecting end for externally connecting with a power source. The invention has the advantages that the directly-heating type functional ceramic substrate is high in far infrared radiation efficiency, adjustable in wavelength range, uniform in temperature field, strong in thermal shock resistance, environment-friendly, efficient and energy-saving, safe and reliable as well as wide in application range.
Description
Technical field
The present invention relates to the electric heating element technical field, relate to a kind of rare earth thick film circuit electric heating element and preparation method thereof in particular.
Background technology
Efficient infrared radiation ceramic is meant ceramic material and the goods that in corresponding serviceability temperature and wider wave, have higher emissivity.Thermal radiation is also referred to as infrared radiation, is the important way that object conducts heat.Under the condition that convection current and heat conduction are restricted, it is the most effective a kind of heating and radiating mode.Therefore, improve the radiation coefficient of irradiator surface, help the reinforcement of radiant heat transfer.In other words, same high temperature conditions, the heating element liberated heat can be more, and the temperature of heating object can be higher.Different far-infrared ceramic goods have different infrared spectral characteristics; Efficient infrared radiation ceramic has excellent radiance, in aspect extensive application such as industrial energy saving, the raising infrared heater heat efficiency, spacecraft thermal control, health-care hospital, household electrical appliance.Along with developing rapidly of infrared technique, directly-heated type, energy-efficient, the research and development of high radiant rate material become focus.Efficient far-infrared radiation ceramic material enjoys attention with its superior radiance.Infrared ray is a kind of ripple, and the mid and far infrared line is the longest one section light wave with heat-flash effect of infrared ray medium wavelength.Has the different spectrum wavelength characteristic according to different elements; Select some rare earth oxide to make additive; Strengthen functional ceramic substrate electric heating element far infrared emitted energy greatly, wherein be described as the 2.5-25um wavelength ray of " sunlight lifeline ", can activate ability in the animal and plant cell.Be widely used in improve the health, field such as health care, household electrical appliance.Efficient infrared radiation ceramic material can significantly improve the far infrared radiation emissivity through the transition metal oxide of selecting the multiple inorganic compound of utilization, a spot of rare earth of interpolation and trace.At the far infrared wave segment limit, the infrared radiation of material mainly produces because of its particle vibration causes that dipole moment changes, and according to the symmetry selection rule: the symmetry during particle vibration is low more, and the variation of dipole moment is just big more, and its infrared radiation property is just strong more.In far-infared ceramic powder, add the transition metal oxide of rare earths such as Pd2O3 and Y2O3 and trace, cause distortion of lattice when forming solid solution, reduced the symmetry of vibration, it is active to have improved lattice vibration, thereby has improved the far infrared radiation emissivity of material.At present, both at home and abroad in middle high-temperature region mainly with the master that is applied as of far infrared powder coating.Specialized application in the efficient far-infrared ceramic goods that heat then seldom.Famous in the world infrared coating has the ET-4 type coating of Britain CRC company, the C-10A type of U.S. CRC company, 1100,1500 type far ultrared paints of Japanese CRC company etc.These infrared coatings all are that passive heating is produced far infrared wave by radiation, and heat source temperature height, power consumption, radiation efficiency are lower.The specific electromagnetic wave physiotherapy equipment that circulates on the Chinese society promptly so-called " refreshing lamp ".Adopt far ultrared paint on electric furnace (resistance wire) the radiation heating TDP plate, capacity usage ratio is low, the heat efficiency is low, mode of heating is backward.Chinese patent 201020055361.3 is used ceramic heater (resistance wire is cast in the ceramic body) instead and is replaced electric furnace heating TDP plate; Though improve useful life; But leakage problem is arranged, and thermal conductance and thermal expansion factor are inconsistent, and structure causes the temperature field inhomogeneous; Defectives such as radiation efficiency instability, TDP plate coating are prone to come off.Germany ELSTEIN pottery far infra-red heater adopts the method for ceramic material parcel resistance wire.Have complex forming technology, heat source temperature is high, the heat efficiency is low, infrared wavelength is adjusted deficiencies such as difficult.In efficient far infrared radiation field of electric heating; Novel heater element requires " directly-heated type ", the volume that generates heat is little, and it is big that surface thermal load is wanted, and it is high that the heat efficiency is wanted; It is fast that warm start is wanted; The infrared radiation rate wants height, temperature field to want evenly, and thermal shock resistance is eager to excel, environmental protection, low-carbon energy-saving, safe and reliable.
Summary of the invention
It is small and exquisite that the object of the invention is exactly a kind of " directly-heated type " heater that provides for the deficiency that solves prior art; Surface thermal load is big; Far-infrared radiation efficient is high, and wave-length coverage is adjustable, and the temperature field is even; Thermal shock resistance is strong, environmental protection, energy-efficient, the safe and reliable rare earth thick film circuit electric heating element based on the IR-LED ceramic substrate.
