CN116574413B - Preparation method of conductive ink - Google Patents
Preparation method of conductive ink Download PDFInfo
- Publication number
- CN116574413B CN116574413B CN202310634121.0A CN202310634121A CN116574413B CN 116574413 B CN116574413 B CN 116574413B CN 202310634121 A CN202310634121 A CN 202310634121A CN 116574413 B CN116574413 B CN 116574413B
- Authority
- CN
- China
- Prior art keywords
- polyvinyl alcohol
- stirring
- conductive
- parts
- conductive ink
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 81
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 81
- 239000000835 fiber Substances 0.000 claims abstract description 60
- 239000002131 composite material Substances 0.000 claims abstract description 41
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 21
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 21
- 239000000945 filler Substances 0.000 claims abstract description 19
- 239000000049 pigment Substances 0.000 claims abstract description 19
- 239000004020 conductor Substances 0.000 claims abstract description 18
- 239000000839 emulsion Substances 0.000 claims abstract description 16
- 239000004814 polyurethane Substances 0.000 claims abstract description 16
- 229920002635 polyurethane Polymers 0.000 claims abstract description 16
- 239000004094 surface-active agent Substances 0.000 claims abstract description 16
- IUYOGGFTLHZHEG-UHFFFAOYSA-N copper titanium Chemical compound [Ti].[Cu] IUYOGGFTLHZHEG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims description 81
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 47
- 238000010438 heat treatment Methods 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 28
- 239000011259 mixed solution Substances 0.000 claims description 24
- 239000001856 Ethyl cellulose Substances 0.000 claims description 22
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 22
- 229920001249 ethyl cellulose Polymers 0.000 claims description 22
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 22
- 238000009987 spinning Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 12
- 230000008961 swelling Effects 0.000 claims description 11
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 8
- 239000004917 carbon fiber Substances 0.000 claims description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 6
- 238000006136 alcoholysis reaction Methods 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 240000002853 Nelumbo nucifera Species 0.000 claims description 2
- 235000006508 Nelumbo nucifera Nutrition 0.000 claims description 2
- 235000006510 Nelumbo pentapetala Nutrition 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 4
- 239000011231 conductive filler Substances 0.000 abstract description 3
- 230000005855 radiation Effects 0.000 abstract description 3
- 239000002245 particle Substances 0.000 description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 24
- 239000000843 powder Substances 0.000 description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 16
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 15
- 239000000463 material Substances 0.000 description 15
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 12
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 12
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 12
- 239000012153 distilled water Substances 0.000 description 11
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 11
- 238000001694 spray drying Methods 0.000 description 11
- 229910021529 ammonia Inorganic materials 0.000 description 8
- 239000012298 atmosphere Substances 0.000 description 8
- 238000006722 reduction reaction Methods 0.000 description 8
- 238000009210 therapy by ultrasound Methods 0.000 description 8
- 238000010926 purge Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- SLZVKEARWFTMOZ-UHFFFAOYSA-N copper;oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[Ti+4].[Cu+2] SLZVKEARWFTMOZ-UHFFFAOYSA-N 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 4
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 4
- 229940112669 cuprous oxide Drugs 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- KELHQGOVULCJSG-UHFFFAOYSA-N n,n-dimethyl-1-(5-methylfuran-2-yl)ethane-1,2-diamine Chemical compound CN(C)C(CN)C1=CC=C(C)O1 KELHQGOVULCJSG-UHFFFAOYSA-N 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- -1 has powder particles Chemical class 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 description 1
- 239000005750 Copper hydroxide Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 229910001956 copper hydroxide Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
The invention belongs to the technical field of printing ink, and particularly relates to a preparation method of conductive printing ink, wherein the conductive printing ink comprises the following components in parts by mass: 40-50 parts of aqueous polyurethane emulsion, 5-8 parts of aqueous pigment, 10-30 parts of conductive material, 5-10 parts of filler and 2-5 parts of surfactant; the conductive material is formed by combining polyvinyl alcohol fibers and composite metal oxides, and a specific preparation method is provided. The invention solves the defects of the prior conductive ink, utilizes the polyvinyl alcohol fiber and the copper-titanium composite oxide as conductive fillers to form a stable fiber net-shaped conductive system and an origin radiation system, and improves the overall conductive performance.
Description
Technical Field
The invention belongs to the technical field of printing ink, and particularly relates to a preparation method of conductive printing ink.
