CN110165073A - The preparation method of the transparent membrane of the porous carbon composite of graphene-based N doping - Google Patents
The preparation method of the transparent membrane of the porous carbon composite of graphene-based N doping Download PDFInfo
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Abstract
The present invention relates to technical field of composite preparation, in particular to a kind of preparation method of the transparent membrane of the porous carbon composite of graphene-based N doping, it is low that impedance is obtained using the method for fabricated in situ, stability is high and has the transparent membrane of the porous carbon composite of the graphene-based N doping of good planarization, the preparation of the transparent membrane is by the way that ZIF-8@GO composite nano materials are prepared, using having the characteristics that the ZIF-8 of polyhedral structure as persursor material, compare other persursor materials, ZIF-8 phosphorus content is abundant, specific surface area height is more advantageous to graphene point in conjunction with improving electrode conductivuty, and prepare material requested rich content, it is cheap.
Description
Technical field
The present invention relates to technical field of composite preparation, in particular to a kind of porous carbon of graphene-based N doping is compound
The preparation method of the transparent membrane of material.
Background technique
Organic Light Emitting Diode (Organic Light-Emitting Diode, referred to as OLED) is because it is with spontaneous
Light, easily preparation, fast response time, low power consumption and other advantages obtain extensive research and development, and oneself is through being applied to various product, especially
It is that flexible Organic Light Emitting Diode (Flexible OLED, referred to as FOLED) has more frivolous, impact-resistant characteristic, quilt
Being described as " dreamlike display " oneself warp becomes the development trend of a new generation of display field.In the research and development middle-jiao yang, function of the spleen and stomach of OLED device
Pole structure plays the role of very important, and the quality of performance will directly affect device illumination effect and service life.OLED at present
Preparation is generally used as anode using indium tin oxide (ITO), but since ITO material is toxic, cost of manufacture is high, bending is poor and first
The disadvantages of cellulose content gradually decreases makes it that can not be advantageously applied to the preparation of flexible device.The alternative material for studying ITO is made
It is very necessary for the further development of photoelectric display industry for the anode layer of OLED device structure.
Summary of the invention
The technical problems to be solved by the present invention are: providing a kind of the saturating of the porous carbon composite of graphene-based N doping
The preparation method of bright film.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention are as follows:
A kind of preparation method of the transparent membrane of the porous carbon composite of graphene-based N doping, comprising the following steps:
Step 1: graphene powder is added in the ethanol solution that concentration is 1-10mg/ml, obtains the first solution;
Step 2: the first solution that step 1 is obtained is uniformly mixed with polyvinylpyrrolidone, obtains the second conjunction solution;
Step 3: nitric acid Zinc material and 2-methylimidazole are added in the second solution that step 2 obtains, at 20-30 DEG C
At a temperature of stir 5-10h, obtain third solution;
Step 4: the third solution obtained after stirring in step 3 is centrifuged under the revolving speed of 3000-10000rpm/min
3-10min obtains ZIF-8@GO composite nano materials after carrying out carrying out washing treatment by ethanol solution;
Step 5: the ZIF-8@GO composite nano materials that step 4 is obtained carry out calcination operation, obtain graphene-based nitrogen
The porous carbon composite of doping;
Step 6: the porous carbon composite for the graphene-based N doping that step 5 is obtained is added in dispersion solvent, obtains
To the dispersion liquid of the porous carbon composite of graphene-based N doping;
Step 7: the dispersion liquid of the porous carbon composite for the graphene-based N doping that step 6 is obtained carries out at spin coating
Reason, obtains the transparent membrane of the porous carbon composite of graphene-based N doping.
The beneficial effects of the present invention are:
This programme using the method for fabricated in situ obtains that impedance is low, stability is high and graphene-based with good planarization
The transparent membrane of the porous carbon composite of N doping, the preparation of the transparent membrane are that ZIF-8@GO is compound to be received by being prepared
Rice material, using the ZIF-8 with polyhedral structure as persursor material, compare other persursor materials, ZIF-8
Phosphorus content is abundant, specific surface area height is more advantageous to graphene point in conjunction with improving electrode conductivuty, and material needed for preparing
Expect rich content, cheap.In-situ synthesized preparation process is simple, is easily achieved, and device therefor is at low cost.With graphene-based
The transparent membrane of the porous carbon composite of N doping replaces the application of ITO material, more meets saving material resources, reduces life
The Green Development theory for producing cost, is with a wide range of applications in photoelectric display field.
