CN107805827A - The preparation method of the heterojunction nanometer material of sulfur-indium-zinc and titanium dioxide - Google Patents
The preparation method of the heterojunction nanometer material of sulfur-indium-zinc and titanium dioxide Download PDFInfo
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Abstract
The invention discloses a kind of sulfur-indium-zinc and the preparation method of the heterojunction nanometer material of titanium dioxide, the present invention is by hydro-thermal method, in TiO2Growth in situ ZnIn in nano rod2S4Obtain the ZnIn with lattice buffer Rotating fields2S4/TiO2Heterogeneous graded transition junction nano composite material.Method is to prepare TiO with method of electrostatic spinning first2Nano rod, the then TiO by that will obtain2Nano rod is evenly spread in a certain amount of zinc acetate, indium trichloride and thioacetyl amine aqueous solution, then the mixed liquor is transferred in autoclave, (120~180 DEG C) are kept for the regular hour (6~24h) at a certain temperature, can controllable preparation ZnIn2S4The ZnIn of nanometer sheet load capacity2S4/TiO2Hetero-junctions nano composite material.ZnIn of the present invention2S4/TiO2Hetero-junctions nano composite material has inexpensive application prospect in Photocatalytic Activity for Degradation organic matter, photocatalytic water field.
Description
Technical field
The present invention relates to the preparation of functional nano-composites and photocatalysis technology field, in particular to a kind of sulfur-indium-zinc
With the preparation method of the heterojunction nanometer material of titanium dioxide.
Background technology
Energy and environment problem is the needs key subjects urgently to be resolved hurrily that human kind sustainable development is faced.Since day
This scientist Fujishima (Nature, 1972,238,37-38) utilizes ultraviolet light TiO2Since electrode photocatalytic water, light
Catalysis technique develops rapidly, and carry out the depollution of environment and energy conversion using sunshine has turned into the focus of current research.However,
Or most photochemical catalyst sun light utilization efficiency and low (such as TiO of photo-quantum efficiency2), or activity it is high but it is unstable (such as
Sulfide and some narrow band gap oxides).Therefore, new material preparation method is developed to obtain sun light utilization efficiency height, performance
Photochemical catalyst stable, that photocatalytic activity is good is the target that numerous scientific workers competitively chase.
Ternary metal sulfide ZnIn2S4Being one has good visible absorption performance and the adjustable narrow band gap of band gap
Semiconductor.The shortcomings that it has preferable visible light photocatalysis performance and overcomes conventional vulcanized thing easy photoetch, therefore be a kind of
There is the visible-light photocatalyst of development prospect very much.At present, to ZnIn2S4Research be concentrated mainly on Morphological control, crystalline phase is adjusted
Section, doping vario-property, exploitation new preparation process and other semiconductors couplings etc., to improve its photocatalysis performance.
It can both increase the sun using hetero-junctions can be compounded to form with narrow gap semiconductor with the wide band gap semiconducter matched
The absorption of light, separation and the transport efficiency of photo-generated carrier can be strengthened again.And ZnIn2S4With TiO2Can band matching, the two
It is compounded to form and is expected to effectively improve photocatalysis performance.It is low in view of heterojunction material Lattice Matching degree, it is difficult to stable close
Hetero-junctions is combined into, it is also contemplated that being advantageous to the collection of photogenerated charge with high length-diameter ratio structure and transporting and high-ratio surface
Product can improve photocatalysis efficiency.
The content of the invention
A kind of the defects of present invention is directed to prior art, there is provided the heterojunction nanometer material of sulfur-indium-zinc and titanium dioxide
Preparation method, this method prepares that cost is low, technique is simple, catalyst photocatalytic activity is strong, stability is high, it is larger to have
Application potential.