Background
With the rapid development of the electronic industry and the improvement of the human life level, conductive ink is used as a functional material in the industries of electronics, machinery, light industry, metallurgy and the like, can endow the conductive ink with antistatic performance, electromagnetic shielding performance and the like, and has attracted wide attention. At present, the conductive powder materials in the common conductive ink are mainly metal powder materials, carbon powder materials and metal oxide conductive powder materials. Although the metal powder materials have strong conductivity, the metal powder materials have the defects of high price, easy oxidation and poor corrosion resistance, and the metal conductive powder materials have high density, easy precipitation and agglomeration and poor dispersibility in a matrix. Although the carbon conductive powder material has better conductivity and stability, the carbon conductive powder material is difficult to uniformly disperse, has weak high-temperature oxidation resistance, and particularly the product is easy to blacken and is not accepted. The metal oxide conductive powder material is paid attention to by high melting point, strong oxidation resistance and moderate price. However, although the metal oxide has a certain conductive system, the metal oxide mainly has powder particles, and needs a large content to form a stable conductive system, and as the content of the metal oxide increases, the adhesiveness of the ink decreases, and it is difficult to satisfy the use requirements.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of conductive ink, which solves the defects of the conventional conductive ink, and utilizes polyvinyl alcohol fibers and copper-titanium composite oxide as conductive fillers to form a stable fiber net-shaped conductive system and an origin radiation system, thereby improving the overall conductive performance.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of conductive ink comprises the following steps of:
40-50 parts of aqueous polyurethane emulsion, 5-8 parts of aqueous pigment, 10-30 parts of conductive material, 5-10 parts of filler and 2-5 parts of surfactant.
The solid content of the aqueous polyurethane emulsion is 30-40%.
The water-based pigment adopts one of permanent red F2R, permanent red F4R, pigment red 22 and firm red lotus.
The conductive material is formed by combining polyvinyl alcohol fibers and composite metal oxides, the mass ratio of the polyvinyl alcohol fibers to the composite metal oxides is 1:1-2, the polyvinyl alcohol fibers are polyvinyl alcohol fibers containing conjugated double bonds, and the composite metal oxides are copper-titanium composite oxides. Further, the polyvinyl alcohol fiber is a polyvinyl alcohol fiber subjected to heat treatment at a temperature of more than 250 ℃, and active groups contained in the polyvinyl alcohol fiber can be condensed to form a conjugated double bond structure in the high-temperature treatment process, so that excellent conductivity is shown. The polyvinyl alcohol with a fiber structure can be inserted in the ink in a solid state, and an organic conductive network system is achieved by utilizing the fiber insertion structure of the polyvinyl alcohol, and the preparation method of the polyvinyl alcohol fiber comprises the following steps: a1, adding polyvinyl alcohol into water, stirring at uniform speed, heating and stirring to form a swelling liquid, wherein the mass of the polyvinyl alcohol and the mass of the water are 1:9-10, wherein the stirring speed of uniform stirring is 300-500r/min, the temperature of heating and stirring is 70-80 ℃, and the stirring speed is 600-800r/min; the polymerization degree of the polyvinyl alcohol is 1700, and the alcoholysis degree is 88; the method comprises the steps of accelerating absorption of the polyvinyl alcohol to distilled water by using a uniform-speed stirring mode, increasing the flow rate of the distilled water in rapid stirring, accelerating absorption and swelling speed of the polyvinyl alcohol, and homogenizing the polyvinyl alcohol aqueous solution in heating stirring; a2, adding ethyl cellulose into ethanol, uniformly stirring to form a solution, adding the solution into a swelling solution, and homogenizing to obtain a mixed solution, wherein the concentration of the ethyl cellulose in the ethanol is 100-300g/L, the uniform stirring speed is 300-500r/min, the mass ratio of the ethyl cellulose to the polyvinyl alcohol in the mixed solution is 1:10-15, and the homogenizing stirring speed is 1000-2000r/min; the ethyl cellulose is completely dispersed by using ethanol as a dissolution solvent, and simultaneously the ethyl cellulose is carried into the polyvinyl alcohol by using ethanol as a solvent expansion