CN105405487A - Conductive silver paste, preparation method therefor, conductive circuit, and preparation method for conductive circuit - Google Patents
Conductive silver paste, preparation method therefor, conductive circuit, and preparation method for conductive circuit Download PDFInfo
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- CN105405487A CN105405487A CN201410439180.3A CN201410439180A CN105405487A CN 105405487 A CN105405487 A CN 105405487A CN 201410439180 A CN201410439180 A CN 201410439180A CN 105405487 A CN105405487 A CN 105405487A
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Abstract
The invention provides conductive silver paste and a preparation method therefor. The conductive silver paste contains the following components: 65-80wt% of silver powder, 8-25wt% of an adhesive, and 5-15wt% of solvent. The adhesive is thermosetting phenolic resin or thermosetting epoxy resin. The invention also provides a method for preparing a conductive circuit through employing the conductive silver paste, and the conductive circuit prepared through the method. The conductive silver paste provided by the invention can be quickly set in a mode of plasma treatment, greatly shortens the setting time, is very suitable for batch production, and improves the work efficiency. Moreover, the conductive circuit formed after setting is good in electrical performances.
Description
Technical field
The invention belongs to metallic conduction circuit print field, be specifically related to a kind of conductive silver paste and preparation method thereof, a kind of preparation method of conducting wire and the conducting wire that prepared by this preparation method.
Background technology
At present, printing industry, through change for many years, develops into electrically conductive ink by original common ink, and electrically conductive ink is also conducting resinl or conductive silver paste.The printing of existing metal paste is widely applied in the electronic products such as antenna, automotive electronics and electronic tag.
Current conductive silver paste is mainly used in the direction such as thin film switch, flexible circuit, and along with the emergence of China's silk screen printing and flexible circuitry board industry, the research and development of the electrocondution slurry of the soft circuit of film also more and more receives publicity.At present, conductive silver paste after printing, its dry solidification is all adopt discontinuous heated-air circulation oven or continuous far-infrared tunnel oven, infrared ray low-temperature bake 80-100 DEG C, 30 seconds time is first used after conductive silver paste printing, 140 DEG C again, baking more than 30 seconds, finally 120 DEG C, the oven dry of 30 minutes time in heated-air circulation oven.In batch production, adopt this technique to need multiple stage discontinuous heated-air circulation oven or continuous far-infrared tunnel oven, preheating, oven dry, cooling required time are longer, consuming time longer when especially printing thicker circuit.And conductive silver paste conventional in prior art, also have no other curing modes of report.
Summary of the invention
The invention solves the technical problem that when conductive silver paste existed in prior art solidifies, required time is long, and conductive silver paste of a kind of new formula and preparation method thereof is provided, provide a kind of conducting wire and preparation method thereof simultaneously.
Particularly, technical scheme of the present invention is:
A kind of conductive silver paste, containing following component in described conductive silver paste: silver powder 65-80wt%, adhesive 8-25wt%, solvent 5-15wt%; Described adhesive is thermosetting phenolic resin or thermosetting epoxy resin.
A preparation method for conductive silver paste, comprises the following steps: mixed in proportion with solvent by adhesive, adds silver powder, mix and obtain described conductive silver paste after adhesive dissolves.
A preparation method for conducting wire, comprises the following steps: on substrate, print conductive silver paste provided by the invention according to required form, then carries out plasma treatment, namely obtains described conducting wire.
A kind of conducting wire, described conducting wire is prepared by preparation method provided by the invention.
Conductive silver paste provided by the invention, the formula of its uniqueness makes it that the mode of plasma treatment can be adopted to realize rapid curing when subsequent cure, thus greatly shorten curing time, be particularly useful for printing thicker conducting wire, and this curing mode is very suitable for producing in enormous quantities, increases work efficiency.The conducting wire prepared after adopting conductive silver paste rapid curing provided by the invention, has good electrical property.
Embodiment
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearly understand, below in conjunction with embodiment, the present invention is further elaborated.
Particularly, the invention provides a kind of conductive silver paste, containing following component in described conductive silver paste: silver powder 65-80wt%, adhesive 8-25wt%, solvent 5-15wt%; Described adhesive is thermosetting phenolic resin or thermosetting epoxy resin.Inventor finds, in this conductive silver paste ratio range, can realize rapid curing in later use plasma treatment, and the conductor layer formed after ensureing solidification has good electrical property; Otherwise, not in this ratio range, also need longer curing time even if utilize plasma treatment to be cured or can not solidify at all, and solidification after resistance excessive.
