CN114005573B - Preparation method of high-temperature electronic paste - Google Patents

Preparation method of high-temperature electronic paste Download PDF

Info

Publication number
CN114005573B
CN114005573B CN202111332680.3A CN202111332680A CN114005573B CN 114005573 B CN114005573 B CN 114005573B CN 202111332680 A CN202111332680 A CN 202111332680A CN 114005573 B CN114005573 B CN 114005573B
Authority
CN
China
Prior art keywords
powder
temperature electronic
preparation
electronic paste
conductive
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.)
Active
Application number
CN202111332680.3A
Other languages
Chinese (zh)
Other versions
CN114005573A (en
Inventor
王立惠
王家兴
卢宗柳
张小文
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guilin University of Electronic Technology
China Nonferrous Metal Guilin Geology and Mining Co Ltd
Original Assignee
Guilin University of Electronic Technology
China Nonferrous Metal Guilin Geology and Mining Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Guilin University of Electronic Technology, China Nonferrous Metal Guilin Geology and Mining Co Ltd filed Critical Guilin University of Electronic Technology
Priority to CN202111332680.3A priority Critical patent/CN114005573B/en
Publication of CN114005573A publication Critical patent/CN114005573A/en
Application granted granted Critical
Publication of CN114005573B publication Critical patent/CN114005573B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20Conductive material dispersed in non-conductive organic material
    • H01B1/22Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/14Conductive material dispersed in non-conductive inorganic material
    • H01B1/16Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables

Abstract

The invention discloses a preparation method of high-temperature electronic paste, which utilizes the dispersion effect of lacquer tree extracted biological resin to ensure that paste particles are uniformly distributed to form a compact film; the components are environment-friendly, the spontaneous reduction of silver salt on the surface of silver is facilitated, the contact resistance between conductive particles is reduced, the conductive effect of the paste is enhanced, and the performance of the high-temperature electronic paste is improved.

