CN106229030B - A kind of electrically conductive composition, electrically conductive ink, conducting film, preparation method and application - Google Patents
A kind of electrically conductive composition, electrically conductive ink, conducting film, preparation method and application Download PDFInfo
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- CN106229030B CN106229030B CN201610534297.9A CN201610534297A CN106229030B CN 106229030 B CN106229030 B CN 106229030B CN 201610534297 A CN201610534297 A CN 201610534297A CN 106229030 B CN106229030 B CN 106229030B
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- electrically conductive
- carbon black
- weight
- graphite
- conductive ink
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- 239000000203 mixture Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000006229 carbon black Substances 0.000 claims abstract description 79
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000002245 particle Substances 0.000 claims abstract description 45
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 33
- 239000010439 graphite Substances 0.000 claims abstract description 33
- 229910021392 nanocarbon Inorganic materials 0.000 claims abstract description 27
- 239000011521 glass Substances 0.000 claims abstract description 24
- 150000001875 compounds Chemical class 0.000 claims abstract description 18
- 239000000428 dust Substances 0.000 claims abstract description 17
- 238000000498 ball milling Methods 0.000 claims description 54
- 238000010438 heat treatment Methods 0.000 claims description 44
- 239000000758 substrate Substances 0.000 claims description 38
- 239000000843 powder Substances 0.000 claims description 22
- 239000002904 solvent Substances 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 239000004094 surface-active agent Substances 0.000 claims description 6
- 239000002562 thickening agent Substances 0.000 claims description 6
- 239000013008 thixotropic agent Substances 0.000 claims description 6
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims description 4
- 229910033181 TiB2 Inorganic materials 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- 235000012241 calcium silicate Nutrition 0.000 claims description 2
- 239000003610 charcoal Substances 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- 239000000779 smoke Substances 0.000 claims description 2
- 239000000976 ink Substances 0.000 claims 8
- 239000012467 final product Substances 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 15
- 238000011049 filling Methods 0.000 abstract description 5
- 235000019241 carbon black Nutrition 0.000 description 67
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 53
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 48
- 229910052799 carbon Inorganic materials 0.000 description 41
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 30
- 238000001291 vacuum drying Methods 0.000 description 28
- 239000011812 mixed powder Substances 0.000 description 26
- 238000001035 drying Methods 0.000 description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 23
- 238000000227 grinding Methods 0.000 description 21
- 238000000034 method Methods 0.000 description 19
- 239000000463 material Substances 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 16
- 239000008367 deionised water Substances 0.000 description 16
- 229910021641 deionized water Inorganic materials 0.000 description 16
- 235000019441 ethanol Nutrition 0.000 description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
- 235000019325 ethyl cellulose Nutrition 0.000 description 13
- 229920001249 ethyl cellulose Polymers 0.000 description 13
- 239000001856 Ethyl cellulose Substances 0.000 description 12
- 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 description 11
- 238000005507 spraying Methods 0.000 description 11
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 description 11
- 239000011231 conductive filler Substances 0.000 description 10
- 239000011159 matrix material Substances 0.000 description 10
- 239000012528 membrane Substances 0.000 description 9
- 239000007921 spray Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 239000012159 carrier gas Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000007873 sieving Methods 0.000 description 8
- 238000005406 washing Methods 0.000 description 8
- 239000000969 carrier Substances 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000010936 titanium Substances 0.000 description 7
- 229910052719 titanium Inorganic materials 0.000 description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 238000002844 melting Methods 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000003701 mechanical milling Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid group Chemical group C(C=1C(C(=O)O)=CC=CC1)(=O)O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 229920005749 polyurethane resin Polymers 0.000 description 2
- -1 rilanit special Chemical compound 0.000 description 2
- SMNDYUVBFMFKNZ-UHFFFAOYSA-N 2-furoic acid Chemical compound OC(=O)C1=CC=CO1 SMNDYUVBFMFKNZ-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003571 electronic cigarette Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000011297 pine tar Substances 0.000 description 1
- 229940068124 pine tar Drugs 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
-
- A24F47/008—
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/18—Conductive material dispersed in non-conductive inorganic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a kind of electrically conductive composition, by weight, comprising:Graphite 20~40;Carbon black 13~30;Titaniferous compound conducting particles 5~10;Glass dust 5~20.Present invention also offers electrically conductive ink comprising the electrically conductive composition and preparation method thereof.In addition, the application present invention also offers conducting film and the conducting film as made from the electrically conductive ink.Due to using flakey micron graphite in the present invention, spherical micron carbon black, spherical nano carbon black, highly conductive titaniferous compound particle these types different shape, the electrically conductive composition of different-grain diameter size mix, in follow-up sintering into after conducting film, big particle plays the role of chain, small particles play the role of filling the gap of big particle, so as to form close conductive channel, are conducive to increase the electric conductivity of obtained conducting film.
Description
Technical field
The present invention relates to a kind of carbon heating film heating-body and its application, and in particular to carbon heating film heating-body is in electronic smoke
Change the application in device.
