CN103903677A - Medium temperature sintering type electro-conduction slurry with lead-free glass powder and preparation method of medium temperature sintering type electro-conduction slurry - Google Patents
Medium temperature sintering type electro-conduction slurry with lead-free glass powder and preparation method of medium temperature sintering type electro-conduction slurry Download PDFInfo
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- CN103903677A CN103903677A CN201410098673.5A CN201410098673A CN103903677A CN 103903677 A CN103903677 A CN 103903677A CN 201410098673 A CN201410098673 A CN 201410098673A CN 103903677 A CN103903677 A CN 103903677A
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Abstract
The invention discloses a medium temperature sintering type electro-conduction slurry with lead-free glass powder and a preparation method of the medium temperature sintering type electrocondution slurry. The preparation method is characterized by comprising the steps of preparing an organic carrier, preparing the lead-free glass powder, preparing silver powder and preparing the electro-conduction slurry. The electro-conduction slurry comprises, by mass, 0 to 80% of micron-scale spherical silver powder, 5% to 70% of micron-scale flake silver powder, 2% to 25% of the lead-free glass powder and 0 to 25% of the organic carrier. The lead-free glass powder comprises, by mass, 25% to 75% of Bi2O3, 20% to 60% of B2O3, 0 to 20% of ZnO, 0 to 20% of Sb2O3, 0 to 10% of Al2O3 and 0 to 8% of alkali metal oxide. The organic carrier comprises, by mass, 50% to 80% of terpilenol, 10% to 40% ofbutyl carbitol acetic ester, 0 to 10% of tributyl citrate, 3% to 10% of ethocel, 0 to 2% of hydrogenated castor oil and 0 to 3% of addition agent.
Description
Technical field
The present invention relates to a kind of preparation of electrocondution slurry, particularly disclose a kind of intermediate sintering temperature type electrocondution slurry that contains lead-free glass powder and preparation method thereof, be specially adapted to Al
2o
3silver slurry for substrate thick-film conductor circuit, belongs to technical field of electronic materials.
Background technology
Because silver has excellent conduction and heat conductivility, flint glass has low-temperature sintering performance and good adhesive property, leaded silver slurry, as microelectronics Packaging, electrode and interconnecting material etc., is to have gathered subject technology a kind of high-tech electronics functional materials such as chemical industry, electronics, metallurgy.The contained PbO of glass in most of plumbous series conductive slurry is more than 70%, due to Lead pollution environment, harmful, makes its application in silver slurry be subject to serious restriction.The research of the unleaded conductive silver paste of current domestic intermediate sintering temperature type is less, and the intermediate sintering temperature type electrocondution slurry of preparation take lead-free glass powder as Binder Phase become a kind of inexorable trend.
Unleaded conductive silver paste is made up of silver powder, lead-free glass powder and organic carrier three.The factors such as the shape of silver powder, dispersiveness, granularity, affect pattern and the density of conductive thick film after sintering, have affected the electrical property of conductive thick film on largely.Owing to contacting as main take face contact or line between flake silver powder particle, between spherical silver powder particles take a contact as main, spherical and flake silver powder is mixed with silver slurry, in conductive thick film after sintering, spherical silver powder can, in the flake silver powder effect that " conduction bridge " do not played in the position of abundant overlapping contact, improve thick-film conductor performance.At present, spherical, sheet is mixed silver powder and in conducting resinl, is applied more extensive, the report using in slug type silver slurry is less, S.P. the Wu spherical and flake silver powder mixing manufacture that once to utilize mass ratio be 80:20 a kind of high-temperature electric conduction silver slurry, after this slurry silk screen printing sintering, electric conductivity and adhesive strength all improve a lot, but the impact of the mixing silver powder that he does not study different proportion in great detail on silver slurry performance.
