CN101817637A - Leadless aluminum dielectric material and preparation method thereof - Google Patents

Leadless aluminum dielectric material and preparation method thereof Download PDF

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Publication number
CN101817637A
CN101817637A CN201010160731A CN201010160731A CN101817637A CN 101817637 A CN101817637 A CN 101817637A CN 201010160731 A CN201010160731 A CN 201010160731A CN 201010160731 A CN201010160731 A CN 201010160731A CN 101817637 A CN101817637 A CN 101817637A
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dielectric material
shrend
parts
leadless
hour
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CN101817637B (en
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邓泰均
孙淑云
李京章
吴胜红
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Taiyang Electronic (Dongguan) Co Ltd
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Taiyang Electronic (Dongguan) Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/50Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57Improving the yield, e-g- reduction of reject rates

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Abstract

The invention provides a leadless aluminum dielectric material used on pure aluminum or aluminum alloy and a preparation method thereof. The preparation method of the invention comprises the following steps: firstly, mixing SiO2, B2O3, TiO2, Al2O3, ZnO, MgO, K2O, Na2O, Li2O and Bi2O3 in a certain proportion, melting the mixture in a heating furnace at 1000 DEG C, and quenching with water; then carrying out wet milling in a corundum ball milling tank for one hour and drying to obtain the leadless aluminum dielectric material; then mixing the leadless aluminum dielectric material and a certain amount of organic solvent and putting the mixture into the corundum ball milling tank for ball milling to obtain a printing material; printing the printing material onto the pure aluminum or the aluminum alloy; and then drying and sintering. The leadless aluminum dielectric material of the invention has the characteristics of no lead pollution to the environment, acid and alkaline corrosion resistance, high rigidity, good chemical stability, capability of well combining with an aluminum substrate, high insulating property and the like, and is suitable for surface decoration of various colors and insulation voltage resistant protection of the aluminum substrate.

