CN110041762A - A kind of preparation method of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink - Google Patents
A kind of preparation method of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink Download PDFInfo
- Publication number
- CN110041762A CN110041762A CN201910433625.XA CN201910433625A CN110041762A CN 110041762 A CN110041762 A CN 110041762A CN 201910433625 A CN201910433625 A CN 201910433625A CN 110041762 A CN110041762 A CN 110041762A
- Authority
- CN
- China
- Prior art keywords
- silver
- microcrystalline cellulose
- parts
- cellulose base
- carrying nano
- 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.)
- Granted
Links
- 229920000168 Microcrystalline cellulose Polymers 0.000 title claims abstract description 148
- 235000019813 microcrystalline cellulose Nutrition 0.000 title claims abstract description 148
- 239000008108 microcrystalline cellulose Substances 0.000 title claims abstract description 148
- 229940016286 microcrystalline cellulose Drugs 0.000 title claims abstract description 148
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 239000002245 particle Substances 0.000 claims abstract description 108
- 235000010980 cellulose Nutrition 0.000 claims abstract description 74
- 229920002678 cellulose Polymers 0.000 claims abstract description 74
- 239000001913 cellulose Substances 0.000 claims abstract description 74
- 239000013081 microcrystal Substances 0.000 claims abstract description 68
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 19
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 17
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims description 52
- 239000013049 sediment Substances 0.000 claims description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 35
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- 239000006185 dispersion Substances 0.000 claims description 32
- 238000006243 chemical reaction Methods 0.000 claims description 30
- 239000000725 suspension Substances 0.000 claims description 28
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 238000010008 shearing Methods 0.000 claims description 16
- 239000002518 antifoaming agent Substances 0.000 claims description 14
- 238000004945 emulsification Methods 0.000 claims description 14
- 235000019441 ethanol Nutrition 0.000 claims description 14
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 9
- 239000006228 supernatant Substances 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 8
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 229920005610 lignin Polymers 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 229920001169 thermoplastic Polymers 0.000 claims description 6
- 239000004416 thermosoftening plastic Substances 0.000 claims description 6
- 239000004925 Acrylic resin Substances 0.000 claims description 5
- 229920000178 Acrylic resin Polymers 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000005292 vacuum distillation Methods 0.000 claims description 2
- 229920001046 Nanocellulose Polymers 0.000 claims 3
- 230000005611 electricity Effects 0.000 claims 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 claims 1
- 229920006389 polyphenyl polymer Polymers 0.000 claims 1
- 239000000976 ink Substances 0.000 abstract description 108
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 34
- 229910052709 silver Inorganic materials 0.000 abstract description 31
- 239000004332 silver Substances 0.000 abstract description 31
- 239000000126 substance Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 18
- 238000012360 testing method Methods 0.000 description 12
- 229920002120 photoresistant polymer Polymers 0.000 description 11
- 238000002604 ultrasonography Methods 0.000 description 10
- 239000002253 acid Substances 0.000 description 9
- 238000007639 printing Methods 0.000 description 9
- 239000011347 resin Substances 0.000 description 9
- 229920005989 resin Polymers 0.000 description 9
- 150000001336 alkenes Chemical class 0.000 description 8
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 description 8
- 239000003292 glue Substances 0.000 description 8
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 8
- 241000209094 Oryza Species 0.000 description 7
- 235000007164 Oryza sativa Nutrition 0.000 description 7
- 235000009566 rice Nutrition 0.000 description 7
- 238000005299 abrasion Methods 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 6
- 238000011161 development Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N Propene Chemical compound CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 241000894006 Bacteria Species 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
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 210000000795 conjunctiva Anatomy 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 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
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 230000035807 sensation Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
-
- 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
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
-
- 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
- C09D11/14—Printing inks based on carbohydrates
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Molecular Biology (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Conductive Materials (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a kind of preparation methods of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink, the present invention is modified it with after sodium borohydride by the way that silver nitrate solution is added to nano micro crystal cellulose solution, obtains silver-carrying nano microcrystalline cellulose base conductive particle；Polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink is prepared based on this silver-carrying nano microcrystalline cellulose base conductive particle again, can greatly improve the performance of electrically conductive ink.The present invention provides novel silver electrically conductive inks, have preferable chemical stability, are not easy to be oxidized, improve the electric property of silver-colored electrically conductive ink, and reduce production cost.
Description
Technical field
The present invention relates to a kind of preparation methods of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink, belong to and lead
Electric material preparation field.
Background technique
In recent years, with the aggravation of environmental problem, renewable resource becomes the inevitable choice of people.Cellulose is on the earth
The most abundant carbohydrate, it is the natural macromolecular material that plant is synthesized by photosynthesis, is widely present in plant, moves
In object and bacterium, therefore become the emphasis of researcher's concern.And nano micro crystal cellulose not only has the characteristic of cellulose, may be used also
There is other characteristics simultaneously by a series of modifications.Research about nano micro crystal cellulose is also many, micro- from nanometer
The preparation of crystalline cellulose is modified to application, and the research of nano micro crystal cellulose just gradually moves to maturity.Nanotechnology is as 21 generation
The hot spot of discipline field of scientific study has pushed the development of electrically conductive ink.With the development of electronic technology, electrically conductive ink is as printing
One of critical material of electronics.Now, main electrically conductive ink to be used has gold system conductive ink, silver system conductive ink, copper system conductive ink
And carbon series conductive ink etc., wherein not only electric conductivity is excellent for silver, chemical stability is good, is not easy to be oxidized, raw even if being oxidized
At oxide it is also electrically conductive.This advantage is many metal materials condition as not available for copper, but nano silver is being sintered
It is easy cracking in the process.Performance is led to promote printed wiring, printed wiring bond strength can effectively be promoted by needing to develop one kind
With the chain conducing composite material of electric conductivity.
Summary of the invention
The object of the present invention is to provide a kind of preparation sides of polyaniline package silver-carrying nano microcrystalline cellulose base conductive ink
Method.The present invention provides novel silver electrically conductive inks, have preferable chemical stability, are not easy to be oxidized, not only increase silver and lead
The electric property of electric ink, and reduce production cost.
A kind of technical solution of the present invention: preparation side of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink
Method carries out in the steps below:
It a, is 0.2%-0.6% nano micro crystal cellulose solution ultrasonic vibration 10- by 40-60 parts of concentration by mass fraction
20min obtains nano micro crystal cellulose suspension liquor；20-30 parts of concentration are added to nano micro crystal cellulose suspension liquor
For the silver nitrate solution of 0.1%-0.2%, ultrasonic disperse 3-8 minutes；
B, the sodium borohydride solution that 20-30 parts of concentration are 0.05%-0.1%, stirring are slowly added in Xiang Shangshu mixed liquor
3-8 minutes, obtain silver-carrying nano microcrystalline cellulose mixed liquor；It is centrifuged again washing, taking precipitate obtains carrying silver
Nano micro crystal cellulose base conductive particle；
Wherein material obtained in step a is directly used in step b, and the number relationship of the two is corresponding；
C, it is 4- that 10-30 parts of silver-carrying nano microcrystalline cellulose base conductive particles and 65-95 parts of concentration are separately taken by mass fraction
8% and molecular weight be 1000-2000Da lignin sulfonic acid sodium solution be mixed into capable dispersion, form silver-carrying nano microcrystalline cellulose
Base conductive particle stable dispersion solution；
D, 3-8 parts of aniline are added to silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion solution, at 60-70 DEG C
High-speed stirred 0.8-1.2h, then temperature adjust to 8 DEG C hereinafter, be added 0.5-2mol/L hydrochloric acid solution to pH be 1.5-3, then
2-6 parts of ammonium persulfate is added and washing is centrifuged after reaction, taking precipitate obtains in 5 DEG C or less reaction 0.8-1.2h
Polyaniline wraps up silver-carrying nano microcrystalline cellulose base conductive particle；Wherein, the silver-carrying nano microcrystalline cellulose base separately taken in step c
Conductive particle is made of the preparation method in step a and step b, but since silver-carrying nano microcrystalline cellulose base conductive particle is
Object is made from step a and b individually separately to take, the number ratio in number ratio and step a-b in step c and d is not related.
