CN1215484C - Medium sizing agent and its producing process for high-power thick-film circuit based on stainless steel substrate - Google Patents
Medium sizing agent and its producing process for high-power thick-film circuit based on stainless steel substrate Download PDFInfo
- Publication number
- CN1215484C CN1215484C CN 02139896 CN02139896A CN1215484C CN 1215484 C CN1215484 C CN 1215484C CN 02139896 CN02139896 CN 02139896 CN 02139896 A CN02139896 A CN 02139896A CN 1215484 C CN1215484 C CN 1215484C
- Authority
- CN
- China
- Prior art keywords
- stainless steel
- organic binder
- microcrystalline glass
- binder bond
- cao
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
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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
- 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
Abstract
The present invention relates to medium slurry used for high-power thick-film circuits based on stainless steel base plates. The present invention is composed of solid-phase components and organic binding agents with the proportion (weight ratio) of (70 to 90): (30 to 10), wherein the solid-phase components are microcrystalline glass in the system of SiO2-B2O3-Al2O3-CaO which comprises 30 to 70% of SiO2, 1 to 15% of B2O3, 5 to 30% of Al2O3, 20 to 60% of CaO, 1 to 10% of Co2O3, 1 to 10% of TiO2 and the to 10% of ZrO2, and the components of the organic binding agents comprise the compounding ratios (weight ratios) 70 to 98% of tributyl citrate, 0.1 to 10% of 1, 4-butyrolactone, 0.5 to 10% of nitrocellulose, 0.1 to 5% of hydrogenated castor oil and 0.1 to 5% of lecithin. The present invention comprises the preparation technology: A. preparing microcrystalline glass powder, which means placing raw materials into a high-temperature electric furnace after the raw materials are harmoniously mixed in a mixer according to the compounding ratios for smelting, water quenching and ball milling; B. preparing the organic binding agents; C. proportionally placing the microcrystalline glass powder and the organic binding agents in a container to obtain finished products by stirring and rolling.
Description
Technical field: the present invention relates to high-power (tens of watts to thousands of watts) thick film circuit dielectric paste based on stainless steel substrate.Be particularly related to based on the high-power thick film integrated circuit of ferritic stainless steel series such as () 1Cr17 substrate with dielectric paste and preparation technology thereof.
Background technology: characteristics such as the high power density that the large power thick film circuit element has, high mechanical properties, heat shock resistance, anti-vibration propose corresponding mechanics and thermal property requirement to substrate.
Conventional substrate material such as ceramic material class, macromolecular material class etc. have excellent dielectric properties, the series electronic slurry commercialization already that is complementary with it, but as the large power thick film circuit element, with the brittle ceramic materials is that substrate can't satisfy its basic instructions for use, and wherein sixty-four dollar question is frangible in installation and the use.The macromolecular material substrate can't satisfy the hot property requirement of high-power generation.Good mechanics that metal has and physical property might be used it as baseplate material, but bring not matching of the coefficient of expansion and electric slurry commonly used thus again, and the problems such as oxidation of thick film firing process generation.
Stainless steel proposes to be different from the specification requirement of general dielectric paste to the dielectric paste for preparing high-power thick film integrated circuit as baseplate material.1, processing performance: because product power is bigger, the working temperature of this class component is generally higher, therefore multiselect in addition for satisfying the requirement of element electric property, need repeatedly silk screen printing on substrate, is dried, is burnt till etc. with the acquisition adequate thickness with 850 ℃ of high temperature standard firing process during component fabrication.Thus slurry is proposed more complicated technology requirement, comprising: silk screen printing characteristic and refiring capability (850 ℃) repeatedly; 2, physical property: dielectric paste stainless steel surfaces by silk-screen, technology such as burn till and obtain insulating barrier, the acquisition of desirable insulating barrier is obviously relevant with the function phase related physical performance of dielectric paste, these performances comprise: expansion character; Heat conductivility; Heat resistance; Bonding force with stainless steel substrate.3, electric property: as the insulating barrier between stainless steel and resistance track and the electrode, dielectric paste should possess good electric property after silk-screen burns till, comprising: breakdown strength; Insulation resistance; Leakage current.4, environmental requirement: when large power thick film circuit uses as electric heating element, also should propose not contain the requirement of Toxic matter, be exactly not contain elements such as heavy metal such as cadmium, lead, barium to dielectric paste.
In above-mentioned many requirements of dielectric paste, can't satisfy mostly with dielectric paste based on the thick film circuit of ceramic substrate.
