CN117545113A - Graphene heating sheet and preparation method thereof - Google Patents
Graphene heating sheet and preparation method thereof Download PDFInfo
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- CN117545113A CN117545113A CN202311635654.7A CN202311635654A CN117545113A CN 117545113 A CN117545113 A CN 117545113A CN 202311635654 A CN202311635654 A CN 202311635654A CN 117545113 A CN117545113 A CN 117545113A
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 132
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 131
- 238000010438 heat treatment Methods 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 49
- 239000011521 glass Substances 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 21
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 21
- 239000010935 stainless steel Substances 0.000 claims abstract description 21
- 239000002135 nanosheet Substances 0.000 claims abstract description 16
- 229910052582 BN Inorganic materials 0.000 claims abstract description 13
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229920006231 aramid fiber Polymers 0.000 claims abstract description 13
- 239000002966 varnish Substances 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 8
- 238000013329 compounding Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 70
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 55
- 239000002002 slurry Substances 0.000 claims description 29
- 239000011248 coating agent Substances 0.000 claims description 28
- 238000000576 coating method Methods 0.000 claims description 28
- 229910052709 silver Inorganic materials 0.000 claims description 21
- 239000004332 silver Substances 0.000 claims description 21
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 10
- 238000007711 solidification Methods 0.000 claims description 10
- 230000008023 solidification Effects 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 6
- WRDNCFQZLUCIRH-UHFFFAOYSA-N 4-(7-azabicyclo[2.2.1]hepta-1,3,5-triene-7-carbonyl)benzamide Chemical compound C1=CC(C(=O)N)=CC=C1C(=O)N1C2=CC=C1C=C2 WRDNCFQZLUCIRH-UHFFFAOYSA-N 0.000 claims description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 5
- 239000001110 calcium chloride Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- LPNYRYFBWFDTMA-UHFFFAOYSA-N potassium tert-butoxide Chemical compound [K+].CC(C)(C)[O-] LPNYRYFBWFDTMA-UHFFFAOYSA-N 0.000 claims description 5
- 238000004804 winding Methods 0.000 claims description 5
- 239000004760 aramid Substances 0.000 claims description 4
- 229920003235 aromatic polyamide Polymers 0.000 claims description 4
- 238000009413 insulation Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000007650 screen-printing Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000243 solution Substances 0.000 description 5
- 238000007789 sealing Methods 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/145—Carbon only, e.g. carbon black, graphite
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/02—Details
- H05B3/03—Electrodes
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
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- Resistance Heating (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to the technical field of graphene heating sheets, in particular to a graphene heating sheet and a preparation method thereof, wherein graphene powder and glass powder are dispersed in water-based varnish, and a graphene heating film with good conductive heating performance is prepared after baking and sintering; secondly, the heat conduction insulating film prepared by compounding the nano aramid fiber and the boron nitride nano sheet serving as raw materials has good insulation and heat conduction properties, and the heat conduction insulating film is coated on the outer side of the graphene heating film to play a good role in insulation and protection and can rapidly transfer the heat energy of the graphene heating film to the stainless steel substrate for heating; finally, the graphene heating sheet prepared by the invention has smaller volume and sheet shape, and heats in a planar manner, so that the occupied area of the graphene heating sheet can be reduced, and the heating range can be enlarged, and the graphene heating sheet has a better market application prospect.
Description
Technical Field
The invention relates to the technical field of graphene heating sheets, in particular to a graphene heating sheet and a preparation method thereof.
Background
The graphene electrothermal film is formed by liquid phase self-assembly or pressing after being compounded with other carbon materials, is directly manufactured into a film by virtue of self-easy film forming property, has no additive, no volatile organic matter, and is environment-friendly and pollution-free. The graphene is electrified to generate heat, the electric energy is almost completely converted into heat energy, no luminous loss exists, the electric heating conversion rate of the traditional resistance wire is only less than 80%, the traditional resistance wire is electrified to excite the graphene to generate far infrared rays, the heat is radiated to the space, and then the surrounding objects emit radiant heat, so that the effect of improving the temperature heating is achieved.