At present common slug type electrocondution slurry exists following not enough: (1), although some electrocondution slurry combination property is better, contains the chemical element that lead, chromium etc. are harmful to human and environment.(2) slurry sintering temperature is higher, does not meet efficient, energy-conservation requirement.(3) mesh permeability is not good when silk screen printing, and depth-width ratio is not ideal enough, and after sintering, sheet resistance high electrical conductivity is poor.(4) in order to improve electric conductivity, increase the content of conductive phase, improve the preparation cost of slurry.(5) after sintering, the soldering resistance of conductive thick film can be poor.
In order to meet the requirement of environmental protection, the Chinese patent that application number is 200810039730.7 discloses a kind of lead-free silver slurry for high-temperature sintered automobile glass heating wire, and this silver slurry uses lead-free glass powder by Bi
2o
3, SiO
2, B
2o
3, ZnO, Al
2o
3, TiO
2, the composition such as Ag, but its softening temperature is higher, causes slurry sintering temperature higher, and the conductive thick film soldering resistance obtaining after this slurry sintering is poor.In order to improve thick film soldering resistance energy, reduce sintering temperature, the patent No. is that the Chinese patent of CN201010190544.0 discloses the thick film conductor paste that a kind of aluminum oxide substrate uses, in the silver powder of this slurry, adulterated a certain amount of palladium powder or platinum powder, can improve the erosion-resisting characteristics of thick film in welding process; In addition, in this slurry glassy phase, increased Bi
2o
3content reduced the sintering temperature of slurry, but after this slurry sintering, the conductivity of thick film is poor.
Summary of the invention
Object of the present invention addresses the deficiencies of the prior art, and a kind of intermediate sintering temperature type electrocondution slurry that contains lead-free glass powder and preparation method thereof is provided, and is a kind of intermediate sintering temperature type conductive paste composition being applicable to take aluminium oxide as substrate.
The present invention is achieved in that a kind of intermediate sintering temperature type electrocondution slurry that contains lead-free glass powder and preparation method thereof, it is characterized in that: described electrocondution slurry comprises following component and quality percentage composition: micron level spherical silver powder 0～80%, micron-stage sheet-like silver powder 5～70%, lead-free glass powder 2～25% and organic carrier 0～25%; The particle diameter of described micron level spherical silver powder is 0.5～2.5 μ m, and the particle diameter of described micron-stage sheet-like silver powder is 2.0～6.0 μ m, and the component of described lead-free glass powder and quality percentage composition are: Bi
2o
325～75%, B
2o
320～60%, ZnO 0～20%, Sb
2o
30～20%, Al
2o
30～10% and alkali metal oxide 0～8%, described alkali metal oxide is Li
2o, the component of described organic carrier and quality amount percentage composition are: terpinol 50～80%, butyl carbitol acetate 10～40%, tributyl citrate 0～10%, ethyl cellulose 3～10%, rilanit special 0～2% and auxiliary agent 0～3%, described auxiliary agent is selected a kind of in soybean lecithin, BYK-354, BYK-9076.
The tap density of described micron level spherical silver powder is 1.0～2.5g/ml, and the tap density of described micron-stage sheet-like silver powder is 1.0～4.5 g/ml.The peak firing temperature of described lead-free glass powder is: 550～750 ℃.
Described preparation method comprises the following steps:
1) prepare organic carrier: carry out proportioning according to the component of described organic carrier and quality amount percentage composition, at 80～120 ℃, dissolve, obtain the organic binder bond of transparent and homogeneous;
2) prepare lead-free glass powder: take raw material according to the component of described lead-free glass powder and quality percentage composition proportioning, utilize planetary ball mill to mix take ethanol as medium ball milling 30～60min, the oxide that obtains mixing after being dried, is packed into Al
2o
3in crucible, in Si-Mo rod stove, be warming up to 1100～1300 ℃, insulation 0.5～2h, after compound fusing, pour in deionized water and obtain glass dregs, then dry, pack ball grinder ball milling 24h in planetary ball mill into, obtain the lead-free glass powder that D50 is 0～2.5 μ m;
3) prepare silver powder: adopt liquid phase reduction, take gum arabic as dispersant and protective agent, with ascorbic acid be reducing agent reduction liquor argenti nitratis ophthalmicus, having prepared average grain diameter is the micron level spherical silver powder of 0.5～2.5 μ m, and re-using high-energy ball milling method, to prepare average grain diameter be 2.0～6.0 μ m micron-stage sheet-like silver powder;
4) prepare electrocondution slurry: described organic carrier, lead-free glass powder, micron level spherical silver powder and micron-stage sheet-like silver powder are mixed by the component of described electrocondution slurry and quality percentage composition proportioning, then being ground to fineness with three-roll grinder is below 10 μ m, the finished product silver slurry that viscosity is 200～250Pa.s.