To achieve the above object, the system of the heterojunction nanometer material of a kind of sulfur-indium-zinc provided by the invention and titanium dioxide
Preparation Method, comprise the following steps:
1) by volume 1~5:2~10:0.5~3 weighs butyl titanate, absolute ethyl alcohol and acetic acid, then by metatitanic acid
Four butyl esters, absolute ethyl alcohol and acetic acid sealing are stirred, and obtain mixed solution;
2) vinyl pyrrolidone is added into mixed solution, sealing stirring, obtains electrostatic spinning predecessor;
3) electrostatic spinning predecessor is positioned in electrostatic spinning machine needle cylinder, electrostatic spinning is carried out, by electrostatic spinning forerunner
Thing is sent into out of electrostatic spinning machine needle cylinder in collection device (collection device is the stainless steel disc covered with aluminium foil), collection device
Obtain collecting product and annealed at 500~600 DEG C 1~3h, obtain TiO2Nano rod;
4) zinc acetate, indium trichloride and thioacetamide are well mixed, obtain mixed liquor;
5) from the standby TiO of step 3)2Nano rod weighs TiO2Nano rod, then it is added to the water progress ultrasound and uniformly divides
Dissipate, obtain suspension;
6) mixed liquor is added into suspension, further ultrasound uniformly, is put into autoclave, autoclave is put into air blast
Drying box, pyroreaction, room temperature is then naturally cooled to, to sediment filtering, cleaning, dry, finally give ZnIn2S4/
TiO2Hetero-junctions nano composite material.
Further, in the step 1), butyl titanate, absolute ethyl alcohol and acetic acid volume ratio are 3~5:6~10:
2.0~3.0.
Yet further, in the step 2), mixed solution is 3.5~18.0 with vinyl pyrrolidone volume ratio:
0.2~4.
Yet further, in the step 3), during electrostatic spinning, voltage is 13~16kV, rate of feed 1.0
~2.0mL/h.
Yet further, in the step 3), collection device is 10~30cm with electrostatic spinning machine needle cylinder distance.
Yet further, in the step 4), zinc acetate, indium trichloride and thioacetamide mol ratio are 1~2:2~
4:4~8.
Yet further, in the step 6), ZnIn2S4/TiO2ZnIn in hetero-junctions nano composite material2S4With
TiO2Mol ratio 2~110:100
Yet further, in the step 6), the temperature of pyroreaction is 120~180 DEG C, 6~24h of reaction time.
The beneficial effects of the present invention are:
The present invention's can be in TiO2Controllable effectively growth ZnIn in nano rod2S4Nanometer sheet and it is uniformly dispersed, obtains
The specific surface area of nano-complex is big, special lattice buffer Rotating fields are advantageous to photo-generated carrier and efficiently collected and separation, can
See under light irradiation and show high photocatalysis performance.
The ZnIn of the present invention2S4/TiO2The pattern of hetero-junctions nano composite material is in the TiO with high length-diameter ratio2Receive
The ZnIn of growth in situ is uniform-distribution with rice bar2S4Nanometer sheet, its specific surface area are 100~500m2/ g, transmitted in high-resolution
Visible ZnIn under electron microscope2S4、TiO2And the buffer layer lattice striped of the two intersection.
Brief description of the drawings
Fig. 1 is different ZnIn2S4And TiO2ZnIn obtained by under molar ratio2S4/TiO2The nano combined material of hetero-junctions
The XRD of material;
In figure, Fig. 1 a and b are respectively ZnIn2S4And TiO2XRD standard spectrums, Fig. 1 c~i are respectively ZnIn2S4And TiO2Rub
You are than being 2:100 (2%), 5:100 (5%), 10:100 (10%), 20:100 (20%), 40:100 (40%), 70:100
And 110 (70%):ZnIn obtained by under the conditions of 100 (110%)2S4/TiO2The XRD of hetero-junctions nano composite material.
Fig. 2 is different ZnIn2S4And TiO2ZnIn obtained by under molar ratio2S4/TiO2The nano combined material of hetero-junctions
The SEM pictures of material;
In figure, Fig. 2 a are pure ZnIn2S4SEM pictures, Fig. 2 a illustrations are pure TiO2The SEM pictures (lower left corner) of nano rod
With the pure ZnIn of amplification2S4SEM pictures (upper right corner), Fig. 2 b~h are respectively ZnIn2S4And TiO2Mol ratio is 2%, 5%,
ZnIn obtained by under the conditions of 10%, 20%, 40%, 70% and 110%2S4/TiO2The SEM figures of hetero-junctions nano composite material
Piece.
