CN109830549A - A kind of indium sulfide/graphene composite film and its preparation method and application - Google Patents
A kind of indium sulfide/graphene composite film and its preparation method and application Download PDFInfo
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Abstract
The invention belongs to composite semiconductor films technical fields, disclose a kind of indium sulfide (In2S3)/graphene composite film and its preparation method and application, the In2S3/ graphene composite film is by inidum chloride, thiocarbamide, polyvinylpyrrolidone is added to configuration reaction precursor liquid in ethylene glycol, there is the FTO Conducting Glass of graphene slurry to be put into micro-wave oven spin coating, under 700~900W of power effect, 180~220 DEG C of progress microwave hydrothermal reactions are made.In of the present invention2S3The object of/graphene composite film mutually uniformly, well-crystallized and purity it is higher.The present invention synthesizes nanometer In using microwave-assisted solution2The laminated film of S and graphene, required equipment and preparation process is simple, low in cost and speed quickly, shorten reaction time, reagent preparation non-toxic and safe.
Description
Technical field
The invention belongs to semiconductor film technique field, more particularly, to a kind of indium sulfide/graphene composite film and
Preparation method and application.
Background technique
Indium sulfide (In2S3) it is a kind of n-type semiconductor, it is typical III~VI family sulfide, has wider forbidden band wide
Degree.In2S3With excellent performance such as optical property, photoelectron performance, acoustical behavior, Electronic Performance etc..Although indium sulfide conduct
A kind of semiconductor material filling transsexual energy with superior catalytic and photoelectricity, but due to its poor electric conductivity, indium sulfide is thin
Application of the film in terms of photoelectrocatalysis is very restricted.The method that existing method prepares indium sulfide composite film material is multiple
Miscellaneous, the reaction time is long, and solvent toxicity is big, this is a difficult point for preparing indium sulfide laminated film.
Summary of the invention
In order to solve above-mentioned the shortcomings of the prior art and disadvantage, the object of the present invention is to provide a kind of In2S3/
Graphene composite film.
Another object of the present invention is the provision of above-mentioned In2S3The preparation method of/graphene composite film.This method uses
Microwave process for synthesizing is with ethylene glycol ((CH2OH)2) it is solvent, inidum chloride (InCl3) it is indium source, thiocarbamide (CH4N2S) is sulphur source, poly- second
Alkene pyrrolidone (PVP) is that surfactant configures reaction precursor liquid, is made in the FTO Conducting Glass that spin coating has graphene
It is standby to obtain In2S3/ graphene composite film.
Still a further object of the present invention is the provision of above-mentioned In2S3The application of/graphene composite film.
The purpose of the present invention is realized by following technical proposals:
A kind of indium sulfide (In2S3)/graphene composite film, the In2S3/ graphene composite film is by inidum chloride, sulphur
Urea and polyvinylpyrrolidone are added to configuration reaction precursor liquid in ethylene glycol, and spin coating is had to the FTO conduction glass of graphene slurry
Glass substrate is put into micro-wave oven, and under 700~900W of power effect, 180~220 DEG C of progress microwave hydrothermal reactions are made.
Preferably, the time of the hydro-thermal reaction is 20~60min.
Preferably, the amount ratio of the inidum chloride, thiocarbamide, polyvinylpyrrolidone and ethylene glycol is (0.1~1) mmol:
(0.1~1) mmol:(0~0.5) g:(20~40) ml.
Preferably, the amount ratio of the inidum chloride, thiocarbamide, polyvinylpyrrolidone and ethylene glycol is (0.2~0.5)
Mmol:(0.2~0.5) mmol:(0.25~0.4) g:(25~35) ml.
Preferably, the graphene slurry is to add terpinol, stone is then added the ethanol solution of ethyl cellulose
Black alkene powder obtains after adding acetylacetone,2,4-pentanedione and OP emulsifier for mixing.
Preferably, the concentration of the ethanol solution of the ethyl cellulose is 8~12wt%, the terpinol and graphene
Mass ratio is (5~10): (0.5~0.1), the volumes of aqueous ethanol ratio of the quality of the terpinol and ethyl cellulose be (1~
2) g:4ml, add the ethanol solution of the ethyl cellulose, acetylacetone,2,4-pentanedione and OP emulsifier volume ratio be 10:(0.1~
0.2): (0.1~0.2).
