CN1424727A - Resistance sizing agent and its producing process for high-power thick-film circuit based on stainless steel substrate - Google Patents
Resistance sizing agent and its producing process for high-power thick-film circuit based on stainless steel substrate Download PDFInfo
- Publication number
- CN1424727A CN1424727A CN 02139894 CN02139894A CN1424727A CN 1424727 A CN1424727 A CN 1424727A CN 02139894 CN02139894 CN 02139894 CN 02139894 A CN02139894 A CN 02139894A CN 1424727 A CN1424727 A CN 1424727A
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- powder
- silver
- stainless steel
- steel substrate
- weight ratio
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
- C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
- C03C3/093—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium containing zinc or zirconium
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
- C03C8/18—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing free metals
Abstract
A resistance slurry for the high-power thick-film circuit on stainless steel substrate is composed of solid-phase component (composite Ag+Pd powder plus microcrystal glass powder) and organic adhesive. Said microcrystal glass is SiO2-B2O3-Al2O3-CaO-Bi2O3 series. Its preparing process includes such steps as preparing microcrystal powder, proportionally preparing composite Ag+Pd powder, preparing organic adhesive, proportioning, stirring, and rolling.
Description
Technical field: the present invention relates to high-power (tens of watts to thousands of watts) thick film circuit resistance slurry based on stainless steel substrate.Be particularly related to based on the large power thick film circuit of ferritic stainless steel series such as () 1Cr17 substrate with resistance slurry and preparation technology thereof.
Background technology: in the thick film circuit technique field, traditional substrate has polymeric substrates and ceramic substrate, and the two all has its limitation.The polymeric substrates thermal conductivity is low, coefficient of expansion height, high temperature (greater than 100 ℃) poor stability.Ceramic substrate comprises Al
2O
3And AlN etc., its size is less, generally is not more than 100 * 100mm
2, and bad mechanical property, complete machine assembling difficulty.The stainless steel substrate of surface insulationization causes that with its good mechanical strength, good hot property, electromagnetic shielding characteristic, large scale, complicated shape and potential comprehensive advantages such as low cost people more and more pay close attention to.The technical characterstic of insulating stainless steel substrate is that to select the 1Cr17 series stainless steel for use be base material, the dielectric paste that will be complementary with the stainless steel rerum natura by silk screen printing, firing process stainless steel surfaces form densification, adhesion strong, satisfy the insulating barrier (＜100 μ m) that insulation and breakdown characteristics etc. require.
Mechanical performance, hot property, the large scale that the insulating stainless steel substrate is good and can be made into rare characteristics such as complicated shape makes its possibility of its application on high-power thick film device of people's special concern.At present, high-power resistance (＞100～1000W), the large power, electrically thermal element (generally all make of the wire resistor silk by the components and parts that application such as＞100～1000W) have a large capacity and a wide range, its size is big, life-span characteristics such as weak point, thermal design difficulty, more and more is difficult to satisfy harsh requirements such as each electric appliances miniaturization, high reliability, long-life.Thick-film resistor paste and thick film conductor paste that the increasingly mature urgent need exploitation and the insulating stainless steel substrate performance of thick film circuit element preparation and application technology is complementary, design preparation small size, complanation, high reliability, long-life, high-power thick film element cheaply are to satisfy the growing market demand.
The resistance track of high-power thick film resistance element and electric heating element and electrode trace are burnt till acquisition by resistance slurry and electrocondution slurry through silk screen printing and oven dry respectively.High-power characteristic requirement component resistance track area is big, resistance is lower and should have alap temperature coefficient of resistance, therefore to the requirement of resistance slurry except necessary resistance and temperature coefficient of resistance, its firing process performance demands is also than low power ceramic substrate thick film circuit element height.
Because the coefficient of expansion of stainless steel substrate is much larger than ceramic substrate, therefore the resistance track rete after burning till based on the thick-film resistor paste of stainless steel substrate should have the bigger coefficient of expansion to be complementary with stainless steel, and the glassy phase in the slurry also should be with compatible based on the dielectric paste of stainless steel substrate and the solid phase composition chemistry in the electrocondution slurry simultaneously.