Summary of the invention: technical problem to be solved by this invention provides a kind of breakdown strength height, good insulation preformance, printing characteristic, burn till characteristic and environmental-protecting performance is good and the thick film circuit that is complementary with stainless steel substrate with dielectric paste and preparation technology thereof.
The present invention solves the problems of the technologies described above the employing following technical proposal, medium pulp for large power thick film circuit based on stainless steel substrate of the present invention, be characterized in it by solid phase composition (microcrystalline glass powder) and organic binder bond by certain preparation technology's gained, the ratio of solid phase composition and organic binder bond (weight ratio) is (70～90): (30～10).
As a further improvement on the present invention, its characteristics are that described solid phase composition is SiO
2-B
2O
3-Al
2O
3-CaO microcrystalline glass in series, all kinds of raw materials and proportioning (weight ratio) are SiO
2(30～70%), B
2O
3(1～15%), Al
2O
3(5～30%), CaO (20～60%), Co
2O
3(1～10%), TiO
2(1～10%), ZrO
2(1～10%); Each set of dispense than (weight ratio) is in the described organic binder bond: tributyl citrate (70～98%), 1,4-butyrolactone (0.1～10%), NC Nitroncellulose (0.5～10%), rilanit special (0.1～5%), lecithin (0.1～5%).
The preparation technology of the medium pulp for large power thick film circuit based on stainless steel substrate of the present invention is:
A, preparation microcrystalline glass powder: by weight percentage with following proportion raw material: SiO
2(30～70%), B
2O
3(1～15%), Al
2O
3(5～30%), CaO (20～60%), Co
2O
3(1～10%), 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, preparation organic binder bond: with organic solvent and thickener, surfactant, thixotropic agent etc. by a certain percentage in 80～100 ℃ of dissolving a few hours, all kinds of raw materials and proportioning are: tributyl citrate (70～98%), 1,4-butyrolactone (0.1～10%), NC Nitroncellulose (0.5～10%), rilanit special (0.1～5%), lecithin (0.1～5%); Adjust the nitrocellulose cellulose content, organic binder bond viscosity is controlled in 200～300mPas scope;
C, with the aforementioned microcrystalline glass powder that makes and organic binder bond in (70～90): the ratio of (30～10) places carries out three-roll rolling after the container dispersed with stirring and gets product.
Major advantage of the present invention is:
1, by to reasonable analysis, select for use devitrified glass as the medium phase based on basic demands such as medium pulp for large power thick film circuit physics, chemical property and the processing performance of stainless steel substrate and environmental protection.By to SiO
2-B
2O
3-Al
2O
3System researches such as-CaO microcrystalline glass in series the coefficient of expansion, vitrification point, softening temperature, crystallite forming core growth dynamics, determine microcrystalline glass formula and melting, ball-milling technology, making it to satisfy with 1Cr17 is the basic demand of 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 ester main solvent to replace traditional one pack system ester main solvent, with the main solvent rational proportion of different boiling and evaporation rate to better meet the basic demand of slurry in each technological processes such as depositing, print, dry, burn till.
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, dielectric paste printing characteristic of the present invention and burn till characteristic good, by the dielectric layer of dielectric paste preparation of the present invention have that breakdown strength is big, insulation resistance is high, with based on the thick film circuit of stainless steel substrate with advantages such as resistance slurry and electrocondution slurry are compatible.
Embodiment:
Embodiment 1:
The dielectric paste that is used for 1Cr17 series stainless steel substrate
1, microcrystalline glass formula: SiO
2(32%), B
2O
3(4%), Al
2O
3(14%), CaO (41%), Co
2O
3(3%), 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, machine binder formula and dissolution process: tributyl citrate (94.5%), NC Nitroncellulose (4%), 1,4-butyrolactone (0.5%), 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.
5, size mixing technology: with glass dust and organic binder bond in proportion (72: 28) carry out three-roll rolling after placing the container dispersed with stirring.
6, size performance:
Electric property when on stainless steel substrate, burning till thickness greater than 80 microns
| Color | Solid content | Viscosity 10RPM | Meshcount | Firing process | Diluent |
| Avy blue | 70％ | 110±20Pas | 90 orders | 850℃ | Tributyl citrate |
| Breakdown strength | Insulation resistance | Leakage current |
| ＞1500VAC | ＞10MΩ(500VDC) | ＜2mA(250VDC) |
Embodiment 2:
The dielectric paste that is used for 1Cr17 series stainless steel substrate
1, microcrystalline glass formula: SiO
2(30%), B
2O
3(5%), Al
2O
3(12%), CaO (43%), Co
2O
3(2%), TiO
2(6%), 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, organic adhesive agent prescription and dissolution process: tributyl citrate (93%), NC Nitroncellulose (5.5%), 1,4-butyrolactone (0.5%), 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.
