CN105161219B - A kind of preparation method of UV photocurings silver nickel coat electrocondution slurry - Google Patents
A kind of preparation method of UV photocurings silver nickel coat electrocondution slurry Download PDFInfo
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- CN105161219B CN105161219B CN201510626803.2A CN201510626803A CN105161219B CN 105161219 B CN105161219 B CN 105161219B CN 201510626803 A CN201510626803 A CN 201510626803A CN 105161219 B CN105161219 B CN 105161219B
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Abstract
The invention discloses a kind of preparation method of UV photocurings silver nickel coat electrocondution slurry, the nickel powder of pretreatment and silver ammonia complex solution are mixed, polyvinylpyrrolidone is added after 60~90 DEG C of heating water bath 6h and reacts 1~2h, then obtains silver coated nickel powder end by centrifugation, cleaning；Photosensitive resin and silver coated nickel powder are well mixed, obtain silver-colored nickel coat conducting resinl；Conducting resinl is subjected to silk-screen printing, and irradiates and produces under uviol lamp.The preparation method of low temperature polymer electrocondution slurry of the present invention, base metal nickel is coated using noble silver, and preparation process is not required to high temperature sintering solidification, significantly reduces production cost；Not only electric conductivity is excellent for the silver-colored nickel coat electric slurry prepared, and can also deposit for a long time.
Description
Technical field
The invention belongs to electrically-conducting paint preparing technical field, and in particular to a kind of system of UV photocurings silver nickel coat electrocondution slurry
Preparation Method.
Background technology
Electrically-conducting paint is because of the advantages that its electric conductivity is high, shield effectiveness is good, and being widely used in every field, (such as aviation is navigated
My god, electronic component etc.).With the miniaturization of circuit and element and integrated, electrically-conducting paint utilizes its stream as connecting material
Dynamic property can directly carry out silk-screen printing and form circuit；On the other hand, electronic product easily by outside electromagnetic interference and to external radiation and
Cause information leakage.Therefore, a kind of electromagnetic shielding conductive slurry of good performance turns into the important trend of industrial materials.
Silver powder doped precious metal electrocondution slurry has been widely used at present.Although its electric conductivity is good, expensive, and
Electron transfer phenomenon occurs during as electrode material and reduces size performance, replaces noble metal to make electrocondution slurry using base metal
Cost can be substantially reduced.Nickel powder has good capability of electromagnetic shielding in metal system, but electric conductivity is not so good as silver powder, and easy to aging.
Conductive paste is prepared with nickel bottoming silver cladding, then can obtain larger economic benefit and social benefit.
Traditional solvent-borne type electrically-conducting paint causes environmental pollution and gradually washed in a pan because of volatile organic content caused by it
Eliminate, low volatile-type, no-solvent type conductive paste turn into research direction.Ultraviolet light (UV) curing process, i.e., triggered using ultraviolet source
Liquid with space charge force is rapidly converted into the process of solid-state.Compared with traditional heat curing process, there is solidification temperature
Spend low, reaction speed is fast, energy-saving and environmental protection, thorough reaction the advantages that.On the basis of existing, the pass of silver coated nickel powder is furtherd investigate
Key technology, keep stable quality, prepare one kind can industrial applications, there is good electric conductivity and absorbing property and anti-oxidant energy
The strong low-temperature environment-friendly type electrocondution slurry of power, so as to reduce manufacturer production cost, improve the market competitiveness.
The content of the invention
It is an object of the invention to provide a kind of preparation method of UV photocurings silver nickel coat electrocondution slurry, solves electrocondution slurry
Cost is high, slow curing and the problem of cause environmental pollution.
The technical solution adopted in the present invention is a kind of preparation method of UV photocurings silver nickel coat electrocondution slurry, specific step
Suddenly it is：
Step 1, the nickel powder of pretreatment and silver ammonia complex solution are mixed, poly- second is added after 60~90 DEG C of heating water bath 6h
Alkene pyrrolidone reacts 1~2h, then obtains silver coated nickel powder end by centrifugation, cleaning；
Step 2, the silver coated nickel powder that photosensitive resin and step 1 obtain is well mixed, obtains silver-colored nickel coat conducting resinl；
Step 3, conducting resinl step 2 obtained carries out silk-screen printing, and is irradiated under uviol lamp, that is, obtains UV solidifications
Low temperature polymer electrocondution slurry.