The In2S3The preparation method of/graphene composite film, comprises the following specific steps that:
S1. terpinol is added in the ethanol solution of ethyl cellulose, is then added graphene powder, magnetic agitation 2~
3h；Add acetylacetone,2,4-pentanedione and OP emulsifier for mixing it is uniform after obtain graphene slurry；
S2. using spin-coating method in FTO spin-on-glass graphene slurry, the good graphene of spin coating is starched in 80~120 DEG C of dryings
Material is sintered at 300~400 DEG C, prepares graphene film in FTO conductive substrates；
S3. 0.1~1mmol inidum chloride, 0.1~1mmol thiocarbamide are sequentially added in the ethylene glycol of 60ml, are then added 0
~0.5g PVP, magnetic agitation to abundant dissolution, with obtaining reaction precursor liquid solution；
S4. the FTO electro-conductive glass of the graphene film prepared in step S2 is put into three-necked flask, and conductive face-up
It places；The precursor solution of step S3 is poured into three-necked flask, three-necked flask is placed in micro-wave oven, power be 700W~
900W reacts at 180~220 DEG C, after the reaction was completed takes out FTO glass, cleaned respectively with dehydrated alcohol and deionized water, then
Its 60~80 DEG C are dried in vacuo, In is made2S3/ graphene composite film.
Preferably, the time of stirring described in step S1 is 2~3h, and the time of drying is 10~20min, step in step S2
The time reacted in rapid S4 is 20~60min.
The In2S3/ graphene composite film is in supercapacitor, lithium ion battery, thin-film solar cells or dyestuff
Application in sensitization solar battery field.
Compared with prior art, the invention has the following advantages:
1. In of the present invention2S3The object of/graphene composite film mutually uniformly, well-crystallized and purity it is higher, there is high ratio table
Area and catalysis and in situ.
2. the present invention is based on microwave-assisted solution to have synthesized nanometer In2The laminated film of S and graphene.Compared to its other party
Method, equipment needed for the present invention and preparation process is simple, low in cost and speed quickly, shorten the reaction time, reagent preparation without
Malicious safety.
3. In of the invention2S3Graphene improves the electric conductivity of film, and THIN COMPOSITE in/graphene composite film
Film has high specific surface area and catalysis and in situ, should have good chemical property.It can be applicable to electrochemical catalytic degradation dirt
Contaminate object, lithium ion cell electrode, solar battery etc..
Detailed description of the invention
Fig. 1 is In in embodiment 22S3The surface SEM photograph of/graphene composite film.
Fig. 2 is In in embodiment 22S3The high-resolution TEM photo of/graphene composite film.
Fig. 3 is In in embodiment 22S3Raman spectrum.
Specific embodiment
The contents of the present invention are further illustrated combined with specific embodiments below, but should not be construed as limiting the invention.
Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagents, method and apparatus.
Embodiment 1
1. preparing the ethanol solution 40ml for the ethyl cellulose that mass fraction is 10wt%, 10g terpinol is added.Then
Ready 0.1g graphene powder is added.Magnetic agitation 2h.It is stirred for evaporating dry dehydrated alcohol.Add 0.6ml levulinic
Graphene slurry is obtained after ketone and 0.6ml OP emulsifier for mixing are uniform.
2. using spin-coating method on the FTO glass conducting surface cleaned up graphitization alkene slurry, place air dry oven 80
DEG C pretreatment 20min.Then it repeats above-mentioned steps to print 6 times, the graphene slurry printed, finally 300 in Muffle furnace
It is sintered under DEG C different temperatures；
3. sequentially add 0.1mmol inidum chloride, 0.1mmol thiocarbamide in the ethylene glycol of 60ml, magnetic agitation is to sufficiently molten
Solution, obtains reaction precursor liquid solution；
4. the FTO electro-conductive glass for preparing graphene film is put into three-necked flask, and conductive placement up；It will be upper
It states the precursor liquid prepared to pour into three-necked flask, three-necked flask is placed in micro-wave oven, reaction temperature is 180 DEG C, micro-wave oven
Power is 700W, reaction time 40min；After the reaction was completed by In2S3The FTO glass of/graphene composite film takes out, respectively
It is cleaned three times with dehydrated alcohol and deionized water, then its 80 DEG C is dried in vacuo, In is made2S3/ graphene composite film.