Compared with prior art, when silk screen printing of the present invention, mesh permeability is good, has good viscosity coefficient, and reasonably combined by spherical and flake silver powder, having reduced on the basis of silver-colored consumption, improved electric conductivity.The present invention has adopted a kind of high Bi
2o
3middle temperature lead-free glass powder, is reduced to 550～750 ℃ by slurry peak firing temperature, the Bi in the time of sintering in this kind of glass
2o
3al easily and in substrate
2o
3there is eutectic reaction, and this kind of glass and Al
2o
3the expansion coefficient mismatching of substrate is good, has improved the adhesive strength of conductive thick film.
The invention has the beneficial effects as follows:
1) lead-free glass powder that the electrocondution slurry that prepared by the inventive method adopts, softening temperature is low, meets the requirement of energy-conserving and environment-protective;
2) electrocondution slurry that prepared by the inventive method has good viscosity coefficient, and when silk screen printing, mesh permeability is better, depth-width ratio ideal, and after sintering, sheet resistance is lower, the minimum 2m Ω/ that reaches, conductivity is better;
3) after sintering, the soldering resistance of conductive thick film can be better;
4) reasonably combined by ball-type and flake silver powder, having reduced on the basis of silver-colored consumption, has improved electric conductivity.
Embodiment
A kind of intermediate sintering temperature type electrocondution slurry that contains lead-free glass powder of the present invention and preparation method thereof, the raw material of electrocondution slurry comprises following component and quality percentage composition: micron level spherical silver powder 0～80%, micron-stage sheet-like silver powder 5～70%, lead-free glass powder 2～25% and organic carrier 0～25%.
Preparation method of the present invention, comprises the following steps:
1, prepare organic carrier: the component of organic carrier and quality amount percentage composition are: terpinol 50～80%, butyl carbitol acetate 10～40%, tributyl citrate 0～10%, ethyl cellulose 3～10%, rilanit special 0～2% and auxiliary agent 0～3%, auxiliary agent is selected a kind of in soybean lecithin, BYK-354, BYK-9076.Take raw material by above-mentioned organic carrier formula, at 80～120 ℃, dissolve, obtain the organic binder bond of transparent and homogeneous.
2, prepare lead-free glass powder: component and quality percentage composition that described lead-free glass powder raw material comprises are: Bi
2o
325～75%, B
2o
320～60%, ZnO 0～20%, Sb
2o
30～20%, Al
2o
30～10% and alkali metal oxide 0～8%.Basic anhydride are Li
2o.Take raw material according to above-mentioned lead-free glass powder formula, utilize planetary ball mill to mix take ethanol as medium ball milling 30～60min, the oxide that obtains mixing after being dried, is packed into Al
2o
3in crucible, in Si-Mo rod stove, be warming up to 1100～1300 ℃, insulation 0.5～2h.After compound fusing, pour in deionized water and obtain glass dregs, then dry, pack ball grinder ball milling 24h in planetary ball mill into, obtain the glass dust that D50 is 0～2.5 μ m.