The features of the present invention also resides in,
The pretreatment of nickel powder in step 1：The nickel powder that average grain diameter is 5 μm is put into acetone, is sufficiently stirred scattered, standing
After filtering is cleaned with deionized water after 8~10min, be added in 5% dilute sulfuric acid and cleaned, then with deionized water clean to
It is neutral.
Silver ammonia complex solution obtains by the following method in step 1：Silver nitrate is dissolved in distilled water and is configured to quality
Concentration is 20~25g/L solution, and then stirring is slowly added to the concentrated ammonia liquor that mass fraction is 28%, starts to generate brown hydrogen-oxygen
Change silver precipitation, finally obtain water white transparency silver ammonia complex solution.
The mass ratio of nickel powder and silver ammonia complex solution is 1 in step 1：1~0.5.
In step 1 centrifuge, clean be using 5000~7000r/min 10~30min of centrifuge after stand 1~
3h, supernatant liquor is outwelled, cleaned twice with deionized water and ethanol.
The mass ratio of photosensitive resin and silver coated nickel powder is 1 in step 2：1~4.
Photosensitive resin is composed of the following components by mass percentage in step 2：40~60% epoxy acrylic resins, 20~
30%N- vinyl pyrrolidones, 10~15% trimethylolpropane tris propylene acid esters, 2~5%1- hydroxycyclohexylphenyl first
Ketone, 1~2% benzophenone, 2~5% Silane coupling reagent KH-570s, 3~4% polyether antifoam agents and 0.2~0.6% acrylic compounds
Levelling agent, above-mentioned mass percent sum are 100%；Above-mentioned each component is well mixed and obtains photosensitive resin.
Concrete operation method is in step 3：The sheet glass that size is 8cm × 2cm × 0.1cm is washed with alcohol or acetone
Only, drying for standby, conducting resinl is carried out on the glass sheet by 220 mesh screen-printing depositions using bar spreader, by what is prepared
It is 103mW/cm that film, which is placed on light intensity,2Ultraviolet light under 10cm radiation 2min, dried after taking-up at be placed on 2 days, whole experiment exists
Carried out in air.
The invention has the advantages that
1. the preparation method of low temperature polymer electrocondution slurry of the present invention, base metal nickel is coated using noble silver, and prepare
Process is not required to high temperature sintering solidification, significantly reduces production cost；The silver-colored nickel coat electric slurry prepared not only electric conductivity
It is excellent, it can also deposit for a long time.
2. the preparation method of low temperature polymer electrocondution slurry of the present invention, the silver-colored nickel coat electricity prepared using the solidification of UV ultraviolet lights
Sub- slurry, the volatilization without organic matter is pollution-free, and curing rate is quickly, available for electrode of solar battery, the integrated electricity of thick film
The low temperature polymer electrocondution slurry of the requirements such as road, LED light source and other electronic components.
Embodiment
With reference to embodiment, the present invention is described in detail.