Embodiment 2
1. preparing the ethanol solution 40ml for the ethyl cellulose that mass fraction is 10wt%, 10g terpinol is added.Then
Ready 0.1g graphene powder is added.Magnetic agitation 2h.It is stirred for evaporating dry dehydrated alcohol.Add 0.6ml levulinic
Graphene slurry is obtained after ketone and 0.6ml OP emulsifier for mixing are uniform.
2. utilizing silk screen print method, graphene slurry is printed in the FTO glass conducting surface cleaned up, places forced air drying
120 DEG C of pretreatment 20min of case.Then it repeats above-mentioned steps to print 6 times, the graphene slurry printed, finally in Muffle furnace
In be sintered under 400 DEG C of different temperatures；
5. sequentially add 0.5mmol inidum chloride, 0.5mmol thiocarbamide in the ethylene glycol of 60ml, then plus 0.25g PVP,
Magnetic agitation obtains reaction precursor liquid solution to abundant dissolution；
6. the FTO electro-conductive glass for preparing graphene film is put into three-necked flask, and conductive placement up；It will be upper
It states the precursor liquid prepared to pour into three-necked flask, three-necked flask is placed in micro-wave oven, reaction temperature is 180 DEG C, micro-wave oven
Power is 800W, reaction time 60min；After the reaction was completed by In2S3The FTO glass of/graphene composite film takes out, respectively
It is cleaned three times with dehydrated alcohol and deionized water, then its 80 DEG C is dried in vacuo, In is made2S3/ graphene composite film.
Fig. 1 is In in the present embodiment2S3The surface SEM photograph of/graphene composite film.Wherein, (a) is multiple (× 2K)
SEM photograph, (b) multiple (× 10K) SEM photograph, (c) multiple (× 20K) SEM photograph, is clear that vulcanization from Fig. 1
Indium (In2S3) load on the surface of graphene, illustrate In2S3And the combination of graphene is very good.Fig. 2 is In in the present embodiment2S3/
The high-resolution TEM photo of graphene composite film.The lattice fringe of indium sulfide and graphene as can be seen from Figure 2, explanation
In2S3It is all very good with graphene crystallinity, also further demonstrate In2S3With the presence of graphene；Fig. 3 is in the present embodiment
In2S3Raman spectrum.As can be known from Fig. 3, there is clearly two peak values, be located at 244cm-1And 3064cm-1, corresponding
In2S3With the Raman peaks of graphene, illustrate In2S3Contain indium sulfide and graphene in/graphene composite film.
Embodiment 3
1. preparing the ethanol solution 40ml for the ethyl cellulose that mass fraction is 10wt%, 10g terpinol is added.Then
Ready 0.2g graphene powder is added, magnetic agitation 4h is stirred for evaporating dry dehydrated alcohol, adds 0.6ml levulinic
Graphene slurry is obtained after ketone and 0.6ml OP emulsifier for mixing are uniform.
2. utilizing silk screen print method, graphene slurry is printed in the FTO glass conducting surface cleaned up, places forced air drying
100 DEG C of pretreatment 20min of case.Then above-mentioned steps are repeated to print 6 times.The graphene slurry printed, finally in Muffle furnace
In be sintered under 350 DEG C of different temperatures；
3. sequentially adding 0.2mmol inidum chloride, 0.2mmol thiocarbamide in the ethylene glycol of 60ml, 0.25PVP is then added,
Magnetic agitation obtains reaction precursor liquid solution to abundant dissolution；
4. the FTO electro-conductive glass for preparing graphene film is put into three-necked flask, and conductive placement up；It will be upper
It states the precursor liquid prepared to pour into three-necked flask, three-necked flask is placed in micro-wave oven, reaction temperature is 200 DEG C, micro-wave oven
Power is 800W, reaction time 50min；After the reaction was completed by In2S3The FTO glass of/graphene composite film takes out, respectively
It is cleaned three times with dehydrated alcohol and deionized water, then its 80 DEG C is dried in vacuo, In is made2S3/ graphene composite film.