E, it separately takes polyaniline to wrap up 30-60 parts of silver-carrying nano microcrystalline cellulose base conductive particle by mass fraction, 20- is added
It is stirred evenly after 50 parts of water and 10-20 parts of ethyl alcohol, adds 0.05-0.2 parts of defoaming agents and continue to stir, be eventually adding 4~8 parts
High temperature sintering thermoplastic acrylic resin carries out emulsification 10-20min under high-speed shearing machine, obtains polyaniline package load silver and receives
Rice microcrystalline cellulose base electrically conductive ink；Wherein, conductive of the polyaniline package silver-carrying nano microcrystalline cellulose base separately taken in step e
Grain is made of the preparation method in step c and step d；But due to conductive, polyaniline package silver-carrying nano microcrystalline cellulose base
Grain is object to be made from step c individually separately to take, therefore the number relationship in step e is individually independent, with the number ratio in step a-d
It is not related.
The preparation method of polyaniline above-mentioned package silver-carrying nano microcrystalline cellulose base electrically conductive ink, in the steps below into
Row:
It a, is 0.3%-0.5% nano micro crystal cellulose solution ultrasonic vibration 14- by 48-52 parts of concentration by mass fraction
18min obtains nano micro crystal cellulose suspension liquor；22-28 parts of concentration are added to nano micro crystal cellulose suspension liquor again
For the silver nitrate solution of 0.13-0.18%, ultrasonic disperse 4-6 minutes；
B, the sodium borohydride solution that 22-28 parts of concentration are 0.06%-0.09%, stirring are slowly added in Xiang Shangshu mixed liquor
3-8 minutes, obtain silver-carrying nano microcrystalline cellulose mixed liquor；It is centrifuged again washing, taking precipitate obtains carrying silver
Nano micro crystal cellulose base conductive particle；
C, it is 5- that 15-25 parts of silver-carrying nano microcrystalline cellulose base conductive particles and 75-85 parts of concentration are separately taken by mass fraction
7% and molecular weight be 1000-2000Da lignin sulfonic acid sodium solution be mixed into capable dispersion, form silver-carrying nano microcrystalline cellulose
Base conductive particle stable dispersion solution；
D, 4-6 parts of aniline are added to silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion solution, at 62-68 DEG C
High-speed stirred 0.9-1.1h, then temperature is adjusted to 8 DEG C hereinafter, the hydrochloric acid solution of 0.8-1.5mol/L is added to pH to 1.8-
2.5,3-5 parts of ammonium persulfate is added, in 5 DEG C or less reaction 0.9-1.1h, washing is centrifuged after reaction, takes precipitating
Object obtains polyaniline package silver-carrying nano microcrystalline cellulose base conductive particle；
E, it separately takes polyaniline to wrap up 35-55 parts of silver-carrying nano microcrystalline cellulose base conductive particle by mass fraction, 25- is added
It is stirred evenly after 45 parts of water and 12-18 parts of ethyl alcohol, adds 0.1-0.18 parts of defoaming agents and continue to stir, be eventually adding 5~7 parts
High temperature sintering thermoplastic acrylic resin carries out emulsification 10-20min under high-speed shearing machine, obtains polyaniline package load silver and receives
Rice microcrystalline cellulose base electrically conductive ink.
The preparation method of polyaniline-coated silver-carrying nano microcrystalline cellulose base conductive particle above-mentioned, in the steps below into
Row:
It a, is that 0.4% nano micro crystal cellulose solution ultrasonic vibration 15min obtains nanometer by 50 parts of concentration by mass fraction
Microcrystalline cellulose suspension liquor；The silver nitrate that 25 parts of concentration are 0.15% is added to nano micro crystal cellulose suspension liquor again
Solution, ultrasonic disperse 5 minutes；
B, it is slowly added to the sodium borohydride solution that 25 parts of concentration are 0.08% in Xiang Shangshu mixed liquor, stirs 5 minutes, makes it
It is uniformly mixed, obtains silver-carrying nano microcrystalline cellulose mixed liquor；It is centrifuged again washing, taking precipitate obtains carrying silver
Nano micro crystal cellulose base conductive particle；
C, 20 parts of silver-carrying nano microcrystalline cellulose base conductive particles are separately taken by mass fraction and 80 parts of concentration be 6.25% and
Molecular weight is 1000-2000Da lignin sulfonic acid sodium solution, forms silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion
Solution；
D, 5 parts of aniline are added to silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion solution, the high speed at 65 DEG C
1.0h is stirred, then temperature is adjusted to 8 DEG C hereinafter, the hydrochloric acid solution that 1.0mol/L is added adds 4 parts of mistake to pH to 2.0
Washing is centrifuged in 5 DEG C or less reaction 1.0h in ammonium sulfate after reaction, taking precipitate obtains polyaniline package load silver and receives
Rice microcrystalline cellulose base conductive particle；
E, it separately takes polyaniline to wrap up 45 parts of silver-carrying nano microcrystalline cellulose base conductive particle by mass fraction, 34 parts of water is added
It is stirred evenly with after 15 parts of ethyl alcohol, adds 0.15 part of defoaming agent and continue to stir, be eventually adding 6 parts of high temperature sintering thermoplasticity third
Olefin(e) acid resin carries out emulsification 15min under high-speed shearing machine, obtains polyaniline package silver-carrying nano microcrystalline cellulose base conductive oil
Ink.
The preparation method of polyaniline above-mentioned package silver-carrying nano microcrystalline cellulose base electrically conductive ink in the step b, is adopted
It is stirred with electric mixer, occurs that its reaction uniformly.
The preparation method of polyaniline above-mentioned package silver-carrying nano microcrystalline cellulose base electrically conductive ink, in the step b
Centrifuge separation washing is to be centrifuged 10min under the revolving speed of 10000rpm, and ultrasound in deionized water is added in obtained sediment and is shaken
Dynamic 30min washing repeats the above process repeatedly until supernatant liquor is white.
The preparation method of polyaniline above-mentioned package silver-carrying nano microcrystalline cellulose base electrically conductive ink, in the step d
Aniline is to carry out vacuum distillation pretreatment in advance, is handled until fraction is colorless and transparent.
The preparation method of polyaniline above-mentioned package silver-carrying nano microcrystalline cellulose base electrically conductive ink, in the step d
High-speed stirred is carried out by high speed shear instrument.
The preparation method of polyaniline above-mentioned package silver-carrying nano microcrystalline cellulose base electrically conductive ink in the step e, makes
The hydrochloric acid of 1mol/L is slowly added to low-speed agitator pH is adjusted.
The preparation method of polyaniline above-mentioned package silver-carrying nano microcrystalline cellulose base electrically conductive ink, in the step d
Centrifuge separation washing is to be centrifuged 10min under the revolving speed of 10000rpm, and ultrasound in deionized water is added in obtained sediment and is shaken
Dynamic 30min washing, repeats the above process repeatedly until sediment becomes navy blue.
The preparation method of polyaniline above-mentioned package silver-carrying nano microcrystalline cellulose base electrically conductive ink, in the step e
The revolving speed of high-speed shearing machine is 3000r/min.