Background technology
Electric radiant Heating Film constantly came out as the product of heating element in recent years, it has more clear advantage, such as thermal efficiency
Height, energy saving, long lifespan, external form alternative is strong, applied widely, processing technology is simple, simple in structure, cost is low, nothing
Naked light, safe and reliable etc..Metal system mainly is used in the prior art, carbon-based material makees the conductive filler of film, although metal based material
Electrical conductivity is high, but it has the shortcomings that as is evident below:It is of high cost that membrane material is done using noble metal, is done membrane material using base metal and is resisted
Oxidisability is bad, it is impossible to continual and steady work.Therefore, sight is gradually transferred to cheap by people, and electric conductivity is preferable, is not easy
Oxidation, performance are stablized, in the carbon-based material of acid and alkali resistance and solvent corrosion.Current most of carbon heating films are all with carbonaceous conductive grain
Son combines macromolecule resin film-forming mode.Such as, the Chinese patent literature of Publication No. CN101624468A discloses one kind
Conductive film of coating of high molecular polymer, Main Components are aromatic polyurethane resins and conductive black, transfer coated by release liners
Method is prepared, and the formula of its floating coat slurry therewith is as follows, in parts by weight:Aromatic polyurethane resins 100;Toluene 120
~160;Dimethylformamide 50~140;Conductive black 8~20;Dispersant 0.5~2.The prior art is as a result of resin
For binding agent, the temperature in use of conducting film is limited.
103146260 A of Publication No. CN disclose a kind of conductive ink composition, including component:Electrically conductive particles, propylene
Acid resin binding agent, organic solvent and additive;The conductive ink composition includes the component of following mass fraction:It is described
Electrically conductive particles are electrically conductive graphite and the mixture of conductive black;The additive includes levelling agent, antioxidant, cohesive force and promotes
At least one of agent, auxiliary rheological agents.
In the prior art, it is general no more than 250 DEG C there is the limitation of heating film temperature in use;General Conductivity Ratio
The shortcomings of metal film two to three orders of magnitude of difference.
The content of the invention
It is low to solve existing existing carbon system heating film (conducting film) temperature in use, it is of the invention the defects of poorly conductive
Purpose is to provide a kind of electrically conductive composition (conductive filler);Additionally provide the electrically conductive ink and its system for including the electrically conductive composition
Preparation Method.
In addition, the application present invention also offers conducting film and the conducting film as made from the electrically conductive ink.
A kind of electrically conductive composition, by weight, comprising
The graphite is flaky graphite, and particle diameter is 1um~80um.
The carbon black is the spherical Nano carbon of spherical the micron carbon black and/or particle diameter 30nm~200nm of particle diameter 1um~60um
It is black.
Preferably, the carbon black is mixed by spherical micron carbon black and spherical nano carbon black, spherical micron carbon black and
The weight part ratio 10~20: 3~10 of spherical nano carbon black.
Titaniferous compound conducting particles is preferably titanium nitride and/or titanium diboride.
The present invention uses glass powder with low melting point, preferably, the glass powder temperature is 400 DEG C~500 DEG C.
Due to using flakey micron graphite, spherical micron carbon black, spherical nano carbon black, highly conductive titaniferous compound in the present invention
Particle these types different shape, the electrically conductive composition of different-grain diameter size mix, in follow-up sintering into after conducting film, big particle
Play the role of chain, small particles play the role of filling the gap of big particle, so as to form close conductive channel, are conducive to increase
The electric conductivity of obtained conducting film.
Present invention also offers a kind of electrically conductive ink (conductive carbon pastes), the electrically conductive composition is included.
Based on electrically conductive ink parts by weight, the electrically conductive ink includes the micron graphite of 20~40 parts by weight, 10~20 weight
Part micron carbon black, the nano carbon blacks of 3~10 parts by weight, the titaniferous compound conducting particles of 5~10 parts by weight, 5~20 parts by weight
The organic carrier of glass dust and 30~60 parts by weight.
Preferably, the electrically conductive ink also includes organic carrier;In terms of electrically conductive ink percetage by weight 100%, have
The percetage by weight of airborne body is 30%~60%.
The organic carrier includes solvent, thickener, thixotropic agent, flow control agent and surfactant;Wherein, solvent,
Thickener, thixotropic agent, the mass parts ratio of flow control agent and surfactant are 86-94: 2-8: 8-14: 1-4: 1-4.
In the present invention, the solvent selected from terpinol, citric acid tri butyl ester, neck dibatyl phithalate at least one
Kind.
Preferably, the solvent is terpinol.
In the present invention, the thickener is selected from least one of ethyl cellulose, nitrocellulose, vistanex.
Preferably, the thickener is ethyl cellulose.
In the present invention, the thixotropic agent is at least one of rilanit special, oleic acid, calcium silicates.
Preferably, the thixotropic agent is rilanit special.
In the present invention, the flow control agent is at least one of furancarboxylic acid, terephthalic acid (TPA), ammonium sulfate.
Preferably, the flow control agent is terephthalic acid (TPA).
In the present invention, the surfactant is at least one of ethanol, toluene, cyclohexanone.
Preferably, the surfactant is ethanol.
Preferably, the organic carrier includes terpinol, ethyl cellulose, rilanit special, terephthalic acid (TPA) and
Ethanol.Under the preferred organic carrier, terpinol, ethyl cellulose, terephthalic acid (TPA), the mass parts ratio of ethanol and rilanit special
Example is 90-93: 3-5: 1-3: 1-3: 8-12.
Still more preferably, by weight, the organic carrier for 92 parts of terpinols, 4 parts of ethyl celluloses, 2 parts it is right
The composition of phthalic acid, 2 parts of ethanol and 10 parts of rilanit specials.