Description

Preparation method of high-temperature electronic paste
Technical Field
The invention relates to the technical field of high-temperature electronic paste, in particular to a preparation method of novel high-temperature electronic paste.
Background
The high-temperature electronic paste has wide application in the industrial production of electronic components and integrated circuits, and is generally composed of a conductive phase, a glass phase and an organic solvent, and can be printed to form conductive nanowires; and (3) carrying out high-temperature sintering, wherein an organic phase and a surfactant are pyrolyzed and volatilized, glass powder is fused on a substrate, and the glass powder is adhered with silver powder to form a conductive compact film. In the process, the distribution of the conductive particles and the contact resistance among the particles have a profound effect on the slurry performance, and the formation of a dense conductive film of the slurry and the conductivity thereof are affected. There are many problems to be solved in high temperature electronic paste, such as: the organic solvent has too many pollutants, and is not friendly to the environment; the surface energy of the conductive phase particles is large, the dispersibility is poor, and the conductive phase particles are easy to agglomerate; the connecting gaps among the conductive phase particles are large, and the contact resistance is large due to unmodified surface morphology, so that the unnecessary energy consumption and the like are caused. Various drawbacks have hampered the progress of industrialization of high temperature electronic pastes.
CN108666002A discloses a metal glass-ceramic powder comprising TeO 2 :10-50wt%,TiO 2 :15-70wt%,ZnO:2-10wt%,SiO 2 :1-15wt% and Li 2 O:5-20wt% of glass phase with high temperature viscosityThe degree is big, is difficult for flowing, and surface tension is big, and the circuit is accurate when printing, but to the adhesion effect of conductive phase poor, conductive powder easily gathers, and the connection space is big, and conductive effect is poor.
CN202011529639.0 discloses that toluene sulfonyl hydrazine is attached to the surface of conductive particles, micro bubbles are generated by hydrolysis to uniformly disperse the conductive particles, the dispersibility of the slurry is improved, but the contact resistance between the conductive particles is improved by the micro bubbles, and the slurry performance is low.
CN20201102070. X discloses a novel glass comprising Bi 2 O 3 :55-75%、B 2 O 3 :5-20%、SiO 2 :5-20%、MgO:1-5%、Al 2 O 3 :1-5%. The glass and the slurry have better dispersibility, and the dispersibility of the conductive phase is improved, but the addition of auxiliary agents such as toluene, xylene and the like has serious environmental pollution.
CN201711337743.8 discloses an electronic paste in which silver-coated copper is used as a conductive phase, the cost of the paste is reduced, but the addition of auxiliary agents such as xylene, isophorone, etc. is serious to environmental pollution.
Therefore, the preparation method of the novel environment-friendly high-temperature electronic paste with good conductive phase dispersion performance and small conductive phase contact resistance is a problem to be solved by the technicians in the field.
Disclosure of Invention
In view of the above, the invention provides a method for preparing novel high-temperature electronic paste and application thereof, in particular to a method for preparing novel high-temperature electronic paste which is environment-friendly, good in conductive phase dispersibility and small in contact resistance and application thereof, and the novel high-temperature electronic paste with environment-friendly high performance is prepared by using lacquer tree extracted biological resin as a dispersing agent and a reducing agent.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the preparation method of the novel high-temperature electronic paste comprises the following steps:
step one: preparation of biological resin extracted from lacquer tree and pretreatment of conductive powder
(1.1) adding 5-10 times of ethanol water solution into the lacquer tree bark, carrying out reflux extraction for 1-3h at 100 ℃, filtering, repeatedly extracting and filtering for 1-3 times, merging filtrate, evaporating and condensing to recover ethanol, eluting by a macroporous resin column, collecting an elution part, and carrying out vacuum drying until the water content is 3-6wt% to obtain lacquer tree biological resin;
(1.2) dispersing conductive phase powder in ethanol, then adding citric acid and the lacquer tree biological resin prepared in the step (1.1), then adding sodium hypophosphite, uniformly mixing, stirring at room temperature, centrifuging at constant temperature, and vacuum drying to obtain pretreated conductive powder;
step two: preparation of novel glass powder