agent of water, and the ethyl cellulose and the polyvinyl alcohol are completely homogenized and mixed by homogenizing; a3, spinning the mixed solution as a spinning solution to obtain composite polyvinyl alcohol fibers, wherein the spinning speed is 20-50m/min, the spinning temperature is 120-130 ℃, in the spinning process, the characteristic that the boiling point of ethanol is lower than that of water is utilized, the ethyl cellulose is matched with the insolubility of the ethyl cellulose in water, the ethyl cellulose is separated out to be used as a crystal nucleus seed structure, and the polyvinyl alcohol is fibrillated along with the evaporation process of distilled water, so as to obtain the composite polyvinyl alcohol fibers, and a4, the composite polyvinyl alcohol fibers are subjected to heating treatment to obtain the polyvinyl alcohol fibers with a porous structure, wherein the heating temperature is 255-260 ℃; in the step, the ethyl cellulose in the composite polyvinyl alcohol forms decomposition treatment at the temperature, so that a pore structure is formed on the polyvinyl alcohol fiber, meanwhile, the polyvinyl alcohol becomes a polymer containing conjugated double bonds at the temperature of more than 250 ℃, the material self maintains a porous structure, the porous structure is favorable for fixing fillers and other resins, the physical position is fixed on the basis of chemical connection, meanwhile, the porous structure is positioned on the fiber, and the fiber can form a stable penetrating structure in the whole ink forming state, so as to form a conductive network structure of an organic system. The preparation method of the copper titanium oxide comprises the following steps: b1, adding high-substituted hydroxypropyl cellulose into ethanol, stirring uniformly to form a dispersion solution, sequentially adding copper chloride and n-butyl titanate, continuously stirring and dissolving completely to obtain a mixed solution, and spray-drying to obtain mixed fine powder, wherein the concentration of the high-substituted hydroxypropyl cellulose in the ethanol is 20-40g/L, the mass ratio of the copper chloride to the n-butyl titanate is 2:1-2, the concentration of the copper chloride in the ethanol is 50-100g/L, the spray speed of spray-drying is 10-20mL/min, and the drying temperature is 80-90 ℃; the method comprises the steps of using ethanol as a solvent, forming mixed dissolution of high-substituted hydroxypropyl cellulose, copper chloride and n-butyl titanate, dispersing solute in a spray drying process to form particles, and simultaneously taking high-substituted hydroxypropyl as an adhesive in each particle and simultaneously containing copper chloride and n-butyl titanate; b2, placing the mixed fine powder into a reaction kettle, standing for 2-3h, then heating for 30-50min, and sweeping to obtain prefabricated particles, wherein the standing atmosphere is a mixed atmosphere of nitrogen, water vapor and ammonia, the volume ratio of the nitrogen, the water vapor and the ammonia is 10-15:2:2, the temperature is 10-20 ℃, and the temperature of the heating is 100-120 ℃; the purging adopts nitrogen at 110 ℃, and the step utilizes an in-situ standing mode to convert copper chloride and n-butyl titanate into titanic acid and copper hydroxide by matching with an ammonia water system formed by water absorption of high-substituted hydroxypropyl cellulose, so that in-situ conversion of copper-titanium oxide is realized; b3, putting the prefabricated particles into distilled water, performing low-temperature ultrasonic treatment, and filtering to obtain porous particles, wherein the mass ratio of the prefabricated particles to the distilled water is 1:10-15, the ultrasonic frequency of the low-temperature ultrasonic treatment is 60-80kHz, and the temperature is 5-10 ℃; b4, carrying out a reduction reaction on the porous particles to obtain copper-titanium composite oxide with the surface containing titanium monoxide and cuprous oxide, wherein the reduction reaction adopts hydrogen, the pressure is 0.2-0.4MPa, and the temperature is 160-180 ℃; the process utilizes copper salt and organic titanium to form stable solution, utilizes the adhesiveness and dispersibility of high-substituted hydroxypropyl cellulose to form homogenized dispersion, forms particles in a spray drying mode, forms the conversion of a copper source and a titanium source in an in-situ hydrolysis mode, reduces copper titanium oxide on the surface through hydrogen, and improves the surface conductivity; in the process, the structure of the high-substituted hydroxypropyl cellulose is not damaged, the recycling can be realized in a spray drying mode, the effect of reducing the cost is achieved, and the residual recycling of copper and titanium can also be realized.
