CN105482554B - Electrically conductive ink - Google Patents

Electrically conductive ink Download PDF

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Publication number
CN105482554B
CN105482554B CN201410522980.1A CN201410522980A CN105482554B CN 105482554 B CN105482554 B CN 105482554B CN 201410522980 A CN201410522980 A CN 201410522980A CN 105482554 B CN105482554 B CN 105482554B
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CN
China
Prior art keywords
electrically conductive
substrate
conductive ink
solvent
ink
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CN201410522980.1A
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Chinese (zh)
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CN105482554A (en
Inventor
林顺茂
沈志强
陈利伟
杨丹
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Star Precision Technology (Guangzhou) Co., Ltd.
Original Assignee
GUANGZHOU GUANGBAO MOBILE ELECTRONICS PARTS Co Ltd
Lite On Technology Corp
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Priority to CN201410522980.1A priority Critical patent/CN105482554B/en
Publication of CN105482554A publication Critical patent/CN105482554A/en
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Abstract

The embodiment of the present invention provides a kind of electrically conductive ink.The electrically conductive ink includes main body ink and substrate solvent.Main body ink accounts for the 60 to 95wt% of electrically conductive ink, and substrate solvent accounts for the 5 to 40wt% of electrically conductive ink.Main body ink further includes multiple conductive particles and bulk solvent, and conductive particle accounts for the 70 to 80wt% of main body ink, and bulk solvent accounts for the 20 to 30wt% of main body ink.In addition, substrate solvent is the solvent for dissolving substrate surface.