Embodiment 4
1. preparing the ethanol solution 40ml for the ethyl cellulose that mass fraction is 10wt%, 10g terpinol is added.Then
Ready 0.2g graphene powder is added, magnetic agitation 4h is stirred for evaporating dry dehydrated alcohol, adds 0.6ml levulinic
Graphene slurry is obtained after ketone and 0.6ml OP emulsifier for mixing are uniform.
2. utilizing silk screen print method, graphene slurry is printed in the FTO glass conducting surface cleaned up, places forced air drying
80-120 DEG C of pretreatment 20min of case.Then above-mentioned steps are repeated to print 6 times.The graphene slurry printed, finally in Muffle
It is sintered under 400 DEG C of different temperatures in furnace；
3. sequentially adding 1.0mmol inidum chloride, 1.0mmol thiocarbamide in the ethylene glycol of 60ml, 0.5g PVP is then added,
Magnetic agitation obtains reaction precursor liquid solution to abundant dissolution；
4. the FTO electro-conductive glass for preparing graphene film is put into three-necked flask, and conductive placement up；It will be upper
It states the precursor liquid prepared to pour into three-necked flask, three-necked flask is placed in micro-wave oven, reaction temperature is 190 DEG C, micro-wave oven
Power is 850W, reaction time 55min；After the reaction was completed by In2S3The FTO glass of/graphene composite film takes out, respectively
It is cleaned three times with dehydrated alcohol and deionized water, then its 80 DEG C is dried in vacuo, In is made2S3/ graphene composite film.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination and simplify,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of indium sulfide/graphene composite film, which is characterized in that the indium sulfide/graphene composite film is by chlorination
Indium, thiocarbamide and polyvinylpyrrolidone are added to configuration reaction precursor liquid in ethylene glycol, have the FTO of graphene slurry to lead spin coating
Electric glass substrate is put into micro-wave oven, and under 700~900W of power effect, 180~220 DEG C of progress microwave hydrothermal reactions are made.
2. indium sulfide/graphene composite film according to claim 1, which is characterized in that the time of the hydro-thermal reaction
For 20~60min.
3. indium sulfide/graphene composite film according to claim 1, which is characterized in that the inidum chloride, gathers thiocarbamide
The amount ratio of vinylpyrrolidone and ethylene glycol is (0.1~1) mmol:(0.1~1) mmol:(0~0.5) g:(20~40) ml.
4. indium sulfide/graphene composite film according to claim 3, which is characterized in that the inidum chloride, gathers thiocarbamide
The amount ratio of vinylpyrrolidone and ethylene glycol is (0.2~0.5) mmol:(0.2~0.5) mmol:(0.25~0.4) g:(25
~35) ml.
5. indium sulfide/graphene composite film according to claim 1, which is characterized in that the graphene slurry be by
The ethanol solution of ethyl cellulose adds terpinol, graphene powder is then added, and adds acetylacetone,2,4-pentanedione and OP emulsifier
It is obtained after stirring.
6. indium sulfide/graphene composite film according to claim 5, which is characterized in that the second of the ethyl cellulose
The concentration of alcoholic solution is 8~12wt%, and the mass ratio of the terpinol and graphene is (5~10): (0.5~0.1), the pine
The quality of oleyl alcohol and the volumes of aqueous ethanol ratio of ethyl cellulose are (1~2) g:4ml, add the second of the ethyl cellulose
The volume ratio of alcoholic solution, acetylacetone,2,4-pentanedione and OP emulsifier is 10:(0.1~0.2): (0.1~0.2).