A kind of preparation method of UV photocurings silver nickel coat electrocondution slurry of the present invention, is concretely comprised the following steps：
Step 1, it is that 5 μm of nickel powder is put into acetone by average grain diameter, is sufficiently stirred scattered, is filtered after standing 8~10min
After being cleaned with deionized water, it is added in 5% dilute sulfuric acid and is cleaned, then cleaned with deionized water to neutrality, obtains pre- place
The nickel powder of reason；
Step 2, silver nitrate is dissolved in the solution for being configured to that mass concentration is 20~25g/L in distilled water, then stirring is slow
It is slow to add the concentrated ammonia liquor that mass fraction is 28%, start to generate brown silver hydroxide precipitation, finally obtain water white transparency silver ammino
Polymer solution；
Step 3, it is 1 in mass ratio by the nickel powder of pretreatment and silver ammonia complex solution：1~0.5 mixing, using 5000~
10000rpm speed magnetic agitation, polyvinylpyrrolidone is added after 60~90 DEG C of heating water bath 6h and reacts 1~2h, is then adopted
With 1~3h is stood after 5000~7000r/min 10~30min of centrifuge, supernatant liquor is outwelled, with deionized water and second
Alcohol cleans twice, obtains silver coated nickel powder end；
Step 4,40~60% epoxy acrylic resins, 20~30%N- vinyl pyrroles are weighed respectively by mass percentage
Alkanone, 10~15% trimethylolpropane tris propylene acid esters, 2~5%1- hydroxycyclohexyl phenyl ketones, 1~2% hexichol first
Ketone, 2~5% Silane coupling reagent KH-570s, 3~4% polyether antifoam agents and 0.2~0.6% acrylic compounds levelling agent, above-mentioned quality
Percentage sum is 100%；Above-mentioned each component is well mixed and obtains photosensitive resin；
Step 5, silver coated nickel powder photosensitive resin and step 1 obtained is 1 in mass ratio：1~4 is well mixed, obtains silver
Nickel coat conducting resinl；
Step 6, the sheet glass that size is 8cm × 2cm × 0.1cm is cleaned with alcohol or acetone, drying for standby, using line
Conducting resinl is carried out 220 mesh screen-printing depositions on the glass sheet by rod coating device, and the film prepared is placed on into light intensity is
103mW/cm2Ultraviolet light under 10cm radiation 2min, dried after taking-up at be placed on 2 days, whole experiment is carried out in atmosphere, is obtained
The low temperature polymer electrocondution slurry of UV solidifications.
The preparation method of low temperature polymer electrocondution slurry of the present invention, base metal nickel is coated using noble silver, and prepared
Cheng Buxu high temperature sinterings solidify, and significantly reduce production cost；Not only electric conductivity is excellent for the silver-colored nickel coat electric slurry prepared
It is different, it can also deposit for a long time.
The preparation method of low temperature polymer electrocondution slurry of the present invention, the silver-colored nickel coat electronics prepared using the solidification of UV ultraviolet lights
Slurry, the volatilization without organic matter is pollution-free, and curing rate is quickly, available for electrode of solar battery, the integrated electricity of thick film
The low temperature polymer electrocondution slurry of the requirements such as road, LED light source and other electronic components.
Embodiment 1
Step 1, the nickel powder that average grain diameter is 5 μm is put into acetone, is sufficiently stirred scattered, filtering use after standing 10min
After deionized water cleaning, it is added in 5% dilute sulfuric acid and is cleaned, then cleaned with deionized water to neutrality, is pre-processed
Nickel powder；
Step 2, silver nitrate is dissolved in the solution for being configured to that mass concentration is 25g/L in distilled water, then stirring slowly adds
Enter the concentrated ammonia liquor that mass fraction is 28%, start to generate brown silver hydroxide precipitation, finally obtain water white transparency silver ammonia complex
Solution；
Step 3, it is 1 in mass ratio by the nickel powder of pretreatment and silver ammonia complex solution：0.5 mixing, using 10000rpm
Speed magnetic agitation, polyvinylpyrrolidone reaction 2h is added after 90 DEG C of heating water bath 6h, then using 7000r/min from
3h is stood after scheming centrifugation 30min, supernatant liquor is outwelled, is cleaned twice with deionized water and ethanol, obtains silver coated nickel powder end；
Step 4, weigh respectively by mass percentage 40% epoxy acrylic resin, 30%N- vinyl pyrrolidones,
15% trimethylolpropane tris propylene acid esters, 5%1- hydroxycyclohexyl phenyl ketones, 2% benzophenone, 4% silane coupler
KH-570,3.4% polyether antifoam agent and 0.6% acrylic compounds levelling agent, above-mentioned mass percent sum are 100%；Will be above-mentioned
Each component is well mixed to obtain photosensitive resin；
Step 5, silver coated nickel powder photosensitive resin and step 1 obtained is 1 in mass ratio：2 is well mixed, obtains silver-colored nickel coat
Conducting resinl；
Step 6, the sheet glass that size is 8cm × 2cm × 0.1cm is cleaned with alcohol or acetone, drying for standby, using line
Conducting resinl is carried out 220 mesh screen-printing depositions on the glass sheet by rod coating device, and the film prepared is placed on into light intensity is
103mW/cm2Ultraviolet light under 10cm radiation 2min, dried after taking-up at be placed on 2 days, whole experiment is carried out in atmosphere, is obtained
The low temperature polymer electrocondution slurry of UV solidifications.