Conductive silver paste provided by the invention, the formula of its uniqueness makes it that the mode of plasma treatment can be adopted to realize rapid curing when subsequent cure, thus greatly shorten curing time, be particularly useful for printing thicker conducting wire, and this curing mode is very suitable for producing in enormous quantities, increases work efficiency.The conducting wire prepared after adopting conductive silver paste rapid curing provided by the invention, has good electrical property.
Under preferable case, in the present invention, the particle diameter of described silver powder is 0.1-5 micron.Inventor find, the silver powder within the scope of this preferable particle size can have good appearance, ensure its silver slurry in good dispersion, finally make formed conducting wire there is good consistency and electric conductivity.
In the present invention, by carrying out great many of experiments discovery in existing adhesive, in the present invention, adopt thermosetting phenolic resin or thermosetting epoxy resin as adhesive of the present invention, and adhesion strength is high, and the content of simultaneously other component of rational allocation, can ensure that the conducting wire of employing conductive silver paste formation of the present invention has good heat resistance, circuit and substrate adhesion high.Under preferable case, described adhesive is selected from least one in phenolic aldehyde-butyronitrile adhesive, phenolic aldehyde-acetal adhesive, phenolic aldehyde-epoxy resin, bisphenol A type epoxy resin.In the curing process, can there is self-crosslinking solidification in adhesive, form coating structure, silver powder is then dispersed in this film.
In the present invention, high boiling solvent selected by described solvent, and boiling point high volatile volatile is little, can ensure the stability of silver slurry.Generally, boiling point can be selected to be the organic solvent of 120-190 DEG C.Such as, described solvent can be selected from least one in the molten acid anhydride acetic acid esters of butyl, butyl acetate, DGDE acetate, isophorone, oxolane, but is not limited to this.
In the present invention, also can contain various auxiliary agent as required in described conductive silver paste, such as, can be selected from least one in curing agent, diluent, sagging inhibitor, adhesion promoter, but be not limited to this.
Wherein, described curing agent is used for, with adhesive, further crosslinking curing occurs, and promotes the formation of film.In the present invention, described curing agent can adopt methylimidazole, but is not limited to this.Described diluent, for regulating the viscosity of conductive silver paste, is convenient to its printing.In the present invention, described diluent can adopt expoxy propane benzylic ether, i.e. epoxy active diluent 692, but is not limited to this.Described sagging inhibitor is used for preventing silver powder particles sedimentation in conductive silver paste, can adopt polyamide wax, but be not limited to this.Described adhesion promoter is for improving when conductive silver paste applies and the adhesive force of substrate, and it can adopt tetraethyl titanate, but is not limited to this.
The content of auxiliary agent is unsuitable too high, otherwise can reduce the content of other component in conductive silver paste, causes the electrical property of the conducting wire formed to decline.Under preferable case, in described conductive silver paste, the content of auxiliary agent is 0.1-2wt%.
Present invention also offers a kind of preparation method of described conductive silver paste, comprise the following steps: adhesive is mixed in proportion with solvent, after adhesive dissolves, add silver powder, mix and obtain described conductive silver paste.As previously mentioned, various auxiliary agent can also be contained as required in described conductive silver paste.Therefore, in the present invention, be also included in the step continuing to add auxiliary agent after adding silver powder.In fact, auxiliary agent also can add before adding silver powder, only needed finally each component to be stirred.
As previously mentioned, conductive silver paste provided by the invention realizes rapid curing by plasma treatment, and has good electrical property after ensureing solidification.Therefore, the invention provides a kind of preparation method of conducting wire, comprise the following steps: on substrate, print conductive silver paste provided by the invention according to required form, then carry out plasma treatment, namely obtain described conducting wire.
Wherein, the method for printing is the common various printing processes in this area, such as, can be silk screen printing or flexographic printing, but be not limited to this.Conductive silver paste provided by the invention has good printing performance, can reach the print thickness of more than 10 microns, meets some special line requirements.Under preferable case, the thickness of the conducting wire that the printing consumption of described conductive silver paste is formed for guarantee is 10-18 micron.