Detailed description of the invention
Fig. 1 is a kind of preparation side of the transparent membrane of the porous carbon composite of graphene-based N doping according to the present invention
The step flow chart of method.
Specific embodiment
To explain the technical content, the achieved purpose and the effect of the present invention in detail, below in conjunction with embodiment and cooperate attached
Figure is explained.
The most critical design of the present invention is: ZIF-8@GO composite nano materials are prepared, and ZIF- will be prepared
8 GO composite nano materials pass through spin coating and spray after obtaining the porous carbon nano-composite material of graphene-based N doping as presoma
Apply the transparent membrane that the porous carbon composite of graphene-based N doping is prepared in technique.
Fig. 1 is please referred to, technical solution provided by the invention:
A kind of preparation method of the porous carbon composite of graphene-based N doping, comprising the following steps:
Step 1: graphene powder is added in the ethanol solution that concentration is 1-10mg/ml, obtains the first solution;
Step 2: the first solution that step 1 is obtained is uniformly mixed with polyvinylpyrrolidone, obtains the second conjunction solution;
Step 3: nitric acid Zinc material and 2-methylimidazole are added in the second solution that step 2 obtains, at 20-30 DEG C
At a temperature of stir 5-10h, obtain third solution;
Step 4: the third solution obtained after stirring in step 3 is centrifuged under the revolving speed of 3000-10000rpm/min
3-10min obtains ZIF-8@GO composite nano materials after carrying out carrying out washing treatment by ethanol solution;
Step 5: the ZIF-8@GO composite nano materials that step 4 is obtained carry out calcination operation, obtain graphene-based nitrogen
The porous carbon composite of doping;
Step 6: the porous carbon composite for the graphene-based N doping that step 5 is obtained is added in dispersion solvent, obtains
To the dispersion liquid of the porous carbon composite of graphene-based N doping;
Step 7: the dispersion liquid of the porous carbon composite for the graphene-based N doping that step 6 is obtained carries out at spin coating
Reason, obtains the transparent membrane of the porous carbon composite of graphene-based N doping.
As can be seen from the above description, the beneficial effects of the present invention are:
This programme using the method for fabricated in situ obtains that impedance is low, stability is high and graphene-based with good planarization
The transparent membrane of the porous carbon composite of N doping, the preparation of the transparent membrane are that ZIF-8@GO is compound to be received by being prepared
Rice material, using the ZIF-8 with polyhedral structure as persursor material, compare other persursor materials, ZIF-8
Phosphorus content is abundant, specific surface area height is more advantageous to graphene point in conjunction with improving electrode conductivuty, and material needed for preparing
Expect rich content, cheap.In-situ synthesized preparation process is simple, is easily achieved, and device therefor is at low cost.With graphene-based
The transparent membrane of the porous carbon composite of N doping replaces the application of ITO material, more meets saving material resources, reduces life
The Green Development theory for producing cost, is with a wide range of applications in photoelectric display field.
Further, the quality of the polyvinylpyrrolidone in step 2 is 30-70mg.
Further, the quality of nitric acid Zinc material is 2-6g in step 3, and the volume of 2-methylimidazole is 3-7ml.
Further, step 5 specifically:
The ZIF-8@GO composite nano materials that step 4 is obtained are added in tube furnace, nitrogen are passed through, at 600-800 DEG C
The heating rate of temperature lower calcination 2-6h, tube furnace are 1-4 DEG C/min, are taken out after the temperature of tube furnace is cooled to 20-30 DEG C,
Obtain the porous carbon composite of graphene-based N doping.
Further, step 7 specifically:
The dispersion liquid of the composite material of the porous carbon for the graphene-based N doping that step 6 obtains is spun on substrate, with
The revolving speed of 300-1000rpm/min carries out drying process after carrying out spin-coat process, and the porous carbon for obtaining graphene-based N doping is multiple
The transparent membrane of condensation material.