The graphene electrothermal film materials on the market are mostly used in the fields of construction, medical treatment, aviation and the like, but the existing heater with the graphene heating sheet inside is large in size and inconvenient to move, if the graphene heating sheet can be miniaturized, the problem that the occupied space is large can be solved, but the heating effect of the graphene heating sheet is correspondingly reduced while the volume of the graphene heating sheet is reduced, so that a novel graphene heating sheet production method is required to be designed, and the prepared graphene heating sheet has a small volume and can also ensure the heating performance.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects in the prior art, the invention provides the graphene heating sheet and the preparation method thereof, so that the prepared graphene heating sheet heats through the surface, and the occupied area of the graphene heating sheet is reduced while the heating performance of the graphene heating sheet is ensured.
Technical proposal
In order to achieve the above purpose, the invention is realized by the following technical scheme:
a preparation method of a graphene heating sheet, comprising the following steps:
step 1, weighing 15-16 parts by weight of graphene powder, dispersing in 46-50 parts by weight of water-based varnish, adding 3-5 parts by weight of glass powder, mixing, stirring, and sieving with a 100-mesh sieve to obtain graphene slurry;
step 2, coating graphene slurry on the surface of a glass sheet, wherein the thickness of the graphene slurry is 30-50 mu m, baking the graphene slurry to prepare a blank to be sintered, separating the blank to be sintered from the surface of the glass sheet, and sintering the blank to obtain a graphene heating film;
step 3, compounding the nanometer aramid fiber and the boron nitride nanometer sheet to prepare a heat-conducting insulating film;
dispersing 12-15 parts by weight of nano silver powder into 25-30 parts by weight of water-based varnish, mixing and stirring, sieving with a 100-mesh sieve, coating the mixture on the surface of a glass sheet to obtain a nano silver blank with the thickness of 30-40 mu m, baking the nano silver blank to obtain a nano silver blank, separating the nano silver blank from the surface of the glass sheet, and sintering the nano silver blank to obtain a sintered silver sheet;
and 5, tiling the sintered silver sheet on the side edge of the cut graphene heating film, winding and coating the heat conduction insulating film on the outer side walls of the graphene heating film and the sintered silver sheet, and finally bonding the obtained sheet body on the cut stainless steel base material to obtain the graphene heating sheet.
And 5, spraying insulating slurry on the stainless steel with the clean surface, sintering the insulating layer, silk-screen printing the graphene slurry, sintering the graphene heating layer, silk-screen printing and sintering the silver wire electrode layer, and finally silk-screen printing and sintering the insulating sealing layer. And obtaining the stainless steel graphene heating sheet.
Further, the stirring speed of the mixing and stirring in the step 1 is 200-300r/min, and the stirring time is 10-15min.
Further, the baking temperature in the step 2 is 180-200 ℃ and the baking time is 5-10min.
Further, the sintering temperature in the step 2 is 650 ℃, and the sintering time is 3min.
Further, the preparation method of the heat conducting and insulating film in the step 3 comprises the following steps:
firstly, weighing 5g of poly-p-phenylene terephthalamide and 5g of potassium tert-butoxide, pouring the mixture into a flask filled with 100mL of dimethyl sulfoxide, adding 4mL of deionized water, heating and uniformly stirring the mixture in a constant-temperature water bath at 60 ℃, and obtaining a nano aramid dispersion;
step two, weighing 1g of boron nitride nanosheets, dispersing in 10mL of dimethyl sulfoxide, uniformly stirring, pouring the nanosheets into the nano aramid dispersion liquid, and continuously stirring for 8-10min to obtain a mixed dispersion component;
and thirdly, coating the mixed and dispersed components on a glass plate by using a coating machine, then placing the coated film in a calcium chloride aqueous solution with the concentration of 1mol/L for solidification, and drying in an oven at 60 ℃ for 24 hours after solidification to obtain the heat-conducting insulating film.
Further, the stirring speed of the stirring in the first step is 200-300r/min, the stirring time is 5-6h, the stirring speed of the stirring in the second step is 300-400r/min, and the stirring time is 3-5min.
Further, the thickness of the coating film in the third step is 60 to 100 μm.
Further, the baking temperature in the step 4 is 180-200 ℃ and the baking time is 5-10min.
Further, the sintering temperature in the step 4 is 520 ℃ and the sintering time is 3min.
The graphene heating sheet is prepared by the preparation method of the graphene heating sheet, and comprises a sintered silver sheet, a graphene heating film, a heat conduction insulating film and a stainless steel substrate.