The solidification process of conductive silver paste is generally hot curing or directly dries, and traditional handicraft adopts baking box to toast for a long time.If print thickness increases, baking time is also elongated, also has corresponding restriction to printing unit, and parts are too large also has requirement to baking box, and impact baking efficiency.And according to method provided by the invention, after printing conductive silver paste, plasma apparatus can be adopted to carry out plasma treatment to slurry printed layers, realize its rapid curing, printed wire can be dried instantaneously.Particularly, after conductive silver paste is completed for printing, when plasma treatment; its negative ions sprayed by plasma apparatus; and high temperature heat is provided, make the slurry of printing rapid curing under the protection of negative ions, solve the problem that in traditional handicraft, baking time is long in an oven.In addition, inventor also finds, adopts plasma treatment printed wire, and ionization post plasma gas can also prevent printed wire from producing pore when high temperature, clean circuit surface, thus plays the effect on solidification and clean circuit surface.
In actual mechanical process, can the nozzle of plasma apparatus is placed on streamline, when there being product to flow through from streamline, plasma apparatus is ejection negative ions and high-temperature gas just, is cured oven dry to product, is applicable to producing in enormous quantities.
Particularly, in the present invention, the gas medium for plasma treatment does not have particular/special requirement, such as, can adopt any at least one in argon gas, oxygen, nitrogen, air, but be not limited to this.The concrete technology parameter of plasma treatment suitably can be selected according to print thickness.Under preferable case, in the present invention, the condition of described plasma treatment comprises: pressure is 50-150KPa; Power is 150-350W; Time is 20-80 second.
In addition, as the common practise of those skilled in the art, during plasma treatment, the nozzle of plasma apparatus at the uniform velocity moves above printed wire, those skilled in the art can select suitable plasma nozzle to the Distance geometry nozzle translational speed of printed wire according to the thickness of printed wire, can be cured printed wire fast like this.
Finally, the invention provides a kind of conducting wire, described conducting wire is prepared by preparation method provided by the invention.Adopt the conducting wire that preparation method provided by the invention obtains, its resistance is lower, and electrical property is good.
Be with it may be noted that, though by means of only experimental verification, conductive silver paste provided by the invention realizes its rapid curing by plasma treatment in the present invention, inventor thinks that plasma treatment fast-curing process provided by the invention is equally also applicable to the rapid curing of other metal pastes such as copper slurry, aluminium paste.
Below by embodiment, the present invention is further illustrated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.In embodiment and comparative example adopt raw material to be all commercially available, the present invention is not particularly limited.
Embodiment 1
(1) conductive silver paste S1 is prepared
Take 180g bisphenol A type epoxy resin and 90g oxolane, bisphenol A type epoxy resin is placed in beaker, drip oxolane with glue head dropper and enter in beaker, stir while dropping, until bisphenol A type epoxy resin dissolves completely.Then take 720g silver powder (particle diameter 0.1 μm, purity 99.99%), and add in beaker, stir, finally taking 10g methylimidazole joins in beaker, and stir and obtain the conductive silver paste of the present embodiment, be designated as S1, it consists of: silver powder 72wt%, adhesive 18%, solvent 9%, auxiliary agent 1%.
(2) conducting wire S10 is prepared
According to required circuitous pattern, by the silk screen printing conductive silver paste S1 that print steps (1) is obtained in substrate; Then the plasma apparatus with respective nozzle shape is selected according to circuitous pattern, argon gas and oxygen mixed gas is selected to be gas medium, wherein ar pressure is 70KPa, oxygen pressure is 60KPa, and the power 200W of setting plasma apparatus, after gas to be mixed enters plasma apparatus, by two pieces of relative pole plates, rise mist and ionize thus carry out plasma treatment to printed wire, the processing time is 30 seconds, forms at substrate surface the conducting wire S10 that thickness is 10 microns.
Embodiment 2
(1) conductive silver paste S2 is prepared
Take 80g phenolic aldehyde-butyronitrile adhesive and 108g butyl acetate, phenolic aldehyde-butyronitrile adhesive is placed in beaker, dripping butyl acetate with glue head dropper enters in beaker, stirs, until phenolic aldehyde-butyronitrile adhesive dissolves completely while dropping.Then 800g silver powder (particle diameter 0.5 μm is taken, purity 99.99%), and add in beaker, stir, finally take 6g epoxy active diluent 692 and 6g polyamide wax joins in beaker, stir and obtain the conductive silver paste of the present embodiment, be designated as S2, it consists of: silver powder 80wt%, adhesive 8%, solvent 10.8%, auxiliary agent 1.2%.