In the present invention, by be combineding with each other for each material of the different structure and particle diameter, can effectively improving use, this is led
The electric conductivity of material prepared by electric composition, in the glass dust of fusion temperature described in coordinated, can effectively improve conductive oil
The temperature in use of conducting film made from ink.
Present invention also offers a kind of preparation method of the electrically conductive ink, comprise the following steps:
Step (1):Graphite, carbon black pretreatment;
Step (2):Ball milling again after being mixed after pretreated carbon black ball milling with graphite, titaniferous compound conducting particles, obtains powder
1;
Step (3):By powder 1 and glass dust mixing and ball milling, powder 2 is obtained;
Step (4):Powder 2 is mixed to prepare electrically conductive ink with organic carrier.
The method of the present invention uses substep ball milling mixing, greatly reducing the agglomeration of carbon black particle, while make difference
Conductive filler mixing evenly, dispersiveness is more preferable, so as to contribute to the electrical conductivity of the follow-up obtained conducting film of increase.
In step (1), graphite, the respective pretreatment of carbon black, wherein preprocess method is identical.
Preprocess method is, for example,:Graphite or carbon black are placed in 50 DEG C~100 DEG C of alkali compounds aqueous solution (such as
NaOH aqueous solutions) in and stir, mixing time is 10min~60min, after stirring with deionized water scouring stone ink, carbon black
To neutrality, filter, 0.5h~3h is dried in vacuo in 60 DEG C~100 DEG C.
The concentration of the aqueous solution of alkali compounds chooses 5%~25%.For example, preprocessing process use weight concentration for
5%~25% NaOH aqueous solutions.
In step (2), first by carbon black pellet ball milling.The carbon black is spherical, the micron charcoal comprising the weight part ratio
Black and nano carbon black.
Carbon black mechanical milling process can be:Pretreated spherical micron carbon black and spherical nano carbon black are mixed, added to existing
There is in general ball-grinding machine (such as zirconia ball grinding jar), ratio of grinding media to material is, for example, 2: 1, then adds certain ball milling solvent
(such as ethanol) carries out ball milling, is filtered after ball milling, and drying removes ball milling solvent to the solid portion of collection again,
In mechanical milling process, rotating speed 300-500r/min;Ball-milling Time is 6-10h.
In the present invention, by the gradation ball milling, the material of different-grain diameter can be uniformly mixed, help further to subtract
Few agglomeration, plays the mutual synergistic effect of each material;So that follow-up sintering, into after conducting film, big particle plays the work of chain
With small particles play the role of filling the gap of big particle, help to form the conductive channel of densification.
Continue ball-milling treatment, ball-milling treatment side after being mixed after carbon black ball milling, drying with graphite, titaniferous compound conducting particles
Formula can be identical with carbon black ball grinding method, is filtered after ball milling, is dried to obtain powder 1.
Preferably, in step (2), the weight ratio of graphite, carbon black and titaniferous compound conducting particles for 20~40: 13~
30: 5~10.
Titaniferous compound conducting particles is titanium nitride and/or titanium diboride, preferably titanium diboride.
By the powder 1 that ball milling obtains continue with glass dust mixing and ball milling, obtain powder 2;The ball grinding method of step (3) can be used for reference
Carbon black ball grinding method.
In step (3), the glass powder temperature is 400 DEG C~500 DEG C, preferably 450 DEG C of melting glass frits.
In the method for the present invention, by the glass dust ball milling mixing into electrically conductive composition, compared to the carbon in most present situation
Be conductive filler with resin solidification into film, the temperature in use for the film that electrically conductive ink of the invention sinters into can greatly improve.
Sieve is crossed after step (3) ball milling, drying, separates ball and material after ball milling, the sieve of sieving is, for example, 80 mesh, is collected
The following particle of 80 mesh is powder 2.
In step (4), powder 2 and organic carrier are mixed to prepare electrically conductive ink.
Powder 2 is ground with organic carrier material using existing equipment, such as three-roll grinder.
The electrically conductive ink viscosity number is preferably 10000cp~40000cp.
Present invention also offers one kind using conducting film (carbon heating film heating-body) made from electrically conductive ink curing.
The electrically conductive ink is sprayed and/or is printed on carrier substrate, is cured up to conducting film.
By taking acid etching is coated with as an example, the conductive carbon pastes are sprayed on quartz glass by carrier substrate after acid etching
Certain galvanic circle is formed on substrate, through drying, sintering, obtains carbon heating film heating-body.
Preferably, the carrier substrate is quartz glass, ceramics or resin substrate.
Preferably, the carrier substrate is preferably quartz glass.Favorably increased using pretreated quartz glass
The bond strength of film and matrix.
The acid corrosion process uses existing conventional method, by taking quartz glass as an example, by quartz glass substrate successively with third
Ketone, each supersound washing 5min~30min of deionized water, is then dried, then with certain density HF aqueous corrosions 0.5min~
15min, is then washed with deionized to neutrality, dry.In HF aqueous solutions, HF concentration is chosen for 5%~40%.
Spraying process can use existing equipment (such as manual spray gun).Its carrier gas is industry N2, operating air pressure is set as
0.2MPa~0.4MPa, spraying number are 6~30 times.
