CN110996411A - Graphene modified inorganic non-metal thick film heating material and preparation method thereof - Google Patents
Graphene modified inorganic non-metal thick film heating material and preparation method thereof Download PDFInfo
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- CN110996411A CN110996411A CN201911244359.2A CN201911244359A CN110996411A CN 110996411 A CN110996411 A CN 110996411A CN 201911244359 A CN201911244359 A CN 201911244359A CN 110996411 A CN110996411 A CN 110996411A
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- 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—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater 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—Heater 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/18—Conductive material dispersed in non-conductive inorganic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
Abstract
The invention discloses a graphene modified inorganic non-metal thick film heating material, which comprises the following steps: uniformly mixing simple substance silicon, nano and sub-nano slag phases to prepare functional phase composite powder, wherein the content of the simple substance silicon accounts for 30-40% of the total weight of the functional phase composite powder; uniformly mixing the functional phase composite powder with glass powder, wherein the content of the glass powder accounts for 20-30% of the total weight of the functional phase composite powder; adding graphene into the mixture powder, wherein the content of the graphene accounts for 0.5-2% of the total weight of the functional phase composite powder; adding an organic solvent into the graphene mixed powder, and uniformly stirring to form thick film slurry; sintering the thick film paste at 1100-1200 ℃ to obtain the required material. The method provided by the invention has the advantages of simple process, good stability of the prepared heating material, good electric and thermal conductivity, low resistance and low energy consumption; can be coated on a plane, curved surface or ring surface substrate in various ways, and can be used in the fields of industry, agriculture, building, household appliances and the like.
Description
Technical Field
The invention relates to the technical field of new material preparation and heating, in particular to a graphene modified inorganic nonmetal thick film heating material and a preparation method thereof.
Background
The heating materials used in the fields of household appliances, industry, agriculture, medicine and the like are mostly resistance wires, the temperature of the resistance wires is higher in a red-hot state under the working state, the resistance wires are easy to oxidize and fuse, the resistance wires generate heat to generate visible light, energy loss is generated, and the resistance wires are used in a spiral state to generate inductive reactance effect. The existing heating material has poor electric conduction, heat conduction, photoelectric conversion and stability.
In 2004, the physicists andrelim and costatin norworth schloff, manchester university, uk, succeeded in separating graphene from graphite by micromechanical exfoliation and studied its quasi-particle nature and magnetic field effects. Subsequently, a great deal of research on graphene shows that graphene also has excellent electrical conductivity, thermal conductivity, light transmittance, stability and the like. Graphene is a polymer made of carbon atoms in sp2The hybrid tracks form a hexagonal honeycomb lattice two-dimensional carbon nanomaterial. Each carbon atom of which is sp2Hybridization is carried out, electrons on a p orbital are contributed to form a large pi bond, pi electrons can move freely, and the electron mobility value of the graphene is up to 2 multiplied by 10 through tests5cm2V · S), therefore, graphene has good conductivity.
Researches show that the thermal conductivity coefficient of the single-layer graphene can reach 5300W/mK, the single-layer graphene is a carbon material with the highest thermal conductivity coefficient at present, the carbon material can be added into a base material to remarkably improve the thermal conductivity of the material, and meanwhile, electrons of the graphene have remarkable plasma resonance effect, so that the graphene has high stability and cannot be attenuated under long-time laser irradiation. The graphene has good light transmission performance, the visible light absorption rate of the single-layer graphene is 2.3%, and the light transmittance is as high as 97.7%. Meanwhile, under the irradiation of light, particularly infrared light, the graphene-based material can generate a remarkable photo-thermal effect, and the thermal effect is transferred to a surrounding medium to increase the temperature of the surrounding medium. In addition, graphene-based materials are essentially infrared-inert, which can greatly reduce the loss of infrared thermal radiation. Due to the performance characteristics, the graphene has very wide application in the fields of energy storage materials, photoelectric materials, electronic devices, heating materials and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a graphene modified inorganic non-metal thick film heating material and a preparation method thereof, and the method can be used for remarkably improving the electric conduction, the heat conduction, the photoelectric conversion and the stability of the material.