(2) conducting wire S20 is prepared
According to required circuitous pattern, by the silk screen printing conductive silver paste S2 that print steps (1) is obtained in substrate; Then the plasma apparatus with respective nozzle shape is selected according to circuitous pattern, argon gas and oxygen mixed gas is selected to be gas medium, wherein ar pressure is 75KPa, oxygen pressure is 65KPa, and the power 200W of setting plasma apparatus, after gas to be mixed enters plasma apparatus, by two pieces of relative pole plates, rise mist and ionize thus carry out plasma treatment to printed wire, the processing time is 38 seconds, forms at substrate surface the conducting wire S20 that thickness is 10 microns.
Embodiment 3
(1) conductive silver paste S3 is prepared
Take 222g phenolic aldehyde-epoxy resin and 121g isophorone, phenolic aldehyde-epoxy resin is placed in beaker, drip isophorone with glue head dropper and enter in beaker, stir while dropping, until phenolic aldehyde-epoxy resin dissolves completely.Then 650g silver powder (particle diameter 4.5 μm is taken, purity 99.99%), and add in beaker, stir, finally take 2g methylimidazole, 1g epoxy active diluent 692,1g polyamide wax and 3g tetraethyl titanate and join in beaker, stir and obtain the conductive silver paste of the present embodiment, be designated as S3, it consists of: silver powder 65wt%, adhesive 22.2%, solvent 12.1%, auxiliary agent 0.7%.
(2) conducting wire S30 is prepared
According to required circuitous pattern, by the silk screen printing conductive silver paste S3 that print steps (1) is obtained in substrate; Then the plasma apparatus with respective nozzle shape is selected according to circuitous pattern, argon gas and oxygen mixed gas is selected to be gas medium, wherein ar pressure is 60KPa, oxygen pressure is 50KPa, and the power 200W of setting plasma apparatus, after gas to be mixed enters plasma apparatus, by two pieces of relative pole plates, rise mist and ionize thus carry out plasma treatment to printed wire, the processing time is 62 seconds, forms at substrate surface the conducting wire S30 that thickness is 10 microns.
Comparative example 1
(1) conductive silver paste DS1 is prepared
Take 250g bisphenol A type epoxy resin and 140g oxolane, bisphenol A type epoxy resin is placed in beaker, drip oxolane with glue head dropper and enter in beaker, stir while dropping, until bisphenol A type epoxy resin dissolves completely.Then 600g silver powder (particle diameter 0.1 μm is taken, purity 99.99%), and add in beaker, stir, finally take 10g methylimidazole and join in beaker, stir and obtain the conductive silver paste of the present embodiment, be designated as S1, it consists of: silver powder 60wt%, adhesive 25%, solvent 14%, auxiliary agent 1%.
(2) conducting wire DS10 is prepared
According to required circuitous pattern, by the silk screen printing conductive silver paste DS1 that print steps (1) is obtained in substrate; Then the plasma apparatus with respective nozzle shape is selected according to circuitous pattern, argon gas and oxygen mixed gas is selected to be gas medium, wherein ar pressure is 70KPa, oxygen pressure is 60KPa, and the power 200W of setting plasma apparatus, after gas to be mixed enters plasma apparatus, by two pieces of relative pole plates, rise mist and ionize thus carry out plasma treatment to printed wire, the processing time is 180 seconds, forms conducting wire DS10 at substrate surface.
Comparative example 2
According to required circuitous pattern, in substrate, print the obtained conductive silver paste S1 of embodiment 1 step (1) by silk screen printing; Then infrared ray low-temperature bake 80 DEG C, 30 seconds time is first used, then 140 DEG C, baking more than 30 seconds, within finally at 120 DEG C 45 minutes in heated-air circulation oven, dry, form at substrate surface the conducting wire DS20 that thickness is 10 microns.
Performance test
Adopt the resistance of universal instrument to conducting wire S10-S30 and DS10-DS20 in embodiment 1-3 and comparative example 1-2 to test, test result is as shown in table 1.
Table 1
As can be seen from the test result of upper table 1, the resistance of the conducting wire adopting conductive silver paste provided by the invention to be solidify to form by plasma treatment is within 4 Europe, has good electrical property, is obviously better than the sample of comparative example 1.Wherein, adopt usual manner to be cured process to conductive silver paste provided by the invention in comparative example 2, although the resistance of its circuit formed is also lower, its curing time is 45 minutes, and operating efficiency is low.And the conductive silver paste in comparative example 1 is not in content ratio range provided by the invention, when adopting method provided by the invention to be cured process (i.e. plasma treatment) to it, required time also longer (180 seconds), inventor found through experiments, if plasma processing time was lower than 180 seconds, circuit is easily wiped off by blade, does not reach the effect of solidification.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (12)
1. a conductive silver paste, is characterized in that, containing following component in described conductive silver paste: silver powder 65-80wt%, adhesive 8-25wt%, solvent 5-15wt%; Described adhesive is thermosetting phenolic resin or thermosetting epoxy resin.