Another object of the present invention is the preparation technology of the rare earth thick film circuit electric heating element of IR-LED ceramic substrate.
The present invention adopts following technical solution to realize above-mentioned purpose: a kind of rare earth thick film circuit electric heating element based on the IR-LED ceramic substrate; It is characterized in that; It comprises quartz-ceramics substrate, serial rare-earth electric slurry; On the quartz-ceramics substrate, thick film circuit has the electrode link of external power supply to the serial rare-earth electric slurry with the prepare of thick film circuit.
As further specifying of such scheme, said quartz base plate is by quartzy (SiO
2-Al
2O
3-B
2O
3-Mg
20
3-ZrO
2) pottery and rare earth oxide composition, each oxide powder proportioning of quartz-ceramics is: SiO
293.5 Al～96.8%,
2O
31.5 B～3%,
2O
30.5 Mg～1%,
20
30.2 ZrO～0.5%,
21～2%, particle size range≤3 η m; Rare earth oxide is one or more in lanthanum, cerium, neodymium, promethium, gadolinium, erbium, scandium, yttrium and the terbium oxide.
Said series electronic slurry comprises packaging slurry, rare earth resistance slurry, rare earth electrode slurry, and the series electronic slurry is formed by function phase, inorganic adhesive phase, organic carrier.
Said rare earth resistance slurry is made up of function phase and organic carrier, and ratio is (65～85) %: (15～35) %; The function phase constituent is made up of silver-colored ruthenium palladium yttrium composite powder and microcrystalline glass powder, and ratio is (55～75): (25～45); The weight ratio of silver ruthenium palladium yttrium powder is (59～75): (15～20.5): (5～20): (0.5～5); Microcrystalline glass powder is CaO-SiO
2-Al
2O
3-B
2O
3-Bi
2O
3-La
2O
3Microcrystalline glass in series, each oxide weight of this devitrified glass is than being CaO10～35%, SiO
220～60%, Al
2O
35～35%, B
2O
31～10%, Bi
2O
310～30%, La
2O
30.3～8%; The nucleus agent is TiO
21～8%, ZrO
21～10%.
Said rare earth resistance slurry organic solvent carrier compound (weight ratio) is: terpinol 68～78%, ATBC 2～18%, ethyl cellulose 0.4～9%, NC Nitroncellulose 0.4～9%, rilanit special 0.1～6%, lecithin 0.1～6%.
Said rare earth electrode slurry is made up of solid phase composition and organic solvent carrier, and its weight ratio is (70～90) %: (10～30) %; Wherein the solid phase composition comprises silver-colored palladium yttrium composite powder and microcrystalline glass powder, and its weight ratio is (94～99.4) %: (0.6～5) %; The weight ratio of this palladium powder, silver powder and yttrium powder is (0.6～10) %: (82～99) %: (0.4～8) %; Said microcrystalline glass powder is SiO
2-Al
2O
3-CaO-B
2O
3-Bi
2O
3-La
2O
3Microcrystalline glass in series, this devitrified glass composition proportion is SiO
220～60%, Al
2O
35～35%, CaO10～35%, B
2O
31～15%, Bi
2O
310～30%, La
2O
30.3～15%, nucleus agent TiO
21～10%, ZrO
21～10%.
Said rare earth electrode slurry organic carrier prescription (weight ratio) is: terpinol 60～98%, ATBC 10～30%, ethyl cellulose 2～10%, NC Nitroncellulose 1～5%, rilanit special 0.1～5%, lecithin 0.1～5%.
Said rare earth packaging slurry is made up of solid phase composition and organic solvent carrier, and proportioning is 70～90%: 10～30%; The solid phase composition is SiO
2-Al
2O
3-CaO-B
2O
3-La
2O
3Microcrystalline glass in series, the composition proportion of each oxide are SiO
2(30～65%), Al
2O
3(5～26%), CaO (18～38%), B
2O
3(2～16%), La
2O
3(0.3～15%), Co
2O
3(0.05～6%); Nucleus agent TiO
2(1～10%), ZrO
2(1～10%).
Said rare earth packaging slurry organic carrier prescription (weight ratio) is BC 66～89%, ATBC 5～15%, ethyl cellulose 0.5～10%, rilanit special 0.1～5%, lecithin 0.1～5%.
A kind of preparation method of the rare earth thick film circuit electric heating element based on the IR-LED ceramic substrate is characterized in that it comprises following processing step:
A, ceramic substrate prepare, through laser, mill, throw, cut, processing line is processed into pdm substrate;
B, serial rare-earth electric slurry are prepared--and carry out homogenized before the printing, draw version, the silk screen printing of serial rare-earth electric slurry on ceramic substrate, process thick film circuit by process: CAD plate-making, light;
C, the preliminary treatment of wet film oxidizing atmosphere, vacuum drying 10～30 minutes, 80～180 ℃ of temperature;
Sintering in the d, the infrared crystallizing and sintering stove of oxidizing atmosphere, 50～120 ℃ of temperature rise rates/time, 750～950 ℃ of high temperature section temperature, the peak value sintering made IR-LED ceramic base rare earth thick film circuit electric heating element in 10～20 minutes;
E, laser marking laser are repaiied resistance, test, packing.
