CN110055031A - A kind of preparation method of width ultravioletvisible absorption Graphene composite thin film material - Google Patents
A kind of preparation method of width ultravioletvisible absorption Graphene composite thin film material Download PDFInfo
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- CN110055031A CN110055031A CN201910449141.4A CN201910449141A CN110055031A CN 110055031 A CN110055031 A CN 110055031A CN 201910449141 A CN201910449141 A CN 201910449141A CN 110055031 A CN110055031 A CN 110055031A
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Abstract
A kind of preparation method of width ultravioletvisible absorption Graphene composite thin film material, comprising the following steps: weigh the phosphoric acid constant volume 250mL that 28.3g mass fraction is 85%；It takes 2g graphene and phosphoric acid solution 5mL to be placed in 60 DEG C of baking oven and activates 5h；By graphene filtering cleaning, it is dry to constant weight and with ferrocene 1:0.5-2 mixed grinding in molar ratio；Polyvinyl alcohol 300mg is taken, 7mL n,N-dimethylacetamide is added, is heated to 120 DEG C of condensing reflux 12h, obtains poly-vinyl alcohol solution；97 DEG C of addition composite material 70mg are cooled to, temperature condensing reflux is kept to obtain mixed liquor for 24 hours；It pipettes and is paved on mixed liquor to culture dish or glass slide, formed a film at room temperature through 2-3 days naturally dries.A kind of preparation method of wide ultravioletvisible absorption Graphene composite thin film material provided by the present invention, has stronger assimilation effect to the ultraviolet-visible under 260-800nm wavelength.
Description
Technical field
The present invention relates to a kind of preparation methods of wide ultravioletvisible absorption Graphene composite thin film material.
Background technique
Composite material (Composite materiaLs) is being macroscopically by two or more material of different nature
Material has the material of new capability by method composition physically or chemically.A variety of materials are complementary to one another in performance, are generated more
Excellent effect makes the comprehensive performance of composite material be better than former composition material and meet the different requirement of various performances.
Graphene, it is considered to be one kind has the following revolutionary material, optics, mechanics, in terms of all
With good performance, the carbon atom inside graphene is each carbon arranged with sp2 hydridization bonding orbital, and internal
Atom can all make the non-bonding electrons being located on pz track free one out, pz track and the plane degree in a vertical angle of adjacent atom
When, then pi bond can be formed, newly formed pi bond shows as partly filling up state.But since graphene is rendered as inert condition, it is easy hair
Raw agglomeration limits its application in many fields, but can generate with the Material cladding of some different performances more excellent
Different performance preferably plays a role.
Ferrocene is a kind of organo-transition metal compound with aromatic nature, is orange-yellow powder under room temperature, has
Camphor smell.Since ferrocene has bigger pi-electron conjugated system and stronger interior molecules electron transfer properties, tool
There is good photoelectric functional property.
The advantages of composite technology has structure designability, can carry out composite structural design, and can not only hold
Connect excellent properties between each component material, and can according to the combination of performance between different materials be associated with to reach single
The comprehensive performance that kind material can not possess.
Now in light absorbing material and photovoltaic material field, due to lacking to broadband (260-800nm) ultraviolet-visible
Strong absorbing material, cause light absorbing material or photovoltaic material not high always to the absorptivity of sunlight, and then affect photovoltaic
The incident photon-to-electron conversion efficiency of material.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of pair of broadband (260-800nm) ultraviolet-visible have compared with
The preparation method of the strong ultravioletvisible absorption thin-film material of strong assimilation effect.
In order to solve the above technical problems, the present invention provides a kind of wide ultravioletvisible absorption Graphene composite thin film materials
Preparation method, comprising the following steps:
(1) it weighs 25.5-31.2g, the phosphoric acid that mass fraction is 85%, is then diluted with water and is settled to 250mL, be made
Phosphoric acid solution；
(2) 2.0g graphene, 4.5-5.5mL phosphoric acid solution are mixed to be placed in 50-70 DEG C of baking oven and activates 1.8-
2.2h；
(3) graphene after activation is filtered out and is wash with distilled water 7 to the pH of waste liquid, then at 100-120 DEG C
Baking oven in dry 1.8-2.2h it is spare to constant weight；
(4) ratio of the graphene by step (3) after dry and ferrocene 1:0.5-2 in molar ratio mix and grind 1.8-
2.2h obtains composite material；
(5) n,N-dimethylacetamide of 7mL is added in 300mg polyvinyl alcohol, is heated to 110-130 DEG C and is condensed back to
12h is flowed, the magnetic agitation of adjoint 450-550r/min, obtains poly-vinyl alcohol solution in heating process；
(6) poly-vinyl alcohol solution of step (5) is cooled to 96-98 DEG C, the composite material of step (4) is then added
70mg maintains heated condition, so that the temperature for the poly-vinyl alcohol solution for being mixed with composite material is maintained at 96-98 DEG C and be condensed back
For 24 hours, mixed liquor is obtained with the magnetic agitation of 450-550r/min in heating process；
(7) it pipettes mixed liquor and paves and be placed in interior, form a film at room temperature through 2-3 days naturally dries.