Fig. 3 is ZnIn2S4And TiO2Mol ratio is 20:ZnIn obtained by under the conditions of 1002S4/TiO2Hetero-junctions nanometer is answered
The TEM pictures of condensation material;
Fig. 3 a~c are ZnIn2S4And TiO2Mol ratio ZnIn resulting under the conditions of being 20%2S4/TiO2Hetero-junctions nanometer
The TEM pictures of the different amplification of material.
Fig. 4 is different ZnIn2S4And TiO2ZnIn obtained by under molar ratio2S4/TiO2The nano combined material of hetero-junctions
Expect photo-catalytic degradation of methyl-orange dyestuff efficiency chart under visible light.
Embodiment
In order to preferably explain the present invention, below in conjunction with the specific embodiment main contents that the present invention is furture elucidated, but
Present disclosure is not limited solely to following examples.
Embodiment 1:
A kind of preparation method of the heterojunction nanometer material 1 of sulfur-indium-zinc and titanium dioxide, comprises the following steps:
1) 5mL butyl titanates, 10mL absolute ethyl alcohols and 3mL acetic acid are weighed, then by butyl titanate, absolute ethyl alcohol
It is placed in acetic acid in glass container, vessel port sealing, solution is continuously stirred into 2h with magnetic stirring apparatus, obtains homogeneous mixing
Solution;
2) 1mL vinyl pyrrolidone is added into mixed solution, sealing stirring, obtains electrostatic spinning predecessor;
3) electrostatic spinning predecessor is positioned in electrostatic spinning machine needle cylinder, voltage be 15kV, rate of feed be
Electrostatic spinning is carried out under the conditions of 1.5mL/h, electrostatic spinning predecessor is sent into apart from electrostatic spinning out of electrostatic spinning machine needle cylinder
In machine needle cylinder 20cm collection device (collection device is the stainless steel disc covered with aluminium foil), collection device obtains collecting product
Anneal 1~3h at 550 DEG C, obtains TiO2Nano rod;
4) 1mmol zinc acetates, 2mmol indium trichlorides and 6mmol thioacetamides are well mixed, obtain the mixed of 20mL
Close liquid;
5) 0.18g TiO are weighed2Nano rod, then progress ultrasound is dispersed in addition 25mL deionized water, obtains
Suspension;
6) mixed liquor is added into suspension, further ultrasound uniformly, is transferred in 50mL autoclave, by autoclave
Air dry oven is put into, the temperature inside the box is set as 160 DEG C, retention time 12h, room temperature is then naturally cooled to, to sediment
Filtering, cleaning, dry, finally give ZnIn2S4/TiO2Hetero-junctions nano composite material 1, wherein, ZnIn2S4/TiO2It is heterogeneous
Tie ZnIn in nano composite material 12S4With TiO2Mol ratio 20:100.
The ZnIn2S4/TiO2Hetero-junctions nano composite material 1XRD figures are shown in Fig. 1 f, and micromorphology SEM is shown in Fig. 2 e,
Transmission electron microscope picture is shown in Fig. 3 a-c, and photocatalysis effect is shown in ZIS20 broken line in Fig. 4.
Embodiment 2
Keep step 1-3 in embodiment 1 constant, and without the step 4-5 in embodiment 1, will directly pass through Static Spinning
The TiO that silk method obtains2Nano rod characterize and photocatalysis test.Obtain TiO2XRD and Fig. 1 the bPDF No.2- of nano rod
387 standard spectrums match, and micromorphology SEM figures are shown in Fig. 2 a, and photocatalysis effect is Fig. 4 TiO2Nanofibers broken lines institute
Show.
Embodiment 3
The present embodiment prepares ZnIn2S4/TiO2The step of method of hetero-junctions nano composite material 2 is with embodiment 1 is basic
Identical, difference is:
TiO in step 52The amount of nano rod is 1.8g, so as to which ZnIn be prepared2S4/TiO2The nano combined material of hetero-junctions
Material 2, ZnIn2S4/TiO2ZnIn in hetero-junctions nano composite material 22S4With TiO2Mol ratio 2:100.