In said processing step b process, in the set-up procedure of serial rare-earth electric slurry, the preparation technology of rare earth resistance slurry wherein is:
1., crystal glass powder preparation, after mixing in R-S01 three-dimensional blender machine by oxide, nucleus agent proportioning, the smelting furnace melting; Temperature is: 1100-1450 ℃; Be incubated after 1-3 hour,, obtain the glass micro mist that little slag ball milling obtains 3 microns of particle diameters the glass melts shrend;
2., silver-colored ruthenium palladium yttrium composite powder preparation, mix in R-S03 high efficient mixed dispersing apparatus by silver-colored ruthenium palladium yttrium grain weight amount proportioning and to obtain composite powder;
3., organic carrier preparation, above-mentioned raw materials is mixed in proportion, dissolving is several hours in 80-100 ℃ water, the adjustment amount of thickener is adjusted at the viscosity of organic carrier solvent in the scope of 180-280mPaS and gets final product;
4., the rare earth resistance slurry is comprehensively modulated; The solid phase composition is made up of silver-colored ruthenium palladium yttrium composite powder and microcrystalline glass powder; By weight solid phase powder, organic carrier solvent are mixed in R-S03 high efficient mixed dispersing apparatus, carry out three-roll rolling and obtain finished product, viscosity number is 150-200PaS/RPM.
In said processing step b process, in the set-up procedure of serial rare-earth electric slurry, the preparation technology of rare earth electrode slurry wherein is:
1. crystal glass powder preparation, than oxide, nucleus agent being mixed the back melting, temperature is 1100-1450 ℃, is incubated 1 ~ 3 hour by raw material weight, and shrend obtains the little slag of glass, and ball milling obtains 3 microns glass micro mists;
2. prepare silver-colored palladium yttrium composite powder, particle diameter is 3 μ m, in the three-dimensional blender machine, mixes by weight modulation;
3. organic carrier preparation mixes the back by the raw material weight ratio and in 80 ~ 100 ℃ of water, dissolved several hours, adjustment ethyl cellulose cellulose content, and viscosity Control is in 150 ~ 280mPas scope;
4. prepare rare earth electrode slurry, it is rolling to go into three-high mill after placing R-S03 three-dimensional blender machine to mix in microcrystalline glass powder, silver-colored palladium yttrium composite powder, organic solvent carrier in proportion, obtains rare earth electrode slurry, viscosity 150-200PaS/RPM.
In said processing step b process, in the set-up procedure of serial rare-earth electric slurry, the preparation technology of rare earth packaging slurry wherein is:
1. prepare the rare earth microcrystalline glass powder: with oxide, nucleus agent melting after mixing, smelting temperature is by weight ratio: 1100-1450 ℃, be incubated after 90-180 minutes, and the shrend of coming out of the stove obtains the little slag of glass; The little slag of ball milling glass is prepared the microcrystalline glass powder of 3 microns of particle diameters;
2. prepare the organic solvent carrier, mix by proportioning, melting bath number hour in 80-100 ℃ water, adjustment ethyl cellulose cellulose content is adjusted at the viscosity of organic carrier in the scope of 150-28OmPaS;
3. packaging slurry modulation, place R-S03 three-dimensional blender machine to mix by weight ratio solid phase composition and the organic solvent carrier after, the rolling finished product that obtains of three rods, viscosity number is 150-200PaS/RPM.
The beneficial effect that the present invention adopts above-mentioned technical solution to reach is:
Substrate of the present invention is a high radiant rate far-infrared function ceramic substrate; The series electronic slurry with the prepare of thick film circuit on substrate; The prescription and the technology of preparing thereof of high radiant rate far-infrared function ceramic substrate, rare earth packaging slurry, rare earth resistance slurry, rare earth electrode slurry are also disclosed simultaneously; " directly-heated type " functional ceramic substrate far-infrared radiation efficient is high, and wave-length coverage is adjustable, and the temperature field is even; Thermal shock resistance is strong, environmental protection, energy-efficient, safe and reliable, applied range.
Description of drawings
Fig. 1 is a structural representation of the present invention;
Fig. 2 is a side-looking structural representation of the present invention.
Description of reference numerals: 1, quartz-ceramics substrate 2, thick film circuit 3, electrode link.
Embodiment
Like Fig. 1, shown in Figure 2; A kind of rare earth thick film circuit electric heating element of the present invention based on the IR-LED ceramic substrate; Comprise quartz-ceramics substrate 1, serial rare-earth electric slurry; On substrate 1, thick film circuit 2 has the electrode link 3 of external power supply to said serial rare-earth electric slurry with the prepare of thick film circuit 2.This serial rare-earth electric slurry comprises packaging slurry, electrode slurry, resistance slurry, and the series electronic slurry is formed by function phase, inorganic adhesive phase, organic carrier.Behind the rare earth thick film circuit power connection, the quartz-ceramics substrate high efficient radiation infrared-ray that directly generates heat.