Preferably, grinding container material used is agate in step (4).
A kind of advantages of the present invention: preparation of wide ultravioletvisible absorption Graphene composite thin film material provided by the present invention
Method, broadband (i.e. wavelength is 260-800nm) ultraviolet-visible have stronger assimilation effect, the experimental results showed that, in wave
In the region of the wider ultraviolet-visible wavelength of a length of 260-800nm, composite film material obtained by the present invention has preferably light
Assimilation effect especially in the utilization of solar energy resources, can be used as ideal light absorbent in later energy development
It may be used in solar battery.
Grinding container material used is agate, can prevent the graphene of grinding from reacting with ferrocene with container itself.
Detailed description of the invention
Fig. 1 is the infrared spectrogram of the embodiment of the present invention one.
Fig. 2 is the infrared spectrogram of the embodiment of the present invention two.
Fig. 3 is the infrared spectrogram of the embodiment of the present invention three.
Fig. 4 is the ultravioletvisible absorption figure of the embodiment of the present invention one.
Fig. 5 is the ultravioletvisible absorption figure of the embodiment of the present invention two.
Fig. 6 is the ultravioletvisible absorption figure of the embodiment of the present invention three.
Fig. 7 is that the composite material film of the embodiment of the present invention two amplifies 3000 times of photo.
Fig. 8 is that the composite material film of the embodiment of the present invention two amplifies 6000 times of photo.
Fig. 9 is that the composite material film of the embodiment of the present invention two amplifies 12000 times of photo.
Specific embodiment
Embodiment one:
A kind of preparation method of width ultravioletvisible absorption Graphene composite thin film material, comprising the following steps:
(1) phosphoric acid that the mass fraction of 25.5g is 85% is weighed in beaker, is then diluted with water and in 250mL capacity
Constant volume in bottle, is made phosphoric acid solution；
(2) 2.0g graphene is weighed in beaker, is measured phosphoric acid solution 4.5mL and is slowly added in beaker, then will fill
The beaker of graphene and phosphoric acid solution is placed in 50 DEG C of baking oven and activates 1.8h；
(3) graphene after activation is filtered out and is wash with distilled water 7 to the pH of waste liquid, then in 100 DEG C of baking
Dry 1.8h is spare to constant weight in case；
(4) graphene by step (3) after dry and the ferrocene ratio mixing of 2:1 in molar ratio are subsequently poured into agate and grind
1.8h is ground in alms bowl, obtains composite material；
(5) it weighs polyvinyl alcohol 300mg in a round bottom flask, 7mL n,N-dimethylacetamide is added, is heated to 110 DEG C
It is condensed back 12h, heating process obtains poly-vinyl alcohol solution with 450r/min magnetic agitation；
(6) stop that poly-vinyl alcohol solution is cooled to 96 DEG C after heating, the composite material of step (4) preparation is then added
70mg maintains heated condition, so that the temperature for the poly-vinyl alcohol solution for being mixed with composite material is maintained at 96 DEG C and is condensed back for 24 hours, adds
Thermal process obtains mixed liquor with 450r/min magnetic agitation；
(7) above-mentioned mixed liquor is moved on culture dish or glass slide with pipette and is paved, it is disposed within, at room temperature through 2-
3 days naturally dry film forming.