After the completion of spraying, temperature programming curing is carried out, is solidificated under vacuum and carries out.Preferably, vacuum solidification
Cheng Zhong, with 2 DEG C/min~10 DEG C/min heating rates to 150 DEG C~200 DEG C, keeps the temperature 5min~30min, then with 2 DEG C/min
~10 DEG C/min heating rates keep the temperature 10min~60min to 500 DEG C~600 DEG C.
In the present invention, a kind of preferable conducting film (carbon heating film heating-body) preparation method, comprises the following steps:
Step a:By carbon black and graphite be respectively placed in 50 DEG C~100 DEG C NaOH aqueous solutions stirring, then spend from
Sub- water is rinsed to neutrality, is filtered, vacuum drying;
The carbon black is the micron carbon black of spherical particle diameter 1um~60um and the nano carbon black of particle diameter 30nm~200nm;It is micro-
The weight part ratio 10~20: 3~10 of rice carbon black and spherical nano carbon black;
The graphite is flakey, and particle diameter is 1um~80um;
Step b:First will be conductive with the graphite and titaniferous compound after the carbon black in a solvent ball milling, filtering, drying
Particle ball milling, filtering, dry powder 1 in a solvent;
Step c:By powder 1 and glass dust in a solvent ball milling, filtering, drying, sieve to obtain powder 2;
Wherein, graphite, carbon black, titaniferous compound conducting particles, glass dust add weight part ratio for 20~40: 13~30: 5~
10: 5~20;
Step d:Powder 2 and organic carrier are mixed to prepare electrically conductive ink;Wherein, the organic carrier includes pine tar
Alcohol, ethyl cellulose, rilanit special, terephthalic acid (TPA) and ethanol;Organic carrier accounts for the 30%~60% of electrically conductive ink weight;
Step e:The electrically conductive ink is sprayed on to the quartz glass substrate on piece after acid etching and forms galvanic circle, it is dry,
Vacuum-sintering, obtains carbon heating film heating-body;During vacuum-sintering, with 2 DEG C/min~10 DEG C/min heating rates to 150 DEG C
~200 DEG C, 5min~30min is kept the temperature, then with 2 DEG C/min~10 DEG C/min heating rates to 500 DEG C~600 DEG C, insulation
10min~60min.
Step b is identical with step c mechanical milling process methods, and ratio of grinding media to material is also identical, and ball milling solvent is also identical, is, for example, ethanol.
Present invention additionally comprises a kind of application of obtained conducting film, and the conducting film is applied to electronic cigarette atomizing
Device.
The temperature in use of of the invention designed and preparation conducting film can be more than or equal to 300 DEG C.
Beneficial effects of the present invention:
(1) present invention is due to using flakey micron graphite, spherical micron carbon black, spherical nano carbon black, highly conductive titanizing
Thing particle these types different shape, the conductive filler of different-grain diameter size mix, and after sintering forms a film, big particle plays chain
Effect, small particles play the role of filling the gap of big particle, so as to form close conductive channel, then electric conductivity greatly increases
Add.
(2) present invention greatly reducing carbon black particle in hybrid conductive filler as a result of substep ball milling mixing
Agglomeration, while different conductive filler is mixed evenly, dispersiveness is more preferable, so that the electrical conductivity after film forming is significantly
Increase.
(3) present invention carries out low-temperature sintering film forming using carbon conductive filler and low-melting glass, compared in most present situation
Carbon conductive filler and resin solidification into film, greatly improve the temperature in use of film.
(4) present invention takes slight erosion to handle matrix quartz glass, the favourable bond strength for increasing film and matrix.
Brief description of the drawings
Fig. 1 is the preparation flow figure of carbon heating film heating-body of the present invention;
Fig. 2 is the schematic diagram of the conductive channel of carbon heating film of the present invention;
Fig. 3 is that a kind of spraying of carbon heating film heating-body of the present invention is film-made schematic diagram.
Embodiment
Following embodiments are implemented by aforesaid operations method:
Following embodiments are using the preparation flow shown in Fig. 1.
Fig. 2 is the schematic diagram of the conductive channel of carbon heating film of the present invention, and the conductive channel of carbon heating film of the invention is distinguished
By flakey micron graphite (a), spherical micron carbon black (b), spherical nano carbon black (c) composition, it can be seen that the heating film is by several
Kind different shape, the conductive filler of different-grain diameter size mix, and after sintering forms a film, big particle plays the role of chain, granule
Son plays the role of filling the gap of big particle, so as to form close conductive channel, then electric conductivity greatly increases.
As can be seen from Figure 3 air gun sprayed coating film mode of the present invention, 1 is spray gun, and 2 be base material, using quartz glass substrate
Piece.
Embodiment 1:
Micron graphite, micron carbon black, nano carbon black are done into following pretreatment respectively:It is electric in 80 DEG C of 10%NaOH solution
Magnetic stirs 15min, then with deionized water rinsing to neutrality, filters, 1h is dried in 80 DEG C of vacuum drying chambers.Pretreatment of raw material
Afterwards, 17g microns of carbon blacks and 3g nano carbon blacks is taken to mix and be put into zirconia ball grinding jar, ratio of grinding media to material 2: 1, then adds a certain amount of
Absolute ethyl alcohol, with the speed ball milling 8h of 300r/min, after ball milling is complete, filters, places into 80 DEG C of dry 2h in vacuum drying chamber, so
Take out afterwards and obtain mixed powder 1 by above-mentioned ball milling drying mode with 40g micron graphites and 5g titanium diborides again, will then obtain
Mixed powder 1 and 5g fusing points obtain mixed powder 2 by above-mentioned ball milling drying mode for 450 DEG C of glass dust, then cross 80 mesh sieves
Son.
By terpinol: ethyl cellulose: terephthalic acid (TPA): ethanol: rilanit special weight part ratio is matched somebody with somebody for 92: 4: 2: 2: 10
Make the organic carrier needed for this experiment.It will take 30g organic carriers that 2h is mixed with the mixed powder 2 after above-mentioned sieving, then use
Three-roll grinder grinds 5 times and obtains conductive carbon pastes repeatedly.
Quartz glass substrate is used into acetone successively, each supersound washing 5min of deionized water, is then placed in air dry oven
80 DEG C of dry 1h, then corrode 15min with 5%HF, then it is washed with deionized to neutrality, is put into air dry oven and does for 80 DEG C
Dry 1h.
Processed quartz glass substrate is lain on experimental bench, with industrial N2For carrier gas, air pressure is set to 0.4MPa, adopts
Conductive carbon pastes obtained above are sprayed on substrate with manual spray gun, circulation spraying 6 times, is then placed in vacuum drying chamber
80 DEG C of dry 1h.After drying, take out sample and be put into vacuum drying oven by following technique sintering:With 2 DEG C/min heating rates to 180
DEG C, 10min is kept the temperature, then with 2 DEG C/min heating rates to 550 DEG C, keeps the temperature 30min.
Obtained a kind of carbon heating film heating-body in embodiment is subjected to resistivity measurement, the performance of its result has excellent
Electric conductivity, its resistivity are 1.6 × 10-4Ω·cm;Through Analysis of Heat Tolerance experimental test, its result performance temperature in use is at least super
Cross 300 DEG C;Measured through attachment fastness, film is 1 grade with the attachment degree of matrix, and performance membrane is high with substrate combinating strength.
Embodiment 2:
Micron graphite, micron carbon black, nano carbon black are done into following pretreatment respectively:It is electric in 100 DEG C of 5%NaOH solution
Magnetic stirs 10min, then with deionized water rinsing to neutrality, filters, 1h is dried in 80 DEG C of vacuum drying chambers.Pretreatment of raw material
Afterwards, 20g microns of carbon blacks and 10g nano carbon blacks is taken to mix and be put into zirconia ball grinding jar, ratio of grinding media to material 2: 1, then adds a certain amount of
Absolute ethyl alcohol, with the speed ball milling 8h of 300r/min, after ball milling is complete, filters, place into 80 DEG C of dry 2h in vacuum drying chamber,
Then take out and obtain mixed powder 1 by above-mentioned ball milling drying mode with 20g micron graphites and 5g titanium diborides again, then incite somebody to action
To mixed powder 1 and 8g fusing points obtain mixed powder 2 by above-mentioned ball milling drying mode for 500 DEG C of glass dust, then cross 80 mesh
Sieve.
By terpinol: ethyl cellulose: terephthalic acid (TPA): ethanol: rilanit special weight part ratio is 91: 5: 3: 1: 10 systems
Organic carrier needed for this experiment.The mixed powder 2 after 37g organic carriers and above-mentioned sieving will be taken to be mixed 2h, then with three
Roller mill grinds 5 times and obtains conductive carbon pastes repeatedly.
Quartz glass substrate is used into acetone successively, each supersound washing 20min of deionized water, is then placed in air dry oven
80 DEG C of dry 1h, then corrode 5min with 20%HF, then it is washed with deionized to neutrality, is put into air dry oven and does for 80 DEG C
Dry 1h.
Processed quartz glass substrate is lain on experimental bench, with industrial N2For carrier gas, air pressure is set to 0.3MPa, adopts
Conductive carbon pastes obtained above are sprayed on substrate with manual spray gun, circulation spraying 10 times, is then placed in vacuum drying chamber
In 80 DEG C of dry 1h.After drying, take out sample and be put into vacuum drying oven by following technique sintering:With 5 DEG C/min heating rates to 200
DEG C, 10min is kept the temperature, then with 5 DEG C/min heating rates to 600 DEG C, keeps the temperature 10min.
Obtained a kind of carbon heating film heating-body in embodiment is subjected to resistivity measurement, the performance of its result has excellent
Electric conductivity, its resistivity are 3.6 × 10-4Ω·cm;Through Analysis of Heat Tolerance experimental test, its result performance temperature in use is at least super
Cross 300 DEG C;Measured through attachment fastness, film is 1 grade with the attachment degree of matrix, and performance membrane is high with substrate combinating strength.
Embodiment 3:
Micron graphite, micron carbon black, nano carbon black are done into following pretreatment respectively:It is electric in 50 DEG C of 25%NaOH solution
Magnetic stirs 15min, then with deionized water rinsing to neutrality, filters, 1h is dried in 80 DEG C of vacuum drying chambers.Pretreatment of raw material
Afterwards, 12g microns of carbon blacks and 5g nano carbon blacks is taken to mix and be put into zirconia ball grinding jar, ratio of grinding media to material 2: 1, then adds a certain amount of
Absolute ethyl alcohol, with the speed ball milling 8h of 300r/min, after ball milling is complete, filters, places into 80 DEG C of dry 2h in vacuum drying chamber, so
Take out afterwards and obtain mixed powder 1 by above-mentioned ball milling drying mode with 20g micron graphites, 5g titanium diborides, 5g titanium nitrides again, connect
The mixed powder 1 that will be obtained and obtain mixed powder 2 by above-mentioned ball milling drying mode with 20g fusing points for 400 DEG C of glass dust, then
Cross 80 mesh sieve.