One, the preparation of quartz-ceramics substrate
Quartz-ceramics baseplate material composition is: high purity quartz (SiO
2-Al
2O
3-B
2O
3-Mg
20
3-ZrO
2) pottery and rare earth oxide composition, each oxide powder proportioning of quartz-ceramics is: SiO
293.5%～96.8%:Al
2O
33～1.5%:B
2O
31～0.5%:Mg
20
30.5～0.25%:ZrO
22～1%: granularity≤3 η m.Adopt to annotate and coagulate method of forming cured and prepared, dry, sintering forms.Rare earth oxide is one or more in lanthanum, cerium, neodymium, promethium, gadolinium, erbium, scandium, yttrium and the terbium oxide.Rare earth oxide can be according to the requirement to electrical property, hot property, chemical property, mechanical performance and far-infrared functional of the quartz-ceramics substrate of different size, different temperatures, different purposes; Add the rare earth oxide of variety classes, different shares according to test number reason pattern, increase or change one of IR-LED far-infrared function ceramic substrate oxide components composition requirement or multinomial.
The quartz-ceramics substrate adopts to annotate and coagulates method of forming cured and prepared, dry, sintering and moulding technology.Processing step is following:
1. quartz-ceramics slip preparation
The first step: ball milling prepares screened stock, adds people's quartz powder materials, premixed liquid, compound additive and carries out ball milling.Premixed liquid concentration is 10%-20%, and premixed liquid is mixed by proportioning and fully dissolves with deionized water by monomer, crosslinking agent to be processed; Propylene phthalein amine monomers (chemical pure) adds the people and measures 0.5-2.0%; Di-2-ethylhexylphosphine oxide propylene phthalein amine crosslinker (chemical pure);
Second step: add the oxide particle material by proportioning and mix slurry, be controlled at ball milling total time 20-30 hour, the slip suspension is good, moisture content low (solid concentration 80%).
2. annotate the type that congeals into
Slip adds people's initator, mixes vacuum degassing; Annotate in people's mould, casting process carries out in (mechanical oscillation or ultrasonic wave) vibration, realizes annotating the type DYNAMIC PROCESSization of congealing into; Solidifying under the 50-80 ℃ of temperature more than the 20min, base substrate curing and demolding, drying, burning till.Persulfuric acid is an initator by the aqueous solution: add the people and measure 0.5-2.0ml/ ㎏ slip.
Quartz-ceramics substrate performance of the present invention:
Bulk density (kg/m
3): 2.76
Compression strength (GPa): 3.8
Far infrared wave emissivity:＞91%
Thermal coefficient of expansion (2.3-5 K-1) (RT-100～350 ℃)
Dielectric strength (KV/mm): >=18
Two, the preparation of serial rare-earth electric slurry
1. rare earth resistance slurry: the rare earth resistance slurry by function mutually and organic carrier form, ratio is: (65～85): (15～35); The function phase constituent is made up of silver-colored ruthenium palladium yttrium composite powder and microcrystalline glass powder, and ratio is: (75～55): (25～45); The weight ratio of silver ruthenium palladium yttrium powder is: (59～75): (15～20.5): (5～20): (0.5～5); Said microcrystalline glass powder is: CaO-SiO
2-Al
2O
3-B
2O
3-Bi
2O
3-La
2O
3Microcrystalline glass in series, each oxide weight ratio of this devitrified glass is: CaO (10～35) %, SiO
2(20～60) %, Al
2O
3(5～35) %, B
2O
3(1～10) %, Bi
2O
3(10～30) %, La
2O
3(0.3～8) %, nucleus agent: TiO
2(1～8) %, ZrO
2(1～10) %.
2. rare earth electrode slurry: rare earth electrode slurry is made up of solid phase composition and organic solvent carrier, and its weight ratio is: (70～90): (10～30); Wherein the solid phase composition comprises: silver-colored palladium yttrium composite powder and microcrystalline glass powder, and its weight ratio is: (94～99.4): (0.6～6); This silver palladium yttrium composite powder is made up of following component (weight ratio), and the weight ratio of palladium powder, silver powder and yttrium powder is: (0.6～10): (82～99): (0.4～8); Microcrystalline glass powder is SiO
2-Al
2O
3-CaO-B
2O
3-Bi
2O
3-La
2O
3Microcrystalline glass in series, the composition weight proportion of this each oxide of devitrified glass is: SiO
2(20～60) %, Al
2O
3(5～35) %, CaO (10～35) %, B
2O
3(1～15) %, Bi
2O
3(10～30) %, La
2O
3(0.3～15) %, nucleus agent: TiO
2(1～10) %, ZrO
2(1～10) %.
