WO2008014677A1 - Boue d'électrode de terres rares destinée à un circuit à couche épaisse de terres rares basé sur un substrat métallique et procédé de production correspondant - Google Patents

Boue d'électrode de terres rares destinée à un circuit à couche épaisse de terres rares basé sur un substrat métallique et procédé de production correspondant Download PDF

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Publication number
WO2008014677A1
WO2008014677A1 PCT/CN2007/002223 CN2007002223W WO2008014677A1 WO 2008014677 A1 WO2008014677 A1 WO 2008014677A1 CN 2007002223 W CN2007002223 W CN 2007002223W WO 2008014677 A1 WO2008014677 A1 WO 2008014677A1
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WO
WIPO (PCT)
Prior art keywords
powder
rare earth
glass
palladium
silver
Prior art date
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PCT/CN2007/002223
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English (en)
Chinese (zh)
Inventor
Kezheng Wang
Original Assignee
Kezheng Wang
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Filing date
Publication date
Application filed by Kezheng Wang filed Critical Kezheng Wang
Publication of WO2008014677A1 publication Critical patent/WO2008014677A1/fr

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Classifications

    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/14—Conductive material dispersed in non-conductive inorganic material
    • H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/06—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
    • H01C17/065—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thick film techniques, e.g. serigraphy
    • H01C17/06506—Precursor compositions therefor, e.g. pastes, inks, glass frits
    • H01C17/06513—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component
    • H01C17/06553—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component composed of a combination of metals and oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/06—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
    • H01C17/065—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thick film techniques, e.g. serigraphy
    • H01C17/06506—Precursor compositions therefor, e.g. pastes, inks, glass frits
    • H01C17/06513—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component
    • H01C17/06533—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component composed of oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/06—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
    • H01C17/065—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thick film techniques, e.g. serigraphy
    • H01C17/06506—Precursor compositions therefor, e.g. pastes, inks, glass frits
    • H01C17/06513—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component
    • H01C17/06533—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component composed of oxides
    • H01C17/06546—Oxides of zinc or cadmium
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/013—Heaters using resistive films or coatings
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/017—Manufacturing methods or apparatus for heaters