Its ZnIn2S4/TiO2The micromorphology SEM of hetero-junctions nano composite material 2 is Fig. 2 b, and photocatalysis effect is inside Fig. 4
Shown in ZIS2 broken lines.
Embodiment 4
The present embodiment prepares ZnIn2S4/TiO2The step of method of hetero-junctions nano composite material 3 is with embodiment 1 is basic
Identical, difference is:
TiO in step 52The amount of nano rod is 0.72g, so as to which ZnIn be prepared2S4/TiO2The nano combined material of hetero-junctions
Material 3, ZnIn2S4/TiO2ZnIn in hetero-junctions nano composite material 32S4With TiO2Mol ratio 5:100.
Its ZnIn2S4/TiO2The micromorphology SEM of hetero-junctions nano composite material 3 is Fig. 2 c, and photocatalysis effect is inside Fig. 4
Shown in ZIS5 broken lines.
Embodiment 5
The present embodiment prepares ZnIn2S4/TiO2The step of method of hetero-junctions nano composite material 4 is with embodiment 1 is basic
Identical, difference is:
TiO in step 52The amount of nano rod is 0.36g, so as to which ZnIn be prepared2S4/TiO2The nano combined material of hetero-junctions
Material 4, ZnIn2S4/TiO2ZnIn in hetero-junctions nano composite material 42S4With TiO2Mol ratio 10:100.
Its ZnIn2S4/TiO2The micromorphology SEM of hetero-junctions nano composite material 4 is Fig. 2 d, and photocatalysis effect is inside Fig. 4
Shown in ZIS10 broken lines.
Embodiment 6
The present embodiment prepares ZnIn2S4/TiO2The step of method of hetero-junctions nano composite material 5 is with embodiment 1 is basic
Identical, difference is:
TiO in step 52The amount of nano rod is 0.36g, so as to which ZnIn be prepared2S4/TiO2The nano combined material of hetero-junctions
Material 5, ZnIn2S4/TiO2ZnIn in hetero-junctions nano composite material 52S4With TiO2Mol ratio 40:100.
Its ZnIn2S4/TiO2The micromorphology SEM of hetero-junctions nano composite material 5 is Fig. 2 f, and photocatalysis effect is inside Fig. 4
Shown in ZIS40 broken lines.
Embodiment 7
The present embodiment prepares ZnIn2S4/TiO2The step of method of hetero-junctions nano composite material 6 is with embodiment 1 is basic
Identical, difference is:
TiO in step 52The amount of nano rod is 0.051g, so as to which ZnIn be prepared2S4/TiO2Hetero-junctions is nano combined
Material 6, ZnIn2S4/TiO2ZnIn in hetero-junctions nano composite material 62S4With TiO2Mol ratio 70:100.
Its ZnIn2S4/TiO2The micromorphology SEM of hetero-junctions nano composite material 6 is Fig. 2 g, and photocatalysis effect is inside Fig. 4
Shown in ZIS70 broken lines.
Embodiment 8
The present embodiment prepares ZnIn2S4/TiO2The step of method of hetero-junctions nano composite material 7 is with embodiment 1 is basic
Identical, difference is:
TiO in step 52The amount of nano rod is 0.033g, so as to which ZnIn be prepared2S4/TiO2Hetero-junctions is nano combined
Material 7, ZnIn2S4/TiO2ZnIn in hetero-junctions nano composite material 72S4With TiO2Mol ratio 110:100.
Its ZnIn2S4/TiO2The micromorphology SEM of hetero-junctions nano composite material 7 is Fig. 2 h, and photocatalysis effect is inside Fig. 4
Shown in ZIS110 broken lines.