3. rare earth packaging slurry: the rare earth packaging slurry is made up of solid phase composition and organic solvent carrier, and weight ratio is: (70～90): (10～30), the solid phase composition is: SiO
2-Al
2O
3-CaO-B
2O
3-La
2O
3Microcrystalline glass in series, the composition weight proportion of each oxide is: SiO
2(30～65) %, Al
2O
3(5～26) %, CaO (18～38) %, B
2O
3(2～16) %, La
2O
3(0.3～15) %, Co
2O
3(0.05～6) %, nucleus agent: TiO
2(1～10) %, ZrO
2(1～10) %.
Above-mentioned rare-earth electric slurry organic solvent carrier is grouped into by one-tenth such as terpinol, ATBC, ethyl cellulose, NC Nitroncellulose, rilanit special, lecithin.The organic carrier prescription of three kinds of rare-earth electric slurries is following:
A. rare earth resistance slurry organic solvent carrier compound (weight ratio) is: terpinol 68～78%, ATBC 2～18%, ethyl cellulose 0.4～9%, NC Nitroncellulose 0.4～9%, rilanit special 0.1～6%, lecithin 0.1～6%;
B. rare earth electrode slurry organic carrier prescription (weight ratio) is: terpinol 60～98%, ATBC 10～30%, ethyl cellulose 2～10%, NC Nitroncellulose 1～5%, rilanit special 0.1～5%, lecithin 0.1～5%;
C. rare earth packaging slurry organic carrier prescription (weight ratio) is BC 66～89%, ATBC 5～15%, ethyl cellulose 0.5～10%, rilanit special 0.1～5%, lecithin 0.1～5%.
The preparation method of above-mentioned serial rare-earth electric slurry:
A. the preparation technology of rare earth resistance slurry:
1. microcrystalline glass powder prepares: after mixing in R-S01 three-dimensional blender machine by above-mentioned oxide, nucleus agent proportioning; The smelting furnace melting, temperature is: 1100 ~ 1450 ℃, be incubated after 1 ~ 3 hour; With the glass melts shrend, obtain the glass micro mist that little slag ball milling obtains 3 microns of particle diameters;
2. silver-colored ruthenium palladium yttrium composite powder prepares: mix in R-S03 high efficient mixed dispersing apparatus by silver-colored ruthenium palladium yttrium grain weight amount proportioning and obtain composite powder;
3. organic carrier preparation: above-mentioned raw materials is mixed in proportion, and dissolving is several hours in 80 ~ 100 ℃ water.Adjust amount of thickener, the viscosity of organic carrier solvent is adjusted at interior the getting final product of scope of 180 ~ 280mPaS.
4. the rare earth resistance slurry is comprehensively modulated: the solid phase composition is made up of silver-colored ruthenium palladium yttrium composite powder and microcrystalline glass powder, by weight solid phase powder, organic carrier solvent are mixed in R-S03 high efficient mixed dispersing apparatus, carries out three-roll rolling and obtains finished product.Viscosity number is 150 ~ 200PaS/RPM;
B. the preparation technology of rare earth electrode slurry:
1. microcrystalline glass powder preparation: than oxide, nucleus agent being mixed the back melting, temperature is by raw material weight: 1100 ~ 1450 ℃, be incubated 1 ~ 3 hour, and shrend obtains the little slag of glass, and ball milling obtains 3 microns glass micro mists;
2. prepare silver-colored palladium yttrium composite powder; Silver palladium yttrium composite powder, particle diameter is: 3 μ m mix by weight modulation in the three-dimensional blender machine;
3. organic carrier preparation; Mix the back by the raw material weight ratio and in 80 ~ 100 ℃ of water, dissolved several hours, adjustment ethyl cellulose cellulose content, viscosity Control is in 150 ~ 280mPas scope;
4. prepare rare earth electrode slurry: it is rolling to go into three-high mill after placing R-S03 three-dimensional blender machine to mix in microcrystalline glass powder, silver-colored palladium yttrium composite powder, organic solvent carrier in proportion, obtains rare earth electrode slurry, viscosity: 150 ~ 200PaS/RPM.