The filler adopts conductive carbon fiber, the material is a high-conductivity material, has excellent comprehensive performance, has incomparable advantages of other materials, has the characteristics of corrosion resistance, wear resistance, high temperature resistance, high strength, light weight and the like besides high conductivity, and is very widely applied. The filler is put into the printing ink, and the conductive carbon fiber belongs to a fiber structure, has certain rigidity and can form an interpenetration fixing effect.
The surfactant is one of BYK-151, BYK-180, BYK-181 and BYK-190.
The preparation method of the conductive ink comprises the following steps:
adding a surfactant and a water-based pigment into the water-based polyurethane emulsion, stirring at a constant temperature of 30-40 ℃ at a stirring speed of 300-500r/min to obtain a prefabricated mixed solution, sequentially adding a conductive material and a filler, and stirring and dispersing for 20-30min to obtain conductive ink; the stirring speed of stirring and dispersing is 700-900r/min.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the defects of the prior conductive ink, utilizes the polyvinyl alcohol fiber and the copper-titanium composite oxide as conductive fillers to form a stable fiber net-shaped conductive system and an origin radiation system, and improves the overall conductive performance.
2. The conductive carbon fiber is used as a filler, has conductive performance, can form a conductive network structure with a conductive material, and ensures that the conductive performance is radiated into the whole ink system.
3. The invention adopts the porous structure polyvinyl alcohol, not only can form a physical curing structure and a penetrating connection structure with the conductive carbon fiber, but also can fix the copper-titanium composite oxide, fill the pores and realize the effective combination of the fiber and the particles.
Detailed Description
The invention is described in detail with reference to examples, but without any limitation to the claims of the invention.
Example 1
A preparation method of conductive ink comprises the following steps of:
40 parts of aqueous polyurethane emulsion, 5 parts of aqueous pigment, 10 parts of conductive material, 5 parts of filler and 2 parts of surfactant.
The solid content of the aqueous polyurethane emulsion is 30%.
The water-based pigment adopts permanent red F2R.
The conductive material is formed by combining polyvinyl alcohol fibers and composite metal oxide, the mass ratio of the polyvinyl alcohol fibers to the composite metal oxide is 1:1, the polyvinyl alcohol fibers are polyvinyl alcohol fibers containing conjugated double bonds, and the composite metal oxide is copper-titanium composite oxide. The preparation method of the polyvinyl alcohol fiber comprises the following steps: a1, adding polyvinyl alcohol into water, stirring at an average speed, and then heating and stirring to form a swelling solution, wherein the mass of the polyvinyl alcohol and the water is 1:9, the stirring speed of the average speed stirring is 300r/min, the temperature of the heating and stirring is 70 ℃, and the stirring speed is 600r/min; the polymerization degree of the polyvinyl alcohol is 1700, and the alcoholysis degree is 88; a2, adding ethyl cellulose into ethanol, uniformly stirring to form a solution, adding the solution into a swelling solution, and homogenizing to obtain a mixed solution, wherein the concentration of the ethyl cellulose in the ethanol is 100g/L, the uniform stirring speed is 300r/min, the mass ratio of the ethyl cellulose in the mixed solution to the polyvinyl alcohol is 1:10, and the stirring speed of the homogenizing is 1000r/min; and a3, spinning the mixed solution as a spinning solution to obtain the composite polyvinyl alcohol fiber, wherein the spinning speed is 20m/min, the spinning temperature is 120 ℃, and a4, heating the composite polyvinyl alcohol fiber to obtain the polyvinyl alcohol fiber with a porous structure, and the heating temperature is 255 ℃. The preparation method of the copper titanium oxide comprises the following steps: b1, adding high-substituted hydroxypropyl cellulose into ethanol, stirring uniformly to form a dispersion solution, sequentially adding copper chloride and n-butyl titanate, continuously stirring and dissolving completely to obtain a mixed solution, and spray-drying to obtain mixed fine powder, wherein the concentration of the high-substituted hydroxypropyl cellulose in the ethanol is 20g/L, the mass ratio of the copper chloride to the n-butyl titanate is 2:1, the concentration of the copper chloride in the ethanol is 50g/L, the spray speed of spray-drying is 10mL/min, and the drying temperature is 80 ℃; b2, placing the mixed fine powder into a reaction kettle, standing for 2 hours, heating for 30 minutes, and purging to obtain prefabricated particles, wherein the standing atmosphere is a mixed atmosphere of nitrogen, water vapor and ammonia, the volume ratio of the nitrogen, the water vapor and the ammonia is 10:2:2, the temperature is 10 ℃, and the temperature of heating is 100 ℃; the purging adopts nitrogen at 110 ℃; b3, putting the prefabricated particles into distilled water, performing low-temperature ultrasonic treatment, and filtering to obtain porous particles, wherein the mass ratio of the prefabricated particles to the distilled water is 1:10, the ultrasonic frequency of the low-temperature ultrasonic treatment is 60kHz, and the temperature is 5 ℃; and b4, carrying out a reduction reaction on the porous particles to obtain the copper-titanium composite oxide with the surface containing titanium monoxide and cuprous oxide, wherein the reduction reaction adopts hydrogen, the pressure is 0.2MPa, and the temperature is 160 ℃.
