CN106205771A - 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
- Publication number
- CN106205771A CN106205771A CN201610515676.3A CN201610515676A CN106205771A CN 106205771 A CN106205771 A CN 106205771A CN 201610515676 A CN201610515676 A CN 201610515676A CN 106205771 A CN106205771 A CN 106205771A
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- Prior art keywords
- preparation
- slurry
- copper conductor
- oxidation resistant
- resistant copper
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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 the preparation method of a kind of oxidation resistant copper conductor slurry, including following several steps: 1) preparation of organic carrier；2) copper powder and glass dust mix homogeneously are i.e. obtained solid-phase mixture, then carry out three roller ground and mixed with organic carrier by three-roll grinder；3) screen process press is passed through by slurry at Al2O3Being printed as special pattern on substrate, the thickness of adjusting process parameter change pulp layer is 20 μm；4) tube furnace under nitrogen atmosphere is protected is sintered.The present invention is by self-control organic carrier, low cost, and volatile performance is good, and atmosphere protection can realize the antioxidation sintering of copper conductor slurry.The conducting wire utilizing copper conductor slurry to prepare achieves replacement silver conductive paste under component environment, and prepared conductor electric conductivity is excellent, and technological process is simple, is a kind of method preparing conductor of high financial profit.
Description
Technical field
The present invention relates to a kind of conductor paste, be specifically related to the preparation method of a kind of oxidation resistant copper conductor slurry.
Background technology
Conductor paste by silk screen printing, the operation such as burn till on substrate, make interconnecting lead, conductor, electric capacity, inductance etc.,
The circuit unit with certain functional requirement can be prepared.Conductor paste is the basic material of development electronic component, is also to make
Slice component and the critical material of 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 significant.
In the technology of preparing of electric slurry, the preparation of conductive phase metal dust is crucial, does not has excellent metal dust
Just not having an excellent electric slurry, metal dust and electric slurry are always mutually promoted and mutually restrict.Conductor is starched
For material, conductive phase based on platinum, palladium, the noble metal powder such as golden and silver-colored, is wherein most widely used with silver conductive paste mostly,
Consumption is the most maximum.In recent years, due to rising violently of noble metal price, cost of sizing agent increases；On the other hand, silver migrates be silver paste from
The shortcoming that body exists, it is impossible to meet the requirement of high-performance electronic components and parts.
Around reducing cost, the novel conductive powder body of searching function admirable, replacing with base metal noble metal to prepare electronics slurry
Material has become the Main way of electric slurry development.Copper powder is due to performances such as the high connductivity of its excellence, heat conduction, in Modern High-Tech
Industry and national defence material are with a wide range of applications, and have become the replacement Precious Metal research of current base metal slurry
Main way, but because its non-oxidizability under air is poor, significantly limit its application, carry out antioxidation on this basis
The conductor paste processed and research and develop cost performance high has important theory significance and construction value.
Along with the progress of copper powder anti-oxidation technology, copper slurry the most progressively grows up.Copper acrylic acid such as Japan Showa electrician
Resin conductor paste, owing to having carried out special handling, long-term good conductivity to copper.Patent CN1472367A is by carrying out copper powder
Electroplate prepares the conductor paste that electric conductivity is excellent.Patent CN201410759034.9 disclose a kind of conductive copper paste and
Its preparation method, its copper powder proportion at 74%-80%, this slurry after silk screen printing under nitrogen, hydrogen mixed gas atmosphere
Sintering, the method prepares the copper conductor that electric conductivity is excellent.
Summary of the invention
Goal of the invention: the invention provides a kind of oxidation resistant copper conductor slurry preparation method, lead for alternative noble metal
The development problem of somaplasm material, carries out the materials containing functional phases of noble metal as an alternative after anti-oxidant treatment by ultra-fine Cu powder, to poly-
On the basis of compound volatility and the research of matrix cementability, self-developing goes out organic carrier of good performance, have developed and is applicable to
The conductor paste of high temperature sintering environment, is the synthetic method of a kind of high financial profit.
Technical scheme: the preparation method of a kind of oxidation resistant copper conductor slurry, including following several steps:
1) preparation of organic carrier, is first blended with 120～150 DEG C of heating after machine solvent, thickening agent mixing, stirs simultaneously
Mixing until being completely dissolved, being subsequently adding rheological agent, thixotropic agent and dispersant thereof, and it is uniform to continue heated and stirred, must have airborne
Body；
2) copper powder and glass dust mix homogeneously are i.e. obtained solid-phase mixture, then entered by three-roll grinder with organic carrier
Row three roller ground and mixed；
3) screen process press is passed through by slurry at 96%Al2O3Special pattern, adjusting process parameter change it is printed as on substrate
The thickness of pulp layer is 20 μm；
4) tube furnace under nitrogen atmosphere is protected is sintered；
Further, described step 1) in mixed organic solvents be terpineol, butyl carbitol and butyl carbitol vinegar
Acid esters, thixotropic agent is castor oil hydrogenated, and thickening agent is ethyl cellulose, and rheological agent is GBL, and dispersant is oleic acid；Step
Rapid 2) particle diameter of described copper powder is 300nm.