Compared with the prior art, the present invention is by being added silver nitrate solution and sodium borohydride to nano micro crystal cellulose solution
It is modified afterwards, obtains silver-carrying nano microcrystalline cellulose base conductive particle；Silver particles are adsorbed on nano microcrystalline fiber at this time
On element, can not only silver particles be made preferably to be dissolved in water, dispersibility can also be improved, while being adsorbed on nano micro crystal cellulose
Silver particles it is smaller, can achieve Nano grade, and there is better electric conductivity, then with this silver-carrying nano microcrystalline cellulose
Polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink is prepared based on plain base conductive particle, can greatly be improved
The performance of electrically conductive ink.Wrapping up conducting wire made of silver-carrying nano microcrystalline cellulose base electrically conductive ink spray printing with polyaniline has more preferably
Electric conductivity, more dense structure, higher resolution ratio and brighter surface, while than silk-screen silver wire have it is stronger
Corrosion-resistant and resistance to moisture ability.And the large specific surface area of the silver particles of Nano grade, the atomicity of unit area is more,
The adhesive ability to substrate can be improved, keep ink not easy to fall off.These advantages can make it print structure on flex plate
Electronic product more complicated, area is bigger.In addition, the present invention has also done further improvement in technique and formula, thus into
Improve to one step the performance of electrically conductive ink.
Detailed description of the invention:
Fig. 1: the principle of the present invention figure；
Fig. 2: the present invention schemes for the phenomenon that centrifuge separation in step b and centrifuge washing；
Fig. 3: the effect picture in the embodiment of the present invention 1 after electrically conductive ink layering；
Fig. 4: the effect picture in the embodiment of the present invention 2 after electrically conductive ink layering；
Fig. 5: the effect picture in the embodiment of the present invention 3 after electrically conductive ink layering；
Fig. 6: the effect picture in the embodiment of the present invention 4 after electrically conductive ink layering；
Fig. 7: nano micro crystal cellulose particle size itself；
Fig. 8: the electrically conductive ink size in the embodiment of the present invention 3；
Fig. 9: the electrically conductive ink size in the embodiment of the present invention 6；
Figure 10: the electrically conductive ink size in the embodiment of the present invention 5；
Figure 11: the electrically conductive ink size in reference examples；
Figure 12: electrically conductive ink of the present invention prints test effect figure；
Figure 13: effect picture before electrically conductive ink abrasion test of the present invention；
Figure 14: effect picture after electrically conductive ink abrasion test of the present invention；.
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawings and examples, but be not intended as to the present invention limit according to
According to.
Embodiment 1: a kind of preparation method of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink, Method And Principle
As shown in Figure 1, simultaneously carrying out in the steps below:
It a, is that 0.3% nano micro crystal cellulose solution ultrasonic vibration 11min obtains nano micro crystal cellulose by 48mL concentration
Suspension liquor；It is 0.1% silver nitrate solution, ultrasound point that 28mL parts of concentration, which are added, to nano micro crystal cellulose suspension liquor again
It dissipates 5 minutes and stirs, be uniformly mixed it；
B, it is slowly added to the sodium borohydride solution that 25mL concentration is 0.1% in Xiang Shangshu mixed liquor, stirs 5 minutes, uses
Electric mixer is uniformly mixed it, obtains silver-carrying nano microcrystalline cellulose mixed liquor；It is centrifuged under the revolving speed of 10000rpm again
Obtained sediment is added ultrasonic vibration 30min in deionized water and washed, repeated the above process repeatedly until upper layer by 10min
Clear liquid is white shown in Fig. 2, and the sediment after then taking washing obtains silver-carrying nano microcrystalline cellulose base conductive particle；
C, it separately takes 20g silver-carrying nano microcrystalline cellulose base conductive particle and 90mL concentration is 6.25% sodium lignin sulfonate
The mixing of (molecular weight 1000-2000Da) solution is dispersed, and silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion is formed
Solution；
D, to stable dispersion solution be added 5mL aniline, the high-speed stirred 1h at 65 DEG C, then temperature adjust to 8 DEG C hereinafter,
The hydrochloric acid solution of 1mol/L is added to pH to 2, adds the ammonium persulfate of 3mL, in 5 DEG C or less reaction 1h, carried out after reaction from
Heart separating, washing is centrifuged 10min under the revolving speed of 10000rpm, and ultrasonic vibration in deionized water is added in obtained sediment
30min washing repeats the above process repeatedly until sediment becomes navy blue, and the sediment after taking washing obtains polyaniline package
Silver-carrying nano microcrystalline cellulose base conductive particle；
E, it separately takes polyaniline to wrap up silver-carrying nano microcrystalline cellulose base conductive particle 4.1g, 3.7mL water and 1.5mL second is added
It is stirred evenly after alcohol, the defoaming agent for adding 0.1mL 15% continues to stir, and is eventually adding the high temperature sintering thermoplasticity third of 0.6g
Olefin(e) acid resin carries out emulsification 10min under high-speed shearing machine, obtains polyaniline package silver-carrying nano microcrystalline cellulose base conductive oil
Ink.
Embodiment 2: a kind of preparation method of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink, and by following
Step carries out:
It a, is that 0.5% nano micro crystal cellulose solution ultrasonic vibration 18min obtains nano micro crystal cellulose by 58mL concentration
Suspension liquor；The silver nitrate solution that 24mL concentration is 0.1%, ultrasound point is added to nano micro crystal cellulose suspension liquor again
It dissipates 5 minutes and stirs, be uniformly mixed it；
B, it is slowly added to that the sodium borohydride solution that 25mL concentration is 0.1% is added in Xiang Shangshu mixed liquor, stirs 5 minutes,
It is uniformly mixed it using electric mixer, obtains silver-carrying nano microcrystalline cellulose mixed liquor；Again under the revolving speed of 10000rpm
Be centrifuged 10min, by obtained sediment be added deionized water in ultrasonic vibration 30min wash, repeat the above process repeatedly until
Supernatant liquor is white, and the sediment after then taking washing obtains silver-carrying nano microcrystalline cellulose base conductive particle；
C, it separately takes 20g silver-carrying nano microcrystalline cellulose base conductive particle and 75mL concentration is 6.25% sodium lignin sulfonate
The mixing of (molecular weight 1000-2000Da) solution is dispersed, and silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion is formed
Solution；
D, to stable dispersion solution be added 7mL aniline, the high-speed stirred 1h at 63 DEG C, then temperature adjust to 8 DEG C hereinafter,
The hydrochloric acid solution of 1mol/L adds the ammonium persulfate of 6mL, in 5 DEG C or less reaction 1h, centrifugation point is carried out after reaction to pH to 2
From washing, it is centrifuged 10min under the revolving speed of 10000rpm, ultrasonic vibration 30min in deionized water is added in obtained sediment
Washing repeats the above process repeatedly until sediment becomes navy blue, and the sediment after taking washing obtains polyaniline package and carries silver
Nano micro crystal cellulose base conductive particle.
E, it separately takes polyaniline to wrap up silver-carrying nano microcrystalline cellulose base conductive particle 4.7g, 3mL water and 1.5mL ethyl alcohol is added
After stir evenly, the defoaming agent for adding 0.1mL 15% continues to stir, and is eventually adding the high temperature sintering thermoplastic propene of 0.6g
Acid resin carries out emulsification 10min under high-speed shearing machine, obtains polyaniline package silver-carrying nano microcrystalline cellulose base conductive oil
Ink.