Summary of the invention: technical problem to be solved by this invention provide that a kind of side resistance is low and adjustable, temperature coefficient of resistance is lower and adjustable, printing characteristic and burn till characteristic good and the thick film circuit that is complementary with the insulating stainless steel substrate with resistance slurry and preparation technology thereof.
The present invention adopts following technical proposal to solve the problems of the technologies described above, large power thick film circuit resistance slurry based on stainless steel substrate of the present invention, be characterized in that it is made up of solid phase components (silver-colored palladium composite powder+microcrystalline glass powder) and organic binder bond, the ratio of solid phase composition and organic binder bond (weight ratio) is (60～80): (40～20), the ratio (weight ratio) (80～60) of silver-colored palladium composite powder and microcrystalline glass powder in the described solid phase composition: (20～40); The particle diameter of palladium powder and silver powder is all less than 2 μ m in the silver palladium composite powder, and the ratio of palladium powder and silver powder (weight ratio) is (3～20): (97～80).
As a further improvement on the present invention, described devitrified glass is SiO
2-B
2O
3-Al
2O
3-CaO-Bi
2O
3Microcrystalline glass in series, all kinds of raw materials and proportioning (weight ratio) are SiO
2(20～70%), B
2O
3(1～15%), Al
2O
3(5～30%), CaO (10～50%), Bi
2O
3(10～30%), TiO
2(1～10%), ZrO
2(1～10%);
Each set of dispense than (weight ratio) is in the described organic binder bond: terpinol (70～98%), tributyl citrate (2～20%), ethyl cellulose (0.5～8%), NC Nitroncellulose (0.5～8%), rilanit special (0.1～5%), lecithin (0.1～5%).
Large power thick film circuit based on stainless steel substrate of the present invention with the preparation technology of resistance slurry is:
A, preparation microcrystalline glass powder: by weight percentage with following proportion raw material: SiO
2(20～70%), B
2O
3(1～15%), Al
2O
3(5～30%), CaO (10～50%), Bi
2O
3(10～30%), TiO
2(1～10%), ZrO
2(1～10%) inserts the high-temperature electric resistance furnace melting after mixing in batch mixer, smelting temperature is 1200～1600 ℃, and temperature retention time is 1～6 hour, and shrend obtains the little slag of glass; The little slag of glass is inserted the ball mill ball milling obtain the micro mist that particle diameter is not more than 5 microns;
B, the silver-colored palladium composite powder of modulation are selected palladium powder, the silver powder of granularity less than 2 μ m for use, press palladium: silver=(3～20): (97～80) are mixed that required silver-colored palladium composite powder is standby;
C, preparation organic binder bond: by a certain percentage in 80～100 ℃ of dissolving a few hours, all kinds of raw materials and proportioning are: terpinol (70～98%), tributyl citrate (2～20%), ethyl cellulose (0.5～8%), NC Nitroncellulose (0.5～8%), rilanit special (0.1～5%), lecithin (0.1～5%) with organic solvent and thickener, surfactant, thixotropic agent etc.; Adjust NC Nitroncellulose, ethyl cellulose cellulose content, organic binder bond viscosity is controlled in 200～300mPas scope;
D, slurry modulation: by silver-colored palladium composite powder: microcrystalline glass powder is: (80～60): the ratio of (20～40) (weight ratio) is prepared the solid phase composition, and in the solid phase composition: organic binder bond=(60～80): the ratio of (40～20) (weight ratio) is carried out three-roll rolling after raw material is placed the container dispersed with stirring, testing size viscosity, range of viscosities are 100～150 ± 20Pas (RPM75).
Binding agent viscosity is controlled in 200～300mPas scope;
Major advantage of the present invention is:
1, by to based on the large power thick film circuit of stainless steel substrate reasonable analysis, select for use devitrified glass as the bonding phase with basic demands such as resistance slurry physics, chemical property and processing performances.By to SiO
2-B
2O
3-Al
2O
3-CaO-Bi
2O
3System researches such as the microcrystalline glass in series coefficient of expansion, vitrification point, softening temperature, crystallite forming core growth dynamics, determine microcrystalline glass formula and melting, ball-milling technology, the coefficient of expansion and the 1Cr17 that make it with the resistor track layer of the compound formation of precious metal powder of proper proportion are stainless steel substrate coupling and good combination.