By terpinol: ethyl cellulose: terephthalic acid (TPA): ethanol: rilanit special weight part ratio is matched somebody with somebody for 93: 3: 2: 2: 12
Make the organic carrier needed for this experiment.It will take 33g organic carriers that 2h is mixed with the mixed powder 2 after above-mentioned sieving, then use
Three-roll grinder grinds 5 times and obtains conductive carbon pastes repeatedly.
Quartz glass substrate is used into acetone successively, each supersound washing 30min of deionized water, is then placed in air dry oven
80 DEG C of dry 1h, then corrode 0.5min with 40%HF, then it is washed with deionized to neutrality, is put into air dry oven 80 DEG C
Dry 1h.
Processed quartz glass substrate is lain on experimental bench, with industrial N2For carrier gas, air pressure is set to 0.25MPa,
Conductive carbon pastes obtained above are sprayed on substrate using manual spray gun, circulation spraying 15 times, is then placed in vacuum drying
80 DEG C of dry 1h in case.After drying, take out sample and be put into vacuum drying oven by following technique sintering:Arrived with 2 DEG C/min heating rates
150 DEG C, 30min is kept the temperature, then with 2 DEG C/min heating rates to 500 DEG C, keeps the temperature 60min.
Obtained a kind of carbon heating film heating-body in embodiment is subjected to resistivity measurement, the performance of its result has excellent
Electric conductivity, its resistivity are 3.0 × 10-4Ω·cm;Through Analysis of Heat Tolerance experimental test, its result performance temperature in use is at least super
Cross 300 DEG C;Measured through attachment fastness, film is 1 grade with the attachment degree of matrix, and performance membrane is high with substrate combinating strength.
Embodiment 4:
Micron graphite, micron carbon black, nano carbon black are done into following pretreatment respectively:It is electric in 60 DEG C of 15%NaOH solution
Magnetic stirs 60min, then with deionized water rinsing to neutrality, filters, 1h is dried in 80 DEG C of vacuum drying chambers.Pretreatment of raw material
Afterwards, 10g microns of carbon blacks and 3g nano carbon blacks is taken to mix and be put into zirconia ball grinding jar, ratio of grinding media to material 2: 1, then adds a certain amount of
Absolute ethyl alcohol, with the speed ball milling 8h of 300r/min, after ball milling is complete, filters, places into 80 DEG C of dry 2h in vacuum drying chamber, so
Take out afterwards and obtain mixed powder 1 by above-mentioned ball milling drying mode with 20g micron graphites and 5g titanium diborides again, then incite somebody to action
To mixed powder 1 and 5g fusing points obtain mixed powder 2 by above-mentioned ball milling drying mode for 480 DEG C of glass dust, then cross 80 mesh
Sieve.
By terpinol: ethyl cellulose: terephthalic acid (TPA): ethanol: rilanit special weight part ratio is matched somebody with somebody for 90: 4: 3: 3: 8
Make the organic carrier needed for this experiment.It will take 57g organic carriers that 2h is mixed with the mixed powder 2 after above-mentioned sieving, then use
Three-roll grinder grinds 5 times and obtains conductive carbon pastes repeatedly.
Quartz glass substrate is used into acetone successively, each supersound washing 10min of deionized water, is then placed in air dry oven
80 DEG C of dry 1h, then corrode 10min with 5%HF, then it is washed with deionized to neutrality, is put into air dry oven and does for 80 DEG C
Dry 1h.
Processed quartz glass substrate is lain on experimental bench, with industrial N2For carrier gas, air pressure is set to 0.2MPa, adopts
Conductive carbon pastes obtained above are sprayed on substrate with manual spray gun, circulation spraying 30 times, is then placed in vacuum drying chamber
In 80 DEG C of dry 1h.After drying, take out sample and be put into vacuum drying oven by following technique sintering:With 2 DEG C/min heating rates to 180
DEG C, 10min is kept the temperature, then with 2 DEG C/min heating rates to 580 DEG C, keeps the temperature 30min.
Obtained a kind of carbon heating film heating-body in embodiment is subjected to resistivity measurement, the performance of its result has excellent
Electric conductivity, its resistivity are 5.4 × 10-4Ω·cm;Through Analysis of Heat Tolerance experimental test, its result performance temperature in use is at least super
Cross 300 DEG C;Measured through attachment fastness, film is 1 grade with the attachment degree of matrix, and performance membrane is high with substrate combinating strength.
Comparative example 1
Micron graphite, micron carbon black, nano carbon black are done into following pretreatment respectively:It is electric in 80 DEG C of 10%NaOH solution
Magnetic stirs 15min, then with deionized water rinsing to neutrality, filters, 1h is dried in 80 DEG C of vacuum drying chambers.Pretreatment of raw material
Afterwards, 17g microns of carbon blacks and 3g nano carbon blacks is taken to mix and be put into zirconia ball grinding jar, ratio of grinding media to material 2: 1, then adds a certain amount of
Absolute ethyl alcohol, with the speed ball milling 8h of 300r/min, after ball milling is complete, filters, places into 80 DEG C of dry 2h in vacuum drying chamber, so
Take out afterwards and obtain mixed powder 1 by above-mentioned ball milling drying mode with 40g micron graphites again, the mixed powder 1 that will then obtain
Mixed powder 2 is obtained by above-mentioned ball milling drying mode for 450 DEG C of glass dust with 5g fusing points, then crosses 80 mesh sieve.
By terpinol: ethyl cellulose: terephthalic acid (TPA): ethanol: rilanit special weight part ratio is matched somebody with somebody for 80: 8: 6: 6: 12
Make the organic carrier needed for this experiment.It will take 30g organic carriers that 2h is mixed with the mixed powder 2 after above-mentioned sieving, then use
Three-roll grinder grinds 5 times and obtains conductive carbon pastes repeatedly.
Quartz glass substrate is used into acetone successively, each supersound washing 5min of deionized water, is then placed in air dry oven
80 DEG C of dry 1h, then corrode 15min with 5%HF, then it is washed with deionized to neutrality, is put into air dry oven and does for 80 DEG C
Dry 1h.
Processed quartz glass substrate is lain on experimental bench, with industrial N2For carrier gas, air pressure is set to 0.4MPa, adopts
Conductive carbon pastes obtained above are sprayed on substrate with manual spray gun, circulation spraying 6 times, is then placed in vacuum drying chamber
80 DEG C of dry 1h.After drying, take out sample and be put into vacuum drying oven by following technique sintering:With 2 DEG C/min heating rates to 180
DEG C, 10min is kept the temperature, then with 2 DEG C/min heating rates to 550 DEG C, keeps the temperature 30min.
Obtained a kind of carbon heating film heating-body in comparative example is subjected to resistivity measurement, its result shows as general lead
Electrically, its resistivity is 5.2 × 10-3Ω·cm;Through Analysis of Heat Tolerance experimental test, its result show temperature in use at least over
300℃;Measured through attachment fastness, film is I grade with the attachment degree of matrix, performance membrane and substrate combinating strength height.
Comparative example 2
Micron graphite, micron carbon black are done into following pretreatment respectively:The electromagnetic agitation in 80 DEG C of 10%NaOH solution
15min, then with deionized water rinsing to neutrality, filters, 1h is dried in 80 DEG C of vacuum drying chambers.After pretreatment of raw material, take
20g microns of carbon blacks, 40g micron graphites, the mixing of 5g titanium diborides are put into zirconia ball grinding jar, and ratio of grinding media to material 2: 1, then adds one
Quantitative absolute ethyl alcohol, with the speed ball milling 8h of 300r/min, after ball milling is complete, filters, places into vacuum drying chamber and do for 80 DEG C
Dry 2h obtains mixed powder 1, is then 450 DEG C of glass dust by above-mentioned ball milling drying side by obtained mixed powder 1 and 5g fusing points
Formula obtains mixed powder 2, then crosses 80 mesh sieve.
By terpinol: ethyl cellulose: terephthalic acid (TPA): ethanol: rilanit special weight part ratio is matched somebody with somebody for 80: 8: 6: 6: 12
Make the organic carrier needed for this experiment.It will take 30g organic carriers that 2h is mixed with the mixed powder 2 after above-mentioned sieving, then use
Three-roll grinder grinds 5 times and obtains conductive carbon pastes repeatedly.
Quartz glass substrate is used into acetone successively, each supersound washing 5min of deionized water, is then placed in air dry oven
80 DEG C of dry 1h, then corrode 15min with 5%HF, then it is washed with deionized to neutrality, is put into air dry oven and does for 80 DEG C
Dry 1h.
Processed quartz glass substrate is lain on experimental bench, with industrial N2For carrier gas, air pressure is set to 0.4MPa, adopts
Conductive carbon pastes obtained above are sprayed on substrate with manual spray gun, circulation spraying 6 times, is then placed in vacuum drying chamber
80 DEG C of dry 1h.After drying, take out sample and be put into vacuum drying oven by following technique sintering:With 2 DEG C/min heating rates to 180
DEG C, 10min is kept the temperature, then with 2 DEG C/min heating rates to 550 DEG C, keeps the temperature 30min.
Obtained a kind of carbon heating film heating-body in comparative example is subjected to resistivity measurement, its result shows as general lead
Electrically, its resistivity is 8.2 × 10-3Ω·cm;Through Analysis of Heat Tolerance experimental test, its result show temperature in use at least over
300℃;Measured through attachment fastness, film is I grade with the attachment degree of matrix, performance membrane and substrate combinating strength height.
Comparative example 3
Micron graphite, micron carbon black, nano carbon black are done into following pretreatment respectively:It is electric in 80 DEG C of 10%NaOH solution
Magnetic stirs 15min, then with deionized water rinsing to neutrality, filters, 1h is dried in 80 DEG C of vacuum drying chambers.Pretreatment of raw material
Afterwards, 17g microns of carbon blacks and 3g nano carbon blacks is taken to mix and be put into zirconia ball grinding jar, ratio of grinding media to material 2: 1, then adds a certain amount of
Absolute ethyl alcohol, with the speed ball milling 8h of 300r/min, after ball milling is complete, filters, places into 80 DEG C of dry 2h in vacuum drying chamber, so
Take out afterwards and obtain mixed powder 1 by above-mentioned ball milling drying mode with 40g micron graphites and 5g titanium diborides again, then cross 80 mesh
Sieve.