Description

Electrically conductive ink
Technical field
The present invention relates to a kind of electrically conductive inks, and in particular to a kind of for forming the conductive oil of conductive layer in substrate surface Ink.
Background technique
It is commonly in the side that the method for line layer is formed on substrate including the use of spraying, dispensing either screen painting at present Conductive material is formed on substrate by method, later using the method for sintering to form line layer on substrate.
During sintering, if the temperature used too it is low may result in line layer substrate surface adhesive force not It is good, and have the situation of disengaging, cause wiring board electric conductivity and reliability decrease.However, having if the temperature of sintering is too high It may result in line layer and substrate deformation, and then influence the quality of wiring board.
Summary of the invention
The embodiment of the present invention provides a kind of electrically conductive ink, this electrically conductive ink can promote conductive layer in the attachment of substrate surface Power.
The embodiment of the present invention provides a kind of electrically conductive ink, including main body ink and substrate solvent.Main body ink accounts for conductive oil The 60 to 95wt% of ink, and substrate solvent accounts for the 5 to 40wt% of electrically conductive ink.Main body ink further include multiple conductive particles and Bulk solvent, conductive particle accounts for the 70 to 80wt% of main body ink, and bulk solvent accounts for the 20 to 30wt% of main body ink.Separately Outside, substrate solvent is the solvent for dissolving substrate surface.
In conclusion the present invention provides a kind of electrically conductive ink, to form a conductive layer in substrate surface, electrically conductive ink packet Including main body ink and substrate solvent, substrate solvent enables main body ink to be embedded in substrate surface dissolving substrate surface, Conductive layer is able to ascend after sintering in the adhesive force of substrate surface.
Be further understood that feature and technology contents of the invention to be enabled, please refer to below in connection with it is of the invention specifically It is bright, but these explanations are intended merely to illustrate the present invention, rather than make any limitation to interest field of the invention.
Specific embodiment
The present invention provides a kind of electrically conductive ink, and to form conductive layer in substrate surface, this electrically conductive ink includes bulk oil Ink, substrate solvent and higher boiling ink.Main body ink accounts for the 60 to 95wt% of electrically conductive ink, and substrate solvent accounts for the 5 of electrically conductive ink To 40wt%, higher boiling ink then accounts for the 5 to 30wt% of electrically conductive ink.In addition, main body ink further includes conductive particle and main body Solvent, conductive particle accounts for the 70 to 80wt% of main body ink, and bulk solvent then accounts for the 20 to 30wt% of main body ink.
In the present embodiment, conductive particle is Argent grain, and so invention is not limited thereto, in other embodiments, conductive Particle can be for example copper particle either other conductive materials.In addition, bulk solvent is selected from by polyalcohol and polyol ethers institute At least one of group of composition, substrate solvent are selected from the group as composed by hydro carbons, esters, phenols, amides and ketone At least one of.High boiling solvent is the solvent that boiling point is greater than 180 DEG C, can be selected from the group as composed by polyalcohol and polyol ethers At least one of group.It should be noted that in the present embodiment, bulk solvent and high boiling solvent select property similar at Point, at the chance analyzed when being used with reducing.
In actual use, user can first mix electrically conductive ink according to aforementioned proportion, and according to actual track Design, in a manner of screen painting, dispensing or spraying, is formed in substrate surface for electrically conductive ink.And then it is coated with leading The substrate of electric ink is sent into oven and is sintered, and after the completion of sintering, conductive layer be will form in substrate surface, to prepare circuit base Plate.It should be noted that in the present embodiment, the material of substrate may include substantially aliphatic hydrocarbon polymer resin, polyamide, polyester Or polyacrylate.
Specifically, since the material of substrate is largely high molecular polymer, when electrically conductive ink is formed in substrate surface When, the substrate solvent in electrically conductive ink can dissolve substrate surface so that between the macromolecular chain of substrate surface, free volume, Away from increase, therefore the main body ink in electrically conductive ink is easier insertion substrate surface.After oversintering, conductive layer is in substrate table Therefore the adhesive force in face can increase.
In addition to this, the high boiling solvent in electrically conductive ink is mainly the evaporation rate to reduce substrate solvent.At this In embodiment, substrate solvent selects the lower ingredient of boiling point, so that electrically conductive ink can permeate and be diffused into substrate surface.So And low-boiling electrically conductive ink evaporation rate is very fast, and in actual use, if the time of applying conductive ink is longer, conductive oil After the completion of ink may solidify before coating is completed, and then the uniformity for influencing electrically conductive ink coating is either sintered, lead Electric layer is in the adhesive force of substrate.
In addition, the embodiment of the present invention is that electrically conductive ink is formed in substrate table in the way of printing, dispensing or spraying etc. Face.In general, the output device of printing, dispensing or spraying, e.g. spray head are open smaller, electrically conductive ink may also can Because of the too fast volatilization of bulk solvent and substrate solvent, and solidifies and be blocked in the output device of printing, dispensing or spraying, shadow Ring the efficiency of coating.For this purpose, addition high boiling solvent can reduce the evaporation rate of substrate solvent, and then reduces electrically conductive ink and exist During coating, the chance that solidifies or block.
It is noted that the amount of addition is controlled since high boiling solvent less easily volatilizees, such as The content for being high boiling solvent can be less than substrate solvent, and electrically conductive ink is difficult to cured situation when reducing sintering.In fact, high Boiling point solvent selective according to actual needs can make an addition in electrically conductive ink, in other embodiments, can not also add High boiling solvent.And when electrically conductive ink does not add high boiling solvent, the preferred proportion of substrate solvent is to account for electrically conductive ink 8 to 25wt%.