5, size mixing technology: with glass dust and organic binder bond in proportion (72: 28) carry out three-roll rolling after placing the container dispersed with stirring.
6, size performance:
Electric property when on stainless steel substrate, burning till thickness greater than 80 microns
| Color | Solid content | Viscosity 10RPM | Meshcount | Firing process | Diluent |
| Avy blue | 70％ | 110±20Pas | 90 orders | 850℃ | Tributyl citrate |
| Breakdown strength | Insulation resistance | Leakage current |
| ＞1500VAC | ＞10MΩ(500VDC) | ＜2mA(250VDC) |
Claims (2)
1, a kind of medium pulp for large power thick film circuit based on stainless steel substrate, it is characterized in that it is by certain preparation technology's gained by solid phase composition and organic binder bond, wherein the solid phase composition is a microcrystalline glass powder, and the weight ratio of solid phase composition and organic binder bond is 70～90: 30～10; Described solid phase composition is SiO
2-B
2O
3-Al
2O
2-CaO microcrystalline glass in series, all kinds of raw materials and weight ratio are SiO
230～70%, B
2O
31～15%, Al
2O
35～30%, CaO 20～60%, Co
2O
31～10%, TiO
21～10%, ZrO
21～10%; The weight ratio of each component is in the described organic binder bond: tributyl citrate 70～98%, 1,4-butyrolactone 0.1～10%, NC Nitroncellulose 0.5～10%, rilanit special 0.1～5%, lecithin 0.1～5%.
2, a kind of preparation is characterized in that based on the preparation technology of the medium pulp for large power thick film circuit of stainless steel substrate:
A, preparation microcrystalline glass powder: by weight percentage with following proportion raw material: SiO
230～70%, B
2O
31～15%, Al
2O
35～30%, CaO 20～60%, Co
2O
31～10%, TiO
21～10%, ZrO
21～10%, insert the high-temperature electric resistance furnace melting after in batch mixer, mixing, 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, preparation organic binder bond: with organic solvent and thickener, surfactant, thixotropic agent by a certain percentage in 80～100 ℃ of dissolving a few hours, all kinds of raw materials and proportioning are: tributyl citrate 70～98%, 1,4-butyrolactone 0.1～10%, NC Nitroncellulose 0.5～10%, rilanit special 0.1～5%, lecithin 0.1～5%; Adjust the nitrocellulose cellulose content, organic binder bond viscosity is controlled in 200～300mPas scope;
C, with the aforementioned microcrystalline glass powder that makes and organic binder bond by 70～90: 30～10 weight ratio places carries out three-roll rolling after the container dispersed with stirring and gets product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02139896 CN1215484C (en) | 2002-12-30 | 2002-12-30 | Medium 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 02139896 CN1215484C (en) | 2002-12-30 | 2002-12-30 | Medium sizing agent and its producing process for high-power thick-film circuit based on stainless steel substrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1424729A CN1424729A (en) | 2003-06-18 |
| CN1215484C true CN1215484C (en) | 2005-08-17 |
Family
ID=4750275
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02139896 Expired - Fee Related CN1215484C (en) | 2002-12-30 | 2002-12-30 | Medium sizing agent and its producing process for high-power thick-film circuit based on stainless steel substrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1215484C (en) |
Cited By (2)
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|---|---|---|---|---|
| CN101740160B (en) * | 2009-11-20 | 2011-06-08 | 湖南利德电子浆料有限公司 | Dielectric paste for metal aluminum substrate thick film circuit and preparation method thereof |
| CN109448887A (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 dielectric paste and preparation method thereof |
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| CN107705879A (en) * | 2017-08-21 | 2018-02-16 | 浙江安扬新能源科技有限公司 | A kind of dielectric paste for stainless steel thick film circuit and preparation method thereof |
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-
2002
- 2002-12-30 CN CN 02139896 patent/CN1215484C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101740160B (en) * | 2009-11-20 | 2011-06-08 | 湖南利德电子浆料有限公司 | Dielectric paste for metal aluminum substrate thick film circuit and preparation method thereof |
| CN109448887A (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 dielectric paste and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1424729A (en) | 2003-06-18 |
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Granted publication date: 20050817 Termination date: 20121230 |