Further, further include step 8:
Multiple spin coating processing is carried out with the identical preparation method of step 7, obtains the graphene-based N doping of different-thickness
The transparent membrane of porous carbon composite;The transparent membrane of the porous carbon composite of the graphene-based N doping with a thickness of
20-200nm。
As can be seen from the above description, passing through the stone of different spin coating revolving speed and the different available different-thickness of spin-coating time
The transparent membrane of the porous carbon composite of mertenyl N doping handles the nanoscale that will be prepared at first by multiple spin coating
The porous carbon composite of other graphene-based N doping tiles and stacks thick graphene-based nitrogen not etc. that obtain large area, high
The porous carbon of the transparent membrane of the porous carbon composite of doping, graphene-based N doping made of being stacked by spin coating technique is multiple
The transparent membrane of condensation material has good profile pattern and electric conductivity, so as to be applied to LCD, OLED, flexibility
In the devices such as OLED and transparence display.
The embodiment of the present invention one are as follows:
A kind of preparation method of the transparent membrane of the porous carbon composite of graphene-based N doping, comprising the following steps:
Step 1: graphene powder is added in the ethanol solution that concentration is 1mg/ml, obtains the first solution;The graphite
Alkene powder is the graphene powder with monolithic layer structure;
Step 2: the first solution that step 1 is obtained is uniformly mixed with 30mg polyvinylpyrrolidone, and it is molten to obtain second
Liquid;
Step 3: 2g nitric acid Zinc material and 3ml 2-methylimidazole are added in the second solution that step 2 obtains, 20
5h is stirred at a temperature of DEG C, obtains third solution;
Step 4: the third solution obtained after stirring in step 3 is centrifuged 3min under the revolving speed of 3000rpm/min, leads to
It crosses after ethanol solution carries out carrying out washing treatment and obtains ZIF-8@GO composite nano materials;
Step 5: the ZIF-8@GO composite nano materials that step 4 is obtained carry out calcination operation, obtain graphene-based nitrogen
The porous carbon composite of doping;Specifically:
The ZIF-8@GO composite nano materials that step 4 is obtained are added in tube furnace, nitrogen are passed through, in 600 DEG C of temperature
The heating rate of lower calcining 6h, tube furnace are 1 DEG C/min, take out after the temperature of tube furnace is cooled to 20 DEG C, obtain graphene
The porous carbon composite of base N doping.
Step 6: the porous carbon composite for the graphene-based N doping that step 5 is obtained is added in dispersion solvent, obtains
To the uniform dispersion of the porous carbon composite of graphene-based N doping;
Step 7: the uniform dispersion of the porous carbon composite for the graphene-based N doping that step 6 obtains is revolved
Painting processing, obtains the transparent membrane of the porous carbon composite of graphene-based N doping;Specifically:
The uniform dispersion of the composite material of the porous carbon for the graphene-based N doping that step 6 obtains is spun to substrate
On, drying process is carried out after carrying out spin-coat process with the revolving speed of 300rpm/min, the porous carbon for obtaining graphene-based N doping is multiple
The transparent membrane of condensation material;The substrate is polyethylene terephthalate (abbreviation PET) substrate.
Further include step 8:
Multiple spin coating processing is carried out with the identical preparation method of step 7, obtains the graphene-based N doping of different-thickness
The transparent membrane of porous carbon composite;The transparent membrane of the porous carbon composite of the graphene-based N doping with a thickness of
20-200nm。
The film thickness for preparing the transparent membrane of the porous carbon composite of the graphene-based N doping of gained through this embodiment is
90nm, square resistance are down to 25.5 Ω/m3, transparency reaches 90%.
The embodiment of the present invention two are as follows:
A kind of preparation method of the transparent membrane of the porous carbon composite of graphene-based N doping, comprising the following steps:
Step 1: graphene powder is added in the ethanol solution that concentration is 4mg/ml, obtains the first solution;
Step 2: the first solution that step 1 is obtained is uniformly mixed with 40mg polyvinylpyrrolidone, and it is molten to obtain second
Liquid;
Step 3: 3g nitric acid Zinc material and 4ml 2-methylimidazole are added in the second solution that step 2 obtains, 28
8h is stirred at a temperature of DEG C, obtains third solution;
Step 4: the third solution obtained after stirring in step 3 is centrifuged 8min under the revolving speed of 6000rpm/min, leads to
It crosses after ethanol solution carries out carrying out washing treatment and obtains ZIF-8@GO composite nano materials;
Step 5: the ZIF-8@GO composite nano materials that step 4 is obtained carry out calcination operation, obtain graphene-based nitrogen
The porous carbon composite of doping;Specifically:
The ZIF-8@GO composite nano materials that step 4 is obtained are added in tube furnace, nitrogen are passed through, in 650 DEG C of temperature
The heating rate of lower calcining 4h, tube furnace are 3 DEG C/min, take out after the temperature of tube furnace is cooled to 28 DEG C, obtain graphene
The porous carbon composite of base N doping.