C. the preparation technology of rare earth packaging slurry:
1. prepare the rare earth microcrystalline glass powder: by weight ratio with oxide, the nucleus agent.Melting after mixing, smelting temperature is: 1 100 ~ 1450 ℃, be incubated after 90 ~ 180 minutes, the shrend of coming out of the stove obtains the little slag of glass; The little slag of ball milling glass is prepared the microcrystalline glass powder of 3 microns of particle diameters;
2. prepare the organic solvent carrier: mix: melting bath number hour in 80 ~ 100 ℃ water by proportioning.Adjustment ethyl cellulose cellulose content is adjusted at the viscosity of organic carrier in the scope of 150 ~ 28OmPaS;
3. packaging slurry modulation: after placing R-S03 three-dimensional blender machine to mix by weight ratio solid phase composition and the organic solvent carrier, the rolling finished product that obtains of three rods.Viscosity number is 150 ~ 200PaS/RPM;
Three, the preparation of the efficient far infrared ceramic base rare earth thick film circuit of IR-LED electric heating element
The preparation technology of the rare earth thick film circuit electric heating element of the efficient far infrared ceramic substrate of IR-LED, process:
1. ceramic substrate is prepared
By the drawing specification requirement through laser, mill, throw, cut, processing line is processed into pdm substrate;
2. the serial rare-earth electric slurry is prepared--carry out homogenized before the printing
Draw version, the silk screen printing of serial rare-earth electric slurry on ceramic substrate by process: CAD plate-making, light, process thick film circuit;
3. wet film oxidizing atmosphere preliminary treatment (drying oven)
Vacuum drying 10～30 minutes, 80～180 ℃ of temperature;
4. sintering furnace
Sintering in the infrared crystallizing and sintering stove of oxidizing atmosphere, 50～120 ℃ of temperature rise rates/time, 750～950 ℃ of high temperature section temperature, the peak value sintering made the efficient far infrared ceramic base rare earth thick film circuit of IR-LED electric heating element in 10～20 minutes.
5. laser marking laser is repaiied resistance;
6. by company standard test, packing.
In the present embodiment, produce φ 120mm by the drawing specification requirement, thickness is the efficient far infrared ceramic substrate of the IR-LED of 6 ㎜ specifications, and is as shown in Figure 1.Subsequent use after the cleaningization processing, the serial rare-earth electric slurry that modulates is contained packaging slurry jz-01, rare earth resistance slurry, rare earth electrode slurry, rare earth packaging slurry, do all and will handle, measure slurry fineness and viscosity, batch process should the side's of making resistance exemplar.By following technology and drawing requirement, the preparation rare earth thick film circuit.
Specification requirement: voltage: 220 ∨ 50Hz 100W surface temperatures: 350 ℃ of max working temperatures: 200 ~ 300 ℃, the temperature field is even, circuitous pattern is rationally distributed.
Manufacture thick film circuit by following technological process:
Technological process:
A. cleaningization processing ceramic substrate → B.CAD light draw version → C. steel mesh printing → D. oven dry sintering → E. and check (laser is repaiied resistance) to pack.
A. thickness of dielectric layers＞60 μ m b. sides hinder film thickness＞8 μ m
B. sintering process: a. heating-cooling speed 50-70 ℃ ∕ min b. peak temperature: 700-900 ℃
Annotate: slurry was placed of a specified duration, need carry out homogenized before using.The jz-01 packaging slurry is selectively fabricated.
After tested, the rare earth thick film circuit heating reaches following designing requirement.Can realize the purpose of staircase control temperature in conjunction with controllable silicon, igbt transistor and converter technique.The rare earth thick film circuit electric heating element performance parameter of the embodiment of the invention:
Surface temperature: 450 ℃ of max working temperatures: 200 ~ 350 ℃
The efficient far infrared ceramic base rare earth thick film circuit of present embodiment IR-LED electric heating element performance:
Bulk density (kg/m
3): 2.76
Compression strength (GPa): 3.8
Far infrared wave emissivity:＞93%
Thermal coefficient of expansion (2-5 K-1) (RT-100-350 ℃)
Dielectric strength (KV/mm): >=18
The rare earth thick-film resistor circuit electrical property of present embodiment:
1. electrical property:
| Resistance | Resolution | TCR/ppm/ ℃ | Aging intensity |
| 450 ± 2m Ω/ | 0.1mm | 1000 ± 150ppm * 10 -6/ ℃ | 10 (N/mm 2) |
2. physical property
| Rheological behavior | Resistive layer thickness | Slurry viscosity | The unit consumption |
| The suitable wire mark of thixotroping | 10 ± 2 μ m | 168 ± 20Pas/10RPM | 86cm 2/ gram |
The rare earth electrode slurry performance of present embodiment:
1. electrical property:
| Side's resistance | Resolution | Tensile strength | Aging intensity |
| ＜3 ± 2m Ω/ | 0.1mm | ＞16 (N/mm2) | 10 (N/mm2) |
2. physical property
| Rheological behavior | Electrode layers thickness | Slurry viscosity | The unit consumption |
| The suitable wire mark of thixotroping | 12 ± 2 μ m | 186PaS/RPM. | The 88cm2/ gram |
The performance parameter of rare earth packaging slurry of the present invention:
1. physical property:
| Color (choosing) | Solids content | The silk screen number | Slurry viscosity | Sintering temperature |
| Blue (ash, black) look | 76% | 180 | 125PaS/RPM | 890 ℃ |
2. electric property:
| Leakage current | Insulation resistance | Breakdown strength |
| ＜3mA (250VDC) | ＞50M Ω (500VDC) | ＞600VAC/＞15 μ m |
Above-described only is preferred implementation of the present invention, should be pointed out that for the person of ordinary skill of the art, under the prerequisite that does not break away from the invention design, can also make some distortion and improvement, and these all belong to protection scope of the present invention.