Advantageous effects
Compared with the prior art, the graphene heating sheet has the following beneficial effects:
according to the invention, graphene powder and glass powder are dispersed in water-based varnish, and a graphene heating film with good conductive heating performance is prepared after baking and sintering; secondly, the heat conduction insulating film prepared by compounding the nano aramid fiber and the boron nitride nano sheet serving as raw materials has good insulation and heat conduction properties, and the heat conduction insulating film is coated on the outer side of the graphene heating film to play a good role in insulation and protection and can rapidly transfer the heat energy of the graphene heating film to the stainless steel substrate for heating; finally, the graphene heating sheet prepared by the invention has smaller volume and sheet shape, and heats in a planar manner, so that the occupied area of the graphene heating sheet can be reduced, and the heating range can be enlarged, and the graphene heating sheet has a better market application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It is evident that the drawings in the following description are only some embodiments of the present invention and that other drawings may be obtained from these drawings without inventive effort for a person of ordinary skill in the art.
FIG. 1 is a schematic cross-sectional view of a graphene heat-generating sheet according to the present invention;
reference numerals in the drawings represent respectively: 1-sintering silver flakes; 2-graphene heating film; 3-a heat conductive insulating film; 4-stainless steel substrate.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention is further described below with reference to examples.
Example 1
The preparation method of the graphene heating sheet of the embodiment comprises the following steps:
step 1, weighing 15 parts by weight of graphene powder, dispersing in 46 parts by weight of water-based varnish, adding 3 parts by weight of glass powder, mixing, stirring, and sieving with a 100-mesh sieve to obtain graphene slurry; wherein the stirring speed of the mixing and stirring is 200r/min, and the stirring time is 10min.
Step 2, coating graphene slurry on the surface of a glass sheet, wherein the thickness of the graphene slurry is 30 mu m, baking the graphene slurry to prepare a blank to be sintered, separating the blank to be sintered from the surface of the glass sheet, and sintering the blank to obtain a graphene heating film; wherein the baking temperature is 180 ℃, the baking time is 5min, the sintering temperature in the step 2 is 650 ℃, and the sintering time is 3min.
Step 3, compounding the nanometer aramid fiber and the boron nitride nanometer sheet to prepare a heat-conducting insulating film;
the preparation method of the heat conduction insulating film comprises the following steps:
firstly, weighing 5g of poly-p-phenylene terephthalamide and 5g of potassium tert-butoxide, pouring the mixture into a flask filled with 100mL of dimethyl sulfoxide, adding 4mL of deionized water, heating and uniformly stirring in a constant-temperature water bath at 60 ℃, and obtaining a nano aramid fiber dispersion liquid, wherein the stirring speed of uniform stirring is 200r/min, and the stirring time is 5h;
step two, weighing 1g of boron nitride nanosheets, dispersing in 10mL of dimethyl sulfoxide, uniformly stirring, pouring the nanosheets into the nano aramid fiber dispersion liquid, continuously stirring for 8min, and marking the nanosheets as mixed dispersed components, wherein the stirring speed of uniform stirring is 300r/min, and the stirring time is 3min;
and thirdly, coating the mixed and dispersed components on a glass plate by using a coating machine, then placing the coated film in a calcium chloride aqueous solution with the concentration of 1mol/L for solidification, and drying in an oven at 60 ℃ for 24 hours after solidification to obtain the heat-conducting insulating film, wherein the thickness of the coated film is 60 mu m.
Step 4, dispersing 12 parts by weight of nano silver powder into 25 parts by weight of water-based varnish, mixing and stirring, sieving with a 100-mesh sieve, coating the mixture on the surface of a glass sheet to obtain a nano silver blank with the thickness of 30 mu m, baking the nano silver blank to obtain a nano silver blank, separating the nano silver blank from the surface of the glass sheet, and sintering the nano silver blank to obtain a sintered silver sheet; wherein the baking temperature is 180 ℃, the baking time is 5min, the sintering temperature is 520 ℃, and the sintering time is 3min.
And 5, tiling the sintered silver sheet on the side edge of the cut graphene heating film, winding and coating the heat conduction insulating film on the outer side walls of the graphene heating film and the sintered silver sheet, and finally bonding the obtained sheet body on the cut stainless steel base material to obtain the graphene heating sheet.
And 5, spraying insulating slurry on the stainless steel with the clean surface, sintering the insulating layer, silk-screen printing the graphene slurry, sintering the graphene heating layer, silk-screen printing and sintering the silver wire electrode layer, and finally silk-screen printing and sintering the insulating sealing layer. And obtaining the stainless steel graphene heating sheet.