Embodiment two:
A kind of preparation method of width ultravioletvisible absorption Graphene composite thin film material, comprising the following steps:
(1) phosphoric acid that the mass fraction of 28.3g is 85% is weighed in beaker, is then diluted with water and in 250mL capacity
Constant volume in bottle, is made phosphoric acid solution；
(2) 2.0g graphene is weighed in beaker, is measured phosphoric acid solution 5mL and is slowly added in beaker, then will fill stone
The beaker of black alkene and phosphoric acid solution is placed in 60 DEG C of baking oven and activates 2h；
(3) graphene after activation is filtered out and is wash with distilled water 7 to the pH of waste liquid, then in 110 DEG C of baking
Dry 2h is spare to constant weight in case；
(4) graphene by step (3) after dry and the ferrocene ratio mixing of 1:1 in molar ratio are subsequently poured into agate and grind
2h is ground in alms bowl, obtains composite material；
(5) it weighs polyvinyl alcohol 300mg in a round bottom flask, 7mL n,N-dimethylacetamide is added, is heated to 120 DEG C
It is condensed back 12h, heating process obtains poly-vinyl alcohol solution with 500r/min magnetic agitation；
(6) stop that poly-vinyl alcohol solution is cooled to 97 DEG C after heating, the composite material of step (4) preparation is then added
70mg maintains heated condition, so that the temperature for the poly-vinyl alcohol solution for being mixed with composite material is maintained at 97 DEG C and is condensed back for 24 hours, adds
Thermal process obtains mixed liquor with 500r/min magnetic agitation；
(7) above-mentioned mixed liquor is moved on culture dish or glass slide with pipette and is paved, it is disposed within, at room temperature through 2-
3 days naturally dry film forming.
Embodiment three:
A kind of preparation method of width ultravioletvisible absorption Graphene composite thin film material, comprising the following steps:
(1) phosphoric acid that the mass fraction of 31.2g is 85% is weighed in beaker, is then diluted with water and in 250mL capacity
Constant volume in bottle, is made phosphoric acid solution；
(2) 2.0g graphene is weighed in beaker, is measured phosphoric acid solution 5.5mL and is slowly added in beaker, then will fill
The beaker of graphene and phosphoric acid solution is placed in 70 DEG C of baking oven and activates 2.2h；
(3) graphene after activation is filtered out and is wash with distilled water 7 to the pH of waste liquid, then in 120 DEG C of baking
Dry 2.2h is spare to constant weight in case；
(4) graphene by step (3) after dry and the ferrocene ratio mixing of 1:2 in molar ratio are subsequently poured into agate and grind
2.2h is ground in alms bowl, obtains composite material；
(5) it weighs polyvinyl alcohol 300mg in a round bottom flask, 7mL n,N-dimethylacetamide is added, is heated to 130 DEG C
It is condensed back 12h, heating process obtains poly-vinyl alcohol solution with 550r/min magnetic agitation；
(6) stop that poly-vinyl alcohol solution is cooled to 98 DEG C after heating, the composite material of step (4) preparation is then added
70mg maintains heated condition, so that the temperature for the poly-vinyl alcohol solution for being mixed with composite material is maintained at 98 DEG C and is condensed back for 24 hours, adds
Thermal process obtains mixed liquor with 550r/min magnetic agitation；
(7) above-mentioned mixed liquor is moved on culture dish or glass slide with pipette and is paved, it is disposed within, at room temperature through 2-
3 days naturally dry film forming.
In above-described embodiment, the reagent specification of use and the place of production are as shown in the table:
| Reagent name | Specification | The place of production |
| Multi-layer graphene | The rich science and technology of Suzhou carbon | |
| C10H10Fe | >=98% | Sinopharm Chemical Reagent Co., Ltd. |
| DMAC N,N' dimethyl acetamide | It analyzes pure | Tianjin Yong Da chemical reagent Co., Ltd |
Structural characterization:
Respectively according to a kind of width ultravioletvisible absorption graphene composite film material described in embodiment one to embodiment three
The preparation method of material produces composite material film, then carry out infrared detection to it respectively, by infared spectrum to film at
Divide and structure is characterized, the experimental result of embodiment one to embodiment three respectively corresponds Fig. 1-Fig. 3, abscissa in Fig. 1-Fig. 3
For wave number (cm-1), ordinate is reflectivity (%).
As shown in Figure 1-Figure 3, the 3300cm in figure-1For the hydroxyl characteristic absorption peak in the middle part of polyvinyl alcohol.1790cm-1For
Carbonyl characteristic absorption peak, the 1500cm of partial oxidation in graphene-1Nearby occur be in graphene on phenyl ring carbon-carbon bond it is flexible
Vibration peak.1000cm-1And 1100cm-1It is nearby the characteristic peak of ferrocene.Show to contain ferrocene in prepared thin-film material
And graphene.