Description

Leadless aluminum dielectric material and preparation method
Technical field
The present invention relates to a kind of production technique of leadless aluminum dielectric material, particularly relate to a kind of leadless aluminum dielectric material of on aluminium or aluminium alloy base plate, using and preparation method.
Background technology
At present, in field of electric heating, had stainless steel to be used for heated substrates, still, stainless steel is as the substrate quality weight, and heat-up rate is slow, and the product of the board materials production of usefulness unit mass is few, and the firing temperature height, causes cost higher.The lighter weight of metallic aluminium or aluminium alloy, fast, the low price of thermal conduction, but melt temperature is lower, probably about 630 ℃, so the sintering temperature of aluminium or aluminium alloy covered material can not be higher than 600 ℃.The coating that now is used for aluminium or aluminum alloy surface, low sintering requirement for satisfied 600 ℃, added a large amount of lead therein, yet high-load plumbous oxide can cause very big pollution to environment in the production of product and later use, and the heater element major part is to contact with tap water, will work the mischief to human body like this.
Summary of the invention
The objective of the invention is to overcome above-mentioned the deficiencies in the prior art part, also take into account the adaptive leadless aluminum dielectric material preparation method of product when technical problem to be solved provides a kind of enhancing productivity, reach aluminum dielectric material leadless environment-friendly, that meet requirements such as surface characteristic and proof voltage test.
For reaching above-mentioned purpose, leadless aluminum dielectric material of the present invention and preparation method are achieved by following technical proposals:
At first prepare unleaded aluminium medium base mateiral, raw material comprises following each component by mass percentage:
Silicon-dioxide SiO 2: 25%~35%
Boron oxide B 2O 3: 11%~18%
Titanium dioxide TiO 2: 8%~14%
Aluminium sesquioxide Al 2O 3: 1%~5%
Zinc oxide ZnO:5%~10%
Magnesium oxide MgO:0.5%~3%
Potassium oxide K 2O:5%~9%
Sodium oxide Na 2O:15%~22%
Lithium Oxide 98min Li 2O:0.5%~3%
Bismuthous oxide bismuth trioxide Bi 2O 3: 9%~15%;
Each oxide compound by above-mentioned mass percent mixes, then this mixture is placed 1000 ℃ process furnace to melt one hour, pass through shrend again, according to material after the shrend: ball: the water ratio is 1: (1~1.2): placed corundum ball grinder ball milling one hour after (1~1.2) mixed, cross 200 mesh sieves then, drying gets final product again; Be placed on according to 100 parts of dielectric materials, 32 parts of organic solvents, 2 parts of mixing of kaolin that ball milling promptly obtains printing slurry in the corundum ball grinder about 2 hours; The surface treatment of aluminium base before the printing: clean zone of oxidation through hot acid earlier, pass through the thermokalite neutralizing treatment again, get final product through clean drying of high temperature washed with de-ionized water then; To print at last slurry use correct printing process with 60 purpose screen printings on aluminium base, oven dry through about 80 ℃, 600 ℃ of sintering can be met the finished product leadless aluminum dielectric material that surface characteristic, proof voltage, acid-alkali-corrosive-resisting, adherence etc. require after 3~5 minutes.
Dielectric material provided by the invention belongs to lead-free low-temperature to be fired and forms, and therefore, can not produce environment and human body in products production and the process used afterwards and pollute and harm.The present invention utilizes silicon-dioxide SiO 2With boron oxide B 2O 3As basic glass-former, utilize titanium dioxide TiO again 2Breast the covering effect that is used for improving dielectric material, simultaneously for promote breast effect, also introduced zinc oxide ZnO, be used for this kind glossiness, improve as turbidity the increase unit elongation.The present invention introduces a certain amount of aluminium oxide Al 2O 3, the high temperature viscosity that is used for adjusting dielectric material prevents crystallization with control surface thickness and quality, improves the chemical resistance of concrete ability of dielectric material, improves resistance to impact shock and hardness.Also introduce an amount of magnesium oxide MgO (less than 8%) simultaneously, enlarge sintering range, increase the coefficient of expansion and regulate firing temperature.In order to increase the coefficient of expansion, introduce basic metal, but because the present invention's use is the method for silk screen printing, comprehensive viscosity and flow leveling are considered, the introducing amount of potassium oxide generally is no more than 9%, excessive words will influence the viscosity and the toughness of glass paste, and the introducing amount of sodium oxide is no more than 20%, excessively then chap easily.The auxiliary material that adds other again reaches the function of needs.Leadless aluminum dielectric material of the present invention have to environment do not have Lead contamination, acid-resistant chemical stability good, can with characteristics such as aluminium base good binding, high insulation withstand voltage properties, be applicable to versicolor surface decoration and the protection of insulation proof voltage on fine aluminium or the aluminium alloy base plate.
Embodiment
For further understanding feature of the present invention, technique means and the specific purposes that reached, function, resolve the advantages and spirit of the present invention, by detailed description of the present invention being further understood below in conjunction with embodiment.
Leadless aluminum dielectric material of the present invention, its prescription mainly comprises: silicon-dioxide SiO2, boron oxide B2O3, titanium dioxide TiO2, aluminium sesquioxide Al2O3, zinc oxide ZnO, magnesium oxide MgO, potassium oxide K2O, sodium oxide Na2O, Lithium Oxide 98min Li2O, bismuthous oxide bismuth trioxide Bi2O3, and the preparation method is as follows:
1), the mass percent of each component in unleaded aluminium medium base mateiral composition system is:
Silicon-dioxide SiO 2: 25%~35%
Boron oxide B 2O 3: 11%~18%
Titanium dioxide TiO 2: 8%~14%
Aluminium sesquioxide Al 2O 3: 1%~5%
Zinc oxide ZnO:5%~10%
Magnesium oxide MgO:0.5%~3%
Potassium oxide K 2O:5%~9%
Sodium oxide Na 2O:15%~22%
Lithium Oxide 98min Li 2O:0.5%~3%
Bismuthous oxide bismuth trioxide Bi 2O 3: 9%~15%;