It should be noted that being about 10 by the coating duration that electrically conductive ink is coated on substrate surface in the present embodiment Minute.The temperature of sintering is about between 80 to 250 DEG C, and preferably sintering temperature is between 100 to 200 DEG C.In addition, preferably Sintering temperature be 1 hour.
In addition, corresponding substrate solvent can be used for different substrate materials, to realize preferable solute effect. For example, when the material of the substrate is substantially aliphatic hydrocarbon polymer resin, substrate solvent is selected from by aromatic hydrocarbon, halogenated hydrocarbons And at least one of group composed by esters.When the material of substrate is polyamide, substrate solvent is selected from by phenols and acyl At least one of group composed by amine.When the material of substrate be polyester when, substrate solvent be selected from by phenols, halogenated hydrocarbons and At least one of group composed by amides.In addition, substrate solvent is choosing when the material of the substrate is polyacrylate At least one of group composed by free aromatic hydrocarbon, ketone, esters and halogenated hydrocarbons.Substrate material and corresponding substrate solvent Table 1 listed below:
Table 1
Substrate material Substrate solvent
Substantially aliphatic hydrocarbon polymer resin Aromatic hydrocarbon, halogenated hydrocarbons, esters
Polyamide Phenols, amides
Polyester Phenols, halogenated hydrocarbons, amides
Polyacrylate Aromatic hydrocarbon, ketone, esters, halogenated hydrocarbons
Next, being configured to electrically conductive ink using above-mentioned substrate solvent, main body ink and high boiling solvent for introducing, and apply Cloth is on substrate, to introduce the composition ratio and experiment flow of various embodiments of the present invention.
Embodiment 1
In the electrically conductive ink of embodiment 1, conductive particle selects Argent grain, and bulk solvent selects propylene glycol monomethyl ether, substrate Solvent selects dimethylbenzene, and high boiling solvent selects diethylene glycol dimethyl ether.In addition, Argent grain accounts for the 75wt% of main body ink, account for The 66wt% of electrically conductive ink.Substrate solvent accounts for the 15wt% of electrically conductive ink, and high boiling solvent then accounts for electrically conductive ink 10wt%.
By mentioned component be uniformly mixed be prepared into electrically conductive ink after, can using print in the way of, electrically conductive ink be coated with On the polycarbonate substrate containing 50wt% glass fibre.Coating duration is about 10 minutes, and sintering time is 1 hour, sintering Temperature is 120 DEG C.After the completion of sintering, electrically conductive ink can form conductive layer in substrate surface, to prepare circuit substrate.
Embodiment 2
In the electrically conductive ink of embodiment 2, conductive particle selects Argent grain, and bulk solvent selects propylene glycol monomethyl ether, substrate Solvent selects dimethylformamide, and high boiling solvent selects ethylene glycol.In addition, Argent grain accounts for the 75wt% of main body ink, account for The 66wt% of electrically conductive ink.Substrate solvent accounts for the 13wt% of electrically conductive ink, and high boiling solvent then accounts for electrically conductive ink 12wt%.
By mentioned component be uniformly mixed be prepared into electrically conductive ink after, can using print in the way of, electrically conductive ink be coated with On polyamide substrate.Coating duration is about 10 minutes, and sintering time is 1 hour, and sintering temperature is 190 DEG C.It has been sintered Cheng Hou, electrically conductive ink can form conductive layer in substrate surface, to prepare circuit substrate.
Embodiment 3
In the electrically conductive ink of embodiment 3, conductive particle selects Argent grain, and bulk solvent selects propylene glycol monomethyl ether, substrate Solvent selects hexone, and high boiling solvent selects ethylene glycol.In addition, Argent grain accounts for the 75wt% of main body ink, Account for the 66wt% of electrically conductive ink.Substrate solvent accounts for the 17wt% of electrically conductive ink, and high boiling solvent then accounts for electrically conductive ink 13wt%.
By mentioned component be uniformly mixed be prepared into electrically conductive ink after, can using print in the way of, electrically conductive ink be coated with On polymethyl methacrylate base material.Coating duration is about 10 minutes, and sintering time is 1 hour, and sintering temperature is 120 DEG C. After the completion of sintering, electrically conductive ink can form conductive layer in substrate surface, to prepare circuit substrate.
Comparative example 1
In the electrically conductive ink of comparative example 1, conductive particle selects nano-Ag particles, and nano-Ag particles can be by polyvinyl pyrrole Alkanone resin is coated, and to avoid nano silver reunion, and solvent selects propylene glycol monomethyl ether.In addition, nano-Ag particles account for conduction The 20 to 40wt% of ink, polyvinyl pyrrolidone resin content is the 1 to 5% of nano silver, solvent account for the 60 of electrically conductive ink to 80wt%.
By mentioned component be uniformly mixed be prepared into electrically conductive ink after, can using print in the way of, electrically conductive ink be coated with On polycarbonate substrate.Coating duration is about 10 minutes, and sintering time is 1 hour, and sintering temperature is 200 DEG C.It needs to illustrate , the sintering temperature of comparative example must just be able to achieve preferable adhesive force up to 200 DEG C.After the completion of sintering, electrically conductive ink can be in base Material surface forms conductive layer, to prepare circuit substrate.It should be noted that each ingredient is with ratio included by comparative example 1 For the conducting ink formulation that general industry is common.
And circuit substrate prepared by above-described embodiment 1 to 3 and comparative example 1 will carry out temperature shock, temperature and humidity circulation And the test of adhesive force, to carry out reliability test to the conductive layer on substrate.It should be noted that the embodiment of the present invention institute into Capable reliability test is according to standard " ink reliability test specification " (Reliability test spec for ink Trace), tested.Next, the test mode that temperature shock, temperature and humidity circulation and adhesive force will be introduced.