2, based on reasonable understanding to each organic principle mechanism of action in the slurry, select for use multicomponent alcohol and ester class main solvent to replace traditional one pack system alcohols main solvent, with the main solvent of different boiling and evaporation rate in proportion preparation rationally make slurry balanced volatilization in process such as print, dry, burn till, avoid solvent to concentrate defectives such as volatilization appearance cracking, pin hole.
3, select for use rilanit special as thixotropic agent, in the organic binder bond system, form good colloform texture, make slurry have good thixotropy and anti-heavy effect.
4, resistance slurry printing characteristic of the present invention and burn till characteristic good, low and adjustable by the resistor track layer side of the having resistance of resistance slurry preparation of the present invention, temperature coefficient of resistance is low and adjustable, cost is low and with based on advantages such as thick film circuit usefulness dielectric paste, the electrocondution slurry of stainless steel substrate are compatible.
Embodiment:
Embodiment 1: the resistance slurry 1, the microcrystalline glass formula that are used for the high-power thick film element of 1Cr17 series stainless steel substrate: SiO
2(28%), B
2O
3(9%), Al
2O
3(19%), CaO (19%), Bi
2O
3(19%), TiO
2(5%), ZrO
2(1%); 2, glass melting technology: 1450 ℃, be incubated three hours; 3, ball milling and granularity control: with the vibrator corase grind, the back is finely ground to maximum particle diameter with planetary ball mill or agitating ball mill and is no more than 5 microns; 4, precious metal powder composition design: the palladium-silver ratio is 1: 25, and the powder maximum particle diameter is less than 2 microns; 5, organic adhesive agent prescription and dissolution process: terpinol (76%), tributyl citrate (19%), ethyl cellulose (3%), NC Nitroncellulose (1%), rilanit special (0.5%), lecithin (0.5%).Dissolution process mixes the back for each component that will prepare in proportion and be incubated 5 hours in high temperature (80～90 ℃) water-bath.6, size mixing technology: with the solid phase composition (the palladium-silver composite powder: glass dust=60: 40) and organic binder bond in proportion (72: 28) carry out three-roll rolling after placing the container dispersed with stirring.7, size performance:
Side's resistance: 100 ± 10m Ω/
Temperature coefficient of resistance: 1500 ± 200 * 10
-6/ ℃
Viscosity: 220 ± 20Pas test condition: 10RPM
Embodiment 2: the resistance slurry 1, the microcrystalline glass formula that are used for the high-power thick film element of 1Cr17 series stainless steel substrate: SiO
2(26%), B
2O
3(10%), Al
2O
3(20%), CaO (20%), Bi
2O
3(18%), TiO
2(4%), ZrO
2(2%); 2, glass melting technology: 1450 ℃, be incubated three hours; 3, ball milling and granularity control: with the vibrator corase grind, the back is finely ground to maximum particle diameter with planetary ball mill or agitating ball mill and is no more than 5 microns; 4, precious metal powder composition design: the palladium-silver ratio is 1: 3, and the powder maximum particle diameter is less than 2 microns; 5, organic adhesive agent prescription and dissolution process: terpinol (72%), tributyl citrate (23%), ethyl cellulose (3%), NC Nitroncellulose (1%), rilanit special (0.5%), lecithin (0.5%).Dissolution process mixes the back for each component that will prepare in proportion and be incubated 5 hours in high temperature (80～90 ℃) water-bath.Size mixing technology: with the solid phase composition (the palladium-silver composite powder: glass dust=58: 42) and organic binder bond in proportion (72: 28) carry out three-roll rolling after placing the container dispersed with stirring.6, size performance:
Side's resistance: 100 ± 10m Ω/
Temperature coefficient of resistance: 300 ± 50 * 10
-6/ ℃
Viscosity: 220 ± 20Pas test condition: 10RPM
Claims (4)
1, a kind of large power thick film circuit resistance slurry based on stainless steel substrate, it is characterized in that it is made up of solid phase components (silver-colored palladium composite powder+microcrystalline glass powder) and organic binder bond, the ratio of solid phase composition and organic binder bond (weight ratio) is (60～80): (40～20), and the ratio of silver-colored palladium composite powder and microcrystalline glass powder is (weight ratio) (80～60) in the described solid phase composition: (20～40); The particle diameter of palladium powder and silver powder is all less than 2 μ m in the silver palladium composite powder, and the ratio of palladium powder and silver powder (weight ratio) is (3～20): (97～80).