In order to achieve the above object, the present invention provides the following technical solution, a method for preparing a graphene modified inorganic non-metallic thick film heating material, comprising the following steps:
s1, preparing functional phase composite powder: uniformly mixing simple substance silicon, nano-scale slag and sub-nano-scale slag, wherein the content of the simple substance silicon accounts for 30-40% of the total weight of the functional phase composite powder;
s2, preparing mixture powder: uniformly mixing functional phase composite powder with glass powder, wherein the content of the glass powder accounts for 20-30% of the total weight of the mixture powder;
s3, preparing graphene mixed powder: adding graphene into the mixture powder, wherein the content of the graphene accounts for 0.5-2% of the total weight of the functional phase composite powder;
s4, preparing thick film paste: adding an organic solvent into the graphene mixed powder, and uniformly stirring the mixed material to form thick film slurry, wherein the content of the organic solvent accounts for 30-40% of the total weight of the functional phase composite powder;
s5, sintering and drying the thick film slurry at the temperature of 1100-1200 ℃ to prepare the graphene modified inorganic nonmetal thick film heating material.
Preferably, the slag phase is oxide and salt, and the weight percentage of the oxide to the salt is 1: (0.8-1.5).
Preferably, the slag phase is one or a combination of more of acid oxide, basic oxide, amphoteric oxide, rare earth element oxide and salt.
Preferably, the slag phase is one or a combination of more of silicon oxide, magnesium oxide, aluminum oxide, yttrium oxide, lanthanum oxide and lithium carbonate.
Preferably, the particle size of the glass powder is in the range of 0.1-5 mm.
Preferably, the organic solvent is one or more of castor oil, calcium ricinoleate, ethanol, terpineol, n-butanol, glycerol, ethyl cellulose, nitrocellulose and linseed oil.
Preferably, the sintering time is 60min to 180 min.
Preferably, in step S5, the ceramic substrate is coated with the thick-film paste, and the ceramic substrate coated with the thick-film paste is sintered.
Preferably, the coating thickness of the thick film paste is inversely proportional to the resistance value of the thick film paste, and the resistance value and the coating thickness are in the following relationship: when the coating thickness is W times 3 μm, the resistance becomes 1/W of that when the film thickness is 3 μm.
The invention also discloses the graphene modified inorganic nonmetal thick film heating material prepared by the method.
Compared with the prior art, the invention has the following effects:
1. the preparation process is simple;
2. the prepared graphene modified inorganic non-metal thick film heating material has good stability, is not easy to damage under the condition of heating temperature of 0-900 ℃, can be used under alternating current and direct current voltage of 3-380V, and has good electric conductivity, good thermal conductivity, low resistance and low energy loss;
3. the thick film is firmly combined with the base material;
4. the coating can be applied to a planar, curved or toroidal substrate in a variety of ways;
5. the application is wide, and the method can be used in the fields of industry, agriculture, buildings, household appliances and the like;
additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is described in further detail below to enable those skilled in the art to practice the invention with reference to the description.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
The first embodiment is as follows:
6.2kg of simple substance silicon, 1.8kg of silicon oxide and 2.0kg of magnesium oxide are taken and mixed according to the simple substance elements and the nano-scale silicon oxide and magnesium oxide slag phase materials to prepare the functional phase composite powder.
Adding 2.45kg of lead-free glass and 0.05kg of graphene into 10.0kg of functional phase composite powder, uniformly mixing, adding 37.5kg of organic solvent, wherein the organic solvent is 33.8kg of castor oil, 1.5kg of calcium ricinoleate and 2.2kg of ethanol, uniformly stirring the mixture to form thick film slurry, coating the thick film slurry on a ceramic matrix, putting the ceramic matrix coated with the thick film slurry into a high-temperature furnace for sintering, wherein the sintering temperature is 1100 ℃, the sintering time is 180min, and the sintering atmosphere is air.