Claims (13)
1. rare earth thick film circuit electric heating element based on the IR-LED ceramic substrate; It is characterized in that; It comprises quartz-ceramics substrate, serial rare-earth electric slurry; On the quartz-ceramics substrate, thick film circuit has the electrode link of external power supply to the serial rare-earth electric slurry with the prepare of thick film circuit.
2. the rare earth thick film circuit electric heating element based on the IR-LED ceramic substrate according to claim 1 is characterized in that, said quartz base plate is by quartzy (SiO
2-Al
2O
3-B
2O
3-Mg
20
3-ZrO
2) pottery and rare earth oxide composition, each oxide powder proportioning of quartz-ceramics is: SiO
293.5 Al～96.8%,
2O
31.5 B～3%,
2O
30.5 Mg～1%,
20
30.2 ZrO～0.5%,
21～2%, particle size range≤3 η m; Rare earth oxide is one or more in lanthanum, cerium, neodymium, promethium, gadolinium, erbium, scandium, yttrium and the terbium oxide.
3. the rare earth thick film circuit electric heating element based on the IR-LED ceramic substrate according to claim 1; It is characterized in that; Said series electronic slurry comprises packaging slurry, rare earth resistance slurry, rare earth electrode slurry, and the series electronic slurry is formed by function phase, inorganic adhesive phase, organic carrier.
4. the rare earth thick film circuit electric heating element based on the IR-LED ceramic substrate according to claim 3 is characterized in that, said rare earth resistance slurry is made up of function phase and organic carrier, and ratio is (65～85) %: (15～35) %; The function phase constituent is made up of silver-colored ruthenium palladium yttrium composite powder and microcrystalline glass powder, and ratio is (55～75): (25～45); The weight ratio of silver ruthenium palladium yttrium powder is (59～75): (15～20.5): (5～20): (0.5～5); Microcrystalline glass powder is CaO-SiO
2-Al
2O
3-B
2O
3-Bi
2O
3-La
2O
3Microcrystalline glass in series, each oxide weight of this devitrified glass is than being CaO10～35%, SiO
220～60%, Al
2O
35～35%, B
2O
31～10%, Bi
2O
310～30%, La
2O
30.3～8%; The nucleus agent is TiO
21～8%, ZrO
21～10%.
5. the rare earth thick film circuit electric heating element based on the IR-LED ceramic substrate according to claim 4; It is characterized in that said rare earth resistance slurry organic solvent carrier compound (weight ratio) is: terpinol 68～78%, ATBC 2～18%, ethyl cellulose 0.4～9%, NC Nitroncellulose 0.4～9%, rilanit special 0.1～6%, lecithin 0.1～6%.
6. the rare earth thick film circuit electric heating element based on the IR-LED ceramic substrate according to claim 3 is characterized in that said rare earth electrode slurry is made up of solid phase composition and organic solvent carrier, and its weight ratio is (70～90) %: (10～30) %; Wherein the solid phase composition comprises silver-colored palladium yttrium composite powder and microcrystalline glass powder, and its weight ratio is (94～99.4) %: (0.6～5) %; The weight ratio of this palladium powder, silver powder and yttrium powder is (0.6～10) %: (82～99) %: (0.4～8) %; Said microcrystalline glass powder is SiO
2-Al
2O
3-CaO-B
2O
3-Bi
2O
3-La
2O
3Microcrystalline glass in series, this devitrified glass composition proportion is SiO
220～60%, Al
2O
35～35%, CaO10～35%, B
2O
31～15%, Bi
2O
310～30%, La
2O
30.3～15%, nucleus agent TiO
21～10%, ZrO
21～10%.
7. the rare earth thick film circuit electric heating element based on the IR-LED ceramic substrate according to claim 6; It is characterized in that said rare earth electrode slurry organic carrier prescription (weight ratio) is: terpinol 60～98%, ATBC 10～30%, ethyl cellulose 2～10%, NC Nitroncellulose 1～5%, rilanit special 0.1～5%, lecithin 0.1～5%.
8. the rare earth thick film circuit electric heating element based on the IR-LED ceramic substrate according to claim 3 is characterized in that said rare earth packaging slurry is made up of solid phase composition and organic solvent carrier, and proportioning is 70～90%: 10～30%; The solid phase composition is SiO
2-Al
2O
3-CaO-B
2O
3-La
2O
3Microcrystalline glass in series, the composition proportion of each oxide are SiO
2(30～65%), Al
2O
3(5～26%), CaO (18～38%), B
2O
3(2～16%), La
2O
3(0.3～15%), Co
2O
3(0.05～6%); Nucleus agent TiO
2(1～10%), ZrO
2(1～10%).