Weighing glass raw materials according to a proportion, mixing, placing the mixture in a sintering heat preservation furnace, firing the mixture, cooling the mixture by deionized water, and ball-milling the obtained glass to obtain glass powder;
step three: preparation of slurry support
Weighing an organic solvent, a reducing agent, lacquer tree biological resin, a coupling agent and a thickening agent according to the mass ratio, and stirring at the rotating speed of 150-250r/min for 15-30min at the temperature of 40-65 ℃ to obtain a slurry carrier;
step four: preparation of the slurry
And weighing the pretreated conductive powder, the glass powder and the slurry carrier according to the mass ratio, and uniformly mixing and dispersing to obtain the novel uniform and environment-friendly high-temperature electronic slurry.
Preferably, the aqueous ethanol solution in the first step is 60-80 wt%.
Preferably, the conductive phase powder in the step (1.2) is one or more of silver powder or silver-coated copper powder.
Preferably, the conductive phase powder in the step (1.2) is a granular powder having an average particle diameter of 0.5 to 1 μm and a flake powder having a particle diameter of 7 to 10 μm; wherein the average particle diameter of the granular conductive phase powder is preferably 0.5 μm, 0.7 μm, 0.9 μm,1 μm, and the average particle diameter of the flake conductive phase powder is preferably 7 μm, 8 μm,9 μm,10 μm; the mass ratio is M Granules and method for producing the same :M Sheet = (0.6-1): 2, preferably 0.6:2, 0.7:2, 0.8:2, 0.9:2, 1:2.
Preferably, the centrifugal speed in the first step is 8000-10000rpm, and the time is 5-10min.
Preferably, the preparation method of the glass powder in the second step comprises the following steps:
the proportion is as follows: bi (Bi) 2 O 3 :67-78wt%;B 2 O 3 :5-11wt%;SiO 2 :0-3wt%; znO:8-15wt%; inO:1-7wt%; baO:0-2wt%; cuO:0-2wt%; and (3) uniformly mixing the components, putting the mixture into a sintering heat preservation furnace, heating to 1100 ℃ for firing for 2 hours, pouring the mixture into deionized water for cold quenching, and ball-milling the mixture to 5-40 mu m by using a zirconium ball with the diameter of 1mm and 3mm at a rotating speed of 150-400rpm to obtain glass phase powder.
Preferably, in the third step, the mass ratio of the organic solvent is as follows: reducing agent: lacquer tree biological resin: coupling agent: thickener= (65-85): (5-15): (1-8): (3-10): (2-10).
Preferably, in the third step, the organic solvent is high temperature resistant resin or terpineol; the reducing agent is one or more of citric acid, ascorbic acid and formic acid; the coupling agent is a silane coupling agent; the thickener is ethyl cellulose.
Preferably, in the fourth step, the mass ratio of the pretreated conductive powder, the glass powder and the slurry carrier is = (78-90): (3-5): (7-12).
Preferably, in the fourth step, the stirring and dispersing rotational speed is 9000-15000rpm, and the dispersing time is 15-30min.
Compared with the prior art, the invention discloses a preparation method and application of the novel high-temperature electronic paste, and has the following beneficial effects:
the method has the advantages that the paint tree is used for extracting the reductive reduction conductive phase powder surface silver salt of the biological resin, so that the concave morphology of the particle surface is filled, the contact resistance among conductive particles is reduced, and the conductive capacity of the conductive phase is improved; the conductive phase and the glass phase powder can be orderly arranged by utilizing the dispersion characteristic of the biological resin extracted from the lacquer tree to form a compact conductive phase film, so that the prepared high-temperature electronic paste has good compactness, strong conductive capability, environmental protection and no pollution, and the performance of the paste is improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the novel high-temperature electronic paste comprises the following steps:
step one: preparation of biological resin extracted from lacquer tree and pretreatment of conductive powder
(1.1) adding an aqueous solution of 80wt% ethanol with the weight being 6 times that of 200g of the bark of the lacquer tree, carrying out reflux extraction for 1h at 100 ℃, filtering, repeatedly extracting and filtering for 3 times, merging filtrate, evaporating and condensing to recover ethanol, eluting through a macroporous resin column, collecting an eluting part, and carrying out vacuum drying until the water content is 4wt% to obtain the lacquer tree biological resin mainly comprising catechol resin;
(1.2) dispersing 85g of silver powder in 510mL of ethanol, then adding 5g of citric acid with any proportion and the lacquer tree biological resin prepared in the step (1.1), then adding 6g of sodium hypophosphite, uniformly mixing, stirring at room temperature for 15min, centrifuging at 10000rpm for 10min, and vacuum drying to obtain pretreated conductive powder;