Step 6: the porous carbon composite for the graphene-based N doping that step 5 is obtained is added in dispersion solvent, obtains
To the uniform dispersion of the porous carbon composite of graphene-based N doping;
Step 7: the uniform dispersion of the porous carbon composite for the graphene-based N doping that step 6 obtains is revolved
Painting processing, obtains the transparent membrane of the porous carbon composite of graphene-based N doping;Step 7 specifically:
The uniform dispersion of the composite material of the porous carbon for the graphene-based N doping that step 6 obtains is spun to substrate
On, drying process is carried out after carrying out spin-coat process with the revolving speed of 550rpm/min, the porous carbon for obtaining graphene-based N doping is multiple
The transparent membrane of condensation material;The substrate is polyethylene terephthalate (abbreviation PET) substrate.
Further include step 8:
Multiple spin coating processing is carried out with the identical preparation method of step 7, obtains the graphene-based N doping of different-thickness
The transparent membrane of porous carbon composite;The transparent membrane of the porous carbon composite of the graphene-based N doping with a thickness of
20-200nm。
The film thickness for preparing the transparent membrane of the porous carbon composite of the graphene-based N doping of gained through this embodiment is
95nm, square resistance are down to 25 Ω/m3, transparency reaches 90.9%.
The embodiment of the present invention three are as follows:
A kind of preparation method of the transparent membrane of the porous carbon composite of graphene-based N doping, comprising the following steps:
Step 1: graphene powder is added in the ethanol solution that concentration is 8mg/ml, obtains the first solution;
Step 2: the first solution that step 1 is obtained is uniformly mixed with 50mg polyvinylpyrrolidone, and it is molten to obtain second
Liquid;
Step 3: 5g nitric acid Zinc material and 5ml 2-methylimidazole are added in the second solution that step 2 obtains, 25
5h is stirred at a temperature of DEG C, obtains third solution;
Step 4: the third solution obtained after stirring in step 3 is centrifuged 10min under the revolving speed of 3000rpm/min,
ZIF-8@GO composite nano materials are obtained after carrying out carrying out washing treatment by ethanol solution;
Step 5: the ZIF-8@GO composite nano materials that step 4 is obtained carry out calcination operation, obtain graphene-based nitrogen
The porous carbon composite of doping;Specifically:
The ZIF-8@GO composite nano materials that step 4 is obtained are added in tube furnace, nitrogen are passed through, in 700 DEG C of temperature
The heating rate of lower calcining 5h, tube furnace are 2 DEG C/min, take out after the temperature of tube furnace is cooled to 25 DEG C, obtain graphene
The porous carbon composite of base N doping.
Step 6: the porous carbon composite for the graphene-based N doping that step 5 is obtained is added in dispersion solvent, obtains
To the uniform dispersion of the porous carbon composite of graphene-based N doping;
Step 7: the uniform dispersion of the porous carbon composite for the graphene-based N doping that step 6 obtains is revolved
Painting processing, obtains the transparent membrane of the porous carbon composite of graphene-based N doping;Specifically:
The uniform dispersion of the composite material of the porous carbon for the graphene-based N doping that step 6 obtains is spun to substrate
On, drying process is carried out after carrying out spin-coat process with the revolving speed of 300rpm/min, the porous carbon for obtaining graphene-based N doping is multiple
The transparent membrane of condensation material;The substrate is polyethylene terephthalate (abbreviation PET) substrate.
Further include step 8:
Multiple spin coating processing is carried out with the identical preparation method of step 7, obtains the graphene-based N doping of different-thickness
The transparent membrane of porous carbon composite;The transparent membrane of the porous carbon composite of the graphene-based N doping with a thickness of
20-200nm。
The film thickness for preparing the transparent membrane of the porous carbon composite of the graphene-based N doping of gained through this embodiment is
100nm, square resistance are down to 24 Ω/m3, transparency reaches 91.2%.