Embodiment 9
The preparation method of the heterojunction nanometer material 8 of sulfur-indium-zinc and titanium dioxide, comprises the following steps:
1) 1mL butyl titanates, 10mL absolute ethyl alcohols and 0.5mL acetic acid are weighed, then by butyl titanate, anhydrous second
Alcohol and acetic acid are placed in glass container, vessel port sealing, solution are continuously stirred into 2h with magnetic stirring apparatus, obtain homogeneous mix
Close solution;
2) 1mL vinyl pyrrolidone is added into mixed solution, sealing stirring, obtains electrostatic spinning predecessor;
3) electrostatic spinning predecessor is positioned in electrostatic spinning machine needle cylinder, voltage be 15kV, rate of feed be
Electrostatic spinning is carried out under the conditions of 1.5mL/h, electrostatic spinning predecessor is sent into apart from electrostatic spinning out of electrostatic spinning machine needle cylinder
In machine needle cylinder 20cm collection device (collection device is the stainless steel disc covered with aluminium foil), collection device obtains collecting product
Anneal 1~3h at 600 DEG C, obtains TiO2Nano rod;
4) 1mmol zinc acetates, 4mmol indium trichlorides and 8mmol thioacetamides are well mixed, obtain the mixed of 20mL
Close liquid;
5) 0.18g TiO are weighed2Nano rod, then progress ultrasound is dispersed in addition 25mL deionized water, obtains
Suspension;
6) mixed liquor is added into suspension, further ultrasound uniformly, is transferred in 50mL autoclave, by autoclave
Air dry oven is put into, the temperature inside the box is set as 120 DEG C, retention time 24h, room temperature is then naturally cooled to, to sediment
Filtering, cleaning, dry, finally give ZnIn2S4/TiO2Hetero-junctions nano composite material 8, wherein, ZnIn2S4/TiO2It is heterogeneous
Tie ZnIn in nano composite material 82S4With TiO2Mol ratio 20:100.
Embodiment 10
The preparation method of the heterojunction nanometer material 9 of sulfur-indium-zinc and titanium dioxide, comprises the following steps:
1) 3mL butyl titanates, 8mL absolute ethyl alcohols and 2mL acetic acid are weighed, then by butyl titanate, absolute ethyl alcohol and
Acetic acid is placed in glass container, vessel port sealing, solution is continuously stirred into 2h with magnetic stirring apparatus, it is molten to obtain homogeneous mixing
Liquid;
2) 1mL vinyl pyrrolidone is added into mixed solution, sealing stirring, obtains electrostatic spinning predecessor;
3) electrostatic spinning predecessor is positioned in electrostatic spinning machine needle cylinder, voltage be 15kV, rate of feed be
Electrostatic spinning is carried out under the conditions of 1.5mL/h, electrostatic spinning predecessor is sent into apart from electrostatic spinning out of electrostatic spinning machine needle cylinder
In machine needle cylinder 20cm collection device (collection device is the stainless steel disc covered with aluminium foil), collection device obtains collecting product
Anneal 1~3h at 500 DEG C, obtains TiO2Nano rod;
4) 1mmol zinc acetates, 3mmol indium trichlorides and 6mmol thioacetamides are well mixed, obtain the mixed of 20mL
Close liquid;
5) 0.18g TiO are weighed2Nano rod, then progress ultrasound is dispersed in addition 25mL deionized water, obtains
Suspension;
6) mixed liquor is added into suspension, further ultrasound uniformly, is transferred in 50mL autoclave, by autoclave
Air dry oven is put into, the temperature inside the box is set as 120 DEG C, retention time 24h, room temperature is then naturally cooled to, to sediment
Filtering, cleaning, dry, finally give ZnIn2S4/TiO2Hetero-junctions nano composite material 9, wherein, ZnIn2S4/TiO2It is heterogeneous
Tie ZnIn in nano composite material 92S4With TiO2Mol ratio 20:100.
As shown in Figure 1:ZnIn is understood with standard diagram contrast2S4For hexagonal phase structure, TiO2To be anatase structured.
Find out TiO shown in Fig. 2 a2The average aspect ratio of nano rod is more than 5:1;From Fig. 2 as can be seen that with mol ratio
Increase ZnIn2S4Nanometer sheet is in TiO2Nano rod appendix is more and more, but is distributed very evenly on bar.
From visible ZnIn under Fig. 3 c high resolution transmission electron microscopy pieces2S4、 TiO2And the two intersection is slow
Layer lattice fringe is rushed, 0.35nm corresponds to TiO2(101) crystal face, 0.24nm corresponds to ZnIn2S4(112) crystal face.