The graphene heating sheet is prepared by the preparation method of the graphene heating sheet, and comprises a sintered silver sheet 1, a graphene heating film 2, a heat conducting insulating film 3 and a stainless steel substrate 4.
Example 2
The preparation method of the graphene heating sheet of the embodiment comprises the following steps:
step 1, weighing 16 parts by weight of graphene powder, dispersing in 50 parts by weight of water-based varnish, adding 5 parts by weight of glass powder, mixing, stirring, and sieving with a 100-mesh sieve to obtain graphene slurry; wherein the stirring speed of the mixing and stirring is 300r/min, and the stirring time is 15min.
Step 2, coating graphene slurry on the surface of a glass sheet, wherein the thickness of the graphene slurry is 50 mu m, baking the graphene slurry to prepare a blank to be sintered, separating the blank to be sintered from the surface of the glass sheet, and sintering the blank to obtain a graphene heating film; wherein the baking temperature is 200 ℃, the baking time is 10min, the sintering temperature in the step 2 is 650 ℃, and the sintering time is 3min.
Step 3, compounding the nanometer aramid fiber and the boron nitride nanometer sheet to prepare a heat-conducting insulating film;
the preparation method of the heat conduction insulating film comprises the following steps:
firstly, weighing 5g of poly-p-phenylene terephthalamide and 5g of potassium tert-butoxide, pouring the mixture into a flask filled with 100mL of dimethyl sulfoxide, adding 4mL of deionized water, heating and uniformly stirring in a constant-temperature water bath at 60 ℃, and obtaining a nano aramid fiber dispersion liquid, wherein the stirring speed of uniform stirring is 300r/min, and the stirring time is 6h;
step two, weighing 1g of boron nitride nanosheets, dispersing in 10mL of dimethyl sulfoxide, uniformly stirring, pouring the nanosheets into the nano aramid fiber dispersion liquid, continuously stirring for 10min, and marking the nanosheets as mixed dispersed components, wherein the stirring speed of uniform stirring is 400r/min, and the stirring time is 5min;
and thirdly, coating the mixed and dispersed components on a glass plate by using a coating machine, then placing the coated film in a calcium chloride aqueous solution with the concentration of 1mol/L for solidification, and drying in an oven at 60 ℃ for 24 hours after solidification to obtain the heat-conducting insulating film, wherein the thickness of the coating film is 100 mu m.
Step 4, dispersing 15 parts by weight of nano silver powder into 30 parts by weight of water-based varnish, mixing and stirring, sieving with a 100-mesh sieve, coating the mixture on the surface of a glass sheet to obtain a nano silver blank with the thickness of 40 mu m, baking the nano silver blank to obtain a nano silver blank, separating the nano silver blank from the surface of the glass sheet, and sintering the nano silver blank to obtain a sintered silver sheet; wherein the baking temperature is 200 ℃, the baking time is 10min, the sintering temperature is 520 ℃, and the sintering time is 3min.
And 5, tiling the sintered silver sheet on the side edge of the cut graphene heating film, winding and coating the heat conduction insulating film on the outer side walls of the graphene heating film and the sintered silver sheet, and finally bonding the obtained sheet body on the cut stainless steel base material to obtain the graphene heating sheet.
And 5, spraying insulating slurry on the stainless steel with the clean surface, sintering a bottom insulating layer, silk-screen printing the graphene slurry, sintering a graphene heating layer, silk-screen printing and sintering a silver wire electrode layer, and finally silk-screen printing and sintering an insulating sealing layer. And obtaining the stainless steel graphene heating sheet.
The graphene heating sheet is prepared by the preparation method of the graphene heating sheet, and comprises a sintered silver sheet 1, a graphene heating film 2, a heat conducting insulating film 3 and a stainless steel substrate 4.
Example 3
The preparation method of the graphene heating sheet of the embodiment comprises the following steps:
step 1, weighing 15 parts by weight of graphene powder, dispersing in 48 parts by weight of water-based varnish, adding 4 parts by weight of glass powder, mixing, stirring, and sieving with a 100-mesh sieve to obtain graphene slurry; wherein the stirring speed of the mixing and stirring is 300r/min, and the stirring time is 13min.
Step 2, coating graphene slurry on the surface of a glass sheet, wherein the thickness of the graphene slurry is 40 mu m, baking the graphene slurry to prepare a blank to be sintered, separating the blank to be sintered from the surface of the glass sheet, and sintering the blank to obtain a graphene heating film; wherein the baking temperature is 190 ℃, the baking time is 8min, the sintering temperature in the step 2 is 650 ℃, and the sintering time is 3min.
Step 3, compounding the nanometer aramid fiber and the boron nitride nanometer sheet to prepare a heat-conducting insulating film;
the preparation method of the heat conduction insulating film comprises the following steps:
firstly, weighing 5g of poly-p-phenylene terephthalamide and 5g of potassium tert-butoxide, pouring the mixture into a flask filled with 100mL of dimethyl sulfoxide, adding 4mL of deionized water, heating and uniformly stirring in a constant-temperature water bath at 60 ℃, and obtaining a nano aramid fiber dispersion liquid, wherein the stirring speed of uniform stirring is 300r/min, and the stirring time is 6h;
step two, weighing 1g of boron nitride nanosheets, dispersing in 10mL of dimethyl sulfoxide, uniformly stirring, pouring the nanosheets into the nano aramid fiber dispersion liquid, continuously stirring for 9min, and marking the nanosheets as mixed dispersed components, wherein the stirring speed of uniform stirring is 400r/min, and the stirring time is 4min;
and thirdly, coating the mixed and dispersed components on a glass plate by using a coating machine, then placing the coated film in a calcium chloride aqueous solution with the concentration of 1mol/L for solidification, and drying in an oven at 60 ℃ for 24 hours after solidification to obtain the heat-conducting insulating film, wherein the thickness of the coated film is 80 mu m.
Step 4, dispersing 13 parts by weight of nano silver powder into 28 parts by weight of water-based varnish, mixing and stirring, sieving with a 100-mesh sieve, coating the mixture on the surface of a glass sheet to obtain a nano silver blank with the thickness of 35 mu m, baking the nano silver blank to obtain a nano silver blank, separating the nano silver blank from the surface of the glass sheet, and sintering the nano silver blank to obtain a sintered silver sheet; wherein the baking temperature is 190 ℃, the baking time is 8min, the sintering temperature is 520 ℃, and the sintering time is 3min.
And 5, tiling the sintered silver sheet on the side edge of the cut graphene heating film, winding and coating the heat conduction insulating film on the outer side walls of the graphene heating film and the sintered silver sheet, and finally bonding the obtained sheet body on the cut stainless steel base material to obtain the graphene heating sheet.
And 5, spraying insulating slurry on the stainless steel with the clean surface, sintering the insulating layer, silk-screen printing the graphene slurry, sintering the graphene heating layer, silk-screen printing and sintering the silver wire electrode layer, and finally silk-screen printing and sintering the insulating sealing layer. And obtaining the stainless steel graphene heating sheet.
The graphene heating sheet is prepared by the preparation method of the graphene heating sheet, and comprises a sintered silver sheet 1, a graphene heating film 2, a heat conducting insulating film 3 and a stainless steel substrate 4.
Comparative example 1
The graphene heating sheet provided in this comparative example and the preparation method thereof are substantially the same as those in example 1, and the main differences are that: in this comparative example 1, the glass powder in the graphene slurry of example 1 was replaced with graphene powder.
Comparative example 2
The graphene heating sheet provided in this comparative example and the preparation method thereof are substantially the same as those in example 1, and the main differences are that: in comparative example 2, the mixed dispersion component in the method for producing a thermally conductive and insulating film in example 1 was replaced with a nanoaramid dispersion to which no boron nitride nanosheets were added.
Performance testing
1. The resistivity of the graphene heat-generating films prepared in examples 1 to 3 and comparative example 1 was measured, and the obtained data is recorded in table 1;
2. the graphene heat-generating films prepared in examples 1 to 3 and comparative example 1 were cut into 150X 10X 0.02mm 3 Then using a universal tester with a sensor accuracy of 0.001N, see GB/T1040.3-2006/ISO527-3: the ultimate breaking strength was measured by the standard of 1995, the loading rate was 0.05mm/min, and the obtained data are recorded in Table 1;
3. the heat conductive properties of the heat conductive insulating films prepared in examples 1 to 3 and comparative example 2 were examined, including in-plane heat conductivity K In And vertical thermal conductivity K Out The data obtained are recorded in table 1;
4. the graphene heating sheets prepared in examples 1-3 were connected to a mobile power supply of 5V and 2A, and the temperature changes of 0s, 10s, 30s and 60s were photographed by an FLIRT600 thermal infrared imager at an ambient temperature of 25 ℃, and the obtained data are recorded in table 2.