2. conductive silver paste according to claim 1, is characterized in that, the particle diameter of described silver powder is 0.1-5 micron.
3. conductive silver paste according to claim 1, is characterized in that, described adhesive is selected from least one in phenolic aldehyde-butyronitrile adhesive, phenolic aldehyde-acetal adhesive, phenolic aldehyde-epoxy resin, bisphenol A type epoxy resin.
4. conductive silver paste according to claim 1, is characterized in that, described solvent is selected from least one in the molten acid anhydride acetic acid esters of butyl, butyl acetate, DGDE acetate, isophorone, oxolane.
5. conductive silver paste according to claim 1, is characterized in that, the auxiliary agent also containing 0.1-2wt% in described conductive silver paste; Described auxiliary agent is selected from least one in curing agent, diluent, sagging inhibitor, adhesion promoter.
6. conductive silver paste according to claim 5, is characterized in that, described curing agent is methylimidazole, and diluent is expoxy propane benzylic ether, and sagging inhibitor is polyamide wax, and adhesion promoter is tetraethyl titanate.
7. the preparation method of conductive silver paste according to claim 1, is characterized in that, comprises the following steps: mixed in proportion with solvent by adhesive, adds silver powder, mix and obtain described conductive silver paste after adhesive dissolves.
8. preparation method according to claim 7, is characterized in that, is also included in the step continuing to add auxiliary agent after adding silver powder; Described auxiliary agent is selected from least one in curing agent, diluent, sagging inhibitor, adhesion promoter.
9. a preparation method for conducting wire, is characterized in that, comprises the following steps: according to the conductive silver paste described in any one of required form printing claim 1-6 on substrate, then carry out plasma treatment, namely obtain described conducting wire.
10. preparation method according to claim 9, is characterized in that, the gas medium that described plasma treatment adopts is selected from least one in argon gas, oxygen, nitrogen, air.
11. preparation methods according to claim 9, is characterized in that, the condition of described plasma treatment comprises: pressure is 50-150KPa; Power is 150-350W; Time is 20-80 second.
12. 1 kinds of conducting wires, is characterized in that, described conducting wire is prepared by preparation method according to claim 9.
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| CN106098826A (en) * | 2016-08-05 | 2016-11-09 | 星慧照明工程集团有限公司 | A kind of high-efficiency solar silion cell plate and preparation method, battery component |
| CN106224877A (en) * | 2016-08-05 | 2016-12-14 | 星慧照明工程集团有限公司 | A kind of wind-solar hybrid intelligent LED street lamp and preparation method |
| CN107301887A (en) * | 2017-05-14 | 2017-10-27 | 成都才盖科技有限公司 | A kind of silver-colored conductive silver paste composition of the novel solar battery back of the body and preparation method |
| CN108133767A (en) * | 2017-12-18 | 2018-06-08 | 深圳市思迈科新材料有限公司 | Weatherability glass touch screen conductive silver paste and preparation method thereof |
| CN109215832A (en) * | 2018-09-18 | 2019-01-15 | 江西华莲欣科技有限公司 | A kind of printing conductive silver paste and preparation method thereof |
| CN110172277A (en) * | 2019-06-14 | 2019-08-27 | 广东华祐新材料有限公司 | A kind of conductive material of low-resistance value |
| CN110172276A (en) * | 2019-06-14 | 2019-08-27 | 广东华祐新材料有限公司 | A kind of conductive material and its preparation process |
| CN111326849A (en) * | 2020-03-09 | 2020-06-23 | 广东四维新材料有限公司 | Method for preparing signal receiving/transmitting antenna of automatic driving automobile |
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| CN110172276A (en) * | 2019-06-14 | 2019-08-27 | 广东华祐新材料有限公司 | A kind of conductive material and its preparation process |
| CN111326849A (en) * | 2020-03-09 | 2020-06-23 | 广东四维新材料有限公司 | Method for preparing signal receiving/transmitting antenna of automatic driving automobile |
| CN111326849B (en) * | 2020-03-09 | 2021-07-06 | 广东四维新材料有限公司 | Method for preparing signal receiving/transmitting antenna of automatic driving automobile |
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Application publication date: 20160316 |