The embodiment of the present invention four are as follows:
A kind of preparation method of the transparent membrane of the porous carbon composite of graphene-based N doping, comprising the following steps:
Step 1: graphene powder is added in the ethanol solution that concentration is 10mg/ml, obtains the first solution;
Step 2: the first solution that step 1 is obtained is uniformly mixed with 70mg polyvinylpyrrolidone, and it is molten to obtain second
Liquid;
Step 3: 6g nitric acid Zinc material and 7ml 2-methylimidazole are added in the second solution that step 2 obtains, 30
10h is stirred at a temperature of DEG C, obtains third solution;
Step 4: the third solution obtained after stirring in step 3 is centrifuged 10min under the revolving speed of 10000rpm/min,
ZIF-8@GO composite nano materials are obtained after carrying out carrying out washing treatment by ethanol solution;
Step 5: the ZIF-8@GO composite nano materials that step 4 is obtained carry out calcination operation, obtain graphene-based nitrogen
The porous carbon composite of doping;Specifically:
The ZIF-8@GO composite nano materials that step 4 is obtained are added in tube furnace, nitrogen are passed through, in 800 DEG C of temperature
The heating rate of lower calcining 3h, tube furnace are 4 DEG C/min, take out after the temperature of tube furnace is cooled to 30 DEG C, obtain graphene
The porous carbon composite of base N doping.
Step 6: the porous carbon composite for the graphene-based N doping that step 5 is obtained is added in dispersion solvent, obtains
To the uniform dispersion of the porous carbon composite of graphene-based N doping;
Step 7: the uniform dispersion of the porous carbon composite for the graphene-based N doping that step 6 obtains is revolved
Painting processing, obtains the transparent membrane of the porous carbon composite of graphene-based N doping;Specifically:
The uniform dispersion of the composite material of the porous carbon for the graphene-based N doping that step 6 obtains is spun to substrate
On, drying process is carried out after carrying out spin-coat process with the revolving speed of 1000rpm/min, the porous carbon for obtaining graphene-based N doping is multiple
The transparent membrane of condensation material;The substrate is polyethylene terephthalate (abbreviation PET) substrate.
Further include step 8:
Multiple spin coating processing is carried out with the identical preparation method of step 7, obtains the graphene-based N doping of different-thickness
The transparent membrane of porous carbon composite;The transparent membrane of the porous carbon composite of the graphene-based N doping with a thickness of
20-200nm。
The film thickness for preparing the transparent membrane of the porous carbon composite of the graphene-based N doping of gained through this embodiment is
105nm, square resistance are down to 24.9 Ω/m3, transparency reaches 90.5%.
The above results show that three gained composite property of above-described embodiment is most stable, and preparation gained transparent membrane has
Minimum impedance value and optimal transparency, therefore embodiment three is this patent optimal case.
In conclusion a kind of system of the transparent membrane of the porous carbon composite of graphene-based N doping provided by the invention
Preparation Method obtains that impedance is low, stability is high using the method for fabricated in situ and the graphene-based N doping with good planarization
Porous carbon composite transparent membrane, the preparation of the transparent membrane is by the way that ZIF-8@GO composite Nano material is prepared
Material, using the ZIF-8 with polyhedral structure as persursor material, compare other persursor materials, and ZIF-8 is carbon containing
Amount is abundant, specific surface area height is more advantageous to graphene point in conjunction with improving electrode conductivuty, and prepares material requested and contain
Amount is abundant, cheap.In-situ synthesized preparation process is simple, is easily achieved, and device therefor is at low cost.Pass through different spin coatings
The thin transparent of the porous carbon composite of the graphene-based N doping of revolving speed and the available different-thickness of different spin-coating times
Film is handled by multiple spin coating and puts down the porous carbon composite of the graphene-based N doping for the Nano grade being prepared at first
Paving and stacking obtain the transparent membrane of large area, graphene-based N doping of varying thickness porous carbon composite, pass through
The transparent membrane of the porous carbon composite of graphene-based N doping made of spin coating technique stacks has good surfacing
Property and electric conductivity, so as to be applied to LCD, OLED, in the flexibility devices such as OLED and transparence display.It is mixed with graphene-based nitrogen
The transparent membrane of miscellaneous porous carbon composite replaces the application of ITO material, more meets saving material resources, reduction is produced into
This Green Development theory, is with a wide range of applications in photoelectric display field.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalents made by bright specification and accompanying drawing content are applied directly or indirectly in relevant technical field, similarly include
In scope of patent protection of the invention.
