CN103895319A - Method for preparing composite film by spraying high-performance composite graphene conductive coating - Google Patents

Method for preparing composite film by spraying high-performance composite graphene conductive coating Download PDF

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Publication number
CN103895319A
CN103895319A CN201410159864.8A CN201410159864A CN103895319A CN 103895319 A CN103895319 A CN 103895319A CN 201410159864 A CN201410159864 A CN 201410159864A CN 103895319 A CN103895319 A CN 103895319A
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spraying
graphite alkene
composite
coating
conducting paint
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CN201410159864.8A
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CN103895319B (en
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黄晓明
姚海波
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Lefu Home Nanomaterials Co., Ltd.
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Suzhou Xuandong Three-Dimensional Space Science & Technology Co Ltd
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Abstract

The invention discloses a method for preparing a composite film by spraying a high-performance composite graphene conductive coating. The method comprises the steps of firstly preparing the composite graphene conductive coating, dispersing the conductive coating into a DMF (dimethyl formamide) solution, then spraying the solution to a substrate with waste heat, and finally carrying out thermal treatment on a coating, so as to obtain the composite film with good optical, electrical and mechanical properties. The composite film has wide application values in the fields of photoelectric devices, electronic circuits and the like.

Description

The method of composite membrane is prepared in a kind of spraying of high performance composite graphite alkene electrically-conducting paint
Technical field
The present invention is specifically related to a kind of method that composite membrane is prepared in high-performance Graphene composite electrically-conducting paint spraying, belongs to spraying coating process field.
 
Background technology
Electrically-conducting paint refers to and can be applied on non-conductive ground by various spraying methods, a kind of new type functional coating that makes it to there is conductive electric current and get rid of accumulate static charge ability, electrical conductivity after film is generally greater than 10S/m, has been widely applied at present every field.
Electrically-conducting paint can be divided into structural conductive coating and addition type electrically-conducting paint according to electrical conduction mechanism and composition at present.Wherein addition type electrically-conducting paint is simple, easy to operate, with low cost and can be coated on the advantages such as various surfaces of complex shape owing to having equipment, is deeply subject to everybody welcome.People develop multiple strong electric conductivity electrically-conducting paint in succession, as conductive filler mainly contains compound and charcoal system (graphite, carbon black) of metal system (silver powder, copper powder, nickel powder etc.), glass/metal etc.But, these electrically-conducting paints, the mechanical strength and the conductance that prepare coating are difficult to improve simultaneously, and the density of coating is larger, and these problems limit its range of application greatly.Also there are the people to prepare electrically-conducting paint with Graphene, then improved the conductive and mechanical properties of spraying, but existed cost higher, and the performance deficiency improving that needs.
Simultaneously, how prepared electrically-conducting paint is sprayed into laminated film by suitable method, also be the emphasis that everybody studies, particularly select suitable spraying condition according to the physical and chemical performance of composite coating, the physical and chemical performance of optimized reservation composite coating, a kind of suitable spraying coating process of searching of urgently returning home is greatly prepared laminated film.
 
Summary of the invention
The object of the invention is for the problems referred to above, the present invention is by optimizing temperature and the spraying condition of composite coating, substrate, prepared the conductive film with high optical property, electric property and mechanical property, this film, in the field such as photoelectric device and electronic circuit, is with a wide range of applications.
For achieving the above object, the present invention studies the method that composite membrane is prepared in the spraying of having prepared a kind of high performance composite graphite alkene electrically-conducting paint, comprises following preparation process
1) prepare composite graphite alkene electrically-conducting paint, predominant quantity part of this graphene conductive coating is:
Graphene 100-115 part
Inorganic silicon dioxide nano particle 3-8 part
Described nano SiO 2 particle diameter is 10-100 nanometer
Inorganic metal copper nano particles 5-7 part
Described copper nano particles diameter is 30-100 nanometer
Dispersant 1-2 part
Nertralizer Propanolamine 1-2 part
Levelling agent butyl ether 1-2 part
Defoamer 1-2 part
Crosslinking agent 2-3 part
Ethanol 50-80 part
Water 200-300 part
2) this composite graphite alkene electrically-conducting paint is added in organic solvent DMF, prepare Graphene composite coating DMF solution;
3), by substrate preheating, the temperature of preheating is 100-150 DEG C;
4) adopt the mode of spraying to spray in substrate composite graphite alkene coating, wherein the temperature of spraying is 60-80 DEG C, and the distance of nozzle and substrate surface is 1-3cm, and the angle of spraying is 30-60 °, and spray time is 1-2min;
5) repeating step 3) and 4), by the spraying that repeats of 5-7 time, obtain good compactness, the coating that thickness is suitable;
6) obtained coating is put into vacuum tube furnace, under the protection of argon gas, in 500-550 DEG C of annealing 2 hours, thereby obtain the composite membrane of composite graphite alkene conductive coating.
The preparation method of Graphene is preferably natural flake graphite, potassium peroxydisulfate and phosphorus pentoxide is joined in the concentrated sulfuric acid of 10ml/ part according to the weight portion ratio of 1:1:1, and ultrasonic 10min stirs 2 hours under 80 degrees Celsius; And then add a certain amount of potassium permanganate, and under the condition of ice bath, stir 2 hours; At room temperature add afterwards the deionized water of 1000ml/ part, stirring at room temperature 2 hours; After stirring finishes, then the hydrogen peroxide that adds 8ml/ part, obtain the suspension of jonquilleous graphene oxide; After separating-purifying, obtain pure Graphene.
Substrate is wherein preferably glass or silicon chip.
The temperature that spraying coating process is wherein optimized for spraying is 70 DEG C, and the distance of nozzle and substrate surface is 2cm, and the angle of spraying is 50 °, and spray time is 2min
The beneficial effect that the present invention has:
Spraying coating process of the present invention is simple to operate, and the laminated film good uniformity of preparation, due to the composition of its material, therefore, its electric property is good, and according to regulating spraying coating process, this film is at suprabasil strong adhesion, and specific area is large, also there is good flexibility, can process once again the various devices of preparation as elementary cell, in the field such as photoelectric device and electronic circuit, be with a wide range of applications.
Detailed description of the invention
For further illustrating the present invention, below in conjunction with the concrete example of implementing, the present invention is done to further detailed description.
Embodiment 1:
A method for composite membrane is prepared in the spraying of high performance composite graphite alkene electrically-conducting paint, comprises following preparation process
1) prepare composite graphite alkene electrically-conducting paint, predominant quantity part of this graphene conductive coating is:
115 parts of Graphenes
8 parts of inorganic silicon dioxide nano particles
Described nano SiO 2 particle diameter is 100 nanometers
7 parts of inorganic metal copper nano particles
Described copper nano particles diameter is 100 nanometers
2 parts of dispersants
2 parts of nertralizer Propanolamines
2 parts of levelling agent butyl ether
2 parts of defoamers
3 parts of crosslinking agents
80 parts of ethanol
300 parts, water
2) this composite graphite alkene electrically-conducting paint is added in organic solvent DMF, prepare Graphene composite coating DMF solution;
3), by substrate preheating, the temperature of preheating is 150 DEG C;
4) adopt the mode of spraying to spray in substrate composite graphite alkene coating, wherein the temperature of spraying is 80 DEG C, and the distance of nozzle and substrate surface is 3cm, and the angle of spraying is 60 °, and spray time is 2min;
5) repeating step 3) and 4), by the spraying that repeats of 7 times, obtain good compactness, the coating that thickness is suitable;
6) obtained coating is put into vacuum tube furnace, under the protection of argon gas, in 550 DEG C of annealing 2 hours, thereby obtain the composite membrane of composite graphite alkene conductive coating.
 
Embodiment 2:
A method for composite membrane is prepared in the spraying of high performance composite graphite alkene electrically-conducting paint, comprises following preparation process
1) prepare composite graphite alkene electrically-conducting paint, predominant quantity part of this graphene conductive coating is:
100 parts of Graphenes
3 parts of inorganic silicon dioxide nano particles
Described nano SiO 2 particle diameter is 10 nanometers
5 parts of inorganic metal copper nano particles
Described copper nano particles diameter is 30 nanometers
1 part of dispersant
1 part of nertralizer Propanolamine
1 part of levelling agent butyl ether
1 part of defoamer
2 parts of crosslinking agents
50 parts of ethanol
200 parts, water
2) this composite graphite alkene electrically-conducting paint is added in organic solvent DMF, prepare Graphene composite coating DMF solution;
3), by substrate preheating, the temperature of preheating is 100 DEG C;
4) adopt the mode of spraying to spray in substrate composite graphite alkene coating, wherein the temperature of spraying is 60 DEG C, and the distance of nozzle and substrate surface is 1cm, and the angle of spraying is 30 °, and spray time is 1min;
5) repeating step 3) and 4), by the spraying that repeats of 5-7 time, obtain good compactness, the coating that thickness is suitable;
6) obtained coating is put into vacuum tube furnace, under the protection of argon gas, in 500 DEG C of annealing 2 hours, thereby obtain the composite membrane of composite graphite alkene conductive coating.
 
Embodiment 3:
A method for composite membrane is prepared in the spraying of high performance composite graphite alkene electrically-conducting paint, comprises following preparation process
1) prepare composite graphite alkene electrically-conducting paint, predominant quantity part of this graphene conductive coating is:
110 parts of Graphenes
8 parts of inorganic silicon dioxide nano particles
Described nano SiO 2 particle diameter is 100 nanometers
5 parts of inorganic metal copper nano particles
Described copper nano particles diameter is 60 nanometers
1 part of dispersant
2 parts of nertralizer Propanolamines
1 part of levelling agent butyl ether
1 part of defoamer
2 parts of crosslinking agents
60 parts of ethanol
200 parts, water
2) this composite graphite alkene electrically-conducting paint is added in organic solvent DMF, prepare Graphene composite coating DMF solution;
3), by substrate preheating, the temperature of preheating is 1200 DEG C;
4) adopt the mode of spraying to spray in substrate composite graphite alkene coating, wherein the temperature of spraying is 70 DEG C, and the distance of nozzle and substrate surface is 2cm, and the angle of spraying is 45 °, and spray time is 1.5min;
5) repeating step 3) and 4), by the spraying that repeats of 5 times, obtain good compactness, the coating that thickness is suitable;
6) obtained coating is put into vacuum tube furnace, under the protection of argon gas, in 525 DEG C of annealing 2 hours, thereby obtain the composite membrane of composite graphite alkene conductive coating.
 
Embodiment 4:
A method for composite membrane is prepared in the spraying of high performance composite graphite alkene electrically-conducting paint, comprises following preparation process
1) prepare composite graphite alkene electrically-conducting paint, predominant quantity part of this graphene conductive coating is:
110 parts of Graphenes
4 parts of inorganic silicon dioxide nano particles
Described nano SiO 2 particle diameter is 50 nanometers
6 parts of inorganic metal copper nano particles
Described copper nano particles diameter is 70 nanometers
1 part of dispersant
1 part of nertralizer Propanolamine
1 part of levelling agent butyl ether
2 parts of defoamers
3 parts of crosslinking agents
70 parts of ethanol
280 parts, water
2) this composite graphite alkene electrically-conducting paint is added in organic solvent DMF, prepare Graphene composite coating DMF solution;
3), by substrate preheating, the temperature of preheating is 120 DEG C;
4) adopt the mode of spraying to spray in substrate composite graphite alkene coating, wherein the temperature of spraying is 70 DEG C, and the distance of nozzle and substrate surface is 2cm, and the angle of spraying is 50 °, and spray time is 1min;
5) repeating step 3) and 4), by the spraying that repeats of 5 times, obtain good compactness, the coating that thickness is suitable;
6) obtained coating is put into vacuum tube furnace, under the protection of argon gas, in 500 DEG C of annealing 2 hours, thereby obtain the composite membrane of composite graphite alkene conductive coating.
 
Embodiment 5:
A method for composite membrane is prepared in the spraying of high performance composite graphite alkene electrically-conducting paint, comprises following preparation process
1) prepare composite graphite alkene electrically-conducting paint, predominant quantity part of this graphene conductive coating is:
120 parts of Graphenes
4 parts of inorganic silicon dioxide nano particles
Described nano SiO 2 particle diameter is 50 nanometers
6 parts of inorganic metal copper nano particles
Described copper nano particles diameter is 70 nanometers
1 part of dispersant
1 part of nertralizer Propanolamine
1 part of levelling agent butyl ether
2 parts of defoamers
3 parts of crosslinking agents
70 parts of ethanol
280 parts, water
2) this composite graphite alkene electrically-conducting paint is added in organic solvent DMF, prepare Graphene composite coating DMF solution;
3), by substrate preheating, the temperature of preheating is 120 DEG C;
4) adopt the mode of spraying to spray in substrate composite graphite alkene coating, wherein the temperature of spraying is 60 DEG C, and the distance of nozzle and substrate surface is 2cm, and the angle of spraying is 45 °, and spray time is 1min;
5) repeating step 3) and 4), by the spraying that repeats of 5 times, obtain good compactness, the coating that thickness is suitable;
6) obtained coating is put into vacuum tube furnace, under the protection of argon gas, in 550 DEG C of annealing 2 hours, thereby obtain the composite membrane of composite graphite alkene conductive coating.

Claims (4)

1. a method for composite membrane is prepared in the spraying of high performance composite graphite alkene electrically-conducting paint, it is characterized in that: comprise following preparation process
1) prepare composite graphite alkene electrically-conducting paint, predominant quantity part of this graphene conductive coating is:
Graphene 100-115 part
Inorganic silicon dioxide nano particle 3-8 part
Described nano SiO 2 particle diameter is 10-100 nanometer
Inorganic metal copper nano particles 5-7 part
Described copper nano particles diameter is 30-100 nanometer
Dispersant 1-2 part
Nertralizer Propanolamine 1-2 part
Levelling agent butyl ether 1-2 part
Defoamer 1-2 part
Crosslinking agent 2-3 part
Ethanol 50-80 part
Water 200-300 part
2) this composite graphite alkene electrically-conducting paint is added in organic solvent DMF, prepare Graphene composite coating DMF solution;
3), by substrate preheating, the temperature of preheating is 100-150 DEG C;
4) adopt the mode of spraying to spray in substrate composite graphite alkene coating, wherein the temperature of spraying is 60-80 DEG C, and the distance of nozzle and substrate surface is 1-3cm, and the angle of spraying is 30-60 °, and spray time is 1-2min;
5) repeating step 3) and 4), by the spraying that repeats of 5-7 time, obtain good compactness, the coating that thickness is suitable;
6) obtained coating is put into vacuum tube furnace, under the protection of argon gas, in 500-550 DEG C of annealing 2 hours, thereby obtain the composite membrane of composite graphite alkene conductive coating.
2. the method for composite membrane is prepared in the spraying of high performance composite graphite alkene electrically-conducting paint as claimed in claim 1, it is characterized in that: the preparation method of Graphene joins natural flake graphite, potassium peroxydisulfate and phosphorus pentoxide in the concentrated sulfuric acid of 10ml/ part according to the weight portion ratio of 1:1:1, ultrasonic 10min stirs 2 hours under 80 degrees Celsius; And then add a certain amount of potassium permanganate, and under the condition of ice bath, stir 2 hours; At room temperature add afterwards the deionized water of 1000ml/ part, stirring at room temperature 2 hours; After stirring finishes, then the hydrogen peroxide that adds 8ml/ part, obtain the suspension of jonquilleous graphene oxide; After separating-purifying, obtain pure Graphene.
3. the method for composite membrane is prepared in the spraying of high performance composite graphite alkene electrically-conducting paint as claimed in claim 1 or 2, it is characterized in that: substrate is glass or silicon chip.
4. the method for composite membrane is prepared in the spraying of high performance composite graphite alkene electrically-conducting paint as claimed in claim 3, it is characterized in that: the temperature of spraying is 70 DEG C, and the distance of nozzle and substrate surface is 2cm, and the angle of spraying is 50 °, and spray time is 2min.
CN201410159864.8A 2014-04-21 2014-04-21 The method of composite membrane is prepared in a kind of spraying of high performance composite graphite alkene electrically-conducting paint Active CN103895319B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107779038A (en) * 2017-10-30 2018-03-09 汪涛 Based on graphene water-base resin electrically-conducting paint and preparation method thereof
CN110218469A (en) * 2019-06-25 2019-09-10 东方电气集团东方汽轮机有限公司 A kind of high temperature resistant graphene conductive water-based anticorrosive paint
CN113690456A (en) * 2021-08-06 2021-11-23 米库玻璃纤维增强塑料泰州有限责任公司 High-performance graphene bipolar plate for fuel cell and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05105828A (en) * 1991-10-16 1993-04-27 Matsushita Electric Works Ltd Conductive paste
JP2011134483A (en) * 2009-12-22 2011-07-07 Iwatsu Electric Co Ltd Method of manufacturing conductive coating, and transparent conductive film
CN102977742A (en) * 2012-12-19 2013-03-20 中国科学院宁波材料技术与工程研究所 Conducting paint
CN103131232A (en) * 2013-03-27 2013-06-05 北京大学 High-performance aqueous graphene paint and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05105828A (en) * 1991-10-16 1993-04-27 Matsushita Electric Works Ltd Conductive paste
JP2011134483A (en) * 2009-12-22 2011-07-07 Iwatsu Electric Co Ltd Method of manufacturing conductive coating, and transparent conductive film
JP5304629B2 (en) * 2009-12-22 2013-10-02 岩崎通信機株式会社 Method for producing conductive paint and transparent conductive film
CN102977742A (en) * 2012-12-19 2013-03-20 中国科学院宁波材料技术与工程研究所 Conducting paint
CN103131232A (en) * 2013-03-27 2013-06-05 北京大学 High-performance aqueous graphene paint and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107779038A (en) * 2017-10-30 2018-03-09 汪涛 Based on graphene water-base resin electrically-conducting paint and preparation method thereof
CN110218469A (en) * 2019-06-25 2019-09-10 东方电气集团东方汽轮机有限公司 A kind of high temperature resistant graphene conductive water-based anticorrosive paint
CN110218469B (en) * 2019-06-25 2021-04-20 东方电气集团东方汽轮机有限公司 High-temperature-resistant graphene conductive water-based anticorrosive paint
CN113690456A (en) * 2021-08-06 2021-11-23 米库玻璃纤维增强塑料泰州有限责任公司 High-performance graphene bipolar plate for fuel cell and preparation method thereof
CN113690456B (en) * 2021-08-06 2022-07-22 米库玻璃纤维增强塑料泰州有限责任公司 High-performance graphene bipolar plate for fuel cell and preparation method thereof

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