9. the rare earth thick film circuit electric heating element based on the IR-LED ceramic substrate according to claim 8; It is characterized in that said rare earth packaging slurry organic carrier prescription (weight ratio) is BC 66～89%, ATBC 5～15%, ethyl cellulose 0.5～10%, rilanit special 0.1～5%, lecithin 0.1～5%.
10. preparation method based on the rare earth thick film circuit electric heating element of IR-LED ceramic substrate is characterized in that it comprises following processing step:
A, ceramic substrate prepare, through laser, mill, throw, cut, processing line is processed into pdm substrate;
B, serial rare-earth electric slurry are prepared--and carry out homogenized before the printing, draw version, the silk screen printing of serial rare-earth electric slurry on ceramic substrate, process thick film circuit by process: CAD plate-making, light;
C, the preliminary treatment of wet film oxidizing atmosphere, vacuum drying 10～30 minutes, 80～180 ℃ of temperature;
Sintering in the d, the infrared crystallizing and sintering stove of oxidizing atmosphere, 50～120 ℃ of temperature rise rates/time, 750～950 ℃ of high temperature section temperature, the peak value sintering made IR-LED ceramic base rare earth thick film circuit electric heating element in 10～20 minutes;
E, laser marking laser are repaiied resistance, test, packing.
11. the preparation method of the rare earth thick film circuit electric heating element based on the IR-LED ceramic substrate according to claim 10; It is characterized in that; In said processing step b process, in the set-up procedure of serial rare-earth electric slurry, the preparation technology of rare earth resistance slurry wherein is:
1., crystal glass powder preparation, after mixing in R-S01 three-dimensional blender machine by oxide, nucleus agent proportioning, the smelting furnace melting; Temperature is: 1100-1450 ℃; Be incubated after 1-3 hour,, obtain the glass micro mist that little slag ball milling obtains 3 microns of particle diameters the glass melts shrend;
2., silver-colored ruthenium palladium yttrium composite powder preparation, mix in R-S03 high efficient mixed dispersing apparatus by silver-colored ruthenium palladium yttrium grain weight amount proportioning and to obtain composite powder;
3., organic carrier preparation, above-mentioned raw materials is mixed in proportion, dissolving is several hours in 80-100 ℃ water, the adjustment amount of thickener is adjusted at the viscosity of organic carrier solvent in the scope of 180-280mPaS and gets final product;
4., the rare earth resistance slurry is comprehensively modulated; The solid phase composition is made up of silver-colored ruthenium palladium yttrium composite powder and microcrystalline glass powder; By weight solid phase powder, organic carrier solvent are mixed in R-S03 high efficient mixed dispersing apparatus, carry out three-roll rolling and obtain finished product, viscosity number is 150-200PaS/RPM.
12. the preparation method of the rare earth thick film circuit electric heating element based on the IR-LED ceramic substrate according to claim 10; It is characterized in that; In said processing step b process, in the set-up procedure of serial rare-earth electric slurry, the preparation technology of rare earth electrode slurry wherein is:
1. crystal glass powder preparation, than oxide, nucleus agent being mixed the back melting, temperature is 1100-1450 ℃, is incubated 1 ~ 3 hour by raw material weight, and shrend obtains the little slag of glass, and ball milling obtains 3 microns glass micro mists;
2. prepare silver-colored palladium yttrium composite powder, particle diameter is 3 μ m, in the three-dimensional blender machine, mixes by weight modulation;
3. organic carrier preparation mixes the back by the raw material weight ratio and in 80 ~ 100 ℃ of water, dissolved several hours, adjustment ethyl cellulose cellulose content, and viscosity Control is in 150 ~ 280mPas scope;
4. prepare rare earth electrode slurry, it is rolling to go into three-high mill after placing R-S03 three-dimensional blender machine to mix in microcrystalline glass powder, silver-colored palladium yttrium composite powder, organic solvent carrier in proportion, obtains rare earth electrode slurry, viscosity 150-200PaS/RPM.
13. the preparation method of the rare earth thick film circuit electric heating element based on the IR-LED ceramic substrate according to claim 10; It is characterized in that; In said processing step b process, in the set-up procedure of serial rare-earth electric slurry, the preparation technology of rare earth packaging slurry wherein is:
1. prepare the rare earth microcrystalline glass powder: with oxide, nucleus agent melting after mixing, smelting temperature is by weight ratio: 1100-1450 ℃, be incubated after 90-180 minutes, and the shrend of coming out of the stove obtains the little slag of glass; The little slag of ball milling glass is prepared the microcrystalline glass powder of 3 microns of particle diameters;
2. prepare the organic solvent carrier, mix by proportioning, melting bath number hour in 80-100 ℃ water, adjustment ethyl cellulose cellulose content is adjusted at the viscosity of organic carrier in the scope of 150-28OmPaS;
3. packaging slurry modulation, place R-S03 three-dimensional blender machine to mix by weight ratio solid phase composition and the organic solvent carrier after, the rolling finished product that obtains of three rods, viscosity number is 150-200PaS/RPM.
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