step two: preparation of novel glass powder
The proportion is as follows: bi (Bi) 2 O 3 :72wt%;B 2 O 3 :8wt%;SiO 2 :3wt%; znO:11wt%; inO:3wt%; baO:1wt%; cuO:2wt%; uniformly mixing the components, putting the mixture into a sintering heat preservation furnace, heating to 1100 ℃ for firing for 2 hours, pouring the mixture into deionized water for cold quenching, ball-milling the mixture to 5-40 mu m by using zirconium balls with diameters of 1mm and 3mm and a rotating speed of 200rpm to obtain glass phase powder;
step three: preparation of slurry support
Weighing raw materials according to the mass ratio of terpineol, citric acid, lacquer tree biological resin, silane coupling agent and ethylcellulose=78:9:2:6:5, and stirring at the speed of 150r/min for 20min at the temperature of 50 ℃ to obtain a slurry carrier;
step four: preparation of the slurry
The novel uniform and environment-friendly high-temperature electronic paste is obtained by pre-treating conductive powder, glass powder and paste carrier=85:5:10 in a mass ratio, weighing, mixing at 9000rpm and dispersing for 20 min.
The silver powder is granular powder with average particle diameter of 0.7 μm and flaky powder with mass ratio of M Granules and method for producing the same :M Sheet =0.7:2。
Example 2
The preparation method of the novel high-temperature electronic paste comprises the following steps:
step one: preparation of biological resin extracted from lacquer tree and pretreatment of conductive powder
(1.1) adding an aqueous solution of 70wt% ethanol with the weight being 8 times that of 200g of the bark of the lacquer tree, carrying out reflux extraction for 2 hours at 100 ℃, filtering, repeatedly extracting and filtering for 2 times, merging filtrate, evaporating and condensing to recover ethanol, eluting through a macroporous resin column, collecting an eluting part, and carrying out vacuum drying until the water content is 5wt% to obtain the lacquer tree biological resin mainly comprising catechol resin;
(1.2) dispersing 85g of silver-coated copper powder in 510mL of ethanol, then adding 5g of the lacquer tree biological resin prepared in the step (1.1) of citric acid with any proportion, then adding 6g of sodium hypophosphite, uniformly mixing, stirring at room temperature for 15min, centrifuging at 9000rpm for 10min, and vacuum drying to obtain pretreated conductive powder;
step two: preparation of novel glass powder
The proportion is as follows: bi (Bi) 2 O 3 :72wt%;B 2 O 3 :8wt%;SiO 2 :3wt%; znO:11wt%; inO:3wt%; baO:1wt%; cuO:2wt%; uniformly mixing the components, putting the mixture into a sintering heat preservation furnace, heating to 1100 ℃ for firing for 2 hours, pouring the mixture into deionized water for cold quenching, ball-milling the mixture to 5-40 mu m by using zirconium balls with diameters of 1mm and 3mm at a rotating speed of 300rpm, and obtaining glass phase powder;
step three: preparation of slurry support
Weighing raw materials according to the mass ratio of terpineol, citric acid, lacquer tree biological resin, silane coupling agent and ethylcellulose=76:8:6:5:5, and stirring at the speed of 150r/min for 20min at the temperature of 50 ℃ to obtain a slurry carrier;
step four: preparation of the slurry
The novel high-temperature electronic paste is prepared by pre-treating conductive powder, glass powder and paste carrier=85:5:10 according to the mass ratio, mixing the materials and dispersing the materials for 20 minutes at 10000 rpm.
The silver-coated copper powder is granular powder with the average particle diameter of 0.9 mu m and flaky powder with the average particle diameter of 9 mu m; mass ratio is M Granules and method for producing the same :M Sheet =0.9:2。
Example 3
The preparation method of the novel high-temperature electronic paste comprises the following steps:
step one: preparation of biological resin extracted from lacquer tree and pretreatment of conductive powder
(1.1) adding an aqueous solution of 80wt% ethanol with the weight being 9 times that of 200g of the bark of the lacquer tree, carrying out reflux extraction for 3 hours at 100 ℃, filtering, evaporating and condensing to recover the ethanol, eluting by a macroporous resin column, collecting the eluted part, and carrying out vacuum drying until the water content is 6wt% to obtain the lacquer tree biological resin mainly comprising catechol resin;
(1.2) dispersing 85g of silver powder in 510mL of ethanol, then adding 5g of citric acid with any proportion and the lacquer tree biological resin mixture prepared in the step (1.1), then adding 6g of sodium hypophosphite, uniformly mixing, stirring at room temperature for 15min, centrifuging at 10000rpm for 10min, and vacuum drying to obtain pretreated conductive powder;
step two: preparation of novel glass powder
