CN108641486A - Capacitive touch screen carbon conductive ink and the preparation method and application thereof - Google Patents

Capacitive touch screen carbon conductive ink and the preparation method and application thereof Download PDF

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CN108641486A
CN108641486A CN201810328868.2A CN201810328868A CN108641486A CN 108641486 A CN108641486 A CN 108641486A CN 201810328868 A CN201810328868 A CN 201810328868A CN 108641486 A CN108641486 A CN 108641486A
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conductive ink
nitrogen
preparation
added
doped graphene
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李宪荣
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Chongqing Photoelectric Display Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/52Electrically conductive inks
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/03Printing inks characterised by features other than the chemical nature of the binder
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/10Printing inks based on artificial resins
    • C09D11/102Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
    • GPHYSICS
    • G06COMPUTING; CALCULATING OR COUNTING
    • G06FELECTRIC DIGITAL DATA PROCESSING
    • G06F3/00Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
    • G06F3/01Input arrangements or combined input and output arrangements for interaction between user and computer
    • G06F3/03Arrangements for converting the position or the displacement of a member into a coded form
    • G06F3/041Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
    • G06F3/044Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means by capacitive means
    • GPHYSICS
    • G06COMPUTING; CALCULATING OR COUNTING
    • G06FELECTRIC DIGITAL DATA PROCESSING
    • G06F2203/00Indexing scheme relating to G06F3/00 - G06F3/048
    • G06F2203/041Indexing scheme relating to G06F3/041 - G06F3/045
    • G06F2203/04103Manufacturing, i.e. details related to manufacturing processes specially suited for touch sensitive devices

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Engineering & Computer Science (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Human Computer Interaction (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Conductive Materials (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)

Abstract

The present invention relates to touch screen technology field more particularly to capacitive touch screen carbon conductive ink and the preparation method and application thereof, carbon conductive ink includes the raw material of following parts by weight:15~20 parts of 44~60 parts of compounded mix, 8~15 parts of macromolecule resin, 2~5 parts of surfactant, 1~3 part of dispersion stabilizer and solvent, the compounded mix is that carboxylic carbon nano-tube, nitrogen-doped graphene and pyrroles's polymerization are made, and carboxylic carbon nano-tube, nitrogen-doped graphene and the mass ratio of pyrroles are 1 in raw material prepared by the compounded mix:1:(0.1~0.2).The electrically conductive ink that the present invention is prepared takes full advantage of the excellent conductive capability of carbon nanotube and graphene, forms and is uniformly dispersed, the conductive network of stereoscopic three-dimensional structure.