3, prepare silver powder: adopting liquid phase reduction, take gum arabic as dispersant and protective agent, is that reducing agent reduces liquor argenti nitratis ophthalmicus with ascorbic acid, and having prepared average grain diameter is the micron level spherical silver powder of 0.5～2.5 μ m; Take above-mentioned micron level spherical silver powder as raw material, using high-energy ball milling method to prepare average grain diameter is 2.0～6.0 μ m micron-stage sheet-like silver powder.
4, prepare electrocondution slurry: above-mentioned organic carrier, lead-free glass powder and silver powder are mixed according to above-mentioned conductive paste composition proportioning, and being then ground to fineness with three-roll grinder is that the finished product silver that viscosity is 200～250Pa.s is starched below 10 μ m.
Below in conjunction with specific embodiment, further set forth the present invention, the following examples are to be only not used in restriction composition range of the present invention for the present invention is described.
Embodiment 1:
An intermediate sintering temperature type electrocondution slurry that contains lead-free glass powder, the quality percentage composition of its constitutive material is: micron level spherical silver powder 63%, micron-stage sheet-like silver powder 7%, lead-free glass powder 7% and organic carrier 23%.
The preparation method of conductive silver paste comprises the following steps:
1, prepare organic carrier: organic carrier component and quality percentage composition are: terpinol 55.2%, butyl carbitol acetate 27.6%, tributyl citrate 9.2%, ethyl cellulose 6%, rilanit special 1%, soybean lecithin 1%.Take raw material by above-mentioned organic carrier formula, at 100 ℃, dissolve, obtain the organic binder bond of transparent and homogeneous.
2, prepare lead-free glass powder: the component of lead-free glass powder and quality percentage composition are: Bi
2o
325%, B
2o
360%, ZnO 10%, Sb
2o
32%, Al
2o
32% and Li
2o 1%.Take raw material according to above-mentioned lead-free glass powder formula, utilize planetary ball mill to mix take ethanol as medium ball milling 30～60min, the oxide that obtains mixing after being dried, is packed into Al
2o
3in crucible, in Si-Mo rod stove, be warming up to 1200 ℃, insulation 0.5h.After compound fusing, pour in deionized water and obtain glass dregs, then dry, pack ball grinder ball milling 24h in planetary ball mill into, obtain the glass dust that D50 is 0～2.5 μ m.
3, prepare silver powder: adopt liquid phase reduction, the mixed solution of preparation gum arabic and ascorbic acid, the concentration of ascorbic acid is 0.17mol/L, the consumption of gum arabic is for dripping AgNO
3the 12.7wt% of amount, the liquor argenti nitratis ophthalmicus that is 0.24mol/L by concentration is added drop-wise in above-mentioned mixed solution with the speed of 1/S, adopts concentrated ammonia liquor to regulate the pH=4 of reaction solution, and mixing speed is 900 r/min, reaction at 25 ℃, having prepared average grain diameter is the micron level spherical silver powder of 2.0 μ m; Take above-mentioned micron level spherical silver powder as raw material, using high-energy ball milling method to prepare average grain diameter is 2.0～6.0 μ m micron-stage sheet-like silver powder.
4, prepare electrocondution slurry: above-mentioned organic carrier, lead-free glass powder and silver powder are mixed according to the proportioning of above-mentioned electrocondution slurry, and being then ground to fineness with three-roll grinder is 7～8 μ m, viscosity is the finished product silver slurry of 220Pa.s left and right.
Embodiment 2:
An intermediate sintering temperature type electrocondution slurry that contains lead-free glass powder, the quality percentage composition of its constitutive material is: micron level spherical silver powder 56%, micron-stage sheet-like silver powder 14%, lead-free glass powder 14% and organic carrier 16%.
The method of conductive silver paste comprises the following steps:
1, prepare organic carrier: organic carrier component and quality percentage composition are: terpinol 70%, butyl carbitol acetate 12%, tributyl citrate 5%, ethyl cellulose 10%, rilanit special 2%, BYK-354 1%.Take raw material by above-mentioned organic carrier formula, at 100 ℃, dissolve, obtain the organic binder bond of transparent and homogeneous.