2), each oxide compound by above-mentioned mass percent mixes, then with this mixture as in 1000 ℃ the process furnace fusing one hour, pass through shrend again, according to material after the shrend: ball: the water ratio is 1: (1~1.2): placed corundum ball grinder ball milling one hour after (1~1.2) mixed, cross 200 mesh sieves then, drying can obtain dielectric material again;
3), be placed on according to 100 parts of dielectric materials, 32 parts of organic solvents, 2 parts of mixing of kaolin that ball milling promptly obtains printing slurry in the corundum ball grinder about 2 hours;
4), the surface treatment of aluminium base before the printing: clean zone of oxidation through hot acid earlier, pass through hot alkali treatment again, get final product through clean drying of high temperature washed with de-ionized water then;
5), respectively organizing mass percent in the above-mentioned organic solvent is:
Terpineol 350: 60~80%, ethyl cellulose: 1~8%
Citric acid tri butyl ester: 10~30% hydrogenated castor oils: 0.5~3%
Flow agent: 0.5~1% defoamer: 0~0.5%
Regulating various ratios makes viscosity at 100~200mPas;
6), will print slurry at last uses correct printing process to be printed on the aluminium base with 60 mesh sieves, oven dry through about 80 ℃, 600 ℃ of sintering can be met the finished product leadless aluminum dielectric material that surface characteristic, proof voltage, acid-alkali-corrosive-resisting, adherence etc. require after 3~5 minutes.
The present invention is preferable following embodiment:
Embodiment one: all kinds of raw materials according to mass ratio are in the unleaded medium base mateiral: 25% SiO 2, 16% B 2O 3, 10% TiO 2, 4.5% Al 2O 3, 7% ZnO, 1.5% MgO, 8% K 2O, 15% Na 2O, 1% Li 2O and 12% Bi 2O 3Mix, then this mixture is placed the process furnace about 1000 ℃ to melt one hour, pour the material after the fusing in cold water shrend, with the material after the shrend according to shrend after material: ball: the water ratio is 1: (1~1.2): placed corundum ball grinder ball milling one hour after (1~1.2) mixed, cross 200 mesh sieves then, drying can obtain dielectric material again; 100 parts of dielectric materials, 32 parts of organic solvents, 2 parts of mixing of kaolin are placed on ball milling promptly obtains printing slurry in the corundum ball grinder about 2 hours; Use correct printing process to be printed on the surface-treated aluminium base with 60 mesh sieves, oven dry through about 80 ℃, 600 ℃ of sintering can be met the finished product leadless aluminum dielectric material that surface characteristic, proof voltage, acid-alkali-corrosive-resisting, adherence etc. require after 3~5 minutes.
Embodiment two: all kinds of raw materials according to mass ratio are in the unleaded aluminium medium base mateiral: 26% SiO 2, 15% B 2O 3, 12% TiO 2, 1.5% Al 2O 3, 8.5% ZnO, 0.5% MgO, 5% K 2O, 17% Na 2O, 0.5% Li 2O and 14% Bi 2O 3Mix, then this mixture is placed the process furnace about 1000 ℃ to melt one hour, pour the material after the fusing in cold water shrend, with the material after the shrend according to shrend after material: ball: the water ratio is 1: (1~1.2): placed corundum ball grinder ball milling one hour after (1~1.2) mixed, cross 200 mesh sieves then, drying can obtain dielectric material again; 100 parts of dielectric materials, 32 parts of organic solvents, 2 parts of mixing of kaolin are placed on ball milling promptly obtains printing slurry in the corundum ball grinder about 2 hours; Use correct printing process to be printed on the surface-treated aluminium base with 60 mesh sieves, oven dry through about 80 ℃, 600 ℃ of sintering can be met the finished product leadless aluminum dielectric material that surface characteristic, proof voltage, acid-alkali-corrosive-resisting, adherence etc. require after 3~5 minutes.
Embodiment three: all kinds of raw materials according to mass ratio are in the unleaded aluminium medium base mateiral: 29% SiO 2, 14% B 2O 3, 8% TiO 2, 2% Al 2O 3, 6% ZnO, 3% MgO, 9% K 2O, 16% Na 2O, 3% Li 2O and 10% Bi 2O 3Mix, then this mixture is placed the process furnace about 1000 ℃ to melt one hour, pour the material after the fusing in cold water shrend, with the material after the shrend according to shrend after material: ball: the water ratio is 1: (1~1.2): placed corundum ball grinder ball milling one hour after (1~1.2) mixed, cross 200 mesh sieves then, drying can obtain dielectric material again; 100 parts of dielectric materials, 32 parts of organic solvents, 2 parts of mixing of kaolin are placed on ball milling promptly obtains printing slurry in the corundum ball grinder about 2 hours; Use correct printing process to be printed on the surface-treated aluminium base with 60 mesh sieves, oven dry through about 80 ℃, 600 ℃ of sintering can be met the finished product leadless aluminum dielectric material that surface characteristic, proof voltage, acid-alkali-corrosive-resisting, adherence etc. require after 3~5 minutes.
Embodiment four: all kinds of raw materials according to mass ratio are in the unleaded aluminium medium base mateiral: 32% SiO 2, 12% B 2O 3, 14% TiO 2, 1% Al 2O 3, 5% ZnO, 1% MgO, 6% K 2O, 18% Na 2O, 2% Li 2O and 9% Bi 2O 3Mix, then this mixture is placed the process furnace about 1000 ℃ to melt one hour, pour the material after the fusing in cold water shrend, with the material after the shrend according to shrend after material: ball: the water ratio is 1: (1~1.2): placed corundum ball grinder ball milling one hour after (1~1.2) mixed, cross 200 mesh sieves then, drying can obtain dielectric material again; 100 parts of dielectric materials, 32 parts of organic solvents, 2 parts of mixing of kaolin are placed on ball milling promptly obtains printing slurry in the corundum ball grinder about 2 hours; Use correct printing process to be printed on the surface-treated aluminium base with 60 mesh sieves, oven dry through about 80 ℃, 600 ℃ of sintering can be met the finished product leadless aluminum dielectric material that surface characteristic, proof voltage, acid-alkali-corrosive-resisting, adherence etc. require after 3~5 minutes.
Above illustrated embodiment is only with for conveniently illustrating the present invention, only for the present invention's preferred embodiment, be not that the present invention is implemented any pro forma restriction, have in the technical field under any and know the knowledgeable usually, if in the scope that does not break away from technical characterictic that the present invention carries, utilize disclosed technology contents to make the local equivalent embodiment that more should equalization changes or modify, and do not break away from technical characterictic content of the present invention, all still belong in the covering scope of the technology of the present invention feature.