Further, step 2) described in solid-phase mixture to account for the content of total mixture be 60～90%, preferably 80%；
Further, it is 0.5～6% that glass dust accounts for the content of solid-phase mixture, preferably 4%；
Further, the sintering temperature of step (4) is 550～700 DEG C, preferably 600 DEG C, temperature retention time be 5～
30min, preferably 10min.
Beneficial effect: the present invention is by self-control organic carrier, and low cost, volatile performance is good, and atmosphere protection can realize copper
The antioxidation sintering of conductor paste.The conducting wire utilizing copper conductor slurry to prepare achieves and replaces silver conductor slurry under component environment
Material, the conductor electric conductivity prepared is excellent, and technological process is simple, is a kind of method preparing conductor of high financial profit.
Detailed description of the invention
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, this embodiment
It is only used for explaining the present invention, is not intended that limiting the scope of the present invention.
Material therefor and performance parameter in following example, manufacturer is as follows:
Terpineol boiling point is 214～224 DEG C, and manufacturer is Shanghai Ling Feng chemical reagent company limited；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 raw
Product producer is Chemical Reagent Co., Ltd., Sinopharm Group.
Glass dust is the micron order raw material that Kunming Nuo Man Electron Material Co., Ltd produces.
Al2O3Substrate production producer is Linzhou City milky way high-tech development company limited.
The preparation of organic carrier: by mixed organic solvents (terpineol 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 baths heating, mechanical agitation is until being completely dissolved again simultaneously
Add the GBL of 20g, the castor oil hydrogenated of 1g and the oleic acid of 4g, and it be uniform to continue heated and stirred, i.e. prepare have airborne
Body, its viscosity is 6.5Pa s.
Embodiment 1
Organic carrier 20g, mean diameter is that glass dust 3.2g, the 300nm copper powder 76.8g of 0.93 μm adds three-roll grinder
In carry out three roller grindings, the conductor paste of mix homogeneously is by being screen printed onto 96%Al2O3Special pattern it is printed as on substrate,
Adjusting process parameter makes the thickness of pulp layer be 20 μm.This printed substrate is positioned over evacuation in vacuum drying oven, is passed through nitrogen
700 DEG C of this slurry, as protective atmosphere, is sintered and is incubated 5min by gas, prepare copper conductive traces, test its sheet resistance be 1.7m Ω/
□.Conductor is carried out tin welding, and the welding area in its surface is the 70% of the gross area.
Embodiment 2
Organic carrier 10g, mean diameter is that glass dust 3.6g, the 300nm copper powder 86.4g of 0.93 μm adds three-roll grinder
In carry out three roller grindings, the conductor paste of mix homogeneously is by being screen printed onto 96%Al2O3Special pattern it is printed as on substrate,
Adjusting process parameter makes the thickness of pulp layer be 20 μm.This printed substrate is positioned over evacuation in vacuum drying oven, is passed through nitrogen
700 DEG C of this slurry, as protective atmosphere, is sintered and is incubated 5min by gas, prepares copper conductive traces, and testing its sheet resistance is 59.2m
Ω/□.Conductor is carried out tin welding, and the welding area in its surface is the 45% of the gross area.
Embodiment 3
Organic carrier 20g, mean diameter is that glass dust 4.8g, the 300nm copper powder 75.2g of 0.93 μm adds three-roll grinder
In carry out three roller grindings, the conductor paste of mix homogeneously is by being screen printed onto 96%Al2O3Special pattern it is printed as on substrate,
Adjusting process parameter makes the thickness of pulp layer be 20 μm.This printed substrate is positioned over evacuation in vacuum drying oven, is passed through nitrogen
700 DEG C of this slurry, as protective atmosphere, is sintered and is incubated 5min by gas, prepare copper conductive traces, test its sheet resistance be 2.8m Ω/
□.Conductor is carried out tin welding, and the welding area in its surface is the 75% of the gross area.
Embodiment 4
Organic carrier 20g, mean diameter is that glass dust 3.2g, the 300nm copper powder 76.8g of 0.93 μm adds three-roll grinder
In carry out three roller grindings, the conductor paste of mix homogeneously is by being screen printed onto 96%Al2O3Special pattern it is printed as on substrate,
Adjusting process parameter makes the thickness of pulp layer be 20 μm.This printed substrate is positioned over evacuation in vacuum drying oven, is passed through nitrogen
600 DEG C of this slurry, as protective atmosphere, is sintered and is incubated 5min by gas, prepare copper conductive traces, test its sheet resistance be 1.1m Ω/
□.Conductor is carried out tin welding, and the welding area in its surface is the 60% of the gross area.