Definitions

  • the invention relates to a rare earth electrode slurry for a rare earth thick film circuit based on a metal substrate, in particular to a ferritic stainless steel series substrate, for example, a rare earth electrode paste for a high power rare earth thick film circuit such as a national standard brand lCrl5, lCrl7, 00Crl2 and the like Its preparation process technology.
  • the new heating element requires small volume, high power, small thermal inertia, large surface thermal load, low power consumption, high thermal efficiency, fast hot start, stable power, uniform temperature field, and process. Good sex, self-controlled temperature, safe and reliable operation, long life, adapt to the scope of the wide. At present, there is no heating element that can meet the above requirements, so the research of a new type of electric heating element such as a rare earth thick film electric heating element is imperative.
  • the object of the present invention is to provide a rare earth thick based on a metal substrate which has good electrical conductivity, strong adhesion, excellent printing characteristics, sintering characteristics, environmental performance, and excellent wettability with metal substrates, resistor blades, and dielectric pastes.
  • Membrane circuit rare earth electrode paste is to provide a rare earth thick based on a metal substrate which has good electrical conductivity, strong adhesion, excellent printing characteristics, sintering characteristics, environmental performance, and excellent wettability with metal substrates, resistor blades, and dielectric pastes.
  • Another object of the present invention is to provide a rare earth thick film circuit based on the above metal substrate. Preparation process of soil electrode slurry.
  • the rare earth electrode slurry of the rare earth thick film circuit based on the metal substrate is composed of a solid phase component and an organic solvent carrier, and the weight ratio thereof is: (70 to 90): (30 to 10).
  • the solid phase component comprises: a silver-palladium-ruthenium composite powder and a glass-ceramic powder, the weight ratio of which is: (99.4 ⁇ 94): (0.6 ⁇ 6), the palladium powder, the silver powder and the tantalum powder in the silver-palladium-ruthenium composite powder The particle size is less than 2 ⁇ ⁇ .
  • the weight ratio of palladium powder, silver powder and strontium powder is: (0.6 ⁇ 10) : (99 ⁇ 82) : (0.4 ⁇ 8).
  • the glass ceramic is a SiO 2 -Al 2 0 3 -CaO-B 2 0 3 -Bi 2 0 3 -La 2 0 3 -based glass ceramic, and the weight ratio of each oxide component is: Si0 2 ( 20 ⁇ 60%), A1 2 0 3 (5 ⁇ 35%), CaO (10 ⁇ 35%), B 2 0 3 (1 ⁇ 15%), La 2 0 3 (0 ⁇ 3 ⁇ 15%), Bi 2 0 3 (10 ⁇ 30%), Ti0 2 (Bu 10%), Zr0 2 (1 ⁇ 10%).
  • the group distribution ratio (by weight) of the organic solvent carrier is: terpineol (60 to 98%), tributyl citrate (10 to 30%), ethyl cellulose (2 to 10%), and nitrocellulose. (1 ⁇ 5%), hydrogenated castor oil (0.1 ⁇ 5%), lecithin (0.1 ⁇ 5%).
  • the preparation process of the invention is as follows: (1) Preparation of rare earth glass-ceramic powder-2 Preparation of silver-palladium-composite powder-3 Preparation of organic solvent carrier-four-dimensional three-dimensional mixing three-rolling rolling one 5 rare earth electrode paddle preparation one 6 bottled for use .
  • the expansion coefficient is matched with the metal substrate and the dielectric slurry, and the combination is firm, and the electrical conductivity, the breakdown strength and the insulation performance are effectively improved.
  • the electrode paste and the metal substrate are enhanced in oxidation resistance and ductility, and the bonding strength is improved.
  • Rare earth lanthanum (La) doping greatly changes the sintering properties, microstructure, density, phase composition and physical and mechanical properties of the glass-ceramic material phase. Thereby, the dielectric strength, electrical performance, process performance of the rare earth thick film circuit electric heating element and the wettability, compatibility and molecular bonding strength of the electronic paddle are improved. Improve the process and significantly improve the product's excellent rate.
  • the rare earth electrode paddle of the rare earth thick film circuit of the invention has excellent printing performance and sintering performance. It has excellent wettability and compatibility with rare earth resist paste and medium paste.
  • an excellent solvent such as hydrogenated castor oil is used as a thixotropic agent to form a good colloidal structure, so that the slurry has good thixotropy and anti-settling effect.
  • the rare earth functional electrode paste of the present invention can be prepared not only on a metal substrate but also on a glass ceramic, ceramic and other metal non-metal substrate. It can be prepared not only on a flat surface but also on a curved surface.
  • the rare earth electrode slurry of the invention has good electrical conductivity, good enthalpy performance, good contact performance, good solder joint integrity and firm connection; the material of the invention does not need to rely on import, 100% localization, reduce precious metal dosage, low cost, material consumption Less, energy-saving; in line with the new industrialization road of circular economy advocated by China (high scientific and technological content, good economic efficiency, low resource consumption, low environmental pollution), and has a strong prospect of foreign exchange earning.
  • the rare earth electrode slurry for rare earth thick film circuit of the invention and the preparation technique thereof are applicable to a ferritic series stainless steel substrate.
  • a ferritic series stainless steel substrate For example: national brand number lCrl5, lCrl7, 00Crl2, etc., foreign brand number 429#, 430#, 410L# and so on.
  • the electrode paddle is compatible with a variety of metal substrate dielectric materials and resistor pastes.
  • metal substrate dielectric materials and resistor pastes For example, an alumina substrate (A1 2 0 3 ), an aluminum nitride (AIN) substrate, a glass-ceramic substrate, a metal alloy aluminum, a titanium alloy substrate, or the like.
  • the heating element adopting the invention is the only one that meets the requirements of small volume, high power, small thermal inertia, large surface heat load, low power consumption, high thermal efficiency, fast heat start, stable power, uniform temperature field, good processability, and self-property. Electric heating element with temperature control, safe and reliable operation, long service life and wide range of requirements. detailed description .
  • Embodiment 1 is a diagrammatic representation of Embodiment 1:
  • This embodiment is a rare earth electrode paste for a rare earth thick film circuit used for a 1CT15 (429#) series stainless steel substrate.
  • the electrode slurry is composed of a solid phase component and an organic solvent carrier, and the solid phase component comprises a silver palladium ruthenium composite powder and a glass ceramic powder.
  • the specific formulation and process are as follows -
  • Glass-ceramic formula The weight ratio of each oxide component is: Si0 2 (28%), Al 2 0 3 (l, 6 D /.), Ca0 (14%), B 2 0 3 (7% ), La 2 0 3 (5%), Bi 2 0 3 ' (22%), Ti0 2 (5%), Zr0 2 (2%):
  • Glass-ceramic smelting process The smelting temperature is: 1350 ⁇ After 120 minutes of heat preservation, it is quickly quenched by water to obtain glass micro slag. The glass slag was placed in a two-stage ball mill to prepare a glass-ceramic powder having a particle diameter of less than 3 ⁇ m.
  • the particle size of the palladium powder, the silver powder and the niobium powder in the silver-palladium-ruthenium composite powder is less than 2 ⁇ m.
  • the weight ratio of palladium powder, silver powder and strontium powder is: 2: 97: 1.
  • Organic solvent carrier formulation and dissolution process The distribution ratio (weight) of each group of organic solvent carrier is: terpineol (78%), tributyl citrate (18%), ethyl cellulose (4%), nitrate Cellulose (2), hydrogenated castor oil (0.6%), lecithin (0.8%).
  • the above mixed organic solvent is mixed and dissolved in 85 ⁇ water temperature for several hours to adjust the content of ethyl cellulose and nitrocellulose to make organic
  • the solvent carrier viscosity was controlled in the range of 245 mPas.
  • the slurry consists of a solid phase component and an organic solvent carrier.
  • the weight ratio is: 78: 22.
  • the weight ratio of the silver-palladium-ruthenium composite powder to the glass-ceramic powder is 98. 5: 1. 5.
  • the particle size of the palladium powder, the silver powder and the niobium powder in the silver-palladium-ruthenium composite powder is less than 2 ⁇ m.
  • the above-mentioned proportioning raw materials were placed in a three-dimensional mixer and stirred and dispersed, and then placed in a three-roll mill to obtain a rare earth electrode slurry.
  • the viscosity of the test slurry was 186 PaS/RPM.
  • Embodiment 2 is a diagrammatic representation of Embodiment 1:
  • the present embodiment is a rare earth electrode pad for a rare earth thick film circuit for a lCrl7 (430#) series stainless steel substrate, the electrode slurry is composed of a solid phase component and an organic solvent carrier, and the solid phase component comprises a silver palladium ruthenium composite powder and a micro Crystal glass powder, its specific process and formula are as follows -
  • Glass-ceramic formula The weight ratio of each oxide component is: Si0 2 (30%), Al 2 0 3 (16%), Ca0 (13%). B 2 0 3 (8%), La 2 0 3 (6%), Bi 2 0 3 (26%), Ti0 2 (6%), Zr0 2 (3%):
  • Glass-ceramic smelting process The smelting temperature is: 135CTC After 120 minutes of heat preservation, it is quickly quenched by water to obtain glass micro slag. The glass slag was placed in a two-stage ball mill to prepare a glass-ceramic powder having a particle diameter of less than 3 ⁇ m.
  • Modulation of silver-palladium-ruthenium composite powder The particle size of the palladium powder, the silver powder and the niobium powder in the silver-palladium-ruthenium composite powder is less than 2 ⁇ m.
  • the weight ratio of palladium powder, silver powder and tantalum powder is 1: 98: 1.
  • Organic solvent carrier formulation and dissolution process The distribution ratio of each group of organic solvent carrier is (by weight): terpineol (76%), tributyl citrate (17 ° /.), ethyl cellulose (3%) ), nitrocellulose (3), hydrogenated castor oil (0.7%), lecithin (0.3%).
  • the above mixed organic solvent was mixed and dissolved in 85 Torr of water for several hours to adjust the content of ethyl cellulose and nitrocellulose to control the viscosity of the organic solvent carrier to be in the range of 250 mPas.
  • the slurry consists of a solid phase component and an organic solvent carrier.
  • the weight ratio is: 77: 23.
  • the weight ratio of the silver-palladium-ruthenium composite powder to the glass-ceramic powder in the solid phase component is 98:2.
  • the particle size of the palladium powder, the silver powder and the niobium powder in the silver-palladium-ruthenium composite powder is less than 2 ⁇ m.
  • the above-mentioned proportioning raw materials were placed in a three-dimensional mixer and stirred and dispersed, and then placed in a three-roll mill to obtain a rare earth electrode slurry.
  • the viscosity of the test slurry was 190 PaS/RPM.

