CN107129752B - A kind of graphene silver nanowires composite mortar and preparation method thereof - Google Patents
A kind of graphene silver nanowires composite mortar and preparation method thereof Download PDFInfo
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- CN107129752B CN107129752B CN201710514222.9A CN201710514222A CN107129752B CN 107129752 B CN107129752 B CN 107129752B CN 201710514222 A CN201710514222 A CN 201710514222A CN 107129752 B CN107129752 B CN 107129752B
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- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
It is to be used in conjunction with silver nanowires, graphene powder and carbon black the invention discloses a kind of graphene silver nanowires composite mortar and preparation method thereof.Composite mortar of the invention is using high additive graphene cooperation low-dosage silver nanowires and carbon black, it is improved largely in conductivity, electromagnetic shielding, sterilization, far infrared heating effect performance, excellent effect, while the present invention has the characteristic of no pollution to the environment using aqueous solvent.
Description
Technical field
The present invention relates to electrocondution slurry technical fields, and in particular to a kind of graphene silver nanowires composite mortar and its preparation
Method.
Background technique
Traditional electrocondution slurry, which is substantially added in polymer in the form of filler by conductive unit powder, to be prepared,
Wherein conductive unit powder mainly includes carbon, metal and compound three classes.To improve performance, the improvement and spy of conductive filler
Suo Yingyong new material is the development trend of electrocondution slurry research both at home and abroad at present.
Conductive carbon paste is mixed with carbon-based material and fluoropolymer resin, is had good electric conductivity, is answered extensively
For communication article (mobile phone), computer, portable electronic product, consumer electronics, the network hardware (server etc.), medical instrument
The electronic equipments such as device, domestic electronic appliances and space flight and national defence.Film layer, film layer are formed after the heated solidification of conductive carbon paste
Not oxidizable, acid and alkali resistance and solvent corrosion can be stablized, protection and conductive effect can be played.
Metal conductive paste has excellent electric conductivity such as gold, silver and copper paste printing ink, and resistivity can reach 10-2-10-3
Ωcm.Metal powder ink performance is good, but price is more expensive, silver itself there is it is easy to migrate, vulcanization, anti-scolding tin erosiveness it is poor, burning
Knot process is easy the defects of cracking.Copper paste printing ink, which can generate oxide layer under air and water effect, keeps electric conductivity unstable.
Conductive silver paste is generally made of silver powder, glass powder and organic component.The dispersing uniformity pair of silver powder in conductive silver paste
The electric conductivity of conductive silver paste has a great impact.Conductive silver paste is the electric conductivity the problem of: one, since silver powder is easy to roll into a ball
It is poly-, two, the presence of non-conductive substance glass powder.These electric conductivity for typically resulting in conductive silver paste are deteriorated.Existing conductive carbon paste
Although there is high cost performance, its resistive performance is lower than conductive silver paste, so the effect in utilization compared with conductive silver paste
It is limited, in the product for requiring high conduction performance, using being restricted.
At present about far infrared heating, safety sterilization, high conductivity comprehensive performance conductive carbon paste research it is less.For
The slurry of above-mentioned high comprehensive performance is obtained, slurry is mixed with using graphene and silver nanowires medium, there is slurry
Electric conductivity, far infrared heating, the composite performance sterilized safely are a preferable technology paths.But how by graphene and
Silver nanowires is good to be dispersed into slurry system and the problem for becoming urgent need to resolve is used in combination.
In addition, commonly using organic solvent in electrocondution slurry is epoxy resin, phenolic resin, polyvinyl acetate, polyamide resin
Rouge, these solvents are not readily dissolved in water, there is pollution, toxic, do not have good environmental-protecting performance.
Summary of the invention
The present invention be to avoid above-mentioned the deficiencies in the prior art in place of, provide that a kind of collection infrared heating, safety is sterilized, height is led
Electrically in the graphene silver nanowires composite mortar and preparation method thereof of one.
The present invention solves technical problem, adopts the following technical scheme that
Graphene silver nanowires composite mortar of the invention, each raw material press the composition of mass fraction are as follows:
1~20 part of 1~100mg/mL silver nanowires dispersion liquid, 20~50 parts of graphene powder, 1~20 part of carbon black, it is aqueous
20~50 parts of polyurethane resin, 1~50 part of aqueous epoxy resins, 1~20 part of water-based acrylic resin, 0.1~5 part of dispersing agent,
0.1~2 part of curing agent hexamethylene diamine, 0.1~10 part of pH buffer, 20~50 parts of water.
Preferably, the diameter of silver nanowires is 40~200nm in the silver nanowires dispersion liquid, and length is 10~500 μm.
Preferably, the partial size of the graphene powder is 2~50 μm, and the partial size of the carbon black is 0.1~10 μm.
Preferably, the dispersing agent is selected from lauryl sodium sulfate, cetyl benzenesulfonic acid sodium, hydroxypropyl methyl fiber
One of element, sodium carboxymethylcellulose are a variety of.
Preferably, the pH buffer configures as follows: in 25mL boronic acid containing 0.2mol/L, potassium chloride 0.2mol/L
Mixed liquor in, be added 4mL 0.1mol/L sodium hydroxide solution be diluted with water to 100mL after mixing, i.e., acquisition pH
Buffer.
The preparation method of graphene silver nanowires composite mortar of the present invention, includes the following steps:
A, graphene powder, carbon black, dispersing agent and water are stirred 0.5-6h according to the ratio, re-ultrasonic dispersion 1-10h, so
After waterborne polyurethane resin is added, and in the ball mill high speed ball milling disperse, most afterwards through 250 mesh screen cloths filter, obtain mixing slurry
Expect A；
B, silver nanowires dispersion liquid, aqueous epoxy resins and water-based acrylic resin are added to vacuum in de-airing mixer
Deaeration is uniformly mixed, and obtains mixed liquid B；
C, mixed slurry A is added in de-airing mixer, under continuous stirring, it is 8 that pH buffer, which is added, and adjusts pH, then
Mixed liquid B and curing agent hexamethylene diamine are sequentially added, continues to stir evenly, is i.e. acquisition graphene silver nanowires composite mortar.
The principle of the present invention are as follows: using the good conductive, conductive structure of graphene powder as filler, auxiliary addition silver is received
Rice noodles and carbon black prepare slurry, and slurry can be fabricated to heating element by coating technique after hot setting.In energization situation
Under, graphene powder working principle is to generate " Brownian movement " by graphene powder particle cluster under the initiation excitation of electricity, by
Mutual shock and friction between carbon molecules generate a large amount of infrared radiation, electric energy and thermal energy conversion rate to generate thermal energy
It is high, it can achieve 99%, wherein thermal energy is distributed to generate a large amount of infrared radiation, and efficiency can achieve 85%.
Compared with the prior art, the beneficial effects of the present invention are embodied in:
1, composite mortar of the invention is using high additive graphene cooperation low-dosage silver nanowires and carbon black, conductivity,
Electromagnetic shielding is sterilized, is improved largely in far infrared heating effect performance, excellent effect, while the present invention is using aqueous molten
Agent has the characteristic of no pollution to the environment.
2, the present invention prepares slurry using graphene auxiliary addition silver nanowires and carbon black, and graphene and silver nanowires is good
Good is dispersed in conductive carbon pastes system, and triplicity is used, and cooperates, further increases the electric conductivity of conductive carbon paste
Can, while having given full play to the far infrared radiation efficiency of grapheme material and the sterilization idiocratic of silver nanowires.
3, graphene silver nanowires composite mortar prepared by the present invention, which is coated in flexible parent metal surface, has excellent attachment
Power, abrasion-resistant, resistance to rubbing, high temperature resistant, water-fastness, resistant to bending, ageing-resistant performance is excellent.
4, each raw material of graphene silver nanowires composite mortar of the invention can market buy, can also be by straightforward procedure system
It is standby, it has a good application prospect.
Detailed description of the invention
Fig. 1 is to send out slurry prepared by the present invention coated in the far infrared being powered after drying on 25 μm of Kapton
Thermal map.
Specific embodiment
Embodiment is presented below, clearly elaboration explanation is done to technical solution of the present invention.
Raw materials used model and producer are as follows in following embodiments:
Graphene powder be originated from Hefei micro crystal material Science and Technology Ltd., can market buy；
Silver nanowires dispersion liquid be originated from Hefei micro crystal material Science and Technology Ltd., can market buy；
Waterborne polyurethane resin: producer's Jitian's chemical industry, trade mark F0328；
Aqueous epoxy resins: producer's Jitian's chemical industry, trade mark E0430；
Water-based acrylic resin: Guangzhou Ao Yate composite material Co., Ltd, producer, trade mark 802C；
Curing agent hexamethylene diamine: using the 1,6- hexamethylene diamine of Aladdin.
Embodiment 1
The present embodiment prepares graphene silver nanowires composite mortar as follows:
A, graphene powder 35g, carbon black 5g, dispersing agent hydroxypropyl methyl cellulose 2g and water 30g is taken first to stir according to the ratio
0.5h is mixed, 20g waterborne polyurethane resin then re-ultrasonic dispersion 1h, is added, and high speed ball milling disperses in the ball mill, finally
It is filtered through 250 mesh screen cloths, obtains mixed slurry A；
B, by 10g 10mg/mL silver nanowires dispersion liquid (diameter 100nm, 50-100 μm long), 2g aqueous epoxy resins and
2g water-based acrylic resin is added to vacuum defoamation in de-airing mixer, is uniformly mixed, and obtains mixed liquid B；
C, mixed slurry A is added in de-airing mixer, under continuous stirring, it is 8 that pH buffer, which is added, and adjusts pH, then
Mixed liquid B and curing agent hexamethylene diamine 2g are sequentially added, continues to stir evenly, is i.e. acquisition graphene silver nanowires composite mortar.
Each raw material dosage in embodiment 1 is adjusted by table 1, and carries out the system of composite mortar in the same fashion
It is standby.Wherein dispersing agent used in Examples 1 to 5 is hydroxypropyl methyl cellulose, and dispersing agent used in embodiment 6~7 is that carboxymethyl is fine
Tie up plain sodium.
The raw material of each embodiment composite mortar of table 1 configures
Conductive silver paste prepared by above-described embodiment is tested for the property:
Sample preparation method one: electrocondution slurry prepared by above-described embodiment is coated in 25 μm of Kapton
On, then in 120 DEG C of baking ovens 30min is kept the temperature, obtain sample.Then be tested for the property as follows: electric performance test is (using sheet resistance
Instrument test resistance), adhesive force test (is vertically drawn, draw nothing to fall off twice in succession) using 3M600 adhesive tape, ageing-resistant test (setting
Temperature is 65 DEG C, humidity 90%RH, and the retention time is 21 days, and test sheet resistance variation is qualification less than 10%, is not otherwise conformed to
Lattice), slurry (it is uniform to be coated on after drying on Kapton the observation far infrared heating that is powered by infrared heating uniformity test
Property), bacteriostasis rate tests (sending slurry sample to Guangdong Province microorganism detection center)；The results are shown in Table 2.
Sample preparation method two: electrocondution slurry prepared by above-described embodiment is coated in 25 μm of 6*6cm polyimides
On foamed film, length and width are sticked respectively in two opposite side of film and are the conductive copper adhesive tape of 10*0.5cm, then enclose one layer on slurry
Kapton finally keeps the temperature 30min in 120 DEG C of baking ovens, obtains sample.Then it is tested for the property as follows: soaked reality
It tests and (impregnates sample in water for 24 hours, otherwise observation front and back resistance variations do not conform to if it is qualification that front and back resistance, which becomes smaller in 10%,
Lattice)；Rubbing experiment (sample is placed in washing machine and washs 45min, observation front and back resistance variations after drying, if front and back resistance
Variation is qualification less than 10%, otherwise unqualified)；Crooked experiment (by 180 ° of sample horizontal buckling, continuously bend 10,20,30,
40,60,80,120 times, the bending number before and after record bending when resistance difference 10%)；Sample (is powered and sends out by high temperature resistant test
Heat is observed using infra-red radiation, and record generates the temperature destroyed)；The results are shown in Table 3.
The test result of each embodiment of table 2
The test result of each embodiment of table 3
Finally, it should be noted that obviously, the above embodiment is merely an example for clearly illustrating the present invention, and simultaneously
The non-restriction to embodiment.For those of ordinary skill in the art, it can also do on the basis of the above description
Other various forms of variations or variation out.There is no necessity and possibility to exhaust all the enbodiments.And thus drawn
The obvious changes or variations that Shen goes out are still in the protection scope of this invention.
Claims (4)
1. a kind of graphene silver nanowires composite mortar, which is characterized in that each raw material presses the composition of mass fraction are as follows:
1~20 part of 1~100mg/mL silver nanowires dispersion liquid, 20~50 parts of graphene powder, 1~20 part of carbon black, aqueous poly- ammonia
20~50 parts of ester resin, 1~50 part of aqueous epoxy resins, 1~20 part of water-based acrylic resin, 0.1~5 part of dispersing agent, solidification
0.1~2 part of agent hexamethylene diamine, 0.1~10 part of pH buffer, 20~50 parts of water；
The diameter of silver nanowires is 40~200nm in the silver nanowires dispersion liquid, and length is 10~500 μm；The graphene
The partial size of powder is 2~50 μm, and the partial size of the carbon black is 0.1~10 μm.
2. graphene silver nanowires composite mortar according to claim 1, it is characterised in that: the dispersing agent is selected from 12
One of sodium alkyl sulfate, cetyl benzenesulfonic acid sodium, hydroxypropyl methyl cellulose, sodium carboxymethylcellulose are a variety of.
3. graphene silver nanowires composite mortar according to claim 1, it is characterised in that: the pH buffer is by as follows
Method configuration: 25mL boronic acid containing 0.2mol/L, potassium chloride 0.2mol/L mixed liquor in, the hydrogen-oxygen of 4mL0.1mol/L is added
Change sodium solution and be diluted with water to 100mL after mixing, is i.e. acquisition pH buffer.
4. the preparation method of graphene silver nanowires composite mortar, feature described in a kind of any one of claims 1 to 3 exist
In including the following steps:
A, graphene powder, carbon black, dispersing agent and water are stirred 0.5-6h according to the ratio, re-ultrasonic dispersion 1-10h, then added
Enter waterborne polyurethane resin, and high speed ball milling disperses in the ball mill, most filtered afterwards through 250 mesh screen cloths, obtains mixed slurry A；
B, silver nanowires dispersion liquid, aqueous epoxy resins and water-based acrylic resin vacuum in de-airing mixer is added to take off
Bubble is uniformly mixed, and obtains mixed liquid B；
C, mixed slurry A is added in de-airing mixer, under continuous stirring, it is 8 that pH buffer, which is added, and adjusts pH, then successively
Mixed liquid B and curing agent hexamethylene diamine is added, continues to stir evenly, is i.e. acquisition graphene silver nanowires composite mortar.
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| CN107635296B (en) * | 2017-09-13 | 2020-11-06 | 合肥微晶材料科技有限公司 | Compound flexible heating film subassembly of graphite alkene silver nanometer line |
| CN107910099A (en) * | 2017-10-31 | 2018-04-13 | 南京旭羽睿材料科技有限公司 | A kind of compound silver paste of graphene and preparation method thereof |
| CN111071630A (en) * | 2018-10-22 | 2020-04-28 | 上海海洋大学 | Microwave action element, microwave food package and processing method thereof |
| CN110449169B (en) * | 2019-07-04 | 2021-03-12 | 中山大学 | Semi-metal material Te nanowire/graphene hydrogel composite material and preparation method and application thereof |
| CN113436805A (en) * | 2021-04-29 | 2021-09-24 | 哈工大机器人集团(无锡)科创基地研究院 | Preparation method and application of low-silver aqueous conductive silver paste |
| CN114702887A (en) * | 2022-02-28 | 2022-07-05 | 江苏威久科技发展有限公司 | Graphene silver nanowire composite slurry and preparation method thereof |
| CN115093692A (en) * | 2022-06-27 | 2022-09-23 | 中国石油大学(北京) | Graphene composite electromagnetic shielding film and preparation method thereof |
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