Fig. 4 can be seen that the ZnIn being prepared when embodiment 12S4/TiO2In hetero-junctions nano composite material 1
ZnIn2S4And TiO2When mol ratio is 20%, photocatalysis effect is optimal.
ZnIn prepared by embodiment 1 and embodiment 9~102S4/TiO2Hetero-junctions nano composite material is compared,
ZnIn2S4/TiO2The photocatalysis effect of hetero-junctions nano composite material 1 is optimal.
Other unspecified parts are prior art.Although above-described embodiment is made that in detail to the present invention
Description, but it is only part of the embodiment of the present invention, rather than whole embodiments, people can also exist according to the present embodiment
Without other embodiment is obtained under the premise of creativeness, these embodiments belong to the scope of the present invention.
Claims (8)
- A kind of 1. preparation method of the heterojunction nanometer material of sulfur-indium-zinc and titanium dioxide, it is characterised in that:Comprise the following steps:1) by volume 1~5:2~10:0.5~3 weighs butyl titanate, absolute ethyl alcohol and acetic acid, then by the fourth of metatitanic acid four Ester, absolute ethyl alcohol and acetic acid sealing are stirred, and obtain mixed solution;2) vinyl pyrrolidone is added into mixed solution, sealing stirring, obtains electrostatic spinning predecessor;3) electrostatic spinning predecessor is positioned in electrostatic spinning machine needle cylinder, carry out electrostatic spinning, by electrostatic spinning predecessor from It is sent into collection device in electrostatic spinning machine needle cylinder, collection device obtains collecting product and annealed at 500~600 DEG C 1~3h, obtains To TiO2Nano rod, it is standby;4) zinc acetate, indium trichloride and thioacetamide are well mixed, obtain mixed liquor;5) from the standby TiO of step 3)2Nano rod weighs TiO2Nano rod, be then added to the water progress ultrasound it is dispersed, obtain Suspension;6) mixed liquor is added into suspension, further ultrasound uniformly, is put into autoclave, autoclave is put into forced air drying Case, pyroreaction, room temperature is then naturally cooled to, to sediment filtering, cleaning, dry, finally give ZnIn2S4/TiO2It is heterogeneous Tie nano composite material.
- 2. the preparation method of the heterojunction nanometer material of sulfur-indium-zinc and titanium dioxide according to claim 1, it is characterised in that: In the step 1), butyl titanate, absolute ethyl alcohol and acetic acid volume ratio are 3~5:6~10:2.0~3.0.
- 3. the preparation method of the heterojunction nanometer material of sulfur-indium-zinc and titanium dioxide according to claim 1, it is characterised in that: In the step 2), mixed solution is 3.5~18.0 with vinyl pyrrolidone volume ratio:0.2~4.
- 4. the preparation method of the heterojunction nanometer material of sulfur-indium-zinc and titanium dioxide according to claim 1, it is characterised in that: In the step 3), during electrostatic spinning, voltage is 13~16kV, rate of feed is 1.0~2.0mL/h.
- 5. the preparation method of the heterojunction nanometer material of sulfur-indium-zinc and titanium dioxide according to claim 1, it is characterised in that: In the step 3), collection device is 10~30cm with electrostatic spinning machine needle cylinder distance.
- 6. the preparation method of the heterojunction nanometer material of sulfur-indium-zinc and titanium dioxide according to claim 1, it is characterised in that: In the step 4), zinc acetate, indium trichloride and thioacetamide mol ratio are 1~2:2~4:4~8.
- 7. the preparation method of the heterojunction nanometer material of sulfur-indium-zinc and titanium dioxide according to claim 1, it is characterised in that: In the step 6), ZnIn2S4/TiO2ZnIn in hetero-junctions nano composite material2S4With TiO2Mol ratio 2~110:100.
- 8. the preparation method of the heterojunction nanometer material of sulfur-indium-zinc and titanium dioxide according to claim 1, it is characterised in that: In the step 6), the temperature of pyroreaction is 120~180 DEG C, 6~24h of reaction time.
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