Example two:
5.5kg of simple substance silicon, 2.1kg of silicon oxide, 2.2kg of magnesium oxide and 0.2kg of yttrium oxide are taken, and the functional phase composite powder is prepared by mixing the simple substance elements with sub-nanometer level silicon oxide, magnesium oxide and yttrium oxide slag phase materials.
Adding 2.45kg of lead-free glass and 0.05kg of graphene into 10.0kg of functional phase composite powder, uniformly mixing, adding 37.5kg of organic solvent, wherein the organic solvent is 31.9kg of castor oil, 1.1kg of calcium ricinoleate, 1.9kg of ethanol and 2.6kg of terpineol, uniformly stirring the mixture to form thick film slurry, coating the thick film slurry on a ceramic matrix, putting the ceramic matrix coated with the thick film slurry into a high-temperature furnace for sintering, wherein the sintering temperature is 1200 ℃, the sintering time is 60min, and the sintering atmosphere is air.
Example three:
5.5kg of simple substance silicon, 2.2kg of silicon oxide, 1.8kg of magnesium oxide, 0.3kg of yttrium oxide and 0.2g of lithium carbonate are taken and mixed with nanoscale silicon oxide, magnesium oxide, yttrium oxide and lithium carbonate slag phase materials to prepare the functional phase composite powder.
Adding 2.45kg of lead-free glass and 0.05kg of graphene into 10.0kg of functional phase composite powder, uniformly mixing, adding 37.5kg of organic solvent, wherein the organic solvent is 31.9kg of castor oil, 1.1kg of calcium ricinoleate, 1.9kg of ethanol and 2.6kg of terpineol, uniformly stirring the mixture to form thick film slurry, coating the thick film slurry on a ceramic matrix, putting the ceramic matrix coated with the thick film slurry into a high-temperature furnace for sintering, wherein the sintering temperature is 1100 ℃, the sintering time is 180min, and the sintering atmosphere is air.
Example four:
6.2kg of simple substance silicon, 1.8kg of silicon oxide and 2.0kg of magnesium oxide are taken and mixed according to the simple substance elements and the sub-nanometer level silicon oxide and magnesium oxide slag phase materials to prepare the functional phase composite powder.
Adding 2.4kg of lead-free glass and 0.1kg of graphene into 10.0kg of functional phase composite powder, uniformly mixing, adding 37.5kg of organic solvent, wherein the organic solvent is 33.8kg of castor oil, 1.5kg of calcium ricinoleate and 2.2kg of ethanol, uniformly stirring the mixture to form thick film slurry, coating the thick film slurry on a ceramic matrix, putting the ceramic matrix coated with the thick film slurry into a high-temperature furnace for sintering, wherein the sintering temperature is 1200 ℃, the sintering time is 120min, and the sintering atmosphere is air.
Example five:
taking 1.0kg of simple substance silicon, 1.4kg of magnesium oxide, 1.4kg of aluminum oxide and 0.2kg of yttrium oxide, and mixing the simple substance elements with nano simple substance silicon, magnesium oxide, aluminum oxide and yttrium oxide slag phase materials to prepare the functional phase composite powder.
Adding 2.4kg of lead-free glass and 0.2kg of graphene into 10.0kg of functional phase composite powder, uniformly mixing, adding 37.4kg of organic solvent, wherein the organic solvent is 31.0kg of castor oil, 1.5kg of calcium ricinoleate, 1.9kg of ethanol, 1.9kg of terpineol and 1.1kg of n-butyl alcohol, uniformly stirring the mixture to form thick film slurry, coating the thick film slurry on a ceramic matrix, putting the ceramic matrix coated with the thick film slurry into a high-temperature furnace for sintering, wherein the sintering temperature is 1200 ℃, the sintering time is 60min, and the sintering atmosphere is air.
Comparative example 1
The graphene-modified inorganic non-metallic thick film heating material was prepared according to the method of example 1, except that graphene was not added.