7. the preparation method of indium sulfide/graphene composite film according to claim 1-6, which is characterized in that
It comprises the following specific steps that:
S1. terpinol is added in the ethanol solution of ethyl cellulose, graphene powder, 2~3h of magnetic agitation is then added；Again
Graphene slurry is obtained after addition acetylacetone,2,4-pentanedione and OP emulsifier for mixing are uniform；
S2. using spin-coating method in FTO spin-on-glass graphene slurry, 80~120 DEG C of dryings exist the good graphene slurry of spin coating
300~400 DEG C are sintered, and prepare graphene film in FTO conductive substrates；
S3. 0.1~1mmol inidum chloride, 0.1~1mmol thiocarbamide are sequentially added in the ethylene glycol of 60ml, then be added 0~
0.5g PVP, magnetic agitation to abundant dissolution, with obtaining reaction precursor liquid solution；
S4. the FTO electro-conductive glass of the graphene film prepared in step S2 is put into three-necked flask, and conduction is put up
It sets；The precursor solution of step S3 is poured into three-necked flask, three-necked flask is placed in micro-wave oven, power be 700W~
900W reacts at 180~220 DEG C, after the reaction was completed takes out FTO glass, cleaned respectively with dehydrated alcohol and deionized water, then
Its 60~80 DEG C are dried in vacuo, In is made2S3/ graphene composite film.
8. the preparation method of indium sulfide/graphene composite film according to claim 7, which is characterized in that in step S1
The time of the stirring is 2~3h, and the dry time is 10~20min in step S2, the time reacted in step S4 is 20~
60min。
9. indium sulfide/graphene composite film according to claim 1-6 is in supercapacitor, lithium-ion electric
Application in pond, thin-film solar cells or field of dye-sensitized solar cells.
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Cited By (7)
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| CN110739155A (en) * | 2019-09-24 | 2020-01-31 | 广东工业大学 | nickel sulfide/graphene composite film and preparation method and application thereof |
| CN112209367A (en) * | 2019-07-12 | 2021-01-12 | 哈尔滨理工大学 | Preparation of indium sulfide nanosphere/foam graphene and electrochemical detection of levodopa |
| CN112209368A (en) * | 2019-07-12 | 2021-01-12 | 哈尔滨理工大学 | Preparation and application of indium sulfide nanosheet array/foamed graphene electrode |
| CN112216525A (en) * | 2019-07-12 | 2021-01-12 | 哈尔滨理工大学 | Preparation of indium sulfide nanosheet array/three-dimensional foam graphene supercapacitor electrode |
| CN112209369A (en) * | 2019-07-12 | 2021-01-12 | 哈尔滨理工大学 | Preparation and application of indium oxide nanosheet array/foamed graphene electrode |
| CN113078300A (en) * | 2021-02-23 | 2021-07-06 | 中科院过程工程研究所南京绿色制造产业创新研究院 | Preparation method of core-shell type indium sulfide microsphere sulfur-loaded composite material and lithium-sulfur battery thereof |
| CN115125560A (en) * | 2022-06-14 | 2022-09-30 | 杭州电子科技大学 | Preparation method of beta-phase indium sulfide micron sheet array |
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| CN112209367A (en) * | 2019-07-12 | 2021-01-12 | 哈尔滨理工大学 | Preparation of indium sulfide nanosphere/foam graphene and electrochemical detection of levodopa |
| CN112209368A (en) * | 2019-07-12 | 2021-01-12 | 哈尔滨理工大学 | Preparation and application of indium sulfide nanosheet array/foamed graphene electrode |
| CN112216525A (en) * | 2019-07-12 | 2021-01-12 | 哈尔滨理工大学 | Preparation of indium sulfide nanosheet array/three-dimensional foam graphene supercapacitor electrode |
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| CN110739155B (en) * | 2019-09-24 | 2021-10-19 | 广东工业大学 | Nickel sulfide/graphene composite film and preparation method and application thereof |
| CN113078300A (en) * | 2021-02-23 | 2021-07-06 | 中科院过程工程研究所南京绿色制造产业创新研究院 | Preparation method of core-shell type indium sulfide microsphere sulfur-loaded composite material and lithium-sulfur battery thereof |
| CN113078300B (en) * | 2021-02-23 | 2022-05-06 | 中科南京绿色制造产业创新研究院 | Preparation method of core-shell type indium sulfide microsphere sulfur-loaded composite material and lithium-sulfur battery thereof |
| CN115125560A (en) * | 2022-06-14 | 2022-09-30 | 杭州电子科技大学 | Preparation method of beta-phase indium sulfide micron sheet array |
| CN115125560B (en) * | 2022-06-14 | 2023-10-17 | 杭州电子科技大学 | Preparation method of beta-phase indium sulfide micro-sheet array |
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