Description

Capacitive touch screen carbon conductive ink and the preparation method and application thereof
Technical field
The present invention relates to touch screen technology fields more particularly to capacitive touch screen carbon conductive ink and preparation method thereof With application.
Background technology
Touch screen is also known as " touch screen ", " touch panel ", is a kind of induction type liquid of the input signals such as receivable contact Crystal device, when contacting the graphic button on screen, the haptic feedback system on screen can be according to the journey of preprogramming Formula drives various connection devices, is substituted for mechanical push button panel, and produces by liquid crystal display picture lively Visual and sound effects.Touch screen is as a kind of newest computer input apparatus, it is most simple at present, conveniently, naturally one kind is man-machine Interactive mode.It imparts multimedia with brand-new looks, is extremely attractive completely new multimedia interactive equipment.Main application In the inquiry of public information, leader's office, Industry Control, military commanding, electronic game, choosing song or selecting dish, multimedia teaching, premises Produce presell etc..
Touchscreen pattern conducting wire requirement resistivity is low, circuit is fine, is usually formed by curing by electrically conductive ink.Nothing Machine electrically conductive ink has many advantages, such as that reliability is high, storge quality is high, stability is good, be widely used in integrated circuit, RFID, The electronic products such as wiring board, thin film switch are the hot spots of research and development recent years.According to the type of conductive material, inorganic conductive oil Ink can be specifically divided into gold system, silver-colored system, copper system, carbon series conductive ink.The various performances of gold system electrically conductive ink are all very excellent, but its valence Lattice are expensive, using significantly being limited, have the product of particular/special requirement using thick film integrated circuit etc. is limited only to.Silver powder With good high conduction performance and chemical stability, silver is that the electric conductivity of electrically conductive ink is slightly less than gold system, but has a wide range of application, It can be largely used to the printing of the high appliance circuit of reliability, the excellent conduction of metallic silver and thermal conductivity become electronics industry spy It is not the important materials in microelectronics industry, but there are electromigration problems for silver-colored conducting wire.Copper system electrically conductive ink cost performance Height, but copper powder is oxidizable.
Carbon series conductive ink can avoid above-mentioned gold system, silver is, all problems of copper system, but current carbon system leads
Electric ink technology is also immature, and one of most commonly used raw material graphene has the characteristics that conduction is excellent, density is low, The service life of electrically conductive ink can be improved and reduce the density of electrically conductive ink by inserting graphene.However graphene is in process In be easy irreversible stacking, bad dispersibility the shortcomings of limit performance of the graphene in electrocondution slurry excellent properties.
Invention content
In view of this, the object of the present invention is to provide capacitive touch screen carbon conductive ink and preparation method thereof with answer With, the electrically conductive ink being prepared takes full advantage of the excellent conductive capability of carbon nanotube and graphene, forms and is uniformly dispersed, The conductive network of stereoscopic three-dimensional structure reduces resistance, improves electric conductivity.
The present invention solves above-mentioned technical problem by following technological means:
Capacitive touch screen carbon conductive ink includes the raw material of following parts by weight:44~60 parts of compounded mix, high score 8~15 parts of subtree fat, 2~5 parts of surfactant, 1~3 part of dispersion stabilizer and solvent, the compounded mix are carboxylated carbon Nanotube, nitrogen-doped graphene and pyrroles's polymerization are made.
Further, carboxylic carbon nano-tube, nitrogen-doped graphene and the matter of pyrroles in the raw material that prepared by the compounded mix Amount is than being 1:1:(0.1~0.2).
Further, the macromolecule resin is epoxy resin, and the surfactant is polyacrylamide, and the dispersion is steady It is sodium carboxymethylcellulose or polyvinylpyrrolidone to determine agent, and the solvent is isopropanol.
In addition, the invention also discloses the preparation method of above-mentioned capacitive touch screen carbon conductive ink, including it is following Step:
The preparation of carboxylic carbon nano-tube/nitrogen-doped graphene compound:Take carboxylic carbon nano-tube that deionized water is added In be dispersed with stirring, be made into the carboxylic carbon nano-tube aqueous solution of 3~4mg/mL, take nitrogen-doped graphene be added deionized water in stir Dispersion is mixed, the nitrogen-doped graphene aqueous solution of 12~16mg/mL is made into, by carboxylic carbon nano-tube aqueous solution and N doping graphite Aqueous solution by volume 4:1 mixing, stirs 3~5h, obtains mixed solution, 40~45h of freeze-drying process obtains carboxylated Carbon nanotube/nitrogen-doped graphene compound;