2, prepare lead-free glass powder: the component of lead-free glass powder and quality percentage composition are: Bi
2o
350%, B
2o
330%, ZnO 7%, Sb
2o
35%, Al
2o
35% and Li
2o 3%.Take raw material according to above-mentioned lead-free glass powder formula, utilize planetary ball mill to mix take ethanol as medium ball milling 30～60min, the oxide that obtains mixing after being dried, is packed into Al
2o
3in crucible, in Si-Mo rod stove, be warming up to 1200 ℃, insulation 0.5h.After compound fusing, pour in deionized water and obtain glass dregs, then dry, pack ball grinder ball milling 24h in planetary ball mill into, obtain the glass dust that D50 is 0～2.5 μ m.
3, prepare silver powder: adopt liquid phase reduction, the mixed solution of preparation gum arabic and ascorbic acid, the concentration of ascorbic acid is 0.17mol/L, the consumption of gum arabic is for dripping AgNO
3the 12.7wt% of amount, the liquor argenti nitratis ophthalmicus that is 0.24mol/L by concentration is added drop-wise in above-mentioned mixed solution with the speed of 1/S, adopts concentrated ammonia liquor to regulate the pH=4 of reaction solution, and mixing speed is 900 r/min, reaction at 25 ℃, having prepared average grain diameter is the micron level spherical silver powder of 2.0 μ m; Take above-mentioned micron level spherical silver powder as raw material, using high-energy ball milling method to prepare average grain diameter is 2.0～6.0 μ m micron-stage sheet-like silver powder.
4, prepare electrocondution slurry: above-mentioned organic carrier, lead-free glass powder and silver powder are mixed according to the proportioning of above-mentioned electrocondution slurry, and being then ground to fineness with three-roll grinder is 7～8 μ m, viscosity is the finished product silver slurry of 220Pa.s left and right.
Embodiment 3:
An intermediate sintering temperature type electrocondution slurry that contains lead-free glass powder, the quality percentage composition of its constitutive material is: micron level spherical silver powder 41%, micron-stage sheet-like silver powder 29%, lead-free glass powder 25% and organic carrier 5%.
The method of conductive silver paste comprises the following steps:
1, prepare organic carrier: organic carrier component and quality percentage composition are: terpinol 80%, butyl carbitol acetate 12.5%, tributyl citrate 1%, ethyl cellulose 3%, rilanit special 0.5% and BYK-9076 3%.Take raw material by above-mentioned organic carrier formula, at 100 ℃, dissolve, obtain the organic binder bond of transparent and homogeneous.
2, prepare lead-free glass powder: the component that lead-free glass powder raw material comprises and quality percentage composition are: Bi
2o
370%, B
2o
320%, ZnO 5%, Sb
2o
32%, Al
2o
32% and Li
2o 1%.Formula according to above-mentioned lead-free glass powder takes raw material, utilizes planetary ball mill to mix take ethanol as medium ball milling 30～60min, and the oxide that obtains mixing after being dried, is packed into Al
2o
3in crucible, in Si-Mo rod stove, be warming up to 1200 ℃, insulation 0.5h.After compound fusing, pour in deionized water and obtain glass dregs, then dry, pack ball grinder ball milling 24h in planetary ball mill into, obtain the glass dust that D50 is 0～2.5 μ m.
3, prepare silver powder: adopt liquid phase reduction, the mixed solution of preparation gum arabic and ascorbic acid, the concentration of ascorbic acid is 0.17mol/L, the consumption of gum arabic is for dripping AgNO
3the 12.7wt% of amount, the liquor argenti nitratis ophthalmicus that is 0.24mol/L by concentration is added drop-wise in above-mentioned mixed solution with the speed of 1/S, adopts concentrated ammonia liquor to regulate the pH=4 of reaction solution, and mixing speed is 900 r/min, reaction at 25 ℃, having prepared average grain diameter is the micron level spherical silver powder of 2.0 μ m; Take above-mentioned micron level spherical silver powder as raw material, using high-energy ball milling method to prepare average grain diameter is 2.0～6.0 μ m micron-stage sheet-like silver powder.