The filler adopts conductive carbon fiber.
The surfactant adopts BYK-151.
The preparation method of the conductive ink comprises the following steps:
adding a surfactant and a water-based pigment into the water-based polyurethane emulsion, stirring at a constant temperature of 30 ℃ at a stirring speed of 300r/min to obtain a prefabricated mixed solution, sequentially adding a conductive material and a filler, and stirring and dispersing for 20min to obtain conductive ink; the stirring speed of the stirring dispersion is 700r/min.
The hardness prepared in this example was 2H, adhesion 5B, conductivity test: the conductive ink is coated on the silicon base plate and forms a loop with the power supply and the light emitting diode. After the power is turned on, the diode emits light to indicate that the conductive ink has good conductivity.
Example 2
A preparation method of conductive ink comprises the following steps of:
50 parts of aqueous polyurethane emulsion, 8 parts of aqueous pigment, 30 parts of conductive material, 10 parts of filler and 5 parts of surfactant.
The solid content of the aqueous polyurethane emulsion is 40%.
The water-based pigment adopts permanent red F4R.
The conductive material is formed by combining polyvinyl alcohol fibers and composite metal oxide, the mass ratio of the polyvinyl alcohol fibers to the composite metal oxide is 1:2, the polyvinyl alcohol fibers are polyvinyl alcohol fibers containing conjugated double bonds, and the composite metal oxide is copper-titanium composite oxide. The preparation method of the polyvinyl alcohol fiber comprises the following steps: a1, adding polyvinyl alcohol into water, stirring at an average speed, and then heating and stirring to form a swelling solution, wherein the mass of the polyvinyl alcohol and the water is 1:10, the stirring speed of the average speed stirring is 500r/min, the temperature of the heating and stirring is 80 ℃, and the stirring speed is 800r/min; the polymerization degree of the polyvinyl alcohol is 1700, and the alcoholysis degree is 88; a2, adding ethyl cellulose into ethanol, uniformly stirring to form a solution, adding the solution into a swelling solution, and homogenizing to obtain a mixed solution, wherein the concentration of the ethyl cellulose in the ethanol is 300g/L, the uniform stirring speed is 500r/min, the mass ratio of the ethyl cellulose in the mixed solution to the polyvinyl alcohol is 1:15, and the stirring speed of the homogenizing is 2000r/min; and a3, spinning the mixed solution as a spinning solution to obtain the composite polyvinyl alcohol fiber, wherein the spinning speed is 50m/min, the spinning temperature is 130 ℃, and a4, heating the composite polyvinyl alcohol fiber to obtain the polyvinyl alcohol fiber with a porous structure, and the heating temperature is 260 ℃. The preparation method of the copper titanium oxide comprises the following steps: b1, adding high-substituted hydroxypropyl cellulose into ethanol, stirring uniformly to form a dispersion solution, sequentially adding copper chloride and n-butyl titanate, continuously stirring and dissolving completely to obtain a mixed solution, and spray-drying to obtain mixed fine powder, wherein the concentration of the high-substituted hydroxypropyl cellulose in the ethanol is 40g/L, the mass ratio of the copper chloride to the n-butyl titanate is 2:2, the concentration of the copper chloride in the ethanol is 100g/L, the spray speed of spray-drying is 20mL/min, and the drying temperature is 90 ℃; b2, placing the mixed fine powder into a reaction kettle, standing for 3 hours, heating for 50 minutes, and purging to obtain prefabricated particles, wherein the standing atmosphere is a mixed atmosphere of nitrogen, water vapor and ammonia, the volume ratio of the nitrogen, the water vapor and the ammonia is 15:2:2, the temperature is 20 ℃, and the temperature of heating is 120 ℃; the purging adopts nitrogen at 110 ℃; b3, putting the prefabricated particles into distilled water, performing low-temperature ultrasonic treatment, and filtering to obtain porous particles, wherein the mass ratio of the prefabricated particles to the distilled water is 1:15, the ultrasonic frequency of the low-temperature ultrasonic treatment is 80kHz, and the temperature is 10 ℃; and b4, carrying out a reduction reaction on the porous particles to obtain the copper-titanium composite oxide with the surface containing titanium monoxide and cuprous oxide, wherein the reduction reaction adopts hydrogen, the pressure is 0.4MPa, and the temperature is 180 ℃.