The preparation of compounded mix:Take acetonitrile and water by volume 6:4 mixing, and cetyl trimethylammonium bromide is added and stirs Mixing is mixed, acetonitrile solution is made, carboxylic carbon nano-tube/nitrogen-doped graphene compound is taken to be added in deionized water, stirring point 30min is dissipated, the hydrochloric acid solution that acetonitrile solution and 0.2mol/L is added stirs and evenly mixs, and pyrrole monomer is added under condition of ice bath, and stir The ferric chloride in aqueous solution that 1.5wt% is slowly added dropwise is mixed, 10~12h, the pH of filtration washing to filter cake are stirred to react after being added dropwise =7, it is dried under vacuum to constant weight in 40~50 DEG C, obtains compounded mix;
The preparation of carbon conductive ink:It takes isopropanol that preparation in deionized water is added and obtains the aqueous isopropanol of 25wt%, it will Compounded mix, macromolecule resin, surfactant, dispersion stabilizer are added in aqueous isopropanol to stir and evenly mix and be led to get to carbon Electric ink.
Further, the nitrogen-doped graphene is that oxidation is prepared by Hummers methods using natural graphite powder as raw material Graphene, then using graphene oxide as raw material, melamine is reducing agent and nitrogen dopant, is prepared by hydro-thermal method.
Further, pyrrole monomer and carboxylic carbon nano-tube/nitrogen-doped graphene are compound in the preparation of the compounded mix The mass ratio of object is 1:(10~20).
Further, the pyrrole monomer and FeCl3·6H2The mass ratio of O is 1:3.5.
In addition, the application for the carbon conductive ink being prepared the invention also discloses the above method, the carbon conductive ink For being formed by curing capacitive touch screen electrode, application process uses screen painting or spray up moulding.
It is carboxylic carbon nano-tube, N doping graphite that compounded mix, compounded mix have been used in the electrically conductive ink of the present invention The compound of alkene and pyrroles, carbon nanotube and graphene are all excellent conductive materials, and by carrying out carboxyl to carbon nanotube Change and be modified, and N doping is carried out to graphene, its dispersion performance can be improved, it is made to be uniformly dispersed, by one-dimensional carbon nanotube and Two-dimensional graphene forms stereoscopic three-dimensional network structure, can reduce resistance preferably with pyrroles's compound structure conductive network, improve Electric conductivity.
Specific implementation mode
Below with reference to specific embodiment, the present invention is described in detail:
The capacitive touch screen carbon conductive ink of the present invention, includes the raw material of following parts by weight:Compounded mix 44~ 60 parts, 8~15 parts of macromolecule resin, 2~5 parts of surfactant, 1~3 part of dispersion stabilizer and solvent, wherein compounded mix It is that carboxylic carbon nano-tube, nitrogen-doped graphene and pyrroles's polymerization are made, carboxylated carbon nanometer in raw material prepared by compounded mix Pipe, nitrogen-doped graphene and the mass ratio of pyrroles are 1:1:(0.1~0.2);Macromolecule resin selects epoxy resin, surface-active Agent selects polyacrylamide, dispersion stabilizer that sodium carboxymethylcellulose or polyvinylpyrrolidone, solvent is selected to select isopropanol.
Embodiment one:The preparation of nitrogen-doped graphene
It weighs stirring under 10g graphite, 5g sodium nitrate condition of ice bath to be added in the 230mL concentrated sulfuric acids, stirs 10min, add 30g potassium permanganates stir 2h, then are placed in 35 DEG C of stirred in water bath 3h, and deionized water is added, and are warming up to 95 DEG C, stir 1h, add Enter 720mL deionized waters stirring 10h, 80mL hydrogen peroxide is added, filters, filter cake is dissolved in 1000mL5mol/L hydrochloric acid, filters Manganese ion is removed, repeats to use 1000mLL5mol/L salt acid elution 3 times, then filter cake is dissolved in 2000mL deionized waters, stand It 1 day, outwells supernatant, deionized water is added, water 10 times or so is changed in repetition until the pH value of solution is more than 4, ultrasonic 10min, It centrifuges, obtains graphene oxide dispersion.It takes melamine to be dissolved in ethyl alcohol and deionized water, is added 4.7mg/mL's Graphene oxide dispersion reacts 10h in 180 DEG C of autoclave, takes out washing to neutrality, freeze-drying obtains N doping Graphene.
Embodiment two:The preparation one of carbon conductive ink
The preparation of carboxylic carbon nano-tube/nitrogen-doped graphene compound:Take carboxylic carbon nano-tube that deionized water is added In be dispersed with stirring, be made into the carboxylic carbon nano-tube aqueous solution of 3mg/mL, take nitrogen-doped graphene be added deionized water in stir Dispersion, is made into the nitrogen-doped graphene aqueous solution of 12mg/mL, and carboxylic carbon nano-tube aqueous solution and nitrogen-doped graphene is water-soluble Liquid by volume 4:1 mixing, stirs 3h, obtains mixed solution, freeze-drying process 40h obtains carboxylic carbon nano-tube/nitrogen and mixes Miscellaneous graphene complex;