Comparative example 2
The graphene-modified inorganic non-metallic thick film heating material was prepared according to the method of example 1, except that no glass frit was added.
Comparative example 3
The graphene-modified inorganic non-metallic thick film heating material was prepared according to the method of example 1, except that no slag phase was added.
Comparative example 4
Taking 3kg of carbon crystal powder, 4kg of graphene and 6kg of titanium powder, fully and uniformly stirring, calcining at the high temperature of 1100 ℃, cooling, filtering out particles above the nanometer level, and adding 1kg of adhesive and 1kg of diluent to prepare the nanometer polymer nanometer heating material.
In order to verify that the technical scheme provided by the invention can achieve the technical effect, test experiments are carried out on the schemes provided by the embodiments and the comparative examples, the optimal conductivity and the thermal expansion coefficient within the temperature range of 25-600 ℃ are measured, and the specific data are shown in table 1.
TABLE 1
The electric conductivity and the photoelectric conversion rate of the graphene modified inorganic non-metallic thick film heating material provided in the embodiments 1 to 5 are higher than those of the graphene modified inorganic non-metallic thick film heating material provided in the comparative example 1, which shows that the electric conductivity, the photoelectric conversion rate and the thermal stability of the heating material can be remarkably improved by adding the graphene with high electron mobility and high thermal conductivity.
The thermal stability and the photoelectric conversion rate of the graphene modified inorganic non-metal thick film heating material provided in the embodiments 1 to 5 are higher than those of the graphene modified inorganic non-metal thick film heating material provided in the comparative example 2 without adding glass powder, which shows that the thermal stability and the photoelectric conversion rate of the heating material can be remarkably improved by adding the glass phase with high light transmittance and higher heat stability.
The thermal stability and the photoelectric conversion rate of the graphene modified inorganic non-metallic thick film heating material provided in examples 1 to 5 are higher than those of the graphene modified inorganic non-metallic thick film heating material without the slag phase provided in comparative example 3, which shows that the photoelectric conversion efficiency of the heating material is significantly improved by the addition of the nano or sub-nano slag phase having the small size effect.
The electrical conductivity, the thermal expansion coefficient and the photoelectric conversion rate of the graphene modified inorganic non-metal thick film heating material provided in the embodiments 1 to 5 are significantly higher than those of the graphene modified heating material provided in the comparative example 4, which shows that the material prepared by uniformly mixing the raw materials and adding the organic solvent to prepare the slurry has better consistency and the heating material obtained by sintering at 1100-.
In conclusion, the preparation method of the graphene modified inorganic non-technical thick film heating material provided by the invention is simple in process, and the electric conductivity of the prepared graphene modified inorganic non-technical thick film heating material is 6 multiplied by 105S/m or more, and a thermal expansion coefficient of 11X 10-6The film has a photoelectric conversion rate of more than 92 percent below K, has excellent conductivity, photoelectric conversion and stability, low resistance and energy loss, is not easy to damage under the condition of heating temperature of 0-900 ℃, is firmly combined with a base material, can be coated on a plane, a curved surface or a ring surface base body in various modes, and can be widely applied to the fields of industry, agriculture, buildings, household appliances and the like.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (10)
1. The preparation method of the graphene modified inorganic nonmetal thick film heating material is characterized by comprising the following steps of:
s1, preparing functional phase composite powder: uniformly mixing simple substance silicon, nano-scale slag and sub-nano-scale slag, wherein the content of the simple substance silicon accounts for 30-40% of the total weight of the functional phase composite powder;
s2, preparing mixture powder: uniformly mixing functional phase composite powder with glass powder, wherein the content of the glass powder accounts for 20-30% of the total weight of the functional phase composite powder;
s3, preparing graphene mixed powder: adding graphene into the mixture powder, wherein the content of the graphene accounts for 0.5-2% of the total weight of the functional phase composite powder;
s4, preparing thick film paste: adding an organic solvent into the graphene mixed powder, and uniformly stirring the mixed material to form thick film slurry, wherein the content of the organic solvent accounts for 30-40% of the total weight of the functional phase composite powder;
s5, sintering and drying the thick film slurry at the temperature of 1100-1200 ℃ to prepare the graphene modified inorganic nonmetal thick film heating material.