Claims (7)

1. the preparation method of a leadless aluminum dielectric material is characterized in that, comprises the steps:
1., at first prepare unleaded aluminium medium base mateiral, raw material comprises following each component by mass percentage:
Silicon-dioxide SiO 2: 25%~35%
Boron oxide B 2O 3: 11%~18%
Titanium dioxide TiO 2: 8%~14%
Aluminium sesquioxide Al 2O 3: 1%~5%
Zinc oxide ZnO:5%~10%
Magnesium oxide MgO:0.5%~3%
Potassium oxide K 2O:5%~9%
Sodium oxide Na 2O:15%~22%
Lithium Oxide 98min Li 2O:0.5%~3%
Bismuthous oxide bismuth trioxide Bi 2O 3: 9%~15%;
2., the unleaded aluminium medium base mateiral with above-mentioned mass percent mixes, then this mixture is thrown in 1000 ℃ process furnace and melted one hour, pass through shrend again, according to material after the shrend: ball: the water ratio is to place corundum ball grinder ball milling one hour after 1: 1~1.2: 1~1.2 mixed, cross 200 mesh sieves then, drying can obtain dielectric material again;
3., dielectric material that above-mentioned steps is obtained, be placed on according to 100 parts of dielectric materials, 32 parts of organic solvents, 2 parts of mixing of kaolin that ball milling promptly obtains printing slurry in the corundum ball grinder about 2 hours;
4., before slurry prints, to the surface treatment of carrying out of aluminium base,, pass through hot alkali treatment more earlier, behind the clean aluminium base of high temperature washed with de-ionized water, dry then and get final product through the zone of oxidation that hot acid cleans aluminium base in printing;
5., at last will print slurry and be printed on the aluminium base with 60 mesh sieves, oven dry through about 80 ℃, 600 ℃ of sintering can obtain the finished product leadless aluminum dielectric material after 3~5 minutes.
2. the preparation method of leadless aluminum dielectric material according to claim 1 is characterized in that:
Step 3. each constituent mass per-cent of described organic solvent is:
Terpineol 350: 60~80%, ethyl cellulose: 1~8%
Citric acid tri butyl ester: 10~30% hydrogenated castor oils: 0.5~3%
Flow agent: 0.5~1% defoamer: 0~0.5%
Regulating various ratios makes viscosity at 100~200mPas.
3. the preparation method of leadless aluminum dielectric material according to claim 1, it is characterized in that: described unleaded aluminium medium base mateiral, all kinds of raw materials and mass percent thereof are: 32% SiO 2, 12% B 2O 3, 14% TiO 2, 1% Al 2O 3, 5% ZnO, 1% MgO, 6% K 2O, 18% Na 2O, 2% Li 2O and 9% Bi 2O 3Mix, then this mixture is placed 1000 ℃ process furnace to melt one hour, pour the material after the fusing in cold water shrend, with the material after the shrend according to shrend after material: ball: the water ratio is to place corundum ball grinder ball milling one hour after 1: 1~1.2: 1~1.2 mixed, cross 200 mesh sieves then, drying can obtain dielectric material again; 100 parts of dielectric materials, 32 parts of organic solvents, 2 parts of mixing of kaolin are placed on ball milling promptly obtains printing slurry in the corundum ball grinder about 2 hours; The printing slurry is printed on the surface-treated aluminium base with 60 mesh sieves, oven dry through about 80 ℃, 600 ℃ of sintering can obtain the finished product leadless aluminum dielectric material after 3~5 minutes.
4. the preparation method of leadless aluminum dielectric material according to claim 1, it is characterized in that: described unleaded aluminium medium base mateiral, all kinds of raw materials and mass ratio thereof are: 25% SiO 2, 16% B 2O 3, 10% TiO 2, 4.5% Al 2O 3, 7% ZnO, 1.5% MgO, 8% K 2O, 15% Na 2O, 1% Li 2O and 12% Bi 2O 3Mix, then this mixture is placed the process furnace about 1000 ℃ to melt one hour, pour the material after the fusing in cold water shrend, with the material after the shrend according to shrend after material: ball: the water ratio is to place corundum ball grinder ball milling one hour after 1: 1~1.2: 1~1.2 mixed, cross 200 mesh sieves then, drying can obtain dielectric material again; 100 parts of dielectric materials, 32 parts of organic solvents, 2 parts of mixing of kaolin are placed on ball milling promptly obtains printing slurry in the corundum ball grinder about 2 hours; The printing slurry is printed on the surface-treated aluminium base with 60 mesh sieves, oven dry through about 80 ℃, 600 ℃ of sintering can obtain the finished product leadless aluminum dielectric material after 3~5 minutes.