The preparation of compounded mix:Take acetonitrile and water by volume 6:4 mixing, and cetyl trimethylammonium bromide is added and stirs Mixing is mixed, acetonitrile solution is made, 5g carboxylic carbon nano-tubes/nitrogen-doped graphene compound is taken to be added in deionized water, stirring Disperse 30min, the hydrochloric acid solution that acetonitrile solution and 0.2mol/L is added stirs and evenly mixs, and it is single that 0.5g pyrroles is added under condition of ice bath Body, and the ferric chloride in aqueous solution that a concentration of 1.5wt% of 120mL are slowly added dropwise is stirred, it is stirred to react 10h after being added dropwise, filters It washs to the pH=7 of filter cake, is dried under vacuum to constant weight in 40 DEG C, obtains compounded mix;
The preparation of carbon conductive ink:It takes isopropanol that preparation in deionized water is added and obtains the aqueous isopropanol of 25wt%, it will 44 parts of compounded mix, 8 parts of epoxy resin, 2 parts of polyacrylamide, 1 part of sodium carboxymethylcellulose are added in aqueous isopropanol and stir Mixing is to get to carbon conductive ink.
Embodiment three:The preparation two of carbon conductive ink
The preparation of carboxylic carbon nano-tube/nitrogen-doped graphene compound:Take carboxylic carbon nano-tube that deionized water is added In be dispersed with stirring, be made into the carboxylic carbon nano-tube aqueous solution of 4mg/mL, take nitrogen-doped graphene be added deionized water in stir Dispersion, is made into the nitrogen-doped graphene aqueous solution of 12mg/mL, and carboxylic carbon nano-tube aqueous solution and nitrogen-doped graphene is water-soluble Liquid by volume 4:1 mixing, stirs 5h, obtains mixed solution, freeze-drying process 45h obtains carboxylic carbon nano-tube/nitrogen and mixes Miscellaneous graphene complex;
The preparation of compounded mix:Take acetonitrile and water by volume 6:4 mixing, and cetyl trimethylammonium bromide is added and stirs Mixing is mixed, acetonitrile solution is made, 10g carboxylic carbon nano-tubes/nitrogen-doped graphene compound is taken to be added in deionized water, stirring Disperse 30min, the hydrochloric acid solution that acetonitrile solution and 0.2mol/L is added stirs and evenly mixs, and it is single that 0.5g pyrroles is added under condition of ice bath Body, and the ferric chloride in aqueous solution that a concentration of 1.5wt% of 120mL are slowly added dropwise is stirred, it is stirred to react 12h after being added dropwise, filters It washs to the pH=7 of filter cake, is dried under vacuum to constant weight in 50 DEG C, obtains compounded mix;
The preparation of carbon conductive ink:It takes isopropanol that preparation in deionized water is added and obtains the aqueous isopropanol of 25wt%, it will 60 parts of compounded mix, 15 parts of epoxy resin, 5 parts of polyacrylamide, 3 parts of polyvinylpyrrolidone are added in aqueous isopropanol and stir Mixing is to get to carbon conductive ink.
Example IV:The preparation three of carbon conductive ink
The preparation of carboxylic carbon nano-tube/nitrogen-doped graphene compound:Take carboxylic carbon nano-tube that deionized water is added In be dispersed with stirring, be made into the carboxylic carbon nano-tube aqueous solution of 3.5mg/mL, take nitrogen-doped graphene be added deionized water in stir Dispersion is mixed, the nitrogen-doped graphene aqueous solution of 14mg/mL is made into, by carboxylic carbon nano-tube aqueous solution and nitrogen-doped graphene water Solution by volume 4:1 mixing, stirs 4h, obtains mixed solution, freeze-drying process 43h obtains carboxylic carbon nano-tube/nitrogen Doped graphene compound;
The preparation of compounded mix:Take acetonitrile and water by volume 6:4 mixing, and cetyl trimethylammonium bromide is added and stirs Mixing is mixed, acetonitrile solution is made, takes 7.5g carboxylic carbon nano-tubes/nitrogen-doped graphene compound to be added in deionized water, stirs Dispersion 30min is mixed, the hydrochloric acid solution that acetonitrile solution and 0.2mol/L is added stirs and evenly mixs, and it is single that 0.5g pyrroles is added under condition of ice bath Body, and the ferric chloride in aqueous solution that 1.5wt% is slowly added dropwise is stirred, 11h, filtration washing to filter cake are stirred to react after being added dropwise PH=7 is dried under vacuum to constant weight in 45 DEG C, obtains compounded mix;
The preparation of carbon conductive ink:It takes isopropanol that preparation in deionized water is added and obtains the aqueous isopropanol of 25wt%, it will 50 parts of compounded mix, 10 parts of epoxy resin, 3 parts of polyacrylamide, 2 parts of sodium carboxymethylcellulose are added in aqueous isopropanol and stir Mixing is to get to carbon conductive ink.
The carbon conductive ink that the above method is prepared can be used for being formed by curing capacitive touch screen electrode, and application process is adopted It is molded method with screen painting or jet drying.
The above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although with reference to preferred embodiment to this hair It is bright to be described in detail, it will be understood by those of ordinary skill in the art that, it can modify to technical scheme of the present invention Or equivalent replacement should all cover the claim in the present invention without departing from the objective and range of technical solution of the present invention In range.Technology that the present invention is not described in detail, shape, construction part are known technology.

Claims (8)

1. capacitive touch screen carbon conductive ink, which is characterized in that include the raw material of following parts by weight:Compounded mix 44~ 60 parts, 8~15 parts of macromolecule resin, 2~5 parts of surfactant, 1~3 part of dispersion stabilizer and solvent, the compounded mix are Carboxylic carbon nano-tube, nitrogen-doped graphene and pyrroles's polymerization are made.
2. capacitive touch screen carbon conductive ink according to claim 1, which is characterized in that prepared by the compounded mix Raw material in carboxylic carbon nano-tube, nitrogen-doped graphene and the mass ratio of pyrroles be 1:1:(0.1~0.2).
3. capacitive touch screen carbon conductive ink according to claim 2, which is characterized in that the macromolecule resin is Epoxy resin, the surfactant are polyacrylamide, and the dispersion stabilizer is sodium carboxymethylcellulose or polyethylene pyrrole Pyrrolidone, the solvent are isopropanols.
4. the preparation method of capacitive touch screen carbon conductive ink according to claim 3, which is characterized in that including with Lower step:
The preparation of carboxylic carbon nano-tube/nitrogen-doped graphene compound:It takes carboxylic carbon nano-tube to be added in deionized water to stir Dispersion is mixed, the carboxylic carbon nano-tube aqueous solution of 3~4mg/mL is made into, takes nitrogen-doped graphene that stirring point in deionized water is added It dissipates, the nitrogen-doped graphene aqueous solution of 12~16mg/mL is made into, by carboxylic carbon nano-tube aqueous solution and nitrogen-doped graphene water Solution by volume 4:1 mixing, stirs 3~5h, obtains mixed solution, 40~45h of freeze-drying process obtains carboxylated carbon and receives Mitron/nitrogen-doped graphene compound;
The preparation of compounded mix:Take acetonitrile and water by volume 6:4 mixing, and it is mixed that cetyl trimethylammonium bromide stirring is added It is even, acetonitrile solution is made, takes carboxylic carbon nano-tube/nitrogen-doped graphene compound to be added in deionized water, is dispersed with stirring 30min, the hydrochloric acid solution that acetonitrile solution and 0.2mol/L is added stir and evenly mix, and pyrrole monomer are added under condition of ice bath, and stir The ferric chloride in aqueous solution of 1.5wt% is slowly added dropwise, 10~12h, the pH=of filtration washing to filter cake are stirred to react after being added dropwise 7, it is dried under vacuum to constant weight in 40~50 DEG C, obtains compounded mix;
The preparation of carbon conductive ink:It takes isopropanol that preparation in deionized water is added and obtains the aqueous isopropanol of 25wt%, it will be compound Filler, macromolecule resin, surfactant, dispersion stabilizer, which are added in aqueous isopropanol, to be stirred and evenly mixed to get oily to carbonaceous conductive Ink.
5. the preparation method of capacitive touch screen carbon conductive ink according to claim 4, which is characterized in that the nitrogen Doped graphene is that graphene oxide is prepared by Hummers methods using natural graphite powder as raw material, then with graphene oxide For raw material, melamine is reducing agent and nitrogen dopant, is prepared by hydro-thermal method.
6. the preparation method of capacitive touch screen carbon conductive ink according to claim 5, which is characterized in that described multiple It is 1 to close the mass ratio of pyrrole monomer and carboxylic carbon nano-tube/nitrogen-doped graphene compound in the preparation of filler:(10~ 20)。
7. the preparation method of capacitive touch screen carbon conductive ink according to claim 6, which is characterized in that the pyrrole Cough up monomer and FeCl3·6H2The mass ratio of O is 1:3.5.
8. the application for the carbon conductive ink that the method according to claim 11 is prepared, which is characterized in that the carbonaceous conductive Ink uses screen painting or spray up moulding for being formed by curing capacitive touch screen electrode, application process.
CN201810328868.2A 2018-04-13 2018-04-13 Capacitive touch screen carbon conductive ink and the preparation method and application thereof Pending CN108641486A (en)

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Application publication date: 20181012