2, the large power thick film circuit resistance slurry based on stainless steel substrate according to claim 1 is characterized in that described devitrified glass is SiO
2-B
2O
3-Al
2O
3-CaO-Bi
2O
3Microcrystalline glass in series, all kinds of raw materials and proportioning (weight ratio) are SiO
2(20～70%), B
2O
3(1～15%), Al
2O
3(5～30%), CaO (10～50%), Bi
2O
3(10～30%), TiO
2(1～10%), ZrO
2(1～10%).
3, the large power thick film circuit resistance slurry based on stainless steel substrate according to claim 1 and 2 is characterized in that each set of dispense than (weight ratio) is in the described organic binder bond: terpinol (70～98%), tributyl citrate (2～20%), ethyl cellulose (0.5～8%), NC Nitroncellulose (0.5～8%), rilanit special (0.1～5%), lecithin (0.1～5%).
4, a kind of according to the preparation technology of the described large power thick film circuit based on stainless steel substrate of claim 1 with resistance slurry, it is characterized in that:
A, preparation microcrystalline glass powder: by weight percentage with following proportion raw material: SiO
2(20～70%), B
2O
3(1～15%), Al
2O
3(5～30%), CaO (10～50%), Bi
2O
3(10～30%), TiO
2(1～10%), ZrO
2(1～10%) inserts the high-temperature electric resistance furnace melting after mixing in batch mixer, smelting temperature is 1200～1600 ℃, and temperature retention time is 1～6 hour, and shrend obtains the little slag of glass; The little slag of glass is inserted the ball mill ball milling obtain the micro mist that particle diameter is not more than 5 microns;
B, the silver-colored palladium composite powder of modulation are selected palladium powder, the silver powder of granularity less than 2 μ m for use, press palladium: silver=(3～20): (97～80) are mixed that required silver-colored palladium composite powder is standby;
C, preparation organic binder bond: by a certain percentage in 80～100 ℃ of dissolving a few hours, all kinds of raw materials and proportioning are: terpinol (70～98%), tributyl citrate (2～20%), ethyl cellulose (0.5～8%), NC Nitroncellulose (0.5～8%), rilanit special (0.1～5%), lecithin (0.1～5%) with organic solvent and thickener, surfactant, thixotropic agent etc.; Adjust NC Nitroncellulose, ethyl cellulose cellulose content, organic binder bond viscosity is controlled in 200～300mPas scope;
D, slurry modulation: by silver-colored palladium composite powder: microcrystalline glass powder is: (80～60): the ratio of (20～40) (weight ratio) is prepared the solid phase composition, and in the solid phase composition: organic binder bond=(60～80): the ratio of (40～20) (weight ratio) is carried out three-roll rolling after raw material is placed the container dispersed with stirring, testing size viscosity, range of viscosities are 100～150 ± 20Pas (RPM75).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02139894 CN1216380C (en) | 2002-12-30 | 2002-12-30 | Resistance sizing agent and its producing process for high-power thick-film circuit based on stainless steel substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02139894 CN1216380C (en) | 2002-12-30 | 2002-12-30 | Resistance sizing agent and its producing process for high-power thick-film circuit based on stainless steel substrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1424727A true CN1424727A (en) | 2003-06-18 |
| CN1216380C CN1216380C (en) | 2005-08-24 |
Family
ID=4750273
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02139894 Expired - Fee Related CN1216380C (en) | 2002-12-30 | 2002-12-30 | Resistance sizing agent and its producing process for high-power thick-film circuit based on stainless steel substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008014677A1 (en) * | 2006-07-28 | 2008-02-07 | Kezheng Wang | Rare earth electrode slurry for rare earth thick-film circuit based on metal substrate and producing process thereof |