The proportion is as follows: bi (Bi) 2 O 3 :72wt%;B 2 O 3 :8wt%;SiO 2 :3wt%; znO:11wt%; inO:3wt%; baO:1wt%; cuO:2wt%; uniformly mixing the components, putting the mixture into a sintering heat preservation furnace, heating to 1100 ℃ for firing for 2 hours, pouring the mixture into deionized water for cold quenching, and ball-milling the mixture to 5-40 mu m by using a rotating speed of 150-400rpm to obtain glass phase powder;
step three: preparation of slurry support
Weighing raw materials according to the mass ratio of terpineol, citric acid, lacquer tree biological resin, silane coupling agent and ethylcellulose=75:7:8:5:5, and stirring at a rotating speed of 150r/min for 20min at 50 ℃ to obtain a slurry carrier;
step four: preparation of the slurry
The novel high-temperature electronic paste is prepared by pre-treating conductive powder, glass powder and paste carrier=85:5:10 in a mass ratio, mixing the materials for 12000rpm and dispersing the materials for 20 minutes, and is uniform and environment-friendly.
The silver powder is granular powder with average particle diameter of 1 μm and flake powder with mass ratio of 10 μm of M Granules and method for producing the same :M Sheet =1:2。
Example 4
The preparation method of the novel high-temperature electronic paste comprises the following steps:
step one: preparation of biological resin extracted from lacquer tree and pretreatment of conductive powder
(1.1) adding 80wt% ethanol aqueous solution with the weight being 10 times that of 200g of cortex lacquer, reflux-extracting for 1h at 100 ℃, filtering, repeatedly extracting and filtering for 3 times, merging filtrate, evaporating and condensing to recover ethanol, eluting by a macroporous resin column, collecting an eluting part, and vacuum-drying until the water content is 4wt% to obtain the lacquer tree biological resin mainly comprising catechol resin;
(1.2) dispersing 85g of silver-coated copper powder in 510mL of ethanol, then adding 7g of citric acid with any proportion and the lacquer tree biological resin prepared in the step (1.1), then adding 6g of sodium hypophosphite, uniformly mixing, stirring at room temperature for 15min, centrifuging at 10000rpm for 10min, and vacuum drying to obtain pretreated conductive powder;
step two: preparation of novel glass powder
And (3) proportioning: bi (Bi) 2 O 3 :72wt%;B 2 O 3 :8wt%;SiO 2 :3wt%; znO:11wt%; inO:3wt%; baO:1wt%; cuO:2wt%; uniformly mixing the components, putting the mixture into a sintering heat preservation furnace, heating to 1100 ℃ for firing for 2 hours, pouring the mixture into deionized water for cold quenching, and ball-milling the mixture to 5-40 mu m by using a rotating speed of 150-400rpm to obtain glass phase powder;
step three: preparation of slurry support
Weighing raw materials according to the mass ratio of terpineol, citric acid, lacquer tree biological resin, silane coupling agent and ethylcellulose=75:7:8:5:5, and stirring at a rotating speed of 150r/min for 20min at 50 ℃ to obtain a slurry carrier;
step four: preparation of the slurry
The novel uniform and environment-friendly high-temperature electronic paste is obtained by pre-treating conductive powder, glass powder and paste carrier=85:5:10 in a mass ratio, weighing, mixing at 9000rpm and dispersing for 20 min.
Wherein the silver-coated copper powder is granular powder with an average particle diameter of 0.5 μm and flaky powder with a mass ratio of M Granules and method for producing the same :M Sheet =0.8:2。
Comparative example 1
The difference from example 3 is that no lacquer tree extraction bio-resin was added in the preparation of the slurry carrier in step three.
Comparative example 2
The difference from example 4 is that the pretreatment preparation of the conductive powder was carried out without adding the lacquer tree extraction bio-resin.
Comparative example 3
Commercial high temperature electronic paste.
Performance test:
the electroconductive pastes provided in examples 1 to 4 and comparative examples 1 to 3 were subjected to film formation:
and (3) adopting a semi-automatic precise printer, carrying out 325 meshes on a screen, curing the screen at 400 ℃ for 10min after printing, and curing the screen at 700 ℃ for 20min to carry out resistance test and adhesive strength test, wherein the thickness of the adhesive film is 30 um.
The results were as follows:
group of Resistivity (Ω cm)
Example 1 6.5
Example 2 5.1
Example 3 3.8
Example 4 3.5
Comparative example 1 9.6
Comparative example 2 8.9
Comparative example 3 11.2
The results show that the product provided by the invention has better electric conductivity; as can be seen from comparison of examples 1-4 and comparative examples 1-3, the invention has the advantages that the dispersion degree of the conductive powder is better, the conductive film is more compact, the reducibility of the conductive film reduces the contact resistance between the conductive phases of the slurry, and the performance of the slurry is improved by using the biological resin extracted from the lacquer tree.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant points refer to the description of the method section.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. The preparation method of the high-temperature electronic paste is characterized by comprising the following steps of:
step one: preparation of biological resin extracted from lacquer tree and pretreatment of conductive powder
(1.1) adding 5-10 times of ethanol water solution into the lacquer tree bark, carrying out reflux extraction for 1-3h at 100 ℃, filtering, repeatedly extracting and filtering for 1-3 times, merging filtrate, evaporating and condensing to recover ethanol, eluting by a macroporous resin column, collecting an elution part, and carrying out vacuum drying until the water content is 3-6wt% to obtain lacquer tree biological resin;
(1.2) dispersing conductive phase powder in ethanol, then adding the lacquer tree biological resin and citric acid prepared in the step (1.1), then adding sodium hypophosphite, uniformly mixing, stirring at room temperature, centrifuging at constant temperature, and vacuum drying to obtain pretreated conductive powder;
step two: preparation of glass powder
Weighing glass raw materials according to a proportion, mixing, placing the mixture in a sintering heat preservation furnace, firing the mixture, cooling the mixture by deionized water, and ball-milling the obtained glass to obtain glass powder;
step three: preparation of slurry support
Weighing an organic solvent, a reducing agent, lacquer tree biological resin, a coupling agent and a thickening agent according to the mass ratio, and stirring at the rotating speed of 150-250r/min for 15-30min at the temperature of 40-65 ℃ to obtain a slurry carrier;
step four: preparation of the slurry
The pretreated conductive powder, the glass powder and the slurry carrier are weighed according to the mass ratio and then mixed and dispersed uniformly, so that the uniform and environment-friendly high-temperature electronic slurry is obtained.
2. The method for preparing high-temperature electronic paste according to claim 1, wherein the aqueous ethanol solution in the first step is 60wt% to 80wt%.
3. The method for preparing high-temperature electronic paste according to claim 1, wherein the conductive phase powder in the step (1.2) is one or more of silver powder or silver-coated copper powder.
4. The method for producing a high-temperature electronic paste according to claim 1, wherein said electroconductive phase powder in step (1.2) is a granular powder having an average particle diameter of 0.5 to 1 μm and a flake powder having a particle diameter of 7 to 10 μm; mass ratio M Granules and method for producing the same :M Sheet =(0.6-1):2。
5. The method for preparing high-temperature electronic paste according to claim 1, wherein the centrifugal rotation speed in the first step is 8000-10000rpm for 5-10min.
6. The method for preparing high-temperature electronic paste according to claim 1, wherein the preparation of the glass powder in the second step is specifically:
the proportion is as follows: bi (Bi) 2 O 3 :67-78wt%;B 2 O 3 :5-11wt%;SiO 2 :0-3wt%; znO:8-15wt%; inO:1-7wt%; baO:0-2wt%; cuO:0-2wt%; and (3) uniformly mixing the components, putting the mixture into a sintering heat preservation furnace, heating to 1100 ℃ for firing for 2 hours, pouring the mixture into deionized water for cold quenching, and ball-milling the mixture to 5-40 mu m by using a zirconium ball with the diameter of 1mm and 3mm at a rotating speed of 150-400rpm to obtain glass phase powder.
7. The method for preparing high-temperature electronic paste according to claim 1, wherein in the third step, the mass ratio of the organic solvent: reducing agent: lacquer tree biological resin: coupling agent: thickener= (65-85): (5-15): (1-8): (3-10): (2-10).
8. The method for preparing high-temperature electronic paste according to claim 1, wherein in the third step, the organic solvent is terpineol; the reducing agent is one or more of citric acid, ascorbic acid and formic acid; the coupling agent is a silane coupling agent; the thickener is ethyl cellulose.
9. The method for preparing the high-temperature electronic paste according to claim 1, wherein in the fourth step, the mass ratio of the conductive powder, the glass powder and the paste carrier is preprocessed= (78-90): (3-5): (7-12).
10. The method for preparing a high temperature electronic paste according to claim 1, wherein the stirring and dispersing rotational speed in the fourth step is 9000-15000rpm, and the dispersing time is 15-30min.
CN202111332680.3A 2021-11-11 2021-11-11 Preparation method of high-temperature electronic paste Active CN114005573B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111332680.3A CN114005573B (en) 2021-11-11 2021-11-11 Preparation method of high-temperature electronic paste