Claims (6)
1. a kind of preparation method of the transparent membrane of the porous carbon composite of graphene-based N doping, which is characterized in that including
Following steps:
Step 1: graphene powder is added in the ethanol solution that concentration is 1-10mg/ml, obtains the first solution;
Step 2: the first solution that step 1 is obtained is uniformly mixed with polyvinylpyrrolidone, obtains the second solution;
Step 3: nitric acid Zinc material and 2-methylimidazole are added in the second solution that step 2 obtains, in 20-30 DEG C of temperature
Lower stirring 5-10h, obtains third solution;
Step 4: the third solution obtained after stirring in step 3 is centrifuged 3- under the revolving speed of 3000-10000rpm/min
10min obtains ZIF-8@GO composite nano materials after carrying out carrying out washing treatment by ethanol solution;
Step 5: the ZIF-8@GO composite nano materials that step 4 is obtained carry out calcination operation, obtain graphene-based N doping
Porous carbon composite;
Step 6: the porous carbon composite for the graphene-based N doping that step 5 is obtained is added in dispersion solvent, obtains stone
The dispersion liquid of the porous carbon composite of mertenyl N doping;
Step 7: the dispersion liquid of the porous carbon composite for the graphene-based N doping that step 6 is obtained carries out spin-coat process,
Obtain the transparent membrane of the porous carbon composite of graphene-based N doping.
2. the preparation method of the transparent membrane of the porous carbon composite of graphene-based N doping according to claim 1,
It is characterized in that, the quality of the polyvinylpyrrolidone in step 2 is 30-70mg.
3. the preparation method of the transparent membrane of the porous carbon composite of graphene-based N doping according to claim 1,
It is characterized in that, the quality of nitric acid Zinc material is 2-6g in step 3, the volume of 2-methylimidazole is 3-7ml.
4. the preparation method of the transparent membrane of the porous carbon composite of graphene-based N doping according to claim 1,
It is characterized in that, step 5 specifically:
The ZIF-8@GO composite nano materials that step 4 is obtained are added in tube furnace, nitrogen are passed through, in 600-800 DEG C of temperature
The heating rate of lower calcining 2-5h, tube furnace are 1-4 DEG C/min, take out, obtain after the temperature of tube furnace is cooled to 20-30 DEG C
The porous carbon composite of graphene-based N doping.
5. the preparation method of the transparent membrane of the porous carbon composite of graphene-based N doping according to claim 1,
It is characterized in that, step 7 specifically:
The dispersion liquid of the composite material of the porous carbon for the graphene-based N doping that step 6 obtains is spun on substrate, with 300-
The revolving speed of 1000rpm/min carries out drying process after carrying out spin-coat process, obtains the porous carbon composite wood of graphene-based N doping
The transparent membrane of material.
6. the preparation method of the transparent membrane of the porous carbon composite of graphene-based N doping according to claim 1,
Further include step 8:
Multiple spin coating processing is carried out with the identical preparation method of step 7, obtains the porous of the graphene-based N doping of different-thickness
The transparent membrane of carbon composite;The transparent membrane of the porous carbon composite of the graphene-based N doping with a thickness of 20-
200nm。
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CN110642236A (en) * | 2019-09-02 | 2020-01-03 | 吉首大学 | Zinc-based aqueous battery negative electrode material and preparation method thereof |
CN110642236B (en) * | 2019-09-02 | 2022-10-11 | 吉首大学 | Zinc-based aqueous battery negative electrode material and preparation method thereof |
CN115101348A (en) * | 2022-08-01 | 2022-09-23 | 浙江光储充能源科技有限公司 | Preparation method and application of carbon composite perovskite nanocrystalline electrode material |
CN115101348B (en) * | 2022-08-01 | 2024-02-09 | 浙江光储充能源科技有限公司 | Preparation method and application of carbon composite perovskite nanocrystalline electrode material |
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