| WO2008014678A1 (en) * | 2006-07-28 | 2008-02-07 | Kezheng Wang | Rare earth base-metal resistance slurry for rare earth thick-film circuit based on metal substrate and producing process thereof |
| WO2008014680A1 (en) * | 2006-07-28 | 2008-02-07 | Kezheng Wang | Rare earth resistance slurry for rare earth thick-film circuit based on metal substrate and producing process thereof |
| WO2008014679A1 (en) * | 2006-07-28 | 2008-02-07 | Ke Zheng Wang | Rare earth medium slurry for rare earth thick-film circuit based on metal substrate and producing process thereof |
| WO2009012621A1 (en) * | 2007-07-24 | 2009-01-29 | Kezheng Wang | An electric heating element of rare earth thick film circuit based on glass ceramic substrate and a method for preparing it |
| CN101868064A (en) * | 2010-06-21 | 2010-10-20 | 陕西科技大学 | Environment-friendly graphite resistance paste and preparation method thereof |
| CN103730189A (en) * | 2014-01-09 | 2014-04-16 | 湖南利德电子浆料有限公司 | Metal substrate based sintering temperature adjustable thick film circuit resistor paste and preparation process thereof |
| CN105047254A (en) * | 2015-06-30 | 2015-11-11 | 苏州洋杰电子有限公司 | Thick film resistor paste and preparation method thereof |
| CN105828465A (en) * | 2016-03-31 | 2016-08-03 | 东莞珂洛赫慕电子材料科技有限公司 | Thick-film resistor slurry based on stainless steel base material and preparation method thereof |
| CN106098140A (en) * | 2016-05-23 | 2016-11-09 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of PTC thermistor slurry based on stainless steel substrate and preparation method thereof |
| CN106128548A (en) * | 2016-06-29 | 2016-11-16 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of resistance slurry of high electric heating conversion ratio |
| CN107424661A (en) * | 2017-06-28 | 2017-12-01 | 西安英诺维特新材料有限公司 | A kind of devitrified glass heating plate medium temperature resistance slurry |
| CN107545946A (en) * | 2017-08-21 | 2018-01-05 | 浙江安扬新能源科技有限公司 | A kind of resistance slurry for stainless steel thick film circuit and preparation method thereof |
| CN108851235A (en) * | 2018-05-24 | 2018-11-23 | 宁夏艾森达新材料科技有限公司 | Aluminium nitride for liquid tobacco tar heating atomization heats substrate |
| CN109448885A (en) * | 2018-11-05 | 2019-03-08 | 浙江亮能机电科技有限公司 | A kind of YH21CT stainless steel thick film circuit resistance slurry and preparation method thereof |
| CN109461517A (en) * | 2018-11-28 | 2019-03-12 | 浙江亮能机电科技有限公司 | A kind of conductor paste and preparation method thereof for stainless steel thick film circuit |
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- 2002-12-30 CN CN 02139894 patent/CN1216380C/en not_active Expired - Fee Related
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|---|---|---|---|---|
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| WO2008014678A1 (en) * | 2006-07-28 | 2008-02-07 | Kezheng Wang | Rare earth base-metal resistance slurry for rare earth thick-film circuit based on metal substrate and producing process thereof |
| WO2008014680A1 (en) * | 2006-07-28 | 2008-02-07 | Kezheng Wang | Rare earth resistance slurry for rare earth thick-film circuit based on metal substrate and producing process thereof |
| WO2008014679A1 (en) * | 2006-07-28 | 2008-02-07 | Ke Zheng Wang | Rare earth medium slurry for rare earth thick-film circuit based on metal substrate and producing process thereof |
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| CN109448885A (en) * | 2018-11-05 | 2019-03-08 | 浙江亮能机电科技有限公司 | A kind of YH21CT stainless steel thick film circuit resistance slurry and preparation method thereof |
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