2. The method for preparing the graphene modified inorganic non-metallic thick film heating material according to claim 1, wherein the slag phase is an oxide and a salt, and the weight percentage of the oxide to the salt is 1: (0.8-1.5).
3. The method for preparing the graphene-modified inorganic non-metallic thick film heating material according to claim 2, wherein the slag phase is one or a combination of several of acidic oxide, basic oxide, amphoteric oxide, rare earth oxide and salts.
4. The method for preparing the graphene-modified inorganic non-metallic thick film heating material according to claim 1, wherein the slag phase is one or a combination of silicon oxide, magnesium oxide, aluminum oxide, yttrium oxide, lanthanum oxide and lithium carbonate.
5. The method for preparing the graphene-modified inorganic non-metallic thick film heating material according to claim 1, wherein the particle size of the glass powder is in the range of 0.1-5 mm.
6. The method for preparing the graphene-modified inorganic non-metallic thick film heating material according to claim 1, wherein the organic solvent is one or more of castor oil, calcium ricinoleate, ethanol, terpineol, n-butanol, glycerol, ethyl cellulose, nitrocellulose, and linseed oil.
7. The method for preparing the graphene-modified inorganic non-metallic thick film heating material according to claim 1, wherein the sintering time is 60min to 180 min.
8. The method of claim 1, wherein in step S5, the ceramic substrate coated with the thick film paste is sintered after the thick film paste is applied on the ceramic substrate.
9. The method of claim 8, wherein the thickness of the thick film paste is inversely proportional to the resistance of the thick film paste.
10. The graphene modified inorganic non-metallic thick film heating material prepared by the method of any one of claims 1 to 9.
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| CN1202511A (en) * | 1998-06-02 | 1998-12-23 | 武汉景辉科技发展有限公司 | Thick film high temperature exothermic material |
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| CN104797016A (en) * | 2015-03-25 | 2015-07-22 | 上海迈永节能新材料科技有限公司 | Inorganic non-metal semiconductor far infrared electric heating film material and preparation process thereof |
| CN105702384A (en) * | 2016-03-24 | 2016-06-22 | 广州市尤特新材料有限公司 | Sintered high-heating paste and preparation method thereof |
| CN107396466A (en) * | 2017-07-03 | 2017-11-24 | 王克政 | Electric slurry and preparation method thereof, thick film circuit chip thermal source and preparation method thereof |
| EP3316662A1 (en) * | 2016-11-01 | 2018-05-02 | Goodrich Corporation | Multilayered panels |
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2019
- 2019-12-06 CN CN201911244359.2A patent/CN110996411A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1202511A (en) * | 1998-06-02 | 1998-12-23 | 武汉景辉科技发展有限公司 | Thick film high temperature exothermic material |
| CN1923749A (en) * | 2006-09-15 | 2007-03-07 | 武汉恒升电子有限公司 | Environment-friendly type nanometer multiple phase ceramic heating material and preparation method |
| CN104797016A (en) * | 2015-03-25 | 2015-07-22 | 上海迈永节能新材料科技有限公司 | Inorganic non-metal semiconductor far infrared electric heating film material and preparation process thereof |
| CN105702384A (en) * | 2016-03-24 | 2016-06-22 | 广州市尤特新材料有限公司 | Sintered high-heating paste and preparation method thereof |
| EP3316662A1 (en) * | 2016-11-01 | 2018-05-02 | Goodrich Corporation | Multilayered panels |
| CN107396466A (en) * | 2017-07-03 | 2017-11-24 | 王克政 | Electric slurry and preparation method thereof, thick film circuit chip thermal source and preparation method thereof |
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