The step of temperature shock test (Temp Shock Test), includes, and above-described embodiment 1 to 3 and comparative example 1 is made The standby circuit substrate come out is first set in 85 DEG C of insulating box 2 hours, then circuit substrate is shifted to 2 in -40 DEG C of insulating box Hour.The time replaced every time is less than or equal to 3 minutes, and is repeated 5 times, time about 20 hours altogether when always surveying.After the completion of test, Whether the surface of observation circuit substrate has defect, color change, removing, deformation or the situation of rupture to generate.
The step of temperature and humidity loop test (Damp Heat Test), includes, firstly, by above-described embodiment 1 to 3 and comparison The prepared circuit substrate come out of example 1 is placed in the climatic chamber that temperature is 25 DEG C, humidity is 93%.Later, by constant temperature The temperature of constant humidity cabinet rises to 55 DEG C in 3 hours, and maintains 55 DEG C of totally 9 hours.Then, by the temperature of climatic chamber 25 DEG C are dropped in 2 hours, and maintains 25 DEG C of totally 16 hours, to complete the circulation of 16 hour.
The circulation of 16 hours carries out 14 circulations in total, wherein can drop humidity when proceeding to the 9th circulation To 50%, and observe whether circuitry testing substrate surface has defect, color change, removing, deformation or the situation of rupture to generate.It Afterwards, then by humidity it adjusts to 93%, to carry out remaining 5 circulations.
In addition, the embodiment of the present invention can also carry out temperature to the circuit substrate come out prepared by embodiment 1 to 3 and comparative example 1 Degree impact and the test (Temperature Shock+Adhesion Test) of attaching power and temperature and humidity circulation and attaching power test (Damp Heat+Adhesion Test).In the test of temperature shock and attaching power, the electricity of embodiment 1 to 3 and comparative example 1 Base board can first carry out above-mentioned temperature shock test.The circuit substrate for having carried out temperature test is placed 2 hours again later, then into The cutting of hundred lattice of row, and observe whether cut edge has defect, removing or the situation of rupture to generate.
Above-mentioned temperature shock and the test for attaching power are using five grades, to define cut edge defect, removing or break The situation split." 0 " grade represents that cut edge is completely smooth, and the situation that do not remove.Grade " 1 " represents the intersection in cutting Place has the conductive layer of flakelet to remove, and the part for removing defect accounts for the 5% of cutting region.Grade " 2 " represent conductive layer along At cut edge, or in the infall of cutting have the situation of removing, and the part for removing defect account for the 5% of cutting region to 15%.Grade " 3 " represents conductive layer along the removing for having part or full wafer at cut edge, and other blocks of cutting region There is the removing of part, the part for removing defect accounts for the 15% to 35% of cutting region.Grade " 4 " represents conductive layer along cutting edge There is large stretch of removing at edge, and other blocks of cutting region also have large stretch of removing, the part for removing defect accounts for cutting region 35% to 65%.The part that grade " 5 " then represents conductive layer removing defect accounts for 65% more than cutting region.
And recycle and attach in temperature and humidity in power test, the circuit substrate of embodiment 1 to 3 and comparative example 1 can be carried out first State temperature and humidity loop test.The circuit substrate for having carried out temperature and humidity loop test is placed 2 hours again later, then carries out hundred lattice and cuts It cuts, and observes whether cut edge has defect, removing or the situation of rupture to generate.It recycles and attaches in example test in temperature and humidity, Be also it is identical as above-mentioned temperature shock and the attaching test of power, classified using five grades, exhaustive division mode is herein not It repeats more.And the circuit substrate of embodiment 1 to 3 and comparative example 1, after above-mentioned reliability test, test result is listed in the table below In 2:
Table 2
From the content of table 2 it is found that the circuit substrate of 1-3 of the embodiment of the present invention is followed in temperature shock test either temperature and humidity Before and after ring test, in appearance all without significant change.That is, the electrically-conductive backing plate surface of embodiment 1-3, there is no obvious The situations such as defect, color change, removing, deformation or rupture.However the circuit substrate of comparative example 1 is whether surveyed in temperature shock Before and after examination either temperature and humidity loop test, conductive layer has the phenomenon that removing or gauffer.
In addition, the circuit substrate of 1-3 of the embodiment of the present invention is in temperature shock and attaches power test either temperature and humidity circulation And after attaching power test, circuit substrate cut edge is relatively smooth, and the situation almost without conductive layer removing occurs, conductive layer The part for removing defect is less than the 5% of cutting region.However, comparative example 1 is either warm and humid in temperature shock and attaching power test After degree circulation and attaching power test, at circuit board cut edge and other blocks of cutting region all have large stretch of conductive layer stripping From the area for removing defect is greater than the 65% of cutting region.From the result of above-mentioned reliability test it is found that compared to comparative example 1, The conductive layer of 1-3 of the embodiment of the present invention has preferable reliability test result.That is, utilizing electrically conductive ink of the invention Prepared conductive layer has preferable adhesive force and reliability for circuit substrate.
In conclusion the present invention provides a kind of electrically conductive ink, to form a conductive layer in substrate surface, electrically conductive ink packet Main body ink, substrate solvent and high boiling solvent are included, substrate solvent enables main body ink to be embedded in dissolve substrate surface Substrate surface is able to ascend conductive layer in the adhesive force of substrate surface after sintering.In addition, high boiling solvent can reduce substrate The evaporation rate of solvent promotes the quality that electrically conductive ink is coated on substrate surface.
The above description is only an embodiment of the present invention, the scope of patent protection being not intended to limit the invention.Any Field technical staff, without departing from the spirit and scope of the invention, the equivalence replacement of made variation and retouching, is still this hair In bright scope of patent protection.