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111332680.3A CN114005573B (en) 2021-11-11 2021-11-11 Preparation method of high-temperature electronic paste

Publications (2)

Publication Number Publication Date
CN114005573A CN114005573A (en) 2022-02-01
CN114005573B true CN114005573B (en) 2023-08-11

Family

ID=79928608

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111332680.3A Active CN114005573B (en) 2021-11-11 2021-11-11 Preparation method of high-temperature electronic paste

Country Status (1)

Country Link
CN (1) CN114005573B (en)

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060079575A (en) * 2005-01-03 2006-07-06 서희동 Manufacturing method for pellet of activated humic substances
KR100908221B1 (en) * 2008-12-31 2009-07-20 (주)피앤피이십일 Aromatic material for preventing illegal poster
CN101826377A (en) * 2010-03-31 2010-09-08 桂林电子科技大学 Thick film thermistor slurry, preparation method thereof and thick film thermistor
CN103450675A (en) * 2012-05-31 2013-12-18 金发科技股份有限公司 Resin composition having laser direct-structuring function and its preparation method and use
CN103854720A (en) * 2012-12-03 2014-06-11 西北稀有金属材料研究院 Solar cell aluminum back surface field slurry material and preparation method thereof
CN107170508A (en) * 2017-05-14 2017-09-15 常州市奥普泰克光电科技有限公司 A kind of preparation method of conductive silver paste
CN111171772A (en) * 2020-02-24 2020-05-19 桂林电子科技大学 Preparation method of epoxy conductive adhesive
CN113421693A (en) * 2021-06-30 2021-09-21 中硕实业(上海)有限公司 Conductive paste and preparation method and application thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060079575A (en) * 2005-01-03 2006-07-06 서희동 Manufacturing method for pellet of activated humic substances
KR100908221B1 (en) * 2008-12-31 2009-07-20 (주)피앤피이십일 Aromatic material for preventing illegal poster
CN101826377A (en) * 2010-03-31 2010-09-08 桂林电子科技大学 Thick film thermistor slurry, preparation method thereof and thick film thermistor
CN103450675A (en) * 2012-05-31 2013-12-18 金发科技股份有限公司 Resin composition having laser direct-structuring function and its preparation method and use
CN103854720A (en) * 2012-12-03 2014-06-11 西北稀有金属材料研究院 Solar cell aluminum back surface field slurry material and preparation method thereof
CN107170508A (en) * 2017-05-14 2017-09-15 常州市奥普泰克光电科技有限公司 A kind of preparation method of conductive silver paste
CN111171772A (en) * 2020-02-24 2020-05-19 桂林电子科技大学 Preparation method of epoxy conductive adhesive
CN113421693A (en) * 2021-06-30 2021-09-21 中硕实业(上海)有限公司 Conductive paste and preparation method and application thereof

Also Published As

Publication number Publication date
CN114005573A (en) 2022-02-01

Similar Documents

Publication Publication Date Title
CN101728001B (en) Lead-free and low-silver photosensitive silver paste and preparation method thereof
CN102324263B (en) Silver paste for solar cells and preparation method thereof
WO2017026722A1 (en) Production method for silver powder for high-temperature sintering type of electrically-conductive paste
CN102403047B (en) Paste for solar cell electrode and electrode using the same and solar cell using the same
CN101271929B (en) Leadless solar battery silver paste and method for producing the same
CN110586959A (en) Preparation method of flake silver powder with high tap density
CN101770829B (en) Special silver electrode paste for touch screen and preparation method thereof
CN102354544A (en) Silver conductive paste for front electrode of crystalline silicon solar cell and preparation method thereof
CN102592704B (en) Aluminum paste for solar energy battery and preparation method thereof
CN113257456A (en) Low-cost conductive paste for heterojunction solar cell and preparation method thereof
CN102354545A (en) Sliver electrode slurry for back electric field of silicon solar cell and preparation method thereof
TW201424887A (en) Silver hybrid copper powder, method for producing same, conductive paste containing silver hybrid copper powder, conductive adhesive, conductive film and electrical circuit
CN104282356A (en) Low-silver-content composite conductive silver paste and preparation method thereof
CN111148345B (en) Blue dielectric paste for thick film circuit, preparation method and application
CN104538085A (en) Environment-friendly conductive silver paste
CN110706842B (en) Front silver paste and preparation method thereof
CN104538084A (en) High-temperature-resistant electric conducting silver paste
CN114005573B (en) Preparation method of high-temperature electronic paste
CN106653145A (en) Medium-and-high temperature thick film circuit conductor paste and preparation method thereof
CN112053796B (en) Silver sulfide resistant electrode paste and preparation method thereof
CN101697317A (en) Preparation method for unleaded silver-palladium inner electrode slurry used for multilayer ceramic capacitor
WO2020021872A1 (en) Electroconductive paste, electrode, and chip resistor
CN113707359B (en) Electrode paste, conductive thick film and preparation method thereof
CN114023511B (en) Method for preparing high-temperature electronic paste based on organic phosphorus salt
CN111128439A (en) Environment-friendly silver electrode slurry for dielectric ceramic filter and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant