CN106205771B - A kind of preparation method of oxidation resistant copper conductor slurry - Google Patents
A kind of preparation method of oxidation resistant copper conductor slurry Download PDFInfo
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- CN106205771B CN106205771B CN201610515676.3A CN201610515676A CN106205771B CN 106205771 B CN106205771 B CN 106205771B CN 201610515676 A CN201610515676 A CN 201610515676A CN 106205771 B CN106205771 B CN 106205771B
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- copper conductor
- oxidation resistant
- organic carrier
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The invention discloses a kind of preparation method of oxidation resistant copper conductor slurry, including the following steps：1) preparation of organic carrier；2) copper powder and glass dust are uniformly mixed up to solid-phase mixture, three roller ground and mixeds is then carried out by three-roll grinder with organic carrier；3) by screen process press by slurry in Al2O3Special pattern is printed as on substrate, the thickness of adjusting process parameter change pulp layer is 20 μm；4) it is sintered in the tube furnace under nitrogen atmosphere protection.The present invention is by making organic carrier by oneself, and cost is low, and volatile performance is good, and atmosphere protection can realize the anti-oxidant sintering of copper conductor slurry.The conducting wire prepared using copper conductor slurry, which is realized, replaces silver conductive paste under component environment, obtained conductor electric conductivity is excellent, and technological process is simple, is a kind of method for preparing conductor of high financial profit.
Description
Technical field
The present invention relates to a kind of conductor paste, and in particular to a kind of preparation method of oxidation resistant copper conductor slurry.
Background technology
Conductor paste by silk-screen printing, the process such as burn till interconnecting lead, conductor, capacitance, inductance etc. made on substrate,
The circuit unit with certain function requirement can be prepared.Conductor paste is the basic material for developing electronic component, and is made
The critical material of slice component and printed circuit, development electric slurry is an important step of electronic information material development, right
The development of China's electronics and information industry is of great significance.
In the technology of preparing of electric slurry, the preparation of conductive phase metal dust is crucial, without excellent metal dust
Just it is always what is mutually promoted and mutually restrict with electric slurry without excellent electric slurry, metal dust.Starched for conductor
For material, conductive phase is mostly based on the noble metal powders such as platinum, palladium, gold and silver, wherein be most widely used with silver conductive paste,
Dosage is also maximum.In recent years, rising violently due to noble metal price, cost of sizing agent increase；On the other hand, silver migration be silver paste from
Body there are the shortcomings that, it is impossible to meet the requirement of high-performance electronic component.
Around reduce cost, find function admirable novel conductive powder, with base metal replace noble metal prepare electronics starch
Material has become the Main way of electric slurry development.Copper powder is due to performances such as its excellent highly conductive, heat conduction, in Modern High-Tech
It is with a wide range of applications in industry and national defence material, and has become current base metal slurry and substituted Precious Metal research
Main way, but because of it, inoxidizability is poor under air, significantly limit its application, carries out on this basis anti-oxidant
Handling and research and develop cost-effective conductor paste has important theory significance and engineering value.
With the progress of copper powder anti-oxidation technology, copper slurry just progressively grows up.Such as the copper acrylic acid of Japanese Showa electrician
Resin conductor paste, due to having carried out specially treated, long-term good conductivity to copper.Patent CN1472367A is by carrying out copper powder
Electroplate prepares the excellent conductor paste of electric conductivity.Patent CN201410759034.9 disclose a kind of conductive copper paste and
Its preparation method, its copper powder proportion is in 74%-80%, and the slurry is after silk-screen printing under nitrogen, hydrogen mixed gas atmosphere
Sintering, the method prepare the excellent copper conductor of electric conductivity.
The content of the invention
Goal of the invention：The present invention provides a kind of oxidation resistant copper conductor slurry preparation method, led for alternative noble metal
The development problem of somaplasm material, as the materials containing functional phases for substituting noble metal after ultra-fine Cu powder is carried out anti-oxidant treatment, to poly-
On the basis of compound volatility and matrix bonding Journal of Sex Research, self-developing goes out organic carrier of good performance, have developed and is suitable for
The conductor paste of high temperature sintering environment, is a kind of synthetic method of high financial profit.
Technical solution：A kind of preparation method of oxidation resistant copper conductor slurry, including the following steps：
1) preparation of organic carrier, is blended with 120~150 DEG C of heating after solvent, thickener mixing, stirs at the same time first
Mix until be completely dissolved, then add rheological agent, thixotropic agent and its dispersant, and it is uniform to continue heating stirring, has to obtain the final product airborne
Body；
2) copper powder and glass dust are uniformly mixed up to solid-phase mixture, then with organic carrier by three-roll grinder into
Three roller ground and mixed of row；
3) by screen process press by slurry in 96%Al2O3Special pattern, adjusting process parameter change are printed as on substrate
The thickness of pulp layer is 20 μm；
4) it is sintered in the tube furnace under nitrogen atmosphere protection；
Further, the mixed organic solvents in the step 1) are terpinol, butyl carbitol and butyl carbitol vinegar
Acid esters, thixotropic agent are rilanit special, and thickener is ethyl cellulose, and rheological agent is 1,4-butyrolactone, and dispersant is oleic acid；Step
The particle diameter of rapid 2) described copper powder is 300nm.
Further, the content that the solid-phase mixture described in step 2) accounts for total mixture is 60~90%, preferably 80%；
Further, the content that glass dust accounts for solid-phase mixture is 0.5~6%, preferably 4%；
Further, the sintering temperature of step (4) is 550~700 DEG C, is preferably 600 DEG C, soaking time for 5~
30min, is preferably 10min.
Beneficial effect：The present invention is by making organic carrier by oneself, and cost is low, and volatile performance is good, and atmosphere protection can realize copper
The anti-oxidant sintering of conductor paste.The conducting wire prepared using copper conductor slurry is realized replaces silver conductor to starch under component environment
Material, obtained conductor electric conductivity is excellent, and technological process is simple, is a kind of method for preparing conductor of high financial profit.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, the embodiment
It is only used for explaining the present invention, is not intended to limit the scope of the present invention..
Material therefor and performance parameter, manufacturer are as follows in following embodiments：
Terpinol boiling point is 214~224 DEG C, and manufacturer is Shanghai Ling Feng chemical reagent Co., Ltd；Butyl carbitol,
The boiling point of butyl carbitol acetate is respectively 230 DEG C, 246.8 DEG C, and manufacturer is East China Normal University chemical plant；Oleic acid is given birth to
Production producer is Sinopharm Chemical Reagent Co., Ltd..
Glass dust is the micron order raw material of Kunming Nuo Man Electron Material Co., Ltd production.
Al2O3Substrate production producer is Linzhou City milky way high-tech development Co., Ltd.
The preparation of organic carrier：By mixed organic solvents (terpinol 42g, butyl carbitol 21g, the butyl carbitol of 70g
Acetate 7g) and the ethyl cellulose mixing of 5g after 120~150 DEG C of oil bath heatings, while mechanical agitation is until be completely dissolved again
Add 1,4-butyrolactone, the rilanit special of 1g and the oleic acid of 4g of 20g, and it is uniform to continue heating stirring, that is, be made have it is airborne
Body, its viscosity are 6.5Pas.
Embodiment 1
Organic carrier 20g, glass dust 3.2g, the 300nm copper powder 76.8g that average grain diameter is 0.93 μm add three-roll grinder
Three roller grindings of middle progress, uniformly mixed conductor paste is by being screen printed onto 96%Al2O3Special pattern is printed as on substrate,
Adjusting process parameter make it that the thickness of pulp layer is 20 μm.The printed wiring board is positioned in vacuum drying oven and is vacuumized, is passed through nitrogen
700 DEG C of this slurry is sintered and keeps the temperature 5min, copper conductive traces are made as protective atmosphere by gas, test its sheet resistance for 1.7m Ω/
□.Tin welding is carried out to conductor, the welding area in its surface is the 70% of the gross area.
Embodiment 2
Organic carrier 10g, glass dust 3.6g, the 300nm copper powder 86.4g that average grain diameter is 0.93 μm add three-roll grinder
Three roller grindings of middle progress, uniformly mixed conductor paste is by being screen printed onto 96%Al2O3Special pattern is printed as on substrate,
Adjusting process parameter make it that the thickness of pulp layer is 20 μm.The printed wiring board is positioned in vacuum drying oven and is vacuumized, is passed through nitrogen
700 DEG C of this slurry is sintered and keeps the temperature 5min, copper conductive traces are made, it is 59.2m to test its sheet resistance as protective atmosphere by gas
Ω/□.Tin welding is carried out to conductor, the welding area in its surface is the 45% of the gross area.
Embodiment 3
Organic carrier 20g, glass dust 4.8g, the 300nm copper powder 75.2g that average grain diameter is 0.93 μm add three-roll grinder
Three roller grindings of middle progress, uniformly mixed conductor paste is by being screen printed onto 96%Al2O3Special pattern is printed as on substrate,
Adjusting process parameter make it that the thickness of pulp layer is 20 μm.The printed wiring board is positioned in vacuum drying oven and is vacuumized, is passed through nitrogen
700 DEG C of this slurry is sintered and keeps the temperature 5min, copper conductive traces are made as protective atmosphere by gas, test its sheet resistance for 2.8m Ω/
□.Tin welding is carried out to conductor, the welding area in its surface is the 75% of the gross area.
Embodiment 4
Organic carrier 20g, glass dust 3.2g, the 300nm copper powder 76.8g that average grain diameter is 0.93 μm add three-roll grinder
Three roller grindings of middle progress, uniformly mixed conductor paste is by being screen printed onto 96%Al2O3Special pattern is printed as on substrate,
Adjusting process parameter make it that the thickness of pulp layer is 20 μm.The printed wiring board is positioned in vacuum drying oven and is vacuumized, is passed through nitrogen
600 DEG C of this slurry is sintered and keeps the temperature 5min, copper conductive traces are made as protective atmosphere by gas, test its sheet resistance for 1.1m Ω/
□.Tin welding is carried out to conductor, the welding area in its surface is the 60% of the gross area.
Embodiment 5
Organic carrier 20g, glass dust 3.2g, the 300nm copper powder 76.8g that average grain diameter is 0.93 μm add three-roll grinder
Three roller grindings of middle progress, uniformly mixed conductor paste is by being screen printed onto 96%Al2O3Special pattern is printed as on substrate,
Adjusting process parameter make it that the thickness of pulp layer is 20 μm.The printed wiring board is positioned in vacuum drying oven and is vacuumized, is passed through nitrogen
600 DEG C of this slurry is sintered and keeps the temperature 10min, copper conductive traces are made, it is 0.8m to test its sheet resistance as protective atmosphere by gas
Ω/□.Tin welding is carried out to conductor, the welding area in its surface is the 80% of the gross area.
Comparative example
Organic carrier 20g, glass dust 3.2g, the 300nm silver powder 76.8g that average grain diameter is 0.93 μm add three-roll grinder
Three roller grindings of middle progress, uniformly mixed conductor paste is by being screen printed onto 96%Al2O3Special pattern is printed as on substrate,
Adjusting process parameter make it that the thickness of pulp layer is 20 μm.The printed wiring board is positioned in Muffle furnace and sinters and protects for 600 DEG C
Warm 5min, is made silver conducting wire, it is 0.4m Ω/ to test its sheet resistance.Tin welding, the welding face in its surface are carried out to conductor
Product is the 100% of the gross area.
From the experimental results, the electric conductivity of the oxidation resistant copper conductor slurry of preparation of the invention is close to silver conductive paste,
The part wiring board of less demanding to solderability drought tolerance can use the electrocondution slurry.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on, should all be included in the protection scope of the present invention god.
Claims (7)
1. a kind of preparation method of oxidation resistant copper conductor slurry, it is characterised in that including the following steps：
1）The preparation of organic carrier, is blended with 120~150 DEG C of heating after solvent, thickener mixing, stirs at the same time first
Until be completely dissolved, rheological agent, thixotropic agent and its dispersant are then added, and it is uniform to continue heating stirring, up to organic carrier;
2）Copper powder and glass dust are uniformly mixed up to solid-phase mixture, then carry out three by three-roll grinder with organic carrier
Roller ground and mixed；
3）By screen process press by slurry in 96%Al2O3Special pattern, adjusting process parameter change slurry are printed as on substrate
The thickness of layer is 20 μm；
4）It is sintered in tube furnace under nitrogen atmosphere protection；
The step 1）In mixed organic solvents be terpinol, butyl carbitol and butyl carbitol acetate, thixotropic agent be
Rilanit special, thickener are ethyl cellulose, and rheological agent is 1,4-butyrolactone, and dispersant is oleic acid, step 2）The copper powder
Particle diameter be 300nm;
The preparation method of the organic carrier is：Terpinol 42g, butyl carbitol 21g and butyl carbitol acetate 7g are mixed
After conjunction, and 120~150 DEG C of oil bath heatings after the ethyl cellulose mixing of 5g, while mechanical agitation adds until being completely dissolved
The oleic acid of the 1,4-butyrolactone of 20g, the rilanit special of 1g and 4g, and it is uniform to continue heating stirring, that is, organic carrier is made, its
Viscosity is 6.5 Pas.
2. the preparation method of oxidation resistant copper conductor slurry according to claim 1, it is characterised in that step 2）Described consolidates
The content that phase mixture accounts for total mixture is 60~90%.
3. the preparation method of oxidation resistant copper conductor slurry according to claim 2, it is characterised in that step 2）Described consolidates
The content that phase mixture accounts for total mixture is 80%.
4. the preparation method of oxidation resistant copper conductor slurry according to claim 1, it is characterised in that glass dust accounts for solid phase and mixes
The content of compound is 0.5~6%.
5. the preparation method of oxidation resistant copper conductor slurry according to claim 4, it is characterised in that glass dust accounts for solid phase and mixes
The content of compound is 4%.
6. the preparation method of oxidation resistant copper conductor slurry according to claim 1, it is characterised in that step（4）Sintering
Temperature is 550~700 DEG C, and soaking time is 5~30min.
7. the preparation method of oxidation resistant copper conductor slurry according to claim 6, it is characterised in that step（4）Sintering
Temperature is 600 DEG C, soaking time 10min.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106887268A (en) * | 2017-01-07 | 2017-06-23 | 东莞易力禾电子有限公司 | Silk-screen printing circuit electrode and preparation method thereof |
| CN106876005B (en) * | 2017-01-11 | 2018-05-18 | 西安工程大学 | Sn-Cu composite electron slurries and preparation method thereof |
| CN108172320A (en) * | 2017-12-27 | 2018-06-15 | 南京足智人信息科技有限公司 | A kind of conductive copper paste |
| CN109461515A (en) * | 2018-11-07 | 2019-03-12 | 刘紫嫣 | A kind of high temperature sintering conductive silver paste and preparation method thereof |
| CN109982516A (en) * | 2019-03-15 | 2019-07-05 | 广东石油化工学院 | Vacuum-sintering precipitation and separation glass circuit substrate plate and preparation method thereof |
| CN111548194A (en) * | 2020-05-29 | 2020-08-18 | 南京凯泰化学科技有限公司 | Preparation method of printed circuit board |
| CN114639506B (en) * | 2022-05-20 | 2022-10-28 | 西安宏星电子浆料科技股份有限公司 | Low-temperature fast-sintering conductive copper paste and preparation method thereof |
| CN115772040B (en) * | 2022-12-20 | 2023-12-12 | 深圳市赛尔美电子科技有限公司 | Manufacturing method of heating component, heating device and heating non-combustion smoking set |
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Effective date of registration: 20191118 Address after: 210000, No. 3 Tan Avenue, Gaochun Economic Development Zone, Nanjing, Jiangsu Patentee after: Nanjing Xinyan New Material Technology Co., Ltd Address before: No. 99 Jiangning Road, Nanjing District hirokage 211169 cities in Jiangsu Province Patentee before: Jinling Institute of Technology |