CN109467985A - A kind of graphene ink preparation method and preparation facilities - Google Patents

A kind of graphene ink preparation method and preparation facilities Download PDF

Info

Publication number
CN109467985A
CN109467985A CN201811212944.XA CN201811212944A CN109467985A CN 109467985 A CN109467985 A CN 109467985A CN 201811212944 A CN201811212944 A CN 201811212944A CN 109467985 A CN109467985 A CN 109467985A
Authority
CN
China
Prior art keywords
bath
water
graphene
added
oil
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.)
Pending
Application number
CN201811212944.XA
Other languages
Chinese (zh)
Inventor
王志辉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Datong Xincheng New Material Co Ltd
Original Assignee
Datong Xincheng New Material Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Datong Xincheng New Material Co Ltd filed Critical Datong Xincheng New Material Co Ltd
Priority to CN201811212944.XA priority Critical patent/CN109467985A/en
Publication of CN109467985A publication Critical patent/CN109467985A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F31/00Mixers with shaking, oscillating, or vibrating mechanisms
    • B01F31/80Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90Heating or cooling systems
    • B01F35/92Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/10Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90Heating or cooling systems
    • B01F2035/99Heating

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)

Abstract

The embodiment of the present application shows a kind of graphene ink preparation method and preparation facilities, method includes: that graphite powder is taken to be put into beaker, it is added after water stirs and is stirred under ultrasound condition, supernatant liquor is outwelled after centrifugation, the precipitating of lower layer is taken out into drying, obtain graphite powder, after mixing by graphite powder and the concentrated sulfuric acid, potassium permanganate is added, after deionized water is added dropwise, hydrogen peroxide is added, graphite oxide is washed with centrifuge and deionized water, by lower layer's graphite oxide precipitating after washing, after drying, obtain pretreatment graphite oxide, pretreatment graphite oxide is stirred to dispersion, nitrification silver and polyvinylpyrrolidone is added, sodium borohydride is added dropwise, preset time is reacted under oil bath later, it obtains carrying silver-colored graphene, silver-colored graphene and water will be carried, binder is uniformly mixed and obtains graphene ink;The present invention, which provides graphene ink preparation method, can not only guarantee the good electric conductivity of graphene ink, and guarantee the use of flexible substrates.

Description

A kind of graphene ink preparation method and preparation facilities
Technical field
The present invention relates to lithium battery electrolytes technical field, in particular to a kind of graphene ink preparation method and detection dress It sets.
Background technique
Graphene is the nano material that known world is most thin, most hard, it is almost fully transparent, only absorption 2.3% Light;Thermal coefficient is up to 5300W/m K, is higher than carbon nanotube and diamond, its electron mobility is more than 15000 under room temperature Cm2/V s, but it is higher than carbon nanotubes or silicon crystal, and about 1 0-8 Ω m of resistivity, it is lower than copper or silver, it is world resistance The smallest material of rate.As a kind of presently found most thin, most hard, the strongest novel nano-material of electrical and thermal conductivity performance, stone Black alkene is referred to as " dark fund ", is " king of new material ", and scientist even foretells that graphene " will thoroughly change 21 century ".Carbon system, Metal nano system and conducting polymer ink are the blue quasi-tradition electrically conductive inks that oneself is widely studied.Although conducting polymer is soft Property display application in there is very big advantage, however they not only conductivity is generally relatively low, but also its thermal stability It is poor PW.Metal nano electrically conductive ink has very big electric conductivity, however they are logical after being deposited in substrate It often needs to carry out high temperature sintering, which limits the uses of flexible substrates.
Summary of the invention
To overcome the problems in correlation technique, the present invention provides a kind of graphene ink preparation method and detection dress It sets, can not only guarantee good electric conductivity, and guarantee the use of flexible substrates.
First aspect of the embodiment of the present invention discloses a kind of graphene ink preparation method, graphene ink preparation side Method the following steps are included:
It takes graphite powder to be put into beaker, is added after water stirs and is stirred under ultrasound condition, supernatant liquor is outwelled after centrifugation, by lower layer Precipitating takes out drying, obtains graphite powder;
The graphite powder and the concentrated sulfuric acid are blended under conditions of ice-water bath after mixing evenly, potassium permanganate is added, is added dropwise After deionized water, hydrogen peroxide is added, washs graphite oxide with centrifuge and deionized water, lower layer's graphite oxide after washing is sunk It forms sediment, after drying, obtains pretreatment graphite oxide;
The pretreatment graphite oxide is stirred to dispersion, is added nitrification silver and polyvinylpyrrolidone, stirring while heats up To 100-120 DEG C, sodium borohydride is added dropwise, reacts preset time under oil bath later, obtains carrying silver-colored graphene;
It is uniformly mixed the silver-colored graphene of the load to obtain the graphene ink with water, binder.
Optionally, graphite powder is put into beaker, is stirred 3-4h under ultrasound condition after addition water stirring 3-4h, is outwelled after centrifugation The precipitating of lower layer is taken out drying, obtains graphite powder by supernatant liquor.
Optionally, the temperature condition that the precipitating of lower layer is taken out drying is 50-60 DEG C, drying time 30-40h.
Optionally, the binder includes polyvinyl butyral and the molten rosin of alcohol.
Optionally, the weight ratio for carrying silver-colored graphene, water and the binder are as follows: 3:2:1.
Optionally, the preparation process carries out in the closed container full of nitrogen.
Using a kind of graphene ink preparation method that first aspect provides, the application is using graphene as a kind of main Conductive phase, and its aqueous phase dispersibility of nanometer human lymph node and electric conductivity are deposited on graphene, first with improved Hummer oxygen Change graft process, under the premise of not adding sodium nitrate, synthesize graphene oxide, then exists in polyethylene of dispersing agent pyrrolidones Under, sodium borohydride is reducing agent, and synchronous reduction silver nitrate and graphite oxide are dilute, to prepare the load silver stone being dispersed in water Black alkene takes water as a solvent then by the way that binder is added and prepares graphene ink;The present invention provides graphene ink preparation side Method can not only guarantee the good electric conductivity of graphene ink, and guarantee the use of flexible substrates.
According to the second aspect of the disclosure, a kind of graphene ink preparation facilities is provided, is used for water-bath or oil bath, comprising: Water-bath cabinet and solution Container, the solution Container are set to the inside of the water-bath cabinet;
The water-bath cabinet includes water-bath box-like body;The first shelf and second that is internally provided with of the water-bath box-like body is put Plate is provided with bain-marie accommodating cavity at the top of first shelf, and the bain-marie accommodating cavity is internally provided with bain-marie, institute Bain-marie is stated for giving solution heating water bath, oil-bath accommodating cavity, the oil-bath accommodating are provided at the top of second shelf Chamber is internally provided with oil-bath, and the oil-bath is for giving solution oil bath heating;
The solution Container includes the first solution Container and the second solution Container, and the first solution accommodating cavity is set to It the top of first shelf and is in contact with the bain-marie, the second solution accommodating cavity is set to first shelf It top and is in contact with the oil-bath.
Optionally, one end far from the solution Container of the bain-marie and the oil-bath is provided with twitch hand Handle.
A kind of graphene ink preparation facilities shown in second aspect is used for water-bath or oil bath, comprising: water-bath cabinet and molten Liquid Container, the solution Container are set to the inside of the water-bath cabinet, and the water-bath cabinet includes water-bath box-like body; The water-bath box-like body is internally provided with the first shelf and the second shelf, is provided with bain-marie at the top of first shelf Accommodating cavity, the bain-marie accommodating cavity are internally provided with bain-marie, and the bain-marie is for giving solution heating water bath, and described the Oil-bath accommodating cavity is provided at the top of two shelves, the oil-bath accommodating cavity is internally provided with oil-bath, and the oil-bath is used In giving solution oil bath heating, the solution Container includes the first solution Container and the second solution Container, and described first is molten Liquid accommodating cavity is set to the top of first shelf and is in contact with the bain-marie, and the second solution accommodating cavity is set to It the top of first shelf and is in contact with the oil-bath;By Man Bingshui double in bain-marie when work, filled in oil-bath Hot oil needs that reaction solution is added to the first solution Container when ice-water bath, reacts under water bath condition, needs to incite somebody to action when oil bath Reaction solution pours into the second solution Container, reacts under the conditions of oil bath, and it is dual-purpose to be achieved a device, improves reaction effect Rate;And guarantee stable reaction temperature, the graphene ink produced can not only guarantee good electric conductivity, Er Qiebao Demonstrate,prove the use of flexible substrates.
Detailed description of the invention
In order to illustrate more clearly of the technical solution of the application, letter will be made to attached drawing needed in the embodiment below Singly introduce, it should be apparent that, for those of ordinary skills, without creative efforts, also Other drawings may be obtained according to these drawings without any creative labor.
Fig. 1 is a kind of flow diagram of graphene ink preparation method provided in an embodiment of the present invention;
Fig. 2 is a kind of structural schematic diagram of graphene ink preparation facilities provided in an embodiment of the present invention.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, below in conjunction with of the invention real The attached drawing in example is applied, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described implementation Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common Technical staff's every other embodiment obtained without making creative work, all should belong to protection of the present invention Range.
Embodiment one
It is a kind of graphene ink preparation method flow chart provided in an embodiment of the present invention, which is characterized in that described referring to Fig. 1 Graphene ink preparation method the following steps are included:
It takes graphite powder to be put into beaker, is added after water stirs and is stirred under ultrasound condition, supernatant liquor is outwelled after centrifugation, by lower layer Precipitating takes out drying, obtains graphite powder;
The graphite powder and the concentrated sulfuric acid are blended under conditions of ice-water bath after mixing evenly, potassium permanganate is added, is added dropwise After deionized water, hydrogen peroxide is added, washs graphite oxide with centrifuge and deionized water, lower layer's graphite oxide after washing is sunk It forms sediment, after drying, obtains pretreatment graphite oxide;
The pretreatment graphite oxide is stirred to dispersion, is added nitrification silver and polyvinylpyrrolidone, stirring while heats up To 100-120 DEG C, sodium borohydride is added dropwise, reacts preset time under oil bath later, obtains carrying silver-colored graphene;
It is uniformly mixed the silver-colored graphene of the load to obtain the graphene ink with water, binder.
The graphene ink preparation method that embodiment one provides, using graphene as a kind of main conductive phase, and Its aqueous phase dispersibility of nanometer human lymph node and electric conductivity are deposited on graphene, graft process are aoxidized with improved Hummer first, not Under the premise of adding sodium nitrate, graphene oxide is synthesized, then in the presence of polyethylene of dispersing agent pyrrolidones, sodium borohydride is Reducing agent, synchronous reduction silver nitrate and graphite oxide are dilute, to prepare the load silver graphene being dispersed in water, then pass through Binder is added, takes water as a solvent and prepares graphene ink;The present invention provides graphene ink preparation method and can not only protect The good electric conductivity of graphene ink is demonstrate,proved, and guarantees the use of flexible substrates.
Embodiment two is a kind of graphene ink preparation method that the preferred embodiment of the invention provides, the graphene oil Black preparation method the following steps are included:
Graphite powder is put into beaker, stirs 3-4h under ultrasound condition after addition water stirring 3-4h, supernatant liquor is outwelled after centrifugation, will The precipitating of lower layer takes out drying, obtains graphite powder.The graphite powder that stirring 3-4h is obtained under ultrasound condition after addition water stirring 3-4h Quality is best.
The graphite powder and the concentrated sulfuric acid are blended under conditions of ice-water bath after mixing evenly, potassium permanganate is added, dropwise After deionized water is added, hydrogen peroxide is added, washs graphite oxide with centrifuge and deionized water, the lower layer after washing is aoxidized into stone Ink precipitating after drying, obtains pretreatment graphite oxide;
The pretreatment graphite oxide is stirred to dispersion, is added nitrification silver and polyvinylpyrrolidone, stirring while heats up To 100-120 DEG C, sodium borohydride is added dropwise, reacts preset time under oil bath later, obtains carrying silver-colored graphene;
It is uniformly mixed the silver-colored graphene of the load to obtain the graphene ink with water, binder.
Embodiment three is a kind of graphene ink preparation method that the preferred embodiment of the invention provides, the graphene oil Black preparation method the following steps are included:
It takes graphite powder to be put into beaker, is added after water stirs and is stirred under ultrasound condition, supernatant liquor is outwelled after centrifugation, by lower layer Precipitating takes out drying, obtains graphite powder;
The graphite powder and the concentrated sulfuric acid are blended under conditions of ice-water bath after mixing evenly, potassium permanganate is added, is added dropwise After deionized water, hydrogen peroxide is added, washs graphite oxide with centrifuge and deionized water, lower layer's graphite oxide after washing is sunk It forms sediment, after drying, obtains pretreatment graphite oxide;
The pretreatment graphite oxide is stirred to dispersion, is added nitrification silver and polyvinylpyrrolidone, stirring while heats up To 100-120 DEG C, sodium borohydride is added dropwise, reacts preset time under oil bath later, obtains carrying silver-colored graphene;
It is uniformly mixed the silver-colored graphene of the load to obtain the graphene ink with water, binder.
The temperature condition that the precipitating of lower layer is taken out drying is 50-60 DEG C, drying time 30-40h.
Example IV is a kind of graphene ink preparation method that the preferred embodiment of the invention provides, the graphene oil Black preparation method the following steps are included:
It takes graphite powder to be put into beaker, is added after water stirs and is stirred under ultrasound condition, supernatant liquor is outwelled after centrifugation, by lower layer Precipitating takes out drying, obtains graphite powder;
The graphite powder and the concentrated sulfuric acid are blended under conditions of ice-water bath after mixing evenly, potassium permanganate is added, is added dropwise After deionized water, hydrogen peroxide is added, washs graphite oxide with centrifuge and deionized water, lower layer's graphite oxide after washing is sunk It forms sediment, after drying, obtains pretreatment graphite oxide;
The pretreatment graphite oxide is stirred to dispersion, is added nitrification silver and polyvinylpyrrolidone, stirring while heats up To 100-120 DEG C, sodium borohydride is added dropwise, reacts preset time under oil bath later, obtains carrying silver-colored graphene;
It is uniformly mixed the silver-colored graphene of the load to obtain the graphene ink with water, binder.
The binder includes polyvinyl butyral and the molten rosin of alcohol.
The adhesion inhibiting properties that good water resistance is combined, (this makes polyvinyl alcohol for good mobility and excellent wet pigments Butyral resin is ideally used to production pigment paste) make polyvinyl butyral resin series be well suited for making the bonding of printing ink Material, if suitably drafting formula, this ink is odorless, tasteless.Because the resin in polyvinyl butyral series is easy It is dissolved in (such as ethyl alcohol) in the solvent without harmful substance, to organic substrate such as cellulose acetate film, mylar and polyphenyl second Alkene and there is excellent adhesiveness to aluminium foil, they are ideal for food packaging offset printing and gravure ink.
Alcohols solvent can be dissolved in but not soluble in water and hydrocarbon natural resin or synthetic resin.It is to prepare the alcohol without drying oil The important source material of matter coating or alcohol varniss.Alcohols solvent can be dissolved in but not soluble in water and hydrocarbon natural resin or synthetic resin. It is the important source material for preparing alcohol matter coating or alcohol varniss without drying oil.The stone that both materials are produced as binder Black alkene ink can more guarantee the use of flexible substrates.
Embodiment five is a kind of graphene ink preparation method that the preferred embodiment of the invention provides, the graphene oil Black preparation method the following steps are included:
It takes graphite powder to be put into beaker, is added after water stirs and is stirred under ultrasound condition, supernatant liquor is outwelled after centrifugation, by lower layer Precipitating takes out drying, obtains graphite powder;
The graphite powder and the concentrated sulfuric acid are blended under conditions of ice-water bath after mixing evenly, potassium permanganate is added, is added dropwise After deionized water, hydrogen peroxide is added, washs graphite oxide with centrifuge and deionized water, lower layer's graphite oxide after washing is sunk It forms sediment, after drying, obtains pretreatment graphite oxide;
The pretreatment graphite oxide is stirred to dispersion, is added nitrification silver and polyvinylpyrrolidone, stirring while heats up To 100-120 DEG C, sodium borohydride is added dropwise, reacts preset time under oil bath later, obtains carrying silver-colored graphene;
It is uniformly mixed the silver-colored graphene of the load to obtain the graphene ink with water, binder.
Wherein, the weight ratio for carrying silver-colored graphene, water and the binder are as follows: 3:2:1.The ratio preparation Ink because conductive phase content it is higher, silver and graphene between connection it is closer, to be formed by conductive channel More, final electric conductivity can also become better and better.When the content of conductive phase reaches a certain level, the side of conductive pattern Block resistance and average change in resistance will very little from cost is saved and electric conductivity angularly considers preferentially select the present embodiment Weight ratio.
Embodiment six is a kind of graphene ink preparation method that the preferred embodiment of the invention provides, the graphene oil Black preparation method the following steps are included:
It takes graphite powder to be put into beaker, is added after water stirs and is stirred under ultrasound condition, supernatant liquor is outwelled after centrifugation, by lower layer Precipitating takes out drying, obtains graphite powder;
The graphite powder and the concentrated sulfuric acid are blended under conditions of ice-water bath after mixing evenly, potassium permanganate is added, is added dropwise After deionized water, hydrogen peroxide is added, washs graphite oxide with centrifuge and deionized water, lower layer's graphite oxide after washing is sunk It forms sediment, after drying, obtains pretreatment graphite oxide;
The pretreatment graphite oxide is stirred to dispersion, is added nitrification silver and polyvinylpyrrolidone, stirring while heats up To 100-120 DEG C, sodium borohydride is added dropwise, reacts preset time under oil bath later, obtains carrying silver-colored graphene;
It is uniformly mixed the silver-colored graphene of the load to obtain the graphene ink with water, binder.
Wherein, the preparation process carries out in the closed container full of nitrogen.Nitrogen can guarantee that various reactions do not have There is the interference of active gases in air.
A kind of graphene ink preparation facilities shown in second aspect is used for water-bath or oil bath, comprising: 1 He of water-bath cabinet Solution Container 2, the solution Container 2 are set to the inside of the water-bath cabinet 1;
The water-bath cabinet 1 includes water-bath box-like body 11;The water-bath box-like body 11 is internally provided with the first shelf 12 With the second shelf 13, the top of first shelf 12 is provided with bain-marie accommodating cavity 14, the bain-marie accommodating cavity 14 it is interior Portion is provided with bain-marie 141, and the bain-marie 141 is provided with oil at the top of second shelf 13 for giving solution heating water bath Bath accommodating cavity 15, the oil-bath accommodating cavity 15 are internally provided with oil-bath 151, and the oil-bath 151 is used for solution Oil bath heating;
The solution Container 2 includes the first solution Container 21 and the second solution Container 22, the first solution accommodating cavity 21 are set to the top of first shelf 12 and are in contact with the bain-marie 141, and the second solution accommodating cavity 22 is arranged In first shelf 13 top and be in contact with the oil-bath 151.
When work, ice water will be filled in bain-marie 141, fills hot oil in oil-bath 151, need to react molten when ice-water bath Liquid is added to the first solution Container 21, reacts under water bath condition, needs that reaction solution is poured into the second solution when oil bath and holds It sets in device 22, is reacted under the conditions of oil bath, it is dual-purpose to be achieved a device, improves reaction efficiency;And guarantee stable anti- Temperature is answered, the graphene ink produced can not only guarantee good electric conductivity, and guarantee the use of flexible substrates.
As preferred embodiment, the separate solution Container 2 of the bain-marie 141 and the oil-bath 151 One end, which is provided with, twitches handle 16, and handle 16 is twitched in addition can be convenient detaching and putting for bain-marie 141 and oil-bath 151 It sets.
Those skilled in the art will readily occur to its of the application after considering specification and practicing application disclosed herein Its embodiment.This application is intended to cover any variations, uses, or adaptations of the application, these modifications, purposes or Person's adaptive change follows the general principle of the application and including the undocumented common knowledge in the art of the application Or conventional techniques.The description and examples are only to be considered as illustrative, and the true scope and spirit of the application are by above Claim is pointed out.
It should be understood that the application is not limited to the accurate process for being described above and being shown in the accompanying drawings, and And various modifications and changes may be made without departing from the scope thereof.Scope of the present application is only limited by the accompanying claims.

Claims (8)

1. a kind of graphene ink preparation method, which is characterized in that the graphene ink preparation method the following steps are included:
It takes graphite powder to be put into beaker, is added after water stirs and is stirred under ultrasound condition, supernatant liquor is outwelled after centrifugation, by lower layer Precipitating takes out drying, obtains graphite powder;
The graphite powder and the concentrated sulfuric acid are blended under conditions of ice-water bath after mixing evenly, potassium permanganate is added, is added dropwise After deionized water, hydrogen peroxide is added, washs graphite oxide with centrifuge and deionized water, lower layer's graphite oxide after washing is sunk It forms sediment, after drying, obtains pretreatment graphite oxide;
The pretreatment graphite oxide is stirred to dispersion, is added nitrification silver and polyvinylpyrrolidone, stirring while heats up To 100-120 DEG C, sodium borohydride is added dropwise, reacts preset time under oil bath later, obtains carrying silver-colored graphene;
It is uniformly mixed the silver-colored graphene of the load to obtain the graphene ink with water, binder.
2. a kind of graphene ink preparation method according to claim 1, which is characterized in that graphite powder is taken to be put into beaker In, 3-4h is stirred under ultrasound condition after addition water stirring 3-4h, supernatant liquor is outwelled after centrifugation, the precipitating of lower layer is taken out and is dried It is dry, obtain graphite powder.
3. a kind of graphene ink preparation method according to claim 1 or 2, which is characterized in that described by the heavy of lower layer The temperature condition taken out and dried of forming sediment is 50-60 DEG C, drying time 30-40h.
4. a kind of graphene ink preparation method according to claim 1, which is characterized in that the binder includes poly- second Enol butyral and the molten rosin of alcohol.
5. a kind of graphene ink preparation method according to claim 1, which is characterized in that the load silver-colored graphene, water And the weight ratio of the binder are as follows: 3:2:1.
6. a kind of graphene ink preparation method according to claim 1, which is characterized in that the preparation process is being filled It is carried out in the closed container of full nitrogen.
7. a kind of graphene ink preparation facilities, which is characterized in that be used for water-bath or oil bath, comprising: water-bath cabinet (1) and solution Container (2), the solution Container (2) are set to the inside of the water-bath cabinet (1);
The water-bath cabinet (1) includes water-bath box-like body (11);The water-bath box-like body (11) is internally provided with first Shelf (12) and the second shelf (13) are provided with bain-marie accommodating cavity (14), the water-bath at the top of first shelf (12) Device accommodating cavity (14) is internally provided with bain-marie (141), and the bain-marie (141) is for giving solution heating water bath, and described the It is provided with oil-bath accommodating cavity (15) at the top of two shelves (13), the oil-bath accommodating cavity (15) is internally provided with oil-bath (151), the oil-bath (151) is for giving solution oil bath heating;
The solution Container (2) includes the first solution Container (21) and the second solution Container (22), first solution Accommodating cavity (21) is set to the top of first shelf (12) and is in contact with the bain-marie (141), second solution Accommodating cavity (22) is set to the top of first shelf (13) and is in contact with the oil-bath (151).
8. a kind of graphene ink preparation facilities according to claim 7, which is characterized in that the bain-marie (141) and One end far from the solution Container (2) of the oil-bath (151), which is provided with, twitches handle (16).
CN201811212944.XA 2018-10-18 2018-10-18 A kind of graphene ink preparation method and preparation facilities Pending CN109467985A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811212944.XA CN109467985A (en) 2018-10-18 2018-10-18 A kind of graphene ink preparation method and preparation facilities

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811212944.XA CN109467985A (en) 2018-10-18 2018-10-18 A kind of graphene ink preparation method and preparation facilities

Publications (1)

Publication Number Publication Date
CN109467985A true CN109467985A (en) 2019-03-15

Family

ID=65665883

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811212944.XA Pending CN109467985A (en) 2018-10-18 2018-10-18 A kind of graphene ink preparation method and preparation facilities

Country Status (1)

Country Link
CN (1) CN109467985A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112993084A (en) * 2021-02-04 2021-06-18 合肥工业大学 Preparation method of Ag-rGO film with excellent photoelectric property
GB2597046A (en) * 2020-05-14 2022-01-19 Graphene Composites Ltd Viral active and/or anti-microbial inks and coatings
CN116219773A (en) * 2022-12-01 2023-06-06 青岛大学 Method for improving fixation fastness of nano silver/reduced graphene oxide UV printing ink
CN117810450A (en) * 2024-02-29 2024-04-02 中国科学院山西煤炭化学研究所 Modified graphite negative electrode material of lithium ion battery and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106887272A (en) * 2017-03-16 2017-06-23 西安晶晟光电科技有限公司 The preparation of chemical reduction method different-grain diameter graphene coated silver powder and the preparation method of slurry
CN207413450U (en) * 2017-11-09 2018-05-29 保定学院 Thermostat water bath with magnetic stirring function

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106887272A (en) * 2017-03-16 2017-06-23 西安晶晟光电科技有限公司 The preparation of chemical reduction method different-grain diameter graphene coated silver powder and the preparation method of slurry
CN207413450U (en) * 2017-11-09 2018-05-29 保定学院 Thermostat water bath with magnetic stirring function

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
常州迅生仪器有限公司: "数显恒温油浴<两孔型>", 《HTTPS://WWW.CHEM17.COM/PRODUCT/DETAIL/26898154.HTML》 *
朱华杨等: "石墨烯/纳米银导电油墨导电性能研究", 《包装工程》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2597046A (en) * 2020-05-14 2022-01-19 Graphene Composites Ltd Viral active and/or anti-microbial inks and coatings
CN112993084A (en) * 2021-02-04 2021-06-18 合肥工业大学 Preparation method of Ag-rGO film with excellent photoelectric property
CN116219773A (en) * 2022-12-01 2023-06-06 青岛大学 Method for improving fixation fastness of nano silver/reduced graphene oxide UV printing ink
CN117810450A (en) * 2024-02-29 2024-04-02 中国科学院山西煤炭化学研究所 Modified graphite negative electrode material of lithium ion battery and preparation method thereof
CN117810450B (en) * 2024-02-29 2024-04-30 中国科学院山西煤炭化学研究所 Modified graphite negative electrode material of lithium ion battery and preparation method thereof

Similar Documents

Publication Publication Date Title
CN109467985A (en) A kind of graphene ink preparation method and preparation facilities
Li et al. A sulfur–polyacrylonitrile/graphene composite cathode for lithium batteries with excellent cyclability
CN105552399B (en) A kind of graphene adulterates conducting polymer modified dual polar plates of proton exchange membrane fuel cell and preparation method thereof
CN105017831B (en) Water-based electric heating nano paint composition and coating and its preparation method and application
CN103466602A (en) Preparation method of graphene powder, and application of graphene powder in lithium ion battery
CN106243836A (en) A kind of graphene conductive carbon slurry and preparation method thereof
CN105140524B (en) Lead storage battery grid containing lead-graphene composite material
CN106752878A (en) A kind of Graphene low-voltage heating coating and preparation method thereof
Raut et al. Porous zinc cobaltite (ZnCo2O4) film by successive ionic layer adsorption and reaction towards solid-state symmetric supercapacitive device
CN103523773B (en) A kind of high connductivity Graphene and grapheme conductive film and preparation method thereof
CN102832392A (en) Current collector carbon coated aluminum foil and its preparation method
CN108831757B (en) A kind of preparation method of N and S codope graphene/carbon nano-tube aeroge
CN107946576A (en) A kind of high magnification graphite cathode material and preparation method thereof, lithium ion battery
CN109003826A (en) N and S codope graphene-graphene nanobelt aeroge preparation method
CN104569093B (en) A kind of electrochemical detection test strip is starched and preparation method thereof and a kind of electrochemical detection test strip and preparation method thereof with carbon
CN105405663B (en) A kind of MoS2The electrochemical preparation method of/graphene combined counter electrode
CN109659540A (en) A kind of preparation method of porous carbon coating antimony telluride nanometer sheet and its application as metal ion cell negative electrode material
CN109830549A (en) A kind of indium sulfide/graphene composite film and its preparation method and application
CN105957584A (en) Graphene oxide/reduced graphene oxide-doped carbon nanotube flexible transparent conductive electrode and preparation method thereof
CN105470522A (en) Conductive coating for lithium ion battery electrode and preparation method for conductive coating, lithium ion battery positive plate and preparation method therefor, and lithium ion battery
CN107641824A (en) Graphene conductive polymer composites and preparation method thereof
Rathinam et al. Rewiring the microbe-electrode interfaces with biologically reduced graphene oxide for improved bioelectrocatalysis
CN109607521A (en) A kind of doped graphene material and its preparation method and application
CN106986331B (en) A kind of graphene-tin-antiomony oxide composite conducting material and preparation method thereof
CN105842438A (en) Preparation method of prussian blue cube / molybdenum disulfide nano composite material

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
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190315