Absorbent properties characterization:
Respectively according to a kind of width ultravioletvisible absorption graphene composite film material described in embodiment one to embodiment three
The preparation method of material produces composite material film, then carries out ultravioletvisible absorption detection to it respectively, is inhaled by UV, visible light
It receives detection to characterize the absorption intensity of prepared thin-film material, embodiment one to three experimental result of embodiment respectively corresponds
Abscissa is wavelength (nm) in Fig. 4-Fig. 6, Fig. 4-Fig. 6, and ordinate is absorption intensity (a.u.).
It is obtained by Fig. 4-Fig. 6 analysis, by a kind of preparation method of wide ultravioletvisible absorption Graphene composite thin film material
The maximum absorption wavelength of the composite material film of production is respectively 268nm, 295nm, 464nm, and composite material film is in 260-
There is very strong ultravioletvisible absorption effect in 800nm wave-length coverage, it can be seen that, the composite material ultravioletvisible absorption range
Wider, the composite film material of the two can do good ultravioletvisible absorption material.
The detection of SEM scanning electron microscope:
Respectively according to a kind of preparation method of width ultravioletvisible absorption Graphene composite thin film material described in embodiment two
Produce composite material film, then carry out SEM scanning electron microscope detection to it respectively, under scanning electron microscope to composite material film according to
Secondary amplification 3000 times, 6000 times, 12000 times, we can be clearly seen that the crystal morphology of film from Electronic Speculum map, and
The situation of plane of crystal.
SEM electromicroscopic photograph as shown in figs. 7 to 9, from Fig. 7 it can be seen that composite material crystal glomeration, particle size are more equal
Even, having a size of several hundred rans, plane of crystal is relatively smooth, and without more hair quality, and composite material surface is with higher
Surface energy.From Fig. 8 it can be seen that film surface is smoother, consistency is high, and cross section is clearly bright and clean；Most of ferrocene is in activity
Disperse relatively uniform in graphene system, compatibility is good, mutually separates there is no apparent；From fig. 9, it can be seen that film surface exists
The loose microcellular structure in part.
Claims (2)
1. a kind of preparation method of width ultravioletvisible absorption Graphene composite thin film material, comprising the following steps:
(1) it weighs 25.5-31.2g, the phosphoric acid that mass fraction is 85%, is then diluted with water and is settled to 250mL, phosphoric acid is made
Solution；
(2) 2.0g graphene, 4.5-5.5mL phosphoric acid solution are mixed to be placed in 50-70 DEG C of baking oven and activates 1.8-2.2h；
(3) graphene after activation is filtered out and is wash with distilled water 7 to the pH of waste liquid, then in 100-120 DEG C of baking
Dry 1.8-2.2h is spare to constant weight in case；
(4) ratio of the graphene by step (3) after dry and ferrocene 1:0.5-2 in molar ratio mix and grind 1.8-
2.2h obtains composite material；
(5) n,N-dimethylacetamide of 7mL is added in 300mg polyvinyl alcohol, is heated to 110-130 DEG C and is condensed back
12h obtains poly-vinyl alcohol solution with the magnetic agitation of 450-550r/min in heating process；
(6) poly-vinyl alcohol solution of step (5) is cooled to 96-98 DEG C, the composite material 70mg of step (4), dimension is then added
Heated condition is held, the temperature for the poly-vinyl alcohol solution for being mixed with composite material is made to be maintained at 96-98 DEG C and is condensed back heating for 24 hours
Mixed liquor is obtained with the magnetic agitation of 450-550r/min in the process；
(7) it pipettes mixed liquor and paves and be placed in interior, form a film at room temperature through 2-3 days naturally dries.
2. a kind of preparation method of wide ultravioletvisible absorption Graphene composite thin film material according to claim 1, special
Sign is: grinding container material used is agate in step (4).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114316955A (en) * | 2021-12-29 | 2022-04-12 | 安徽科技学院 | Preparation method of porous silicon and cuprous thiocyanate compounded optical material |
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| CN114316955A (en) * | 2021-12-29 | 2022-04-12 | 安徽科技学院 | Preparation method of porous silicon and cuprous thiocyanate compounded optical material |
| CN114316955B (en) * | 2021-12-29 | 2023-08-25 | 安徽科技学院 | Preparation method of porous silicon and cuprous thiocyanate composite optical material |
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