TABLE 1
TABLE 2
The data in the table show that the graphene heating film prepared in the embodiment 1-3 has lower resistivity and better mechanical property, and the heat conducting insulating film prepared in the embodiment 1-3 has better heat conducting property, and the graphene heating sheet prepared in the invention can quickly heat and has excellent market popularization value.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the graphene heating sheet is characterized by comprising the following steps of:
step 1, weighing 15-16 parts by weight of graphene powder, dispersing in 46-50 parts by weight of water-based varnish, adding 3-5 parts by weight of glass powder, mixing, stirring, and sieving with a 100-mesh sieve to obtain graphene slurry;
step 2, coating graphene slurry on the surface of a glass sheet, wherein the thickness of the graphene slurry is 30-50 mu m, baking the graphene slurry to prepare a blank to be sintered, separating the blank to be sintered from the surface of the glass sheet, and sintering the blank to obtain a graphene heating film;
step 3, compounding the nanometer aramid fiber and the boron nitride nanometer sheet to prepare a heat-conducting insulating film;
dispersing 12-15 parts by weight of nano silver powder into 25-30 parts by weight of water-based varnish, mixing and stirring, sieving with a 100-mesh sieve, coating the mixture on the surface of a glass sheet to obtain a nano silver blank with the thickness of 30-40 mu m, baking the nano silver blank to obtain a nano silver blank, separating the nano silver blank from the surface of the glass sheet, and sintering the nano silver blank to obtain a sintered silver sheet;
and 5, tiling the sintered silver sheet on the side edge of the cut graphene heating film, winding and coating the heat conduction insulating film on the outer side walls of the graphene heating film and the sintered silver sheet, and finally bonding the obtained sheet body on the cut stainless steel base material to obtain the graphene heating sheet.
2. The method for preparing a graphene heating sheet according to claim 1, wherein the stirring speed of the mixing and stirring in the step 1 is 200-300r/min, and the stirring time is 10-15min.
3. The method for preparing a graphene heating sheet according to claim 2, wherein the baking temperature in the step 2 is 180-200 ℃ and the baking time is 5-10min.
4. The method for preparing a graphene heat-generating sheet according to claim 1, wherein the sintering temperature in the step 2 is 650 ℃ and the sintering time is 3min.
5. The method for preparing a graphene heating sheet according to claim 1, wherein the method for preparing the heat conducting and insulating film in the step 3 is as follows:
firstly, weighing 5g of poly-p-phenylene terephthalamide and 5g of potassium tert-butoxide, pouring the mixture into a flask filled with 100mL of dimethyl sulfoxide, adding 4mL of deionized water, heating and uniformly stirring the mixture in a constant-temperature water bath at 60 ℃, and obtaining a nano aramid dispersion;
step two, weighing 1g of boron nitride nanosheets, dispersing in 10mL of dimethyl sulfoxide, uniformly stirring, pouring the nanosheets into the nano aramid dispersion liquid, and continuously stirring for 8-10min to obtain a mixed dispersion component;
and thirdly, coating the mixed and dispersed components on a glass plate by using a coating machine, then placing the coated film in a calcium chloride aqueous solution with the concentration of 1mol/L for solidification, and drying in an oven at 60 ℃ for 24 hours after solidification to obtain the heat-conducting insulating film.
6. The preparation method of the graphene heating sheet according to claim 5, wherein the stirring speed of stirring uniformly in the first step is 200-300r/min, the stirring time is 5-6h, the stirring speed of stirring uniformly in the second step is 300-400r/min, and the stirring time is 3-5min.
7. The method for preparing a graphene heat-generating sheet according to claim 5, wherein the thickness of the coating film in the third step is 60-100 μm.
8. The method for preparing a graphene heating sheet according to claim 1, wherein the baking temperature in the step 4 is 180-200 ℃ and the baking time is 5-10min.
9. The method for preparing a graphene heat-generating sheet according to claim 1, wherein the sintering temperature in the step 4 is 520 ℃ and the sintering time is 3min.
10. A graphene heating sheet, characterized in that the graphene heating sheet is prepared by the preparation method of the graphene heating sheet according to any one of claims 1 to 9, and comprises a sintered silver sheet (1), a graphene heating film (2), a heat conducting insulating film (3) and a stainless steel substrate (4).
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