5. the preparation method of leadless aluminum dielectric material according to claim 1, it is characterized in that: described unleaded aluminium medium base mateiral, all kinds of raw materials and mass ratio thereof are: 29% SiO 2, 14% B 2O 3, 8% TiO 2, 2% Al 2O 3, 6% ZnO, 3% MgO, 9% K 2O, 16% Na 2O, 3% Li 2O and 10% Bi 2O 3Mix, then this mixture is placed the process furnace about 1000 ℃ to melt one hour, pour the material after the fusing in cold water shrend, with the material after the shrend according to shrend after material: ball: the water ratio is to place corundum ball grinder ball milling one hour after 1: 1~1.2: 1~1.2 mixed, cross 200 mesh sieves then, drying can obtain dielectric material again; 100 parts of dielectric materials, 32 parts of organic solvents, 2 parts of mixing of kaolin are placed on ball milling promptly obtains printing slurry in the corundum ball grinder about 2 hours; The printing slurry is printed on the surface-treated aluminium base with 60 mesh sieves, oven dry through about 80 ℃, 600 ℃ of sintering can obtain the finished product leadless aluminum dielectric material after 3~5 minutes.
6. the preparation method of leadless aluminum dielectric material according to claim 1, it is characterized in that: described unleaded aluminium medium base mateiral, all kinds of raw materials and mass ratio thereof are: 26% SiO 2, 15% B 2O 3, 12% TiO 2, 1.5% Al 2O 3, 8.5% ZnO, 0.5% MgO, 5% K 2O, 17% Na 2O, 0.5% Li 2O and 14% Bi 2O 3Mix, then this mixture is placed the process furnace about 1000 ℃ to melt one hour, pour the material after the fusing in cold water shrend, with the material after the shrend according to shrend after material: ball: the water ratio is to place corundum ball grinder ball milling one hour after 1: 1~1.2: 1~1.2 mixed, cross 200 mesh sieves then, drying can obtain dielectric material again; 100 parts of dielectric materials, 32 parts of organic solvents, 2 parts of mixing of kaolin are placed on ball milling promptly obtains printing slurry in the corundum ball grinder about 2 hours; The printing slurry is printed on the surface-treated aluminium base with 60 mesh sieves, oven dry through about 80 ℃, 600 ℃ of sintering can obtain the finished product leadless aluminum dielectric material after 3~5 minutes.
7. leadless aluminum dielectric material, its composition comprises following each component by weight percentage:
Silicon-dioxide SiO 2: 25%~35%
Boron oxide B 2O 3: 11%~18%
Titanium dioxide TiO 2: 8%~14%
Aluminium sesquioxide Al 2O 3: 1%~5%
Zinc oxide ZnO:5%~10%
Magnesium oxide MgO:0.5%~3%
Potassium oxide K 2O:5%~9%
Sodium oxide Na 2O:15%~22%
Lithium Oxide 98min Li 2O:0.5%~3%
Bismuthous oxide bismuth trioxide Bi 2O 3: 9%~15%.
CN2010101607314A 2010-04-23 2010-04-23 Leadless aluminum dielectric material and preparation method thereof Expired - Fee Related CN101817637B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107540228A (en) * 2017-09-25 2018-01-05 江苏时空雨电子有限公司 A kind of high insulation resistance medium powder, its precursor, preparation method and application

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CN1870838A (en) * 2006-04-29 2006-11-29 吴胜红 Electronic media material on high power stainless steel plate and its preparation method
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CN1424729A (en) * 2002-12-30 2003-06-18 中国人民解放军国防科学技术大学 Medium sizing agent and its producing process for high-power thick-film circuit based on stainless steel substrate
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107540228A (en) * 2017-09-25 2018-01-05 江苏时空雨电子有限公司 A kind of high insulation resistance medium powder, its precursor, preparation method and application

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