The resistivity of low temperature polymer electrocondution slurry prepared by embodiment 1 is 2.5m Ω/.
Embodiment 2
Step 1, the nickel powder that average grain diameter is 5 μm is put into acetone, is sufficiently stirred scattered, filtering use after standing 10min
After deionized water cleaning, it is added in 5% dilute sulfuric acid and is cleaned, then cleaned with deionized water to neutrality, is pre-processed
Nickel powder；
Step 2, silver nitrate is dissolved in the solution for being configured to that mass concentration is 22g/L in distilled water, then stirring slowly adds
Enter the concentrated ammonia liquor that mass fraction is 28%, start to generate brown silver hydroxide precipitation, finally obtain water white transparency silver ammonia complex
Solution；
Step 3, it is 1 in mass ratio by the nickel powder of pretreatment and silver ammonia complex solution：0.8 mixing, using 5000rpm's
Speed magnetic agitation, polyvinylpyrrolidone reaction 1h is added after 60 DEG C of heating water bath 6h, then using 5000r/min centrifugation
1h is stood after machine centrifugation 10min, supernatant liquor is outwelled, is cleaned twice with deionized water and ethanol, obtains silver coated nickel powder end；
Step 4, weigh respectively by mass percentage 50% epoxy acrylic resin, 27%N- vinyl pyrrolidones,
It is 10% trimethylolpropane tris propylene acid esters, 3%1- hydroxycyclohexyl phenyl ketones, 1.8% benzophenone, 5% silane coupled
Agent KH-570,3% polyether antifoam agent and 0.2% acrylic compounds levelling agent, above-mentioned mass percent sum are 100%；Will be above-mentioned
Each component is well mixed to obtain photosensitive resin；
Step 5, silver coated nickel powder photosensitive resin and step 1 obtained is 1 in mass ratio：3 is well mixed, obtains silver-colored nickel coat
Conducting resinl；
Step 6, the sheet glass that size is 8cm × 2cm × 0.1cm is cleaned with alcohol or acetone, drying for standby, using line
Conducting resinl is carried out 220 mesh screen-printing depositions on the glass sheet by rod coating device, and the film prepared is placed on into light intensity is
103mW/cm2Ultraviolet light under 10cm radiation 2min, dried after taking-up at be placed on 2 days, whole experiment is carried out in atmosphere, is obtained
The low temperature polymer electrocondution slurry of UV solidifications.
The resistivity of low temperature polymer electrocondution slurry prepared by embodiment 2 is 5.7m Ω/.