By terpinol: ethyl cellulose: terephthalic acid (TPA): ethanol: rilanit special weight part ratio is 70: 26: 2: 2: 10
Prepare the organic carrier needed for this experiment.It will take 30g organic carriers that 2h is mixed with the mixed powder 1 after above-mentioned sieving, then
Ground repeatedly with three-roll grinder 5 times and obtain conductive carbon pastes.
Quartz glass substrate is used into acetone successively, each supersound washing 5min of deionized water, is then placed in air dry oven
80 DEG C of dry 1h, then corrode 15min with 5%HF, then it is washed with deionized to neutrality, is put into air dry oven and does for 80 DEG C
Dry 1h.
Processed quartz glass substrate is lain on experimental bench, with industrial N2For carrier gas, air pressure is set to 0.4MPa, adopts
Conductive carbon pastes obtained above are sprayed on substrate with manual spray gun, circulation spraying 6 times, is then placed in vacuum drying chamber
120 DEG C cure dry 1h.
Obtained a kind of carbon heating film heating-body in comparative example is subjected to resistivity measurement, its result shows as poor conduction
Property, its resistivity is 4.8 × 10-2Ω·cm;Through Analysis of Heat Tolerance experimental test, its result performance temperature in use is no more than 160
℃;Measured through attachment fastness, film is III level with the attachment degree of matrix, shows membrane and substrate combinating strength is not high.
It can be seen that the carbon heating film good conductivity of the present invention from embodiment 1-4, film use environment temperature is high, adhesive strength
The advantages that high.
If not it can be seen that from embodiment 1 and comparative example 1-2 using the ball of flaky graphite and different-grain diameter in the present invention
Shape carbon black and titaniferous compound mix the conducting particles of composition, and organic carrier ratio formula not using the present invention, then shape
Into heating film electric conductivity it is poor the shortcomings that;If not this it appears that being used in the carbon heating film use present invention in comparative example 3
Low-melting glass sintering film forming mode, the film use environment temperature of formation limited significantly, and with the attachment of base material
Intensity degradation.
Although the foregoing describing the embodiment of the present invention, it will be appreciated by those of skill in the art that these
It is merely illustrative of, after the above of the present invention has been read, those skilled in the art can make the present invention various change
Dynamic or modification, these equivalent forms also fall within the scope of the appended claims of the present application.
Claims (8)
- A kind of 1. electrically conductive composition, it is characterised in that:By weight, comprisingGraphite 20 ~ 40;Carbon black 13 ~ 30;Titaniferous compound conducting particles 5 ~ 10;Glass dust 5 ~ 20;The graphite is flaky graphite, and particle diameter is 1um ~ 80um;The carbon black is the spherical micron charcoal of particle diameter 1um ~ 60um The black and spherical nano carbon black of particle diameter 30nm ~ 200nm;Titaniferous compound conducting particles is titanium nitride and/or titanium diboride;The weight part ratio 10 ~ 20 of spherical micron carbon black and spherical nano carbon black:3~10.
- 2. electrically conductive composition as claimed in claim 1, it is characterised in that:The glass powder temperature is 400 DEG C ~ 500 ℃。
- 3. a kind of electrically conductive ink, it is characterised in that include claim 1-2 any one of them electrically conductive compositions.
- 4. electrically conductive ink as claimed in claim 3, it is characterised in that:Based on electrically conductive ink parts by weight, the electrically conductive ink bag Micron graphite containing 20 ~ 40 parts by weight, the micron carbon black of 10 ~ 20 parts by weight, the nano carbon black of 3 ~ 10 parts by weight, 5 ~ 10 parts by weight Titaniferous compound conducting particles, the glass dust of 5 ~ 20 parts by weight and the organic carrier of 30 ~ 60 parts by weight.
- 5. electrically conductive ink as claimed in claim 4, it is characterised in that:The organic carrier includes solvent, thickener, thixotroping Agent, flow control agent and surfactant;Wherein, the matter of solvent, thickener, thixotropic agent, flow control agent and surfactant It is 86-94 to measure part ratio:2-8:8-14:1-4:1-4;The thixotropic agent is at least one of rilanit special, oleic acid, calcium silicates.
- 6. such as the preparation method of claim 3-5 any one of them electrically conductive inks, it is characterised in that:Comprise the following steps:Step(1):Graphite, carbon black pretreatment;Step(2):Ball milling again after being mixed after pretreated carbon black ball milling with graphite, titaniferous compound conducting particles, obtains powder 1;Step(3):By powder 1 and glass dust mixing and ball milling, powder 2 is obtained;Step(4):Powder 2 is mixed to prepare electrically conductive ink with organic carrier.
- A kind of 7. preparation method of conducting film, it is characterised in that:Claim 3-5 any one of them electrically conductive ink is sprayed And/or be printed on carrier substrate, cure under vacuum to obtain the final product;During vacuum solidification, with 2 DEG C/min ~ 10 DEG C/min liters Warm speed keeps the temperature 5min ~ 30min, then with 2 DEG C/min ~ 10 DEG C/min heating rates to 500 DEG C ~ 600 to 150 DEG C ~ 200 DEG C DEG C, keep the temperature 10min ~ 60min.
- 8. the application of conducting film made from a kind of claim 7, it is characterised in that the conducting film is applied to electronic smoke Change device.
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