The filler adopts conductive carbon fiber.
The surfactant adopts BYK-180.
The preparation method of the conductive ink comprises the following steps:
adding a surfactant and a water-based pigment into the water-based polyurethane emulsion, stirring at a constant temperature of 40 ℃ at a stirring speed of 500r/min to obtain a prefabricated mixed solution, sequentially adding a conductive material and a filler, and stirring and dispersing for 30min to obtain conductive ink; the stirring speed of stirring and dispersing is 900r/min.
The hardness prepared in this example was 2H, adhesion 5B, conductivity test: the conductive ink is coated on the silicon base plate and forms a loop with the power supply and the light emitting diode. After the power is turned on, the diode emits light to indicate that the conductive ink has good conductivity.
Example 3
A preparation method of conductive ink comprises the following steps of:
45 parts of aqueous polyurethane emulsion, 7 parts of aqueous pigment, 20 parts of conductive material, 8 parts of filler and 4 parts of surfactant.
The solid content of the aqueous polyurethane emulsion is 35%.
Pigment red 22 is used as the aqueous pigment.
The conductive material is formed by combining polyvinyl alcohol fibers and composite metal oxide, the mass ratio of the polyvinyl alcohol fibers to the composite metal oxide is 1:2, the polyvinyl alcohol fibers are polyvinyl alcohol fibers containing conjugated double bonds, and the composite metal oxide is copper-titanium composite oxide. The preparation method of the polyvinyl alcohol fiber comprises the following steps: a1, adding polyvinyl alcohol into water, stirring at an average speed, and then heating and stirring to form a swelling solution, wherein the mass of the polyvinyl alcohol and the water is 1:9, the stirring speed of the average speed stirring is 400r/min, the temperature of the heating and stirring is 75 ℃, and the stirring speed is 700r/min; the polymerization degree of the polyvinyl alcohol is 1700, and the alcoholysis degree is 88; a2, adding ethyl cellulose into ethanol, uniformly stirring to form a solution, adding the solution into a swelling solution, and homogenizing to obtain a mixed solution, wherein the concentration of the ethyl cellulose in the ethanol is 200g/L, the uniform stirring speed is 400r/min, the mass ratio of the ethyl cellulose in the mixed solution to the polyvinyl alcohol is 1:13, and the stirring speed of the homogenizing is 1500r/min; and a3, spinning the mixed solution as a spinning solution to obtain the composite polyvinyl alcohol fiber, wherein the spinning speed is 40m/min, the spinning temperature is 125 ℃, and a4, heating the composite polyvinyl alcohol fiber to obtain the polyvinyl alcohol fiber with a porous structure, and the heating temperature is 260 ℃. The preparation method of the copper titanium oxide comprises the following steps: b1, adding high-substituted hydroxypropyl cellulose into ethanol, stirring uniformly to form a dispersion solution, sequentially adding copper chloride and n-butyl titanate, continuously stirring and dissolving completely to obtain a mixed solution, and spray-drying to obtain mixed fine powder, wherein the concentration of the high-substituted hydroxypropyl cellulose in the ethanol is 30g/L, the mass ratio of the copper chloride to the n-butyl titanate is 2:1, the concentration of the copper chloride in the ethanol is 80g/L, the spray speed of spray-drying is 15mL/min, and the drying temperature is 85 ℃; b2, placing the mixed fine powder into a reaction kettle, standing for 3h, heating for 40min, and purging to obtain prefabricated particles, wherein the standing atmosphere is a mixed atmosphere of nitrogen, water vapor and ammonia, the volume ratio of the nitrogen, the water vapor and the ammonia is 13:2:2, the temperature is 15 ℃, and the temperature of heating is 110 ℃; the purging adopts nitrogen at 110 ℃; b3, putting the prefabricated particles into distilled water, performing low-temperature ultrasonic treatment, and filtering to obtain porous particles, wherein the mass ratio of the prefabricated particles to the distilled water is 1:13, the ultrasonic frequency of the low-temperature ultrasonic treatment is 70kHz, and the temperature is 8 ℃; and b4, carrying out a reduction reaction on the porous particles to obtain the copper-titanium composite oxide with the surface containing titanium monoxide and cuprous oxide, wherein the reduction reaction adopts hydrogen, the pressure is 0.3MPa, and the temperature is 170 ℃.