Embodiment 3
Step 1, it is that 5 μm of nickel powder is put into acetone by average grain diameter, is sufficiently stirred scattered, stands to filter after 8min and spend
After ionized water cleaning, it is added in 5% dilute sulfuric acid and is cleaned, then cleaned with deionized water to neutrality, is pre-processed
Nickel powder；
Step 2, silver nitrate is dissolved in the solution for being configured to that mass concentration is 20g/L in distilled water, then stirring slowly adds
Enter the concentrated ammonia liquor that mass fraction is 28%, start to generate brown silver hydroxide precipitation, finally obtain water white transparency silver ammonia complex
Solution；
Step 3, it is 1 in mass ratio by the nickel powder of pretreatment and silver ammonia complex solution：0.6 mixing, using 7000rpm's
Speed magnetic agitation, polyvinylpyrrolidone reaction 1.5h is added after 80 DEG C of heating water bath 6h, then using 6000r/min from
2h is stood after scheming centrifugation 20min, supernatant liquor is outwelled, is cleaned twice with deionized water and ethanol, obtains silver coated nickel powder end；
Step 4, weigh respectively by mass percentage 60% epoxy acrylic resin, 20%N- vinyl pyrrolidones,
11% trimethylolpropane tris propylene acid esters, 2%1- hydroxycyclohexyl phenyl ketones, 1% benzophenone, 2% silane coupler
KH-570,3.6% polyether antifoam agent and 0.4% acrylic compounds levelling agent, above-mentioned mass percent sum are 100%；Will be above-mentioned
Each component is well mixed to obtain photosensitive resin；
Step 5, silver coated nickel powder photosensitive resin and step 1 obtained is 1 in mass ratio：4 is well mixed, obtains silver-colored nickel coat
Conducting resinl；
Step 6, the sheet glass that size is 8cm × 2cm × 0.1cm is cleaned with alcohol or acetone, drying for standby, using line
Conducting resinl is carried out 220 mesh screen-printing depositions on the glass sheet by rod coating device, and the film prepared is placed on into light intensity is
103mW/cm2Ultraviolet light under 10cm radiation 2min, dried after taking-up at be placed on 2 days, whole experiment is carried out in atmosphere, is obtained
The low temperature polymer electrocondution slurry of UV solidifications.
The resistivity of low temperature polymer electrocondution slurry prepared by embodiment 3 is 8.4m Ω/.
Embodiment 4
Step 1, it is that 5 μm of nickel powder is put into acetone by average grain diameter, is sufficiently stirred scattered, stands to filter after 9min and spend
After ionized water cleaning, it is added in 5% dilute sulfuric acid and is cleaned, then cleaned with deionized water to neutrality, is pre-processed
Nickel powder；
Step 2, silver nitrate is dissolved in the solution for being configured to that mass concentration is 20g/L in distilled water, then stirring slowly adds
Enter the concentrated ammonia liquor that mass fraction is 28%, start to generate brown silver hydroxide precipitation, finally obtain water white transparency silver ammonia complex
Solution；
Step 3, it is 1 in mass ratio by the nickel powder of pretreatment and silver ammonia complex solution：1 mixing, using 9000rpm speed
Magnetic agitation is spent, polyvinylpyrrolidone reaction 1.5h is added after 70 DEG C of heating water bath 6h, then using 5000r/min centrifugation
1.5h is stood after machine centrifugation 25min, supernatant liquor is outwelled, is cleaned twice with deionized water and ethanol, obtains silver coated nickel powder end；
Step 4, weigh respectively by mass percentage 45% epoxy acrylic resin, 29%N- vinyl pyrrolidones,
13% trimethylolpropane tris propylene acid esters, 3.5%1- hydroxycyclohexyl phenyl ketones, 1.5% benzophenone, 3.5% silane
Coupling agent kh-570,4% polyether antifoam agent and 0.5% acrylic compounds levelling agent, above-mentioned mass percent sum are 100%；Will
Above-mentioned each component is well mixed to obtain photosensitive resin；
Step 5, silver coated nickel powder photosensitive resin and step 1 obtained is 1 in mass ratio：1 is well mixed, obtains silver-colored nickel coat
Conducting resinl；
Step 6, the sheet glass that size is 8cm × 2cm × 0.1cm is cleaned with alcohol or acetone, drying for standby, using line
Conducting resinl is carried out 220 mesh screen-printing depositions on the glass sheet by rod coating device, and the film prepared is placed on into light intensity is
103mW/cm2Ultraviolet light under 10cm radiation 2min, dried after taking-up at be placed on 2 days, whole experiment is carried out in atmosphere, is obtained
The low temperature polymer electrocondution slurry of UV solidifications.
The resistivity of low temperature polymer electrocondution slurry prepared by embodiment 4 is 3.2m Ω/.
Claims (4)
1. a kind of preparation method of UV photocurings silver nickel coat electrocondution slurry, it is characterised in that concretely comprise the following steps：
Step 1, the nickel powder of pretreatment and silver ammonia complex solution are mixed, the mass ratio of nickel powder and silver ammonia complex solution is 1：
Polyvinylpyrrolidone is added after 1~0.5,60~90 DEG C of heating water bath 6h and reacts 1~2h, is then obtained by centrifugation, cleaning
Silver coated nickel powder end；
Step 2, the silver coated nickel powder that photosensitive resin and step 1 obtain is well mixed, the mass ratio of photosensitive resin and silver coated nickel powder
For 1：1~4, obtain silver-colored nickel coat conducting resinl；Wherein photosensitive resin is composed of the following components by mass percentage：40~60% epoxies
Acrylic resin, 20~30%N- vinyl pyrrolidones, 10~15% trimethylolpropane tris propylene acid esters, 2~5%1- hydroxyls
Butylcyclohexyl phenyl ketone, 1~2% benzophenone, 2~5% Silane coupling reagent KH-570s, 3~4% polyether antifoam agents and 0.2
~0.6% acrylic compounds levelling agent, above-mentioned mass percent sum are 100%；Above-mentioned each component is well mixed and obtains light
Quick resin；
Step 3, the sheet glass that size is 8cm × 2cm × 0.1cm is cleaned with alcohol or acetone, drying for standby, applied using bar
Conducting resinl is carried out 220 mesh screen-printing depositions on the glass sheet by cloth device, and it is 103mW/cm that the film prepared is placed on into light intensity2
Ultraviolet light under 10cm radiation 2min, dried after taking-up at be placed on 2 days, whole experiment is carried out in atmosphere, that is, obtains UV solidifications
Low temperature polymer electrocondution slurry.
2. the preparation method of UV photocurings silver nickel coat electrocondution slurry according to claim 1, it is characterised in that in step 1
The pretreatment of nickel powder：It is that 5 μm of nickel powder is put into acetone by average grain diameter, is sufficiently stirred scattered, is filtered after standing 8~10min
After being cleaned with deionized water, it is added in 5% dilute sulfuric acid and is cleaned, then is cleaned with deionized water to neutrality.
3. the preparation method of UV photocurings silver nickel coat electrocondution slurry according to claim 1, it is characterised in that in step 1
Silver ammonia complex solution obtains by the following method：Silver nitrate is dissolved in distilled water to be configured to mass concentration be 20~25g/L
Solution, then stirring is slowly added to the concentrated ammonia liquor that mass fraction is 28%, starts to generate brown silver hydroxide precipitation, finally
To water white transparency silver ammonia complex solution.
4. the preparation method of UV photocurings silver nickel coat electrocondution slurry according to claim 1, it is characterised in that in step 1
Centrifugation, cleaning are 1~3h of standing after 10~30min of centrifuge using 5000~7000r/min, outwell supernatant liquor,
Cleaned twice with deionized water and ethanol.
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| CN106378448B (en) * | 2016-09-20 | 2019-03-19 | 杨海波 | A kind of nickel powder silver clad surface for circuit brake material is modified |
| CN114447123B (en) * | 2020-11-02 | 2024-05-14 | 苏州阿特斯阳光电力科技有限公司 | Heterojunction solar cell and photovoltaic module |
| CN112643026A (en) * | 2020-12-16 | 2021-04-13 | 重庆云天化瀚恩新材料开发有限公司 | Preparation method of silver-coated nickel powder |
| CN114605894A (en) * | 2022-04-11 | 2022-06-10 | 西安热工研究院有限公司 | Based on AgNWs/Ti3AlC2Corrosion-resistant coating of conductive filler and preparation method thereof |
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| CN103474126B (en) * | 2013-09-16 | 2015-09-16 | 东莞市贝特利新材料有限公司 | Can the electrocondution slurry of UV surface cure and conductive film circuit production method thereof fast |
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Application publication date: 20151216 Assignee: Pucheng Zhenggong Gas Co.,Ltd. Assignor: XI'AN POLYTECHNIC University Contract record no.: X2023980034734 Denomination of invention: A preparation method of UV curable silver coated nickel conductive paste Granted publication date: 20180102 License type: Common License Record date: 20230419 |
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