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  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Glass Compositions (AREA)
  • Conductive Materials (AREA)

Abstract

L'invention concerne une boue d'électrode de terres rares destinée à un circuit à couche épaisse de terres rares basé sur un substrat métallique et un procédé de production correspondant. Cette boue est composée d'un composant en phase solide et d'un support de solvant organique selon un rapport exprimé en poids de (70 -90):(30 -10). Le composant en phase solide comprend une poudre de composé d'Ag-Pd-Y et une poudre de verre microcristallin selon un rapport exprimé en poids de (99,4-94):(0,6-6). Ce rapport exprimé en poids de poudre de Pd, de poudre d'Ag et de poudre d'Y de la poudre de composé d'Ag-Pd-Y équivalent à (0,6-10):(99-82):(0,4-8). La poudre de verre microcristallin consiste en du verre microcristallin à base de SiO2-Al2O3-CaO-B2O3-Bi2O3-La2O3. Le procédé de production de cette boue comprend les étapes consistant: (1) à préparer la poudre de verre microcristallin; (2) à préparer la poudre de composé d'Ag-Pd-Y; (3) à préparer le support de solvant organique; (4) à mélanger l'ensemble de trois rouleaux et à le faire rouler; (5) à préparer la boue d'électrode de terres rares; (6) à la mettre en bouteille.
PCT/CN2007/002223 2006-07-28 2007-07-23 Boue d'électrode de terres rares destinée à un circuit à couche épaisse de terres rares basé sur un substrat métallique et procédé de production correspondant WO2008014677A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CNB2006100367143A CN100499940C (zh) 2006-07-28 2006-07-28 基于金属基板的稀土厚膜电路稀土电极浆料及其制备工艺
CN200610036714.3 2006-07-28

