CN109046384A - A kind of three-dimensional globular In2S3-SnS2The preparation method of compound - Google Patents
A kind of three-dimensional globular In2S3-SnS2The preparation method of compound Download PDFInfo
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- CN109046384A CN109046384A CN201810784914.XA CN201810784914A CN109046384A CN 109046384 A CN109046384 A CN 109046384A CN 201810784914 A CN201810784914 A CN 201810784914A CN 109046384 A CN109046384 A CN 109046384A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
Abstract
The present invention relates to a kind of three-dimensional globular In2S3‑SnS2The preparation method of compound.Indium nitrate, l- isoleucine, sodium borohydride and water are mixed into precursor liquid by the method for the present invention, are placed in hydrothermal reaction kettle and are carried out hydro-thermal reaction, and three-dimensional globular In is obtained2S3；By three-dimensional globular In2S3, SnCl4, thiocarbamide, ethylenediamine and water is mixed into precursor liquid, is placed in hydrothermal reaction kettle and carries out secondary hydro-thermal reaction and obtain three-dimensional globular In2S3‑SnS2Compound.The method of the present invention simple process, easily controllable, high production efficiency.
Description
Technical field
The present invention relates to a kind of three-dimensional globular In2S3-SnS2The preparation method of compound.
Background technique
In2S3It is a kind of novel optoelectronic materials, three-dimensional globular In can be obtained by hydrothermal synthesis by having been reported2S3.It is this
In2S3With large specific surface area, certain photoelectric conversion and catalytic performance, this three-dimensional globular structure or one kind are shown
Highly desirable complex carrier can be easier other compound nano particles because its surface has many tens nanometers of ducts
Material, compound often have better photoelectric conversion and catalytic performance.SnS2It is a kind of flake nano material, does not have been reported that
It can obtain three-dimensional globular In2S3-SnS2Compound, it is found by the applicant that being primarily due to SnS2Nanometer sheet side length is in 50-100nm, hardly possible
To enter In2S3Duct, so wanting to obtain SnS2With In2S3Compound, it is necessary to obtain the lesser SnS of size2Nanometer sheet.Three
Tie up spherical In2S3-SnS2Photoelectric conversion performance and photocatalysis performance can be improved in compound, can be used in photochemical catalyst, solar energy
The fields such as battery.However, SnS2Synthesis condition and three-dimensional globular In2S3Difference is larger, both compatible nano materials obtain compound
There are certain difficulties for object, so the present invention provides a kind of methods of mature and reliable to prepare three-dimensional globular In2S3-SnS2It is compound
Object.
Summary of the invention
It is an object of the present invention to overcome the deficiencies of the prior art and provide a kind of three-dimensional globular In2S3-SnS2It is compound
The preparation method of object.
Provided technical solution is the present invention to solve above-mentioned technical problem:
First prepare three-dimensional globular In2S3, then to three-dimensional globular In2S3Middle addition SnCl4, thiocarbamide, ethylenediamine and water, hydro-thermal it is anti-
Three-dimensional globular In should can be obtained2S3-SnS2Compound, nano-sheet SnS2It is evenly distributed on three-dimensional globular In2S3In gap；
Specifically comprise the following steps:
Step (1) is by indium nitrate, l- isoleucine, sodium borohydride and water according to mass ratio 1:(2~4): (1~2): 60
Mixing, is placed in hydrothermal reaction kettle and carries out hydro-thermal reaction, and hydrothermal temperature is 160~200 DEG C, and constant temperature time is 8~12 small
When；
Solidliquid mixture after hydro-thermal reaction is carried out solid-liquid centrifugation separation by step (2), liquid product is poured out, by solid-state
Product takes out, and dries 5~8 hours at 70~80 DEG C after being washed with deionized 3 times；
Product grind into powder after step (3) will be dried, obtains three-dimensional globular In2S3；
Step (4) is by above-mentioned three-dimensional globular In2S3、SnCl4, thiocarbamide, ethylenediamine and water is according to mass ratio 10:(1~3):
(2~4): (1~3): 50 are mixed into precursor liquid, are placed in hydrothermal reaction kettle and carry out hydro-thermal reaction, hydrothermal temperature be 160~
200 DEG C, constant temperature time is 20~30 hours；
Solidliquid mixture after hydro-thermal reaction is carried out solid-liquid centrifugation separation by step (5), liquid product is poured out, by solid-state
Product takes out, and dries 8~10 hours at 80~90 DEG C after being washed with deionized 3 times；
Product grind into powder after step (6) will be dried, obtains three-dimensional globular In2S3-SnS2Compound.
The beneficial effects of the present invention are: l- isoleucine, sodium borohydride prepares three-dimensional globular In using indium nitrate2S3,
Its three-dimensional chondritic is easy to and nano-sheet SnS2It carries out compound；Using SnCl4, thiocarbamide, ethylenediamine receives as precursor preparation
Rice sheet SnS2；Thiocarbamide, ethylenediamine will not be to three-dimensional globular In2S3Structure is destroyed, while can reduce SnS2Size, can
To guarantee nano-sheet SnS2It is evenly distributed on three-dimensional globular In2S3In gap, guarantee composite effect.
Detailed description of the invention
Fig. 1 is three-dimensional globular In prepared by embodiment 12S3-SnS2The scanning electron microscope (SEM) photograph (SEM) of compound；
Fig. 2 is three-dimensional globular In prepared by embodiment 22S3-SnS2The X ray diffracting spectrum (XRD) of compound；
Fig. 3 is three-dimensional globular In prepared by embodiment 32S3-SnS2The transmission electron microscope picture (TEM) of compound.
Specific embodiment
The present invention is further described with reference to the accompanying drawings and examples, but is not therefore limited the present invention to described
Within scope of embodiments.
Embodiment 1:
10g indium nitrate, 20gl- isoleucine, 10g sodium borohydride and 600g water are mixed according to mass ratio 1:2:1:60,
It is placed in hydrothermal reaction kettle and carries out hydro-thermal reaction, hydrothermal temperature is 160 DEG C, and constant temperature time is 8 hours；After hydro-thermal reaction
Solidliquid mixture carry out solid-liquid centrifugation separation, pour out liquid product, solid product taken out, after being washed with deionized 3 times
It is dried 5 hours at 70 DEG C；Product grind into powder after drying, obtains three-dimensional globular In2S3；By 100g three-dimensional globular
In2S3, 10gSnCl4, 20g thiocarbamide, 10g ethylenediamine and 500g water are mixed into precursor liquid according to mass ratio 10:1:2:1:50, are placed in
Hydro-thermal reaction is carried out in hydrothermal reaction kettle, hydrothermal temperature is 160 DEG C, and constant temperature time is 20 hours；After hydro-thermal reaction
Solidliquid mixture carry out solid-liquid centrifugation separation, pour out liquid product, solid product taken out, after being washed with deionized 3 times
It is dried 8 hours at 80 DEG C；Product grind into powder after drying, obtains three-dimensional globular In2S3-SnS2Compound.
Fig. 1 is three-dimensional globular In prepared by embodiment 12S3-SnS2The scanning electron microscope (SEM) photograph (SEM) of compound；It can therefrom see
Out, three-dimensional globular In prepared by embodiment 12S3-SnS2Compound has three-dimensional globular structure, nano-sheet SnS2It is uniformly distributed
In three-dimensional globular In2S3In gap.X ray diffracting spectrum (XRD) shows three-dimensional globular In2S3-SnS2Contain In in compound2S3
And SnS2Structure, well-crystallized.
Embodiment 2:
10g indium nitrate, 30gl- isoleucine, 10g sodium borohydride and 600g water are mixed according to mass ratio 1:3:1:60,
It is placed in hydrothermal reaction kettle and carries out hydro-thermal reaction, hydrothermal temperature is 180 DEG C, and constant temperature time is 10 hours；By hydro-thermal reaction
Solidliquid mixture afterwards carries out solid-liquid centrifugation separation, pours out liquid product, solid product is taken out, be washed with deionized 3 times
It is dried 6 hours at 80 DEG C afterwards；Product grind into powder after drying, obtains three-dimensional globular In2S3；By 100g three-dimensional globular
In2S3, 20gSnCl4, 30g thiocarbamide, 20g ethylenediamine and 500g water are mixed into precursor liquid according to mass ratio 10:2:3:2:50, are placed in
Hydro-thermal reaction is carried out in hydrothermal reaction kettle, hydrothermal temperature is 180 DEG C, and constant temperature time is 24 hours；After hydro-thermal reaction
Solidliquid mixture carry out solid-liquid centrifugation separation, pour out liquid product, solid product taken out, after being washed with deionized 3 times
It is dried 9 hours at 90 DEG C；Product grind into powder after drying, obtains three-dimensional globular In2S3-SnS2Compound.
Fig. 2 is three-dimensional globular In prepared by embodiment 22S3-SnS2The X ray diffracting spectrum (XRD) of compound；Therefrom may be used
To find out, the three-dimensional globular In of the preparation of embodiment 22S3-SnS2Contain In in compound2S3And SnS2Structure, well-crystallized.Scanning
Electron microscope (SEM) shows three-dimensional globular In2S3-SnS2Compound has three-dimensional globular structure, nano-sheet SnS2It is evenly distributed on
Three-dimensional globular In2S3In gap.
Embodiment 3:
10g indium nitrate, 40gl- isoleucine, 20g sodium borohydride and 600g water are mixed according to mass ratio 1:4:2:60,
It is placed in hydrothermal reaction kettle and carries out hydro-thermal reaction, hydrothermal temperature is 200 DEG C, and constant temperature time is 12 hours；By hydro-thermal reaction
Solidliquid mixture afterwards carries out solid-liquid centrifugation separation, pours out liquid product, solid product is taken out, be washed with deionized 3 times
It is dried 8 hours at 80 DEG C afterwards；Product grind into powder after drying, obtains three-dimensional globular In2S3；By 100g three-dimensional globular
In2S3, 30gSnCl4, 40g thiocarbamide, 30g ethylenediamine and 500g water are mixed into precursor liquid according to mass ratio 10:3:4:3:50, are placed in
Hydro-thermal reaction is carried out in hydrothermal reaction kettle, hydrothermal temperature is 200 DEG C, and constant temperature time is 30 hours；After hydro-thermal reaction
Solidliquid mixture carry out solid-liquid centrifugation separation, pour out liquid product, solid product taken out, after being washed with deionized 3 times
It is dried 10 hours at 90 DEG C；Product grind into powder after drying, obtains three-dimensional globular In2S3-SnS2Compound.
Fig. 3 is three-dimensional globular In prepared by embodiment 32S3-SnS2The transmission electron microscope picture (TEM) of compound；It can therefrom see
Out, nano-sheet SnS2With In2S3Sky is combined with each other.Scanning electron microscope (SEM) photograph (SEM) shows three-dimensional globular In2S3-SnS2Compound
With three-dimensional globular structure, nano-sheet SnS2It is evenly distributed on three-dimensional globular In2S3In gap.
Claims (2)
1. a kind of three-dimensional globular In2S3-SnS2The preparation method of compound, above-mentioned In2S3-SnS2Nano-sheet SnS in compound2
It is evenly distributed on three-dimensional globular In2S3In gap；It is characterized by comprising following steps:
Step (1) is by indium nitrate, l- isoleucine, sodium borohydride and water according to mass ratio 1:(2~4): (1~2): 60 mixing,
It is placed in hydrothermal reaction kettle and carries out hydro-thermal reaction, hydrothermal temperature is 160~200 DEG C, and constant temperature time is 8~12 hours；
Solidliquid mixture after hydro-thermal reaction is carried out solid-liquid centrifugation separation by step (2), liquid product is poured out, by solid product
It takes out, is dried 5~8 hours at 70~80 DEG C after being washed with deionized repeatedly；
Product grind into powder after step (3) will be dried, obtains three-dimensional globular In2S3；
Step (4) is by above-mentioned three-dimensional globular In2S3、SnCl4, thiocarbamide, ethylenediamine and water according to certain mass ratio be mixed into forerunner
Liquid is placed in hydrothermal reaction kettle and carries out hydro-thermal reaction, and hydrothermal temperature is 160~200 DEG C, and constant temperature time is 20~30 small
When；
Solidliquid mixture after hydro-thermal reaction is carried out solid-liquid centrifugation separation by step (5), liquid product is poured out, by solid product
It takes out, is dried 8~10 hours at 80~90 DEG C after being washed with deionized 3 times；
Product grind into powder after step (6) will be dried, obtains three-dimensional globular In2S3-SnS2Compound.
2. a kind of three-dimensional globular In as described in claim 12S3-SnS2The preparation method of compound, it is characterised in that step
(4) three-dimensional globular In2S3、SnCl4, thiocarbamide, ethylenediamine and water mass ratio be 10:(1~3): (2~4): (1~3): 50.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112899710A (en) * | 2021-01-28 | 2021-06-04 | 中国科学院青岛生物能源与过程研究所 | For electrocatalytic reduction of CO2Preparation method of catalyst for preparing formic acid |
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| CN106000424A (en) * | 2016-06-03 | 2016-10-12 | 牛和林 | Indium sulfide photocatalyst with ultrahigh photocatalytic activity and preparation method and application thereof |
| CN107029755A (en) * | 2017-04-16 | 2017-08-11 | 桂林理工大学 | A kind of heterojunction photocatalyst and preparation method thereof |
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| CN108273518A (en) * | 2018-01-17 | 2018-07-13 | 济南大学 | A kind of SnS2/Mn3O4The synthetic method and products obtained therefrom of flower-shaped composite construction |
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- 2018-07-17 CN CN201810784914.XA patent/CN109046384A/en active Pending
Patent Citations (4)
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| CN106000424A (en) * | 2016-06-03 | 2016-10-12 | 牛和林 | Indium sulfide photocatalyst with ultrahigh photocatalytic activity and preparation method and application thereof |
| CN107029755A (en) * | 2017-04-16 | 2017-08-11 | 桂林理工大学 | A kind of heterojunction photocatalyst and preparation method thereof |
| CN107537523A (en) * | 2017-09-22 | 2018-01-05 | 陕西科技大学 | A kind of method that hydro-thermal method prepares stannic disulfide/bismuth oxyiodide composite photo-catalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112899710A (en) * | 2021-01-28 | 2021-06-04 | 中国科学院青岛生物能源与过程研究所 | For electrocatalytic reduction of CO2Preparation method of catalyst for preparing formic acid |
| CN112899710B (en) * | 2021-01-28 | 2021-11-23 | 中国科学院青岛生物能源与过程研究所 | For electrocatalytic reduction of CO2Preparation method of catalyst for preparing formic acid |
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