The filler adopts conductive carbon fiber.
The surfactant adopts BYK-190.
The preparation method of the conductive ink comprises the following steps:
adding a surfactant and a water-based pigment into the water-based polyurethane emulsion, stirring at a constant temperature of 35 ℃ at a stirring speed of 400r/min to obtain a prefabricated mixed solution, sequentially adding a conductive material and a filler, and stirring and dispersing for 25min to obtain conductive ink; the stirring speed of stirring and dispersing is 800r/min.
The hardness prepared in this example was 2H, adhesion 5B, conductivity test: the conductive ink is coated on the silicon base plate and forms a loop with the power supply and the light emitting diode. After the power is turned on, the diode emits light to indicate that the conductive ink has good conductivity.
It is to be understood that the foregoing detailed description of the invention is merely illustrative of the invention and is not limited to the embodiments of the invention. It will be understood by those of ordinary skill in the art that the present invention may be modified or substituted for elements thereof to achieve the same technical effects; as long as the use requirement is met, the invention is within the protection scope of the invention.
Claims (6)
1. A preparation method of conductive ink is characterized in that: the conductive ink comprises the following components in percentage by mass:
40-50 parts of aqueous polyurethane emulsion, 5-8 parts of aqueous pigment, 10-30 parts of conductive material, 5-10 parts of filler and 2-5 parts of surfactant; the conductive material is formed by combining polyvinyl alcohol fibers and composite metal oxides; the mass ratio of the polyvinyl alcohol fiber to the composite metal oxide is 1:1-2; the composite metal oxide is copper-titanium composite oxide;
the polyvinyl alcohol fiber is a polyvinyl alcohol fiber containing conjugated double bonds, and the polyvinyl alcohol fiber is a porous fiber; the preparation method of the polyvinyl alcohol fiber comprises the following steps: a1, adding polyvinyl alcohol into water, stirring at uniform speed, heating and stirring to form a swelling liquid, wherein the mass ratio of the polyvinyl alcohol to the water is 1:9-10, wherein the stirring speed of uniform stirring is 300-500r/min, the temperature of heating and stirring is 70-80 ℃, and the stirring speed is 600-800r/min; the polymerization degree of the polyvinyl alcohol is 1700, and the alcoholysis degree is 88; a2, adding ethyl cellulose into ethanol, uniformly stirring to form a solution, adding the solution into a swelling solution, and homogenizing to obtain a mixed solution, wherein the concentration of the ethyl cellulose in the ethanol is 100-300g/L, the uniform stirring speed is 300-500r/min, the mass ratio of the ethyl cellulose to the polyvinyl alcohol in the mixed solution is 1:10-15, and the homogenizing stirring speed is 1000-2000r/min; a3, spinning the mixed solution as a spinning solution to obtain the composite polyvinyl alcohol fiber, wherein the spinning speed is 20-50m/min, the spinning temperature is 120-130 ℃, and a4, heating the composite polyvinyl alcohol fiber to obtain the polyvinyl alcohol fiber with a porous structure, and the heating temperature is 255-260 ℃.
2. The method for preparing the conductive ink according to claim 1, wherein: the solid content of the aqueous polyurethane emulsion is 30-40%.
3. The method for preparing the conductive ink according to claim 1, wherein: the water-based pigment adopts one of permanent red F2R, permanent red F4R, pigment red 22 and firm red lotus.
4. The method for preparing the conductive ink according to claim 1, wherein: the filler adopts conductive carbon fiber.
5. The method for preparing the conductive ink according to claim 1, wherein: the surfactant is one of BYK-151, BYK-180, BYK-181 and BYK-190.