Embodiment 5
Organic carrier 20g, mean diameter is that glass dust 3.2g, the 300nm copper powder 76.8g of 0.93 μm adds three-roll grinder
In carry out three roller grindings, the conductor paste of mix homogeneously is by being screen printed onto 96%Al2O3Special pattern it is printed as on substrate,
Adjusting process parameter makes the thickness of pulp layer be 20 μm.This printed substrate is positioned over evacuation in vacuum drying oven, is passed through nitrogen
600 DEG C of this slurry, as protective atmosphere, is sintered and is incubated 10min by gas, prepares copper conductive traces, and testing its sheet resistance is 0.8m
Ω/□.Conductor is carried out tin welding, and the welding area in its surface is the 80% of the gross area.
Comparative example
Organic carrier 20g, mean diameter is that glass dust 3.2g, the 300nm argentum powder 76.8g of 0.93 μm adds three-roll grinder
In carry out three roller grindings, the conductor paste of mix homogeneously is by being screen printed onto 96%Al2O3Special pattern it is printed as on substrate,
Adjusting process parameter makes the thickness of pulp layer be 20 μm.This printed substrate is positioned in Muffle furnace 600 DEG C of sintering and protects
Temperature 5min, prepares silver conducting wire, and testing its sheet resistance is 0.4m Ω/.Conductor is carried out tin welding, welding of its surface
Amass 100% for the gross area.
From the experimental results, the electric conductivity of the oxidation resistant copper conductor slurry of the preparation of the present invention close to silver conductive paste,
Part wiring board less demanding to solderability drought tolerance can use this electrocondution slurry.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (7)
1. the preparation method of an oxidation resistant copper conductor slurry, it is characterised in that include following several step:
1) preparation of organic carrier, is first blended with 120～150 DEG C of heating after machine solvent, thickening agent mixing, and stirring is straight simultaneously
To being completely dissolved, it is subsequently adding rheological agent, thixotropic agent and dispersant thereof, and it is uniform to continue heated and stirred, obtains organic carrier；
2) copper powder and glass dust mix homogeneously are i.e. obtained solid-phase mixture, then carry out three with organic carrier by three-roll grinder
Roller ground and mixed；
3) screen process press is passed through by slurry at 96%Al2O3Special pattern, adjusting process parameter change slurry it is printed as on substrate
The thickness of layer is 20 μm；
4) tube furnace under nitrogen atmosphere is protected is sintered；
Described step 1) in mixed organic solvents be terpineol, butyl carbitol and butyl carbitol acetate, thixotropic agent is
Castor oil hydrogenated, thickening agent is ethyl cellulose, and rheological agent is GBL, and dispersant is oleic acid, step 2) described copper powder
Particle diameter be 300nm.
The preparation method of oxidation resistant copper conductor slurry the most according to claim 1, it is characterised in that step 2) described in consolidate
It is 60～90% that phase mixture accounts for the content of total mixture.
The preparation method of oxidation resistant copper conductor slurry the most according to claim 2, it is characterised in that step 2) described in consolidate
It is 80% that phase mixture accounts for the content of total mixture.
The preparation method of oxidation resistant copper conductor slurry the most 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%.
The preparation method of oxidation resistant copper conductor slurry the most according to claim 4, it is characterised in that glass dust accounts for solid phase and mixes
The content of compound is 4%.
The preparation method of oxidation resistant copper conductor slurry the most according to claim 1, it is characterised in that the sintering of step (4)
Temperature is 550～700 DEG C, and temperature retention time is 5～30min.
The preparation method of oxidation resistant copper conductor slurry the most according to claim 6, it is characterised in that the sintering of step (4)
Temperature is 600 DEG C, and temperature retention time is 10min.
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| CN201610515676.3A CN106205771B (en) | 2016-06-30 | 2016-06-30 | A kind of preparation method of oxidation resistant copper conductor slurry |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106876005A (en) * | 2017-01-11 | 2017-06-20 | 西安工程大学 | Sn Cu composite electron slurries and preparation method thereof |
| 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 |
| 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 |
| CN114639506A (en) * | 2022-05-20 | 2022-06-17 | 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 |
| CN115772040A (en) * | 2022-12-20 | 2023-03-10 | 深圳市赛尔美电子科技有限公司 | Method for manufacturing heating assembly, heating device and heating non-combustible smoking set |
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| 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 |
| CN106876005A (en) * | 2017-01-11 | 2017-06-20 | 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 |
| CN114639506A (en) * | 2022-05-20 | 2022-06-17 | 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 |
| 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 |
| CN115772040A (en) * | 2022-12-20 | 2023-03-10 | 深圳市赛尔美电子科技有限公司 | Method for manufacturing heating assembly, heating device and heating non-combustible smoking set |
| 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 |