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Publication number Priority date Publication date Assignee Title
EP2636070A1 (fr) * 2010-10-28 2013-09-11 Heraeus Precious Metals North America Conshohocken LLC Métallisations de pile solaire contenant un additif métallique
CN114009856A (zh) * 2021-09-30 2022-02-08 江苏国瓷泓源光电科技有限公司 抽吸设备的改性电极浆料及制备工艺

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CN101106842B (zh) * 2007-07-24 2011-12-21 王晨 基于微晶玻璃基板的厚膜电路电热元件及其制备工艺
CN101436441B (zh) * 2008-12-09 2011-06-15 彩虹集团公司 一种厚膜纳米金电极浆料及其制备方法
CN101923911B (zh) * 2010-04-27 2011-11-02 电子科技大学 基于不锈钢基板的ybco厚膜电阻浆料及其制备方法
CN102136308B (zh) * 2010-11-23 2012-11-14 湖南威能新材料科技有限公司 银浆料用有机载体及其制备方法和含该有机载体的银浆料及含该银浆料制造的太阳能电池
CN102290117B (zh) * 2011-04-25 2013-03-06 深圳市唯特偶新材料股份有限公司 一种低温烧结纳米银浆及其制备方法
CN102568704B (zh) * 2012-03-16 2015-01-21 广东羚光新材料股份有限公司 一种环保型无铅半导体陶瓷电容电极银浆及其制备方法
CN102646459A (zh) * 2012-05-23 2012-08-22 湖南利德电子浆料有限公司 混合银粉晶体硅基太阳能电池正面银浆料及其制备方法
CN102685942B (zh) * 2012-05-29 2014-05-07 王克政 一种ptc稀土厚膜电路智能电热元件及其制备方法
CN104318979A (zh) * 2014-09-19 2015-01-28 王晨 复合材料基厚膜电路稀土介质浆料及其制备工艺
CN106205773B (zh) * 2016-07-06 2018-04-24 东莞珂洛赫慕电子材料科技有限公司 一种基于不锈钢基材的厚膜电路稀土电极浆料及其制备方法
CN106409380A (zh) * 2016-09-27 2017-02-15 东莞珂洛赫慕电子材料科技有限公司 一种铝合金基板厚膜电路中温烧结电阻浆料及其制备方法
CN107068238A (zh) * 2016-12-09 2017-08-18 东莞珂洛赫慕电子材料科技有限公司 一种铝合金基板用厚膜电路中温烧结全银电极浆料及其制备方法
CN110690010A (zh) * 2019-10-18 2020-01-14 泰阳电子(东莞)有限公司 一种微晶玻璃板用稀土高温碳浆的制备方法
CN113724914B (zh) * 2021-11-01 2022-02-25 西安宏星电子浆料科技股份有限公司 一种耐硫化油位传感器用银钯浆料
CN114360762B (zh) * 2022-03-14 2022-06-10 西安拓库米电子科技有限公司 一种片式电阻用抗银迁移银导体浆料及其制备方法

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US5277844A (en) * 1993-03-29 1994-01-11 Rainey Clifford S Resistor composition
JPH08186006A (ja) * 1994-12-28 1996-07-16 Du Pont Kk 厚膜抵抗体組成物
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2636070A1 (fr) * 2010-10-28 2013-09-11 Heraeus Precious Metals North America Conshohocken LLC Métallisations de pile solaire contenant un additif métallique
EP2636070A4 (fr) * 2010-10-28 2014-04-02 Heraeus Precious Metals North America Conshohocken Llc Métallisations de pile solaire contenant un additif métallique
US9466738B2 (en) 2010-10-28 2016-10-11 Heracus Precious Metals North America Conshohocken LLC Solar cell metallizations containing metal additive
CN114009856A (zh) * 2021-09-30 2022-02-08 江苏国瓷泓源光电科技有限公司 抽吸设备的改性电极浆料及制备工艺

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