Embodiment 3: a kind of preparation method of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink, and by following
Step carries out:
It a, is that 0.4% nano micro crystal cellulose solution ultrasonic vibration 15min obtains nano micro crystal cellulose by 50mL concentration
Suspension liquor；The silver nitrate solution that 25mL concentration is 0.15%, ultrasound is added to nano micro crystal cellulose suspension liquor again
Disperse to stir for 5 minutes, is uniformly mixed it；
B, it is slowly added to that the sodium borohydride solution that 25mL concentration is 0.08% is added in Xiang Shangshu mixed liquor, stirs 5 minutes,
It is uniformly mixed it using electric mixer, obtains silver-carrying nano microcrystalline cellulose mixed liquor；Again under the revolving speed of 10000rpm
Be centrifuged 10min, by obtained sediment be added deionized water in ultrasonic vibration 30min wash, repeat the above process repeatedly until
Supernatant liquor is white, and the sediment after then taking washing obtains silver-carrying nano microcrystalline cellulose base conductive particle；
C, it separately takes 20g silver-carrying nano microcrystalline cellulose base conductive particle and 80mL concentration is 6.25% sodium lignin sulfonate
The mixing of (molecular weight 1000-2000Da) solution is dispersed, and silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion is formed
Solution；
D, to stable dispersion solution be added 5mL aniline, the high-speed stirred 1h at 60-70 DEG C, then temperature adjust to 8 DEG C with
Under, the hydrochloric acid solution of 1mol/L adds the ammonium persulfate of 6mL, in 5 DEG C or less reaction 1h, is centrifuged after reaction to pH to 2
Separating, washing is centrifuged 10min under the revolving speed of 10000rpm, and ultrasonic vibration in deionized water is added in obtained sediment
30min washing repeats the above process repeatedly until sediment becomes navy blue, and the sediment after taking washing is that polyaniline package carries
Silver nanoparticle microcrystalline cellulose base conductive particle.
E, it separately takes polyaniline to wrap up silver-carrying nano microcrystalline cellulose base conductive particle 4.3g, 3.5mL water and 1.5mL second is added
It is stirred evenly after alcohol, the defoaming agent for adding 0.1mL 15% continues to stir, and is eventually adding the high temperature sintering thermoplasticity third of 0.6g
Olefin(e) acid resin carries out emulsification 10min under high-speed shearing machine, obtains polyaniline package silver-carrying nano microcrystalline cellulose base conductive oil
Ink.
Embodiment 4: a kind of preparation method of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink, and by following
Step carries out:
It a, is that 0.4% nano micro crystal cellulose solution ultrasonic vibration 15min obtains nano micro crystal cellulose by 50mL concentration
Suspension liquor；The silver nitrate solution that 25mL concentration is 0.13%, ultrasound is added to nano micro crystal cellulose suspension liquor again
Disperse to stir for 5 minutes, is uniformly mixed it；
B, it is slowly added to that the sodium borohydride solution that 25mL concentration is 0.08% is added in Xiang Shangshu mixed liquor, stirs 5 minutes,
It is uniformly mixed it using electric mixer, obtains silver-carrying nano microcrystalline cellulose mixed liquor；Again under the revolving speed of 10000rpm
Be centrifuged 10min, by obtained sediment be added deionized water in ultrasonic vibration 30min wash, repeat the above process repeatedly until
Supernatant liquor is white, and the sediment after then taking washing obtains silver-carrying nano microcrystalline cellulose base conductive particle；
C, it separately takes 20g silver-carrying nano microcrystalline cellulose base conductive particle and 80mL concentration is 6.25% sodium lignin sulfonate
The mixing of (molecular weight 1000-2000Da) solution is dispersed, and silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion is formed
Solution；
D, to stable dispersion solution be added 5mL aniline, the high-speed stirred 1h at 65 DEG C, then temperature adjust to 8 DEG C hereinafter,
The hydrochloric acid solution of 1mol/L adds the ammonium persulfate of 4mL, in 5 DEG C or less reaction 1h, centrifugation point is carried out after reaction to pH to 2
From washing, it is centrifuged 10min under the revolving speed of 10000rpm, ultrasonic vibration 30min in deionized water is added in obtained sediment
Washing repeats the above process repeatedly until sediment becomes navy blue, and the sediment after taking washing carries silver for polyaniline package and receives
Rice microcrystalline cellulose base conductive particle.
E, it separately takes polyaniline to wrap up silver-carrying nano microcrystalline cellulose base conductive particle 4.3g, 3.5mL water and 1.5mL second is added
It is stirred evenly after alcohol, the defoaming agent for adding 0.1mL 15% continues to stir, and is eventually adding the high temperature sintering thermoplasticity third of 0.6g
Olefin(e) acid resin carries out emulsification 10min under high-speed shearing machine, obtains polyaniline package silver-carrying nano microcrystalline cellulose base conductive oil
Ink.
Embodiment 5: a kind of preparation method of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink, and by following
Step carries out:
It a, is that 0.4% nano micro crystal cellulose solution ultrasonic vibration 15min obtains nano micro crystal cellulose by 50mL concentration
Suspension liquor；The silver nitrate solution that 25mL concentration is 0.12%, ultrasound is added to nano micro crystal cellulose suspension liquor again
Disperse to stir for 5 minutes, is uniformly mixed it；
B, it is slowly added to that the sodium borohydride solution that 25mL concentration is 0.08% is added in Xiang Shangshu mixed liquor, stirs 5 minutes,
It is uniformly mixed it using electric mixer, obtains silver-carrying nano microcrystalline cellulose mixed liquor；Again under the revolving speed of 10000rpm
Be centrifuged 10min, by obtained sediment be added deionized water in ultrasonic vibration 30min wash, repeat the above process repeatedly until
Supernatant liquor is white, and the sediment after then taking washing obtains silver-carrying nano microcrystalline cellulose base conductive particle；
It c, is that 6.25% sodium lignin sulfonate (divides by 20g silver-carrying nano microcrystalline cellulose base conductive particle and 80mL concentration
Son amount 1000-2000Da) solution mixing dispersed, formed silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion it is molten
Liquid；
D, to stable dispersion solution be added 5mL aniline, the high-speed stirred 1h at 65 DEG C, then temperature adjust to 8 DEG C hereinafter,
The hydrochloric acid solution of 1mol/L adds the ammonium persulfate of 4mL, in 5 DEG C or less reaction 1h, centrifugation point is carried out after reaction to pH to 2
From washing, it is centrifuged 10min under the revolving speed of 10000rpm, ultrasonic vibration 30min in deionized water is added in obtained sediment
Washing repeats the above process repeatedly until sediment becomes navy blue, and the sediment after taking washing carries silver for polyaniline package and receives
Rice microcrystalline cellulose base conductive particle.
E, it separately takes polyaniline to wrap up silver-carrying nano microcrystalline cellulose base conductive particle 4.3g, 3.5mL water and 1.5mL second is added
It is stirred evenly after alcohol, the defoaming agent for adding 0.1mL 15% continues to stir, and is eventually adding the high temperature sintering thermoplasticity third of 0.6g
Olefin(e) acid resin carries out emulsification 10min under high-speed shearing machine, obtains polyaniline package silver-carrying nano microcrystalline cellulose base conductive oil
Ink.
Embodiment 6: a kind of preparation method of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink, and by following
Step carries out:
It a, is that 0.4% nano micro crystal cellulose solution ultrasonic vibration 15min obtains nano micro crystal cellulose by 50mL concentration
Suspension liquor；The silver nitrate solution that 25mL concentration is 0.18%, ultrasound is added to nano micro crystal cellulose suspension liquor again
Disperse to stir for 5 minutes, is uniformly mixed it；
B, it is slowly added to that the sodium borohydride solution that 25mL concentration is 0.08% is added in Xiang Shangshu mixed liquor, stirs 5 minutes,
It is uniformly mixed it using electric mixer, obtains silver-carrying nano microcrystalline cellulose mixed liquor；Again under the revolving speed of 10000rpm
Be centrifuged 10min, by obtained sediment be added deionized water in ultrasonic vibration 30min wash, repeat the above process repeatedly until
Supernatant liquor is white, and the sediment after then taking washing obtains silver-carrying nano microcrystalline cellulose base conductive particle；
C, it separately takes 20g silver-carrying nano microcrystalline cellulose base conductive particle and 80mL concentration is 6.25% sodium lignin sulfonate
The mixing of (molecular weight 1000-2000Da) solution is dispersed, and silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion is formed
Solution；
D, to stable dispersion solution be added 5mL aniline, the high-speed stirred 1h at 65 DEG C, then temperature adjust to 8 DEG C hereinafter,
The hydrochloric acid solution of 1mol/L adds the ammonium persulfate of 4mL, in 5 DEG C or less reaction 1h, centrifugation point is carried out after reaction to pH to 2
From washing, it is centrifuged 10min under the revolving speed of 10000rpm, ultrasonic vibration 30min in deionized water is added in obtained sediment and is washed
It washs, repeats the above process repeatedly until sediment becomes navy blue, the sediment after taking washing is that polyaniline wraps up silver-carrying nano
Microcrystalline cellulose base conductive particle.
E, it separately takes polyaniline to wrap up silver-carrying nano microcrystalline cellulose base conductive particle 4.3g, 3.5mL water and 1.5mL second is added
It is stirred evenly after alcohol, the defoaming agent for adding 0.1mL 15% continues to stir, and is eventually adding the high temperature sintering thermoplasticity third of 0.6g
Olefin(e) acid resin carries out emulsification 10min under high-speed shearing machine, obtains polyaniline package silver-carrying nano microcrystalline cellulose base conductive oil
Ink.
Embodiment 7: a kind of preparation method of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink, and by following
Step carries out:
It a, is that 0.4% nano micro crystal cellulose solution ultrasonic vibration 15min obtains nano micro crystal cellulose by 50mL concentration
Suspension liquor；The silver nitrate solution that 25mL concentration is 0.19%, ultrasound is added to nano micro crystal cellulose suspension liquor again
Disperse to stir for 5 minutes, is uniformly mixed it；
B, it is slowly added to that the sodium borohydride solution that 25mL concentration is 0.08% is added in Xiang Shangshu mixed liquor, stirs 5 minutes,
It is uniformly mixed it using electric mixer, obtains silver-carrying nano microcrystalline cellulose mixed liquor；Again under the revolving speed of 10000rpm
Be centrifuged 10min, by obtained sediment be added deionized water in ultrasonic vibration 30min wash, repeat the above process repeatedly until
Supernatant liquor is white, and the sediment after then taking washing obtains silver-carrying nano microcrystalline cellulose base conductive particle；
C, it separately takes 20g silver-carrying nano microcrystalline cellulose base conductive particle and 80mL concentration is 6.25% sodium lignin sulfonate
The mixing of (molecular weight 1000-2000Da) solution is dispersed, and silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion is formed
Solution；
D, to stable dispersion solution be added 5mL aniline, the high-speed stirred 1h at 65 DEG C, then temperature adjust to 8 DEG C hereinafter,
The hydrochloric acid solution of 1mol/L adds the ammonium persulfate of 4mL, in 5 DEG C or less reaction 1h, centrifugation point is carried out after reaction to pH to 2
From washing, it is centrifuged 10min under the revolving speed of 10000rpm, ultrasonic vibration 30min in deionized water is added in obtained sediment
Washing repeats the above process repeatedly until sediment becomes navy blue, and the sediment after taking washing carries silver for polyaniline package and receives
Rice microcrystalline cellulose base conductive particle.
E, it separately takes polyaniline to wrap up silver-carrying nano microcrystalline cellulose base conductive particle 4.3g, 3.5mL water and 1.5mL second is added
It is stirred evenly after alcohol, the defoaming agent for adding 0.1mL 15% continues to stir, and is eventually adding the high temperature sintering thermoplasticity third of 0.6g
Olefin(e) acid resin carries out emulsification 10min under high-speed shearing machine, obtains polyaniline package silver-carrying nano microcrystalline cellulose base conductive oil
Ink.
Embodiment 8: a kind of preparation method of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink, and by following
Step carries out:
It a, is that 0.4% nano micro crystal cellulose solution ultrasonic vibration 15min obtains nano micro crystal cellulose by 50mL concentration
Suspension liquor；The silver nitrate solution that 25mL concentration is 0.2%, ultrasound point is added to nano micro crystal cellulose suspension liquor again
It dissipates 5 minutes and stirs, be uniformly mixed it；
B, it is slowly added to that the sodium borohydride solution that 25mL concentration is 0.08% is added in Xiang Shangshu mixed liquor, stirs 5 minutes,
It is uniformly mixed it using electric mixer, obtains silver-carrying nano microcrystalline cellulose mixed liquor；Again under the revolving speed of 10000rpm
Be centrifuged 10min, by obtained sediment be added deionized water in ultrasonic vibration 30min wash, repeat the above process repeatedly until
Supernatant liquor is white, and the sediment after then taking washing obtains silver-carrying nano microcrystalline cellulose base conductive particle；
C, it separately takes 20g silver-carrying nano microcrystalline cellulose base conductive particle and 80mL concentration is 6.25% sodium lignin sulfonate
The mixing of (molecular weight 1000-2000Da) solution is dispersed, and silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion is formed
Solution；
D, to stable dispersion solution be added 5mL aniline, the high-speed stirred 1h at 65 DEG C, then temperature adjust to 8 DEG C hereinafter,
The hydrochloric acid solution of 1mol/L adds the ammonium persulfate of 4mL, in 5 DEG C or less reaction 1h, centrifugation point is carried out after reaction to pH to 2
From washing, it is centrifuged 10min under the revolving speed of 10000rpm, ultrasonic vibration 30min in deionized water is added in obtained sediment
Washing repeats the above process repeatedly until sediment becomes navy blue, and the sediment after taking washing carries silver for polyaniline package and receives
Rice microcrystalline cellulose base conductive particle.
E, it separately takes polyaniline to wrap up silver-carrying nano microcrystalline cellulose base conductive particle 4.3g, 3.5mL water and 1.5mL second is added
It is stirred evenly after alcohol, the defoaming agent for adding 0.1mL 15% continues to stir, and is eventually adding the high temperature sintering thermoplasticity third of 0.6g
Olefin(e) acid resin carries out emulsification 10min under high-speed shearing machine, obtains polyaniline package silver-carrying nano microcrystalline cellulose base conductive oil
Ink.
Reference examples: take the silver-colored electrically conductive ink of market conventional sales as reference examples.
Detection and analysis:
1, ink stability
Ink stability refer to the properties of ink remained unchanged in storage do not settle, not conjunctiva, not rancid
Performance.On the one hand, nano micro crystal cellulose (NCC) is due to high specific surface area, be on mechanics it is unstable, separately
On the one hand, since effect polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink (calling electrically conductive ink in the following text) of gravity can sink
Drop, but the particle of electrically conductive ink and very little, it can constantly carry out random movement.These reasons make it be both opposite
Stable is again unstable.Thus to the stability of the electrically conductive ink in the electrically conductive ink and reference examples in embodiment 1-6 into
Row test.
Firstly, the electrically conductive ink 1mL in each embodiment is taken to be placed in the bottle that keeps sample, 4mL water is then added.Stand every
1h, 2h, 4h, 6h, 8h, 12h, for 24 hours, 36h, 48h, 72h, 84h it is observed, until be layered, what is compared divides
The layer time is as shown in table 1, is analyzed according to stability of the table 1 to electrically conductive ink.
Table 1
From table 1 it follows that the separation time in embodiment is all larger than the separation time in reference examples, electrically conductive ink
Stability substantially enhances.From the embodiment 1-8 of table 1 as can be seen that embodiment 3 be it is the most stable, wherein Fig. 3 is embodiment
Effect picture in 1 after electrically conductive ink layering, Fig. 4 are the effect pictures in embodiment 2 after electrically conductive ink layering, and Fig. 5 is in embodiment 3
Effect picture after electrically conductive ink layering, Fig. 6 are the effect pictures in embodiment 4 after electrically conductive ink layering；Using control variate method pair
Silver nitrate solution concentration is changed (embodiment 1,2 does not make reference).Data can be seen that phase from embodiment 8- embodiment 3
For silver nitrate content, as the content of nano micro crystal cellulose increases, electrically conductive ink stability is with nano microcrystalline fibre
Dimension element content increase be first increases to reduce afterwards, this is because just start nano micro crystal cellulose content increase when, nano microcrystalline
A possibility that cellulose is in conjunction with silver particles also increase, and stability increases at this time, this shows that nano micro crystal cellulose plays point
The effect of powder.Then when nano micro crystal cellulose content continues to increase, the combination of nano micro crystal cellulose and silver starts to become
It is weak, so as to cause stability decline.
2, grain size analysis
The size distribution of electrically conductive ink in the main measurement embodiment 3 of this detection, embodiment 5, embodiment 6 and reference examples,
Wherein nano micro crystal cellulose particle size itself is as shown in Figure 7 between 100-1000nm；Measure the conductive oil in embodiment 3
Black size as shown in figure 8, electrically conductive ink size in embodiment 6 as shown in figure 9, electrically conductive ink in embodiment 5
Size is as shown in Figure 10, and the electrically conductive ink size in reference examples is as shown in figure 11；It can be seen that from Fig. 7 to Figure 11
The electrically conductive ink size distribution of embodiment 3 and embodiment 6 is also substantially between 100-1000nm, with nano micro crystal cellulose itself
Particle size relatively coincide, and particle size is smaller at this time, and distribution is more uniform, and electric conductivity is preferable.And the particle in reference examples
The size of the smaller far smaller than nano micro crystal cellulose particle size of size itself, causes electric conductivity to weaken.In embodiment 5
Silver base conductive ink granularity partial size becomes smaller, and distribution is also more uniform, but omits with nano micro crystal cellulose particle size itself
There is difference, electric conductivity is slightly insufficient with respect to for embodiment 3 and embodiment 6.
3, silk-screen printing performance
In experiment use sensitizer stencil making method, process flow be painting photosensitive liquid → baking version → printing down → development → baking version →
Colour-separation drafting.
(1) photoresists are poured into glue applicator and (note: pouring into the half of glue applicator volume) first when being coated with photoresists, it will
Silk screen is placed with 75 degree of horizontal sextant angle vertically, then the edge glue applicator Jiao Kou contacted with silk screen surface and slowly tilt make it is photosensitive
Glue is contacted with silk screen surface, then at the uniform velocity moves up glue applicator when until being 2-3cm with silk screen upper end distance and glue applicator leans outward
Tiltedly, flow back into photoresists in glue applicator.Lift glue applicator.This completes the coatings of a photoresists, just by photoresists
Reverse side is respectively coated with three times to ensure photoresists thickness.
(2) silk-screen plate of coated photoresists is put into plate whirler setting temperature is 55 DEG C of drying silk-screen plates, and silk-screen plate dries
Temperature cannot be too high when dry, and otherwise silk thread deformation influences mesh form.Silk-screen plate after drying is rinsed with water under high pressure dry
Only.
(3) film medicine film is faced upward when printing down, is placed on exposure desk.Then silk-screen plate is covered on the film, is adjusted
Whole silk-screen plate position (generally making the film lower position in version).According to the light source of the photobehavior of photoresists and printer spy
Property setting the time for exposure be 120s, turn on the switch.Printer executes printing down instruction automatically.
(4) because this use photoresists the characteristics of be it is not light-exposed water-soluble, the photoresists of areas are
Have no light sensation optical cement, rather than the photoresists of areas are light-exposed that photochemical reaction has occurred, so silk-screen plate is placed on sink
Interior tap water flushing can develop.
(5) silk-screen plate after development is placed in plate whirler and is dried, check halftone.
This test is printed on art paper, wherein to embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment
6 and reference examples tested, it is as shown in Fig. 12 to be ultimately imaged result, in Figure 12 it can be seen from embodiment 2, embodiment 3,
Embodiment 4, embodiment 5, the ink printing effect in embodiment 6 are and embodiment 3, real compared with improving significantly in reference examples
Diffusion phenomena will not occur for the ink printing for applying example 4 and implementation 5, and printing effect is very good, and the ink diffusion phenomenon of embodiment 2
Slightly occur, the black diffusion phenomena in reference examples are extremely serious.
4, ink abrasion resistance is tested
Ink abrasion resistance test is rubbed repeatedly by layer of ink of the quasi-instrument to ink or printed matter, is passed through later
Comparison friction front and back color difference changes to evaluate the wear-resisting property of ink or printed matter, and ink abrasion resistance testing machine can effectively divide
The problems such as layer of ink of analysis printed matter falls off, anti-wiping property is poor and the coating hardness of other products is poor.
Instrument used in this test is ink adhesive strength tester, and setting friction number is 50 circles, after observation friction
The flatness of ink particle tests embodiment 3, and for final result as shown in Figure 13-Figure 14, Figure 12 is the test for implementing 3
Before, after Figure 13 is the test of reference examples, it can be seen that embodiment 3 is after ink abrasion resistance is tested from Figure 13-Figure 14,
Smooth and smooth, fine, the wear-resisting property of ink particle flatness still more of the flatness of ink particle still more
Preferably, ink particle dropping situations are smaller.
5, conductivity measurement
Resistance measurement is carried out to the electrically conductive ink in embodiment 3-8 and reference examples, resistance is bigger, obstruction of the conductor to electric current
Effect is also bigger, illustrates that its electric conductivity is poorer.In this test, all it is measured using identical voltage, forms such as table 2
Shown in resistivity measurements.
Table 2
From Table 2, it can be seen that in embodiment 3- embodiment 8 silver base conductive ink resistance value, respectively less than in reference examples
Conventional silver-colored electrically conductive ink, electric conductivity of the invention significantly improve, from embodiment 8- embodiment 3 as can be seen that with nanometer
The increase of the ratio of microcrystalline cellulose, the electric conductivity of nanometer silver inks first increases to be reduced afterwards, when arriving embodiment 3, electric conductivity
Most preferably, then resistance increases again.This is because when nano micro crystal cellulose starts to increase, due to nano micro crystal cellulose itself
It is non-conductive, therefore when nano micro crystal cellulose content is higher, electric conductivity is begun to decline on the whole, but with point of silver particles
Dissipate property and water-soluble enhancing, electric conductivity gradually increases at this time, electric conductivity achieve the effect that in embodiment 3 it is best,
The dispersed and water-soluble of particle that i.e. nano micro crystal cellulose makes enhances the cooperation being optimal, then again due to nanometer
The nonconducting effect of microcrystalline cellulose itself, starts to reduce in example 4 again.
In conclusion the present invention to nano micro crystal cellulose solution by being added after silver nitrate solution and sodium borohydride to it
It is modified, obtains silver-carrying nano microcrystalline cellulose base conductive particle；Silver particles are adsorbed on nano micro crystal cellulose at this time, no
Can only silver particles be made preferably to be dissolved in water, dispersibility can also be improved, while be adsorbed on the silver granuel on nano micro crystal cellulose
Son is smaller, can achieve Nano grade, and have better electric conductivity, then lead with this silver-carrying nano microcrystalline cellulose base
Polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink is prepared based on electric particle, can greatly improve conductive oil
The performance of ink.Wrapping up conducting wire made of silver-carrying nano microcrystalline cellulose base electrically conductive ink spray printing with polyaniline has preferably conduction
Property, more dense structure, higher resolution ratio and brighter surface, while than silk-screen silver wire have stronger corrosion resistant
Erosion and resistance to moisture ability.And the large specific surface area of the silver particles of Nano grade, the atomicity of unit area is more, Ke Yiti
Height keeps ink not easy to fall off the adhesive ability of substrate.These advantages can make its printed on flex plate structure it is more complicated,
The bigger electronic product of area.
Claims (10)
1. a kind of preparation method of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink, it is characterised in that: by following
Step carries out:
It a, is 0.2%-0.6% nano micro crystal cellulose solution ultrasonic vibration 10-20min by 40-60 parts of concentration by mass fraction,
Obtain nano micro crystal cellulose suspension liquor；20-30 parts of concentration, which are added, to nano micro crystal cellulose suspension liquor is
The silver nitrate solution of 0.1%-0.2%, ultrasonic disperse 3-8 minutes；
B, the sodium borohydride solution that 20-30 parts of concentration are 0.05%-0.1% is slowly added in Xiang Shangshu mixed liquor, stirring 3-8 divides
Clock obtains silver-carrying nano microcrystalline cellulose mixed liquor；It is centrifuged again washing, it is micro- that taking precipitate obtains silver-carrying nano
Crystalline cellulose base conductive particle；
C, 10-30 parts of silver-carrying nano microcrystalline cellulose base conductive particles are separately taken by mass fraction and 65-95 parts of concentration be 4-8% and
The lignin sulfonic acid sodium solution that molecular weight is 1000-2000Da is mixed into capable dispersion, forms silver-carrying nano microcrystalline cellulose base and leads
The particle stabilized dispersion solution of electricity；
D, 3-8 parts of aniline are added to silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion solution, the high speed at 60-70 DEG C
Stir 0.8-1.2h, then temperature adjust to 8 DEG C hereinafter, be added 0.5-2mol/L hydrochloric acid solution to pH be 1.5-3, add
In 5 DEG C or less reaction 0.8-1.2h washing is centrifuged, taking precipitate obtains polyphenyl in 2-6 parts of ammonium persulfate after reaction
Amine wraps up silver-carrying nano microcrystalline cellulose base conductive particle；
E, it separately takes polyaniline to wrap up 30-60 parts of silver-carrying nano microcrystalline cellulose base conductive particle by mass fraction, is added 20-50 parts
It is stirred evenly after water and 10-20 parts of ethyl alcohol, adds 0.05-0.2 parts of defoaming agents and continue to stir, be eventually adding 4~8 parts of high temperature
It is sintered thermoplastic acrylic resin, emulsification 10-20min is carried out under high-speed shearing machine, it is micro- to obtain polyaniline package silver-carrying nano
Crystalline cellulose base electrically conductive ink.
2. the preparation method of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink according to claim 1,
It is characterized in that: carrying out in the steps below:
It a, is 0.3%-0.5% nano micro crystal cellulose solution ultrasonic vibration 14-18min by 48-52 parts of concentration by mass fraction
Obtain nano micro crystal cellulose suspension liquor；22-28 parts of concentration, which are added, to nano micro crystal cellulose suspension liquor again is
The silver nitrate solution of 0.13-0.18%, ultrasonic disperse 4-6 minutes；
B, it is slowly added to the sodium borohydride solution that 22-28 parts of concentration are 0.06%-0.09% in Xiang Shangshu mixed liquor, stirs 3-8
Minute, obtain silver-carrying nano microcrystalline cellulose mixed liquor；It is centrifuged again washing, taking precipitate obtains silver-carrying nano
Microcrystalline cellulose base conductive particle；
C, 15-25 parts of silver-carrying nano microcrystalline cellulose base conductive particles are separately taken by mass fraction and 75-85 parts of concentration be 5-7% and
The lignin sulfonic acid sodium solution that molecular weight is 1000-2000Da is mixed into capable dispersion, forms silver-carrying nano microcrystalline cellulose base and leads
The particle stabilized dispersion solution of electricity；
D, 4-6 parts of aniline are added to silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion solution, the high speed at 62-68 DEG C
Stir 0.9-1.1h, then temperature adjust to 8 DEG C hereinafter, be added 0.8-1.5mol/L hydrochloric acid solution to pH to 1.8-2.5, then
3-5 parts of ammonium persulfate is added and washing is centrifuged after reaction, taking precipitate obtains in 5 DEG C or less reaction 0.9-1.1h
Polyaniline wraps up silver-carrying nano microcrystalline cellulose base conductive particle；
E, it separately takes polyaniline to wrap up 35-55 parts of silver-carrying nano microcrystalline cellulose base conductive particle by mass fraction, is added 25-45 parts
It is stirred evenly after water and 12-18 parts of ethyl alcohol, adds 0.1-0.18 parts of defoaming agents and continue to stir, be eventually adding 5~7 parts of high temperature
It is sintered thermoplastic acrylic resin, emulsification 10-20min is carried out under high-speed shearing machine, it is micro- to obtain polyaniline package silver-carrying nano
Crystalline cellulose base electrically conductive ink.
3. the preparation method of polyaniline-coated silver-carrying nano microcrystalline cellulose base conductive particle according to claim 2,
It is characterized in that: carrying out in the steps below:
It a, is that 0.4% nano micro crystal cellulose solution ultrasonic vibration 15min obtains nano microcrystalline by 50 parts of concentration by mass fraction
Cellulose suspension solution；It is molten that the silver nitrate that 25 parts of concentration are 0.15% is added to nano micro crystal cellulose suspension liquor again
Liquid, ultrasonic disperse 5 minutes；
B, it is slowly added to the sodium borohydride solution that 25 parts of concentration are 0.08% in Xiang Shangshu mixed liquor, stirs 5 minutes, makes its mixing
Uniformly, silver-carrying nano microcrystalline cellulose mixed liquor is obtained；It is centrifuged again washing, taking precipitate obtains silver-carrying nano
Microcrystalline cellulose base conductive particle；
C, it is 6.25% and molecule that 20 parts of silver-carrying nano microcrystalline cellulose base conductive particles and 80 parts of concentration are separately taken by mass fraction
Amount is 1000-2000Da lignin sulfonic acid sodium solution, forms silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion solution；
D, 5 parts of aniline, the high-speed stirred at 65 DEG C is added to silver-carrying nano microcrystalline cellulose base conductive particle stable dispersion solution
1.0h, then temperature is adjusted to 8 DEG C hereinafter, the hydrochloric acid solution that 1.0mol/L is added adds 4 parts of persulfuric acid to pH to 2.0
In 5 DEG C or less reaction 1.0h washing is centrifuged, it is micro- that taking precipitate obtains polyaniline package silver-carrying nano in ammonium after reaction
Crystalline cellulose base conductive particle；
E, it separately takes polyaniline to wrap up 45 parts of silver-carrying nano microcrystalline cellulose base conductive particle by mass fraction, 34 parts of water and 15 is added
It is stirred evenly after part ethyl alcohol, adds 0.15 part of defoaming agent and continue to stir, be eventually adding 6 parts of high temperature sintering thermoplastic acrylic
Resin carries out emulsification 15min under high-speed shearing machine, obtains polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink.
4. the preparation of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink according to claim 1-3
Method, it is characterised in that: in the step b, be stirred using electric mixer, occur that its reaction uniformly.
5. the preparation of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink according to claim 1-3
Method, it is characterised in that: the centrifuge separation washing in the step b is to be centrifuged 10min under the revolving speed of 10000rpm, will be obtained
Sediment be added deionized water in ultrasonic vibration 30min washing, repeat the above process repeatedly until supernatant liquor for white.
6. the preparation of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink according to claim 1-3
Method, it is characterised in that: the aniline in the step d is to carry out vacuum distillation pretreatment in advance, and processing is colorless and transparent to fraction
Until.
7. the preparation of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink according to claim 1-3
Method, it is characterised in that: the high-speed stirred in the step d is carried out by high speed shear instrument.
8. the preparation of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink according to claim 1-3
Method, it is characterised in that: in the step e, be slowly added to the hydrochloric acid of 1mol/L using low-speed agitator pH is adjusted.
9. the preparation of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink according to claim 1-3
Method, it is characterised in that: the centrifuge separation washing in the step d is to be centrifuged 10min under the revolving speed of 10000rpm, will be obtained
Sediment be added deionized water in ultrasonic vibration 30min washing, repeat the above process repeatedly until sediment become navy blue.
10. the system of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink according to claim 1-3
Preparation Method, it is characterised in that: the revolving speed of the high-speed shearing machine in the step e is 3000r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910433625.XA CN110041762B (en) | 2019-05-23 | 2019-05-23 | Preparation method of polyaniline-coated silver-loaded nano microcrystalline cellulose-based conductive ink |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910433625.XA CN110041762B (en) | 2019-05-23 | 2019-05-23 | Preparation method of polyaniline-coated silver-loaded nano microcrystalline cellulose-based conductive ink |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110041762A true CN110041762A (en) | 2019-07-23 |
| CN110041762B CN110041762B (en) | 2022-03-01 |
Family
ID=67283258
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910433625.XA Active CN110041762B (en) | 2019-05-23 | 2019-05-23 | Preparation method of polyaniline-coated silver-loaded nano microcrystalline cellulose-based conductive ink |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110041762B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110860695A (en) * | 2019-11-25 | 2020-03-06 | 天津科技大学 | Preparation method of silver nanoparticles with adjustable size and distribution |
| CN112876744A (en) * | 2021-01-15 | 2021-06-01 | 湖南大学 | Method for enhancing mechanical property of nano cellulose membrane by using lignosulfonate |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020080822A (en) * | 2001-04-18 | 2002-10-26 | (주)펨텍 | Composite of high conductive organic-inorganic hybrid for electromagnetic interference shielding |
| JP4568819B2 (en) * | 2005-03-10 | 2010-10-27 | 国立大学法人大阪大学 | Method for producing metal nanocluster |
| CN105111507A (en) * | 2015-09-08 | 2015-12-02 | 哈尔滨工业大学 | Preparation method and application of bacterial cellulose/polyaniline/carbon nanotube conducting film material |
| CN106147406A (en) * | 2016-08-25 | 2016-11-23 | 周荣 | A kind of preparation method of cellulose base conductive printing ink from polyaniline |
| CN106149460A (en) * | 2016-07-06 | 2016-11-23 | 福建农林大学 | High intensity high antibiotic property water proof type conductive paper and preparation method thereof |
| CN107686688A (en) * | 2017-09-23 | 2018-02-13 | 南京林业大学 | Graphene/polypyrrole/carbon black conductive ink and preparation method and flexible-paper-base writing conducting wire |
| CN108047811A (en) * | 2017-12-27 | 2018-05-18 | 成都新柯力化工科技有限公司 | It is a kind of to improve Nano silver grain method dispersed in aqueous, environmental protective ink |
| CN109535849A (en) * | 2018-12-18 | 2019-03-29 | 盐城工学院 | A kind of ink-jet nano silver conductive ink and preparation method thereof |
-
2019
- 2019-05-23 CN CN201910433625.XA patent/CN110041762B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020080822A (en) * | 2001-04-18 | 2002-10-26 | (주)펨텍 | Composite of high conductive organic-inorganic hybrid for electromagnetic interference shielding |
| JP4568819B2 (en) * | 2005-03-10 | 2010-10-27 | 国立大学法人大阪大学 | Method for producing metal nanocluster |
| CN105111507A (en) * | 2015-09-08 | 2015-12-02 | 哈尔滨工业大学 | Preparation method and application of bacterial cellulose/polyaniline/carbon nanotube conducting film material |
| CN106149460A (en) * | 2016-07-06 | 2016-11-23 | 福建农林大学 | High intensity high antibiotic property water proof type conductive paper and preparation method thereof |
| CN106147406A (en) * | 2016-08-25 | 2016-11-23 | 周荣 | A kind of preparation method of cellulose base conductive printing ink from polyaniline |
| CN107686688A (en) * | 2017-09-23 | 2018-02-13 | 南京林业大学 | Graphene/polypyrrole/carbon black conductive ink and preparation method and flexible-paper-base writing conducting wire |
| CN108047811A (en) * | 2017-12-27 | 2018-05-18 | 成都新柯力化工科技有限公司 | It is a kind of to improve Nano silver grain method dispersed in aqueous, environmental protective ink |
| CN109535849A (en) * | 2018-12-18 | 2019-03-29 | 盐城工学院 | A kind of ink-jet nano silver conductive ink and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| HAO GOU；JINGXIAN HE；ZUNLI MO；ZHONGLI ZHAO: ""Ultrasonic preparation of cellulose/Ag/polyaniline conductive composites and its electrical properties"", 《JOURNAL OF MATERIALS SCIENCE-MATERIALS IN ELECTRONICS》 * |
| 于腾飞: ""导电纤维素复合材料的制备、结构与性能研究"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110860695A (en) * | 2019-11-25 | 2020-03-06 | 天津科技大学 | Preparation method of silver nanoparticles with adjustable size and distribution |
| CN112876744A (en) * | 2021-01-15 | 2021-06-01 | 湖南大学 | Method for enhancing mechanical property of nano cellulose membrane by using lignosulfonate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110041762B (en) | 2022-03-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110041762A (en) | A kind of preparation method of polyaniline package silver-carrying nano microcrystalline cellulose base electrically conductive ink | |
| Zhou et al. | Rapid fabrication of vivid noniridescent structural colors on fabrics with robust structural stability by screen printing | |
| Zheng et al. | Lignin‐Based Encapsulation of Liquid Metal Particles for Flexible and High‐Efficiently Recyclable Electronics | |
| CN104861910B (en) | A kind of graphene coated inorganic filler epoxy resin compound adhesive and preparation method thereof | |
| CN102138188B (en) | Electrically responsive composite material, a method of manufacture and a transducer produced using said material | |
| CN105618734B (en) | A kind of method of the modified sheeted silver powder in surface | |
| CN108668431A (en) | The preparation method and purposes of flexible extensible conducting wire and circuit | |
| CN1654533A (en) | Nano silicon dioxide/acrylate composite emulsion and preparation method thereof | |
| CN106782757A (en) | A kind of printable compliant conductive slurry and its conducting wire and preparation method | |
| CN105304161B (en) | Low-temperature environment-friendly conductive silver paste and preparation method and application | |
| CN103299484A (en) | Anisotropic conductive film | |
| Wen et al. | Insights into the interaction of polycarboxylate with coal and kaolinite and their application in flotation | |
| CN115109294A (en) | Antistatic film and preparation method thereof | |
| CN106952677A (en) | A kind of high temperature resistant sensing conductive carbon paste and preparation method thereof | |
| CN108948867A (en) | A kind of UV electrically conductive ink and its preparation method and application of suitable fabric silk-screen | |
| CN109627849A (en) | A kind of carbon nano-tube/poly pyrroles nanotube composite electron ink and preparation method thereof | |
| He et al. | Preparation of superhydrophobic conductive micro/nano‐graphite/PDMS films on paper by simple spraying method | |
| Chen et al. | Facile Fabrication of Carbon Nanocolloid‐Silver Composite Ink for the Application of All Inkjet‐Printed Wearable Electronics | |
| CN105542655B (en) | A kind of mould release and preparation method thereof for OCA optical adhesive film | |
| CN107868510A (en) | A kind of one-component black matte dielectric ink and preparation method thereof | |
| CN106632910A (en) | Preparation method and application of nano aluminum hydroxide graft | |
| CN114203338B (en) | Conductive paste and preparation method thereof | |
| CN1785816A (en) | Preparation method of star shaped copper sulfide | |
| CN105869705A (en) | Graphene/nano-silver light-sensitive conductive composite paste and preparation method therefor | |
| CN103145139A (en) | Viscosity reducer for improving viscosity of kaolin, and its preparation method |
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 |