Claims (11)

1. a kind of electrically conductive ink, to form conductive layer in a substrate surface, which is characterized in that the electrically conductive ink includes:
One main body ink, accounts for the 60 to 90wt% of the electrically conductive ink, and the main body ink includes:
Multiple conductive particles account for the 70 to 80wt% of the main body ink;And
One bulk solvent accounts for the 20 to 30wt% of the main body ink;
One substrate solvent accounts for the 5 to 35wt% of the electrically conductive ink, and the substrate solvent is the molten of the dissolution substrate surface Agent;And
One high boiling solvent accounts for the 5 to 30wt% of the electrically conductive ink, and the content of the high boiling solvent is less than the substrate The content of solvent, the boiling point of the high boiling solvent is between 180 to 220 DEG C.
2. electrically conductive ink as described in claim 1, wherein the bulk solvent is selected from by polyalcohol and polyol ethers institute group At at least one of group, and the high boiling solvent be in the group as composed by polyalcohol and polyol ethers at least It is a kind of.
3. electrically conductive ink as described in claim 1, wherein the substrate solvent is selected from by hydro carbons, esters, phenols, amides And at least one of group composed by ketone.
4. electrically conductive ink as described in claim 1, wherein the substrate solvent accounts for the 10 to 20wt% of the electrically conductive ink.
5. electrically conductive ink as described in claim 1, wherein the substrate solvent accounts for the 8 to 25wt% of the electrically conductive ink.
6. electrically conductive ink as described in claim 1, wherein the high boiling solvent accounts for the 10 to 20wt% of the electrically conductive ink.
7. electrically conductive ink as claimed in claim 3, wherein the material of the substrate includes: substantially aliphatic hydrocarbon polymer resin, gathers Amide, polyester or polyacrylate.
8. electrically conductive ink as claimed in claim 7, wherein when the material of the substrate is substantially aliphatic hydrocarbon polymer resin, institute Stating substrate solvent is selected from least one of group as composed by aromatic hydrocarbon, halogenated hydrocarbons and esters.
9. electrically conductive ink as claimed in claim 7, wherein the substrate solvent is when the material of the substrate is polyamide Selected from least one of group as composed by phenols and amides.
10. electrically conductive ink as claimed in claim 7, wherein the substrate solvent is when the material of the substrate is polyester Selected from least one of group as composed by phenols, halogenated hydrocarbons and amides.
11. electrically conductive ink as claimed in claim 7, wherein when the material of the substrate is polyacrylate, the substrate Solvent is selected from least one of group as composed by aromatic hydrocarbon, ketone, esters and halogenated hydrocarbons.
CN201410522980.1A 2014-09-30 2014-09-30 Electrically conductive ink Expired - Fee Related CN105482554B (en)

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Publication number Priority date Publication date Assignee Title
KR20200140359A (en) * 2018-05-08 2020-12-15 아그파-게바에르트 엔.브이. Conductive ink

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102719137A (en) * 2012-05-31 2012-10-10 杭州浙大海维特化工科技有限公司 Special jet ink for PVC (polyvinyl chloride) cable
CN103952034A (en) * 2014-05-19 2014-07-30 北京印刷学院 Resin-free nano-silver electrically conductive printing ink as well as preparation method and applications thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102719137A (en) * 2012-05-31 2012-10-10 杭州浙大海维特化工科技有限公司 Special jet ink for PVC (polyvinyl chloride) cable
CN103952034A (en) * 2014-05-19 2014-07-30 北京印刷学院 Resin-free nano-silver electrically conductive printing ink as well as preparation method and applications thereof

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