4, prepare electrocondution slurry: above-mentioned organic carrier, lead-free glass powder and silver powder are mixed according to the proportioning of above-mentioned electrocondution slurry, and being then ground to fineness with three-roll grinder is 7～8 μ m, viscosity is the finished product silver slurry of 220Pa.s left and right.
Claims (4)
1. an intermediate sintering temperature type electrocondution slurry that contains lead-free glass powder, is characterized in that: described electrocondution slurry comprises following component and quality percentage composition: micron level spherical silver powder 0～80%, micron-stage sheet-like silver powder 5～70%, lead-free glass powder 2～25% and organic carrier 0～25%; The particle diameter of described micron level spherical silver powder is 0.5～2.5 μ m, and the particle diameter of described micron-stage sheet-like silver powder is 2.0～6.0 μ m, and the component of described lead-free glass powder and quality percentage composition are: Bi
2o
325～75%, B
2o
320～60%, ZnO 0～20%, Sb
2o
30～20%, Al
2o
30～10% and alkali metal oxide 0～8%, described alkali metal oxide is Li
2o, the component of described organic carrier and quality amount percentage composition are: terpinol 50～80%, butyl carbitol acetate 10～40%, tributyl citrate 0～10%, ethyl cellulose 3～10%, rilanit special 0～2% and auxiliary agent 0～3%, described auxiliary agent is selected a kind of in soybean lecithin, BYK-354, BYK-9076.
2. according to the intermediate sintering temperature type electrocondution slurry that contains lead-free glass powder described in claim 1, it is characterized in that: the tap density of described micron level spherical silver powder is 1.0～2.5g/ml, the tap density of described micron-stage sheet-like silver powder is 1.0～4.5 g/ml.
3. according to described in claim 1, it is characterized in that the intermediate sintering temperature type electrocondution slurry that contains lead-free glass powder: the peak firing temperature of described lead-free glass powder is: 550～750 ℃.
4. a preparation method for the intermediate sintering temperature type electrocondution slurry that contains lead-free glass powder described in any one in claim 1～3, is characterized in that: described preparation method comprises the following steps:
1) prepare organic carrier: carry out proportioning according to the component of described organic carrier and quality amount percentage composition, at 80～120 ℃, dissolve, obtain the organic binder bond of transparent and homogeneous;
2) prepare lead-free glass powder: take raw material according to the component of described lead-free glass powder and quality percentage composition proportioning, utilize planetary ball mill to mix take ethanol as medium ball milling 30～60min, the oxide that obtains mixing after being dried, is packed into Al
2o
3in crucible, in Si-Mo rod stove, be warming up to 1100～1300 ℃, insulation 0.5～2h, after compound fusing, pour in deionized water and obtain glass dregs, then dry, pack ball grinder ball milling 24h in planetary ball mill into, obtain the lead-free glass powder that D50 is 0～2.5 μ m;
3) prepare silver powder: adopt liquid phase reduction, take gum arabic as dispersant and protective agent, with ascorbic acid be reducing agent reduction liquor argenti nitratis ophthalmicus, having prepared average grain diameter is the micron level spherical silver powder of 0.5～2.5 μ m, and re-using high-energy ball milling method, to prepare average grain diameter be 2.0～6.0 μ m micron-stage sheet-like silver powder;
4) prepare electrocondution slurry: described organic carrier, lead-free glass powder, micron level spherical silver powder and micron-stage sheet-like silver powder are mixed by the component of described electrocondution slurry and quality percentage composition proportioning, then being ground to fineness with three-roll grinder is below 10 μ m, the finished product silver slurry that viscosity is 200～250Pa.s.
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