6. The method for preparing the conductive ink according to claim 1, wherein: the preparation method of the conductive ink comprises the following steps:
adding a surfactant and a water-based pigment into the water-based polyurethane emulsion, stirring at a constant temperature of 30-40 ℃ at a stirring speed of 300-500r/min to obtain a prefabricated mixed solution, sequentially adding a conductive material and a filler, and stirring and dispersing for 20-30min to obtain conductive ink; the stirring speed of stirring and dispersing is 700-900r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310634121.0A CN116574413B (en) | 2023-05-31 | 2023-05-31 | Preparation method of conductive ink |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310634121.0A CN116574413B (en) | 2023-05-31 | 2023-05-31 | Preparation method of conductive ink |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116574413A CN116574413A (en) | 2023-08-11 |
| CN116574413B true CN116574413B (en) | 2023-12-19 |
Family
ID=87534018
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310634121.0A Active CN116574413B (en) | 2023-05-31 | 2023-05-31 | Preparation method of conductive ink |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116574413B (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109234831A (en) * | 2018-07-23 | 2019-01-18 | 成都普美怡科技有限公司 | A kind of high-performance conductive vinal and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007119532A (en) * | 2005-10-25 | 2007-05-17 | Bussan Nanotech Research Institute Inc | Electroconductive coating material |
-
2023
- 2023-05-31 CN CN202310634121.0A patent/CN116574413B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109234831A (en) * | 2018-07-23 | 2019-01-18 | 成都普美怡科技有限公司 | A kind of high-performance conductive vinal and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王国建等.《功能高分子材料》.同济大学出版社,2010,(第1版),第128页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116574413A (en) | 2023-08-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105112894B (en) | It is a kind of that process for copper coating on surface is carried out to inorganic particulate by dopamine | |
| CN102837003B (en) | Nano silver particles with multilevel structure and preparation method thereof | |
| CN103849008A (en) | Hybridized particle, polymer-based composite material, their preparation methods and use of polymer-based composite material | |
| CN103102509B (en) | Core-shell type carbon microspheres and preparation method and application thereof | |
| CN105754515A (en) | Degradable recyclable epoxy electroconductive adhesive and preparation, degradation and recycling methods thereof | |
| CN104830247A (en) | Sheet/branch silver-coated copper powder and green halogen-free low-silver-content economical electrically conductive adhesive capable of replacing traditional electrically conductive adhesives with high silver contents | |
| CN101338040B (en) | Method for preparing porous conductive coating on plastic surface | |
| CN109423637A (en) | A kind of preparation method of high conductive material | |
| CN110540775A (en) | Graphene-based printing ink and preparation method thereof | |
| CN116574413B (en) | Preparation method of conductive ink | |
| CN110079266A (en) | A kind of nano silver is carbon nano-tube modified to prepare high heat-conductivity conducting glue and preparation method thereof | |
| CN112980356A (en) | Conductive adhesive, flexible circuit, flexible printed circuit board and flexible electronic element | |
| CN104152882B (en) | Preparation method of chemically-silvered active carbon as composite conductive filler | |
| CN115418880B (en) | Impregnating resin material for densification modification of carbon fiber paper, high-performance carbon fiber paper and preparation method thereof | |
| CN110707326B (en) | Water-system battery current collector, positive electrode, flexible battery, preparation and application thereof | |
| KR20080069897A (en) | Carbon nanofiber for fuel cell, nanocomposite comprising the same, method for making the composite, and fuel cell using the composite | |
| CN114956065B (en) | Amino modified graphene, preparation method thereof, amino modified graphene coating and application | |
| CN111392772A (en) | Preparation method of nano titanium dioxide material with uniform particle size distribution | |
| CN113600167B (en) | Preparation method of palladium-carbon catalyst based on ectoine | |
| CN114974663A (en) | Conductive agent and preparation method thereof, conductive paste and preparation method thereof, and solar cell | |
| CN108408749A (en) | A kind of preparation method of superfine alumina powder | |
| CN112871162B (en) | Preparation method of mesoporous ruthenium-aluminum composite catalyst | |
| CN101230148B (en) | Method for preparing chitosan-ionic liquid-copper nanoparticles composite membrane on electrode negative surface by one-step electic synthesis | |
| CN101980341A (en) | Nano zinc oxide conductive mica powder and preparation process thereof | |
| CN107858713B (en) | A kind of device and method preparing expanded graphite electro-coppering |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |