CN103895319B - The method of composite membrane is prepared in a kind of spraying of high performance composite graphite alkene electrically-conducting paint - Google Patents
The method of composite membrane is prepared in a kind of spraying of high performance composite graphite alkene electrically-conducting paint Download PDFInfo
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- CN103895319B CN103895319B CN201410159864.8A CN201410159864A CN103895319B CN 103895319 B CN103895319 B CN 103895319B CN 201410159864 A CN201410159864 A CN 201410159864A CN 103895319 B CN103895319 B CN 103895319B
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- 239000002131 composite material Substances 0.000 title claims abstract description 74
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 45
- 239000010439 graphite Substances 0.000 title claims abstract description 45
- 238000005507 spraying Methods 0.000 title claims abstract description 45
- -1 graphite alkene Chemical class 0.000 title claims abstract description 42
- 239000003973 paint Substances 0.000 title claims abstract description 38
- 239000012528 membrane Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000000576 coating method Methods 0.000 claims abstract description 55
- 239000011248 coating agent Substances 0.000 claims abstract description 50
- 239000000758 substrate Substances 0.000 claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 32
- 229910021389 graphene Inorganic materials 0.000 claims description 29
- 239000002105 nanoparticle Substances 0.000 claims description 21
- 239000007921 spray Substances 0.000 claims description 19
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 229910052802 copper Inorganic materials 0.000 claims description 14
- 239000010949 copper Substances 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 7
- WUGQZFFCHPXWKQ-UHFFFAOYSA-N Propanolamine Chemical compound NCCCO WUGQZFFCHPXWKQ-UHFFFAOYSA-N 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 7
- 238000000137 annealing Methods 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000003431 cross linking reagent Substances 0.000 claims description 7
- 239000013530 defoamer Substances 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 235000012239 silicon dioxide Nutrition 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000012286 potassium permanganate Substances 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 235000019394 potassium persulphate Nutrition 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- 239000000725 suspension Substances 0.000 claims description 2
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims 1
- 230000003287 optical effect Effects 0.000 abstract description 2
- 230000005611 electricity Effects 0.000 abstract 1
- 239000002918 waste heat Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
- Paints Or Removers (AREA)
Abstract
The method of composite membrane is prepared in the spraying that the invention discloses a kind of high performance composite graphite alkene electrically-conducting paint, first the method prepares composite graphite alkene electrically-conducting paint, again electrically-conducting paint is dispersed in DMF solution, and then by being sprayed on the substrate of waste heat, finally coating is heat-treated, obtain the laminated film with good optical, electricity and mechanical property, this field such as filrn photovoltaic devices and electronic circuit, is with a wide range of applications.
Description
Technical field
The present invention is specifically related to the method that composite membrane is prepared in the spraying of a kind of High-performance graphene composite electrically-conducting paint, belongs to spraying coating process field.
Background technology
Electrically-conducting paint refers to and can be applied on non-conductive substrates by various spraying method, make it a kind of new type functional coating that there is conductive electric current and get rid of accumulate static charge ability, electrical conductivity after film is generally greater than 10S/m, is widely applied to every field at present.
Current electrically-conducting paint can be divided into structural conductive coating and addition type electrically-conducting paint according to electrical conduction mechanism and composition.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, the dark welcome by everybody.People develop multiple strong electric conductivity electrically-conducting paint in succession, as conductive filler mainly contains metal system (silver powder, copper powder, nickel powder etc.), glass/metal compound and charcoal system (graphite, carbon black) etc.But these electrically-conducting paints, the mechanical strength and the conductance that prepare coating are difficult to improve, and the density of coating is comparatively large, and these problems limit its range of application greatly simultaneously.Also there are people to use Graphene to prepare electrically-conducting paint, then improve the conductive and mechanical properties of spraying, but it are higher to there is cost, the deficiency of the raising and performance 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 conditions according to the physical and chemical performance of composite coating, the physical and chemical performance of optimized reservation composite coating, urgently returns home greatly and finds a kind of suitable spraying coating process to prepare laminated film.
Summary of the invention
The object of the invention is for the problems referred to above, the present invention is by optimizing composite coating, the temperature of substrate and spraying conditions, 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 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, the temperature wherein sprayed 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) repeat step 3) and 4), by 5-7 time repeat spray, obtain good compactness, the coating of appropriate thickness;
6) obtained coating is put into vacuum tube furnace, under the protection of argon gas, in 500-550 DEG C of annealing 2 hours, thus obtain the composite membrane of composite graphite alkene conductive coating.
Natural flake graphite, potassium peroxydisulfate and phosphorus pentoxide preferably join in the concentrated sulfuric acid of 10ml/ part according to the weight portion ratio of 1:1:1 by the preparation method of Graphene, ultrasonic 10min, stir 2 hours at 80 degrees celsius; And then add a certain amount of potassium permanganate, and stir 2 hours under the condition of ice bath; At room temperature add the deionized water of 1000ml/ part afterwards, stirring at room temperature 2 hours; After stirring terminates, then add the hydrogen peroxide of 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 uniformity of preparation is good, due to the composition of its material, therefore, its electric property is good, and according to adjustment spraying coating process, this film is at suprabasil strong adhesion, and specific area is large, also there is good flexibility, the various device of preparation can be processed once again 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 implemented, further detailed description is done to the present invention.
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:
Graphene 115 parts
Inorganic silicon dioxide nano particle 8 parts
Described nano SiO 2 particle diameter is 100 nanometers
Inorganic metal copper nano particles 7 parts
Described copper nano particles diameter is 100 nanometers
Dispersant 2 parts
Nertralizer Propanolamine 2 parts
Levelling agent butyl ether 2 parts
Defoamer 2 parts
Crosslinking agent 3 parts
Ethanol 80 parts
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, the temperature wherein sprayed 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) repeat step 3) and 4), by 7 times repeat spraying, obtain good compactness, the coating of appropriate thickness;
6) obtained coating is put into vacuum tube furnace, under the protection of argon gas, in 550 DEG C of annealing 2 hours, thus 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:
Graphene 100 parts
Inorganic silicon dioxide nano particle 3 parts
Described nano SiO 2 particle diameter is 10 nanometers
Inorganic metal copper nano particles 5 parts
Described copper nano particles diameter is 30 nanometers
Dispersant 1 part
Nertralizer Propanolamine 1 part
Levelling agent butyl ether 1 part
Defoamer 1 part
Crosslinking agent 2 parts
Ethanol 50 parts
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, the temperature wherein sprayed 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) repeat step 3) and 4), by 5-7 time repeat spray, obtain good compactness, the coating of appropriate thickness;
6) obtained coating is put into vacuum tube furnace, under the protection of argon gas, in 500 DEG C of annealing 2 hours, thus 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:
Graphene 110 parts
Inorganic silicon dioxide nano particle 8 parts
Described nano SiO 2 particle diameter is 100 nanometers
Inorganic metal copper nano particles 5 parts
Described copper nano particles diameter is 60 nanometers
Dispersant 1 part
Nertralizer Propanolamine 2 parts
Levelling agent butyl ether 1 part
Defoamer 1 part
Crosslinking agent 2 parts
Ethanol 60 parts
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, the temperature wherein sprayed 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) repeat step 3) and 4), by 5 times repeat spraying, obtain good compactness, the coating of appropriate thickness;
6) obtained coating is put into vacuum tube furnace, under the protection of argon gas, in 525 DEG C of annealing 2 hours, thus 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:
Graphene 110 parts
Inorganic silicon dioxide nano particle 4 parts
Described nano SiO 2 particle diameter is 50 nanometers
Inorganic metal copper nano particles 6 parts
Described copper nano particles diameter is 70 nanometers
Dispersant 1 part
Nertralizer Propanolamine 1 part
Levelling agent butyl ether 1 part
Defoamer 2 parts
Crosslinking agent 3 parts
Ethanol 70 parts
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, the temperature wherein sprayed 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) repeat step 3) and 4), by 5 times repeat spraying, obtain good compactness, the coating of appropriate thickness;
6) obtained coating is put into vacuum tube furnace, under the protection of argon gas, in 500 DEG C of annealing 2 hours, thus 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:
Graphene 120 parts
Inorganic silicon dioxide nano particle 4 parts
Described nano SiO 2 particle diameter is 50 nanometers
Inorganic metal copper nano particles 6 parts
Described copper nano particles diameter is 70 nanometers
Dispersant 1 part
Nertralizer Propanolamine 1 part
Levelling agent butyl ether 1 part
Defoamer 2 parts
Crosslinking agent 3 parts
Ethanol 70 parts
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, the temperature wherein sprayed 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) repeat step 3) and 4), by 5 times repeat spraying, obtain good compactness, the coating of appropriate thickness;
6) obtained coating is put into vacuum tube furnace, under the protection of argon gas, in 550 DEG C of annealing 2 hours, thus obtain the composite membrane of composite graphite alkene conductive coating.
Claims (4)
1. a method for composite membrane is prepared in the spraying of 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, the temperature wherein sprayed 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) repeat step 3) and 4), by 5-7 time repeat spray, obtain coating;
6) obtained coating is put into vacuum tube furnace, under the protection of argon gas, in 500-550 DEG C of annealing 2 hours, thus obtain the composite membrane of composite graphite alkene conductive coating.
2. the method for composite membrane is prepared in the spraying of composite graphite alkene electrically-conducting paint as claimed in claim 1, it is characterized in that: natural flake graphite, potassium peroxydisulfate and phosphorus pentoxide join in the concentrated sulfuric acid of 10ml/ part according to the weight portion ratio of 1:1:1 by the preparation method of Graphene, ultrasonic 10min, stirs 2 hours at 80 degrees celsius; And then add a certain amount of potassium permanganate, and stir 2 hours under the condition of ice bath; At room temperature add the deionized water of 1000ml/ part afterwards, stirring at room temperature 2 hours; After stirring terminates, then add the hydrogen peroxide of 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 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 composite graphite alkene electrically-conducting paint as claimed in claim 3, and it is characterized in that: the temperature of spraying is 70 DEG C, the distance of nozzle and substrate surface is 2cm, and the angle of spraying is 50 °, and spray time is 2min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410159864.8A CN103895319B (en) | 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 |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410159864.8A CN103895319B (en) | 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 |
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| CN107779038A (en) * | 2017-10-30 | 2018-03-09 | 汪涛 | Based on graphene water-base resin electrically-conducting paint and preparation method thereof |
| 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 |
| 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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| JPH05105828A (en) * | 1991-10-16 | 1993-04-27 | Matsushita Electric Works Ltd | Conductive paste |
| 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 |
| CN102977742B (en) * | 2012-12-19 | 2015-11-25 | 中国科学院宁波材料技术与工程研究所 | A kind of electrically conducting coating |
| CN103131232B (en) * | 2013-03-27 | 2015-04-15 | 北京大学 | High-performance aqueous graphene paint and preparation method thereof |
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Effective date of registration: 20170310 Address after: 214100 Wuxi, Huishan Province Economic Development Zone, No. Weir Road, building No. 311, room 1702, room 1, No. 1706 Patentee after: WUXI TONGCHUANG GRAPHENE APPLICATION TECHNOLOGY CO., LTD. Address before: Longwan District Wenzhou Road West Wing hit Street No. 168 of 325024 cities in Zhejiang Province Patentee before: Zhang Zuowei |
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Effective date of registration: 20190701 Address after: 610000 1, 3, 1, 366 north section of lakeside road, Tianfu New District, Chengdu, Sichuan Patentee after: Lefu Home Nanomaterials Co., Ltd. Address before: Room 1702 and 1706, Building No. 1, 311 Yanxin Road, Huishan Economic Development Zone, Wuxi City, Jiangsu Province Patentee before: WUXI TONGCHUANG GRAPHENE APPLICATION TECHNOLOGY CO., LTD. |