CN109573962A - A kind of Bi2Se3The preparation method of@C composite - Google Patents
A kind of Bi2Se3The preparation method of@C composite Download PDFInfo
- Publication number
- CN109573962A CN109573962A CN201811564018.9A CN201811564018A CN109573962A CN 109573962 A CN109573962 A CN 109573962A CN 201811564018 A CN201811564018 A CN 201811564018A CN 109573962 A CN109573962 A CN 109573962A
- Authority
- CN
- China
- Prior art keywords
- composite
- preparation
- reaction
- bismuth
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of Bi2Se3The preparation method of@C composite, comprising the following steps: (1) bismuth nitrate and trimesic acid are dissolved in solvent, obtain mixed liquor；(2) mixed liquor is heated to reaction in reaction kettle, it is after the reaction was completed, reaction kettle is cooling, washing is centrifuged in reaction product, obtains bismuth metal-organic framework compound；(3) bismuth metal-organic framework compound is mixed with selenium powder, grinds to obtain powder；(4) under inert gas shielding, to powder selenization, Bi is obtained2Se3@C composite.The bismuth metal-organic framework compound that the present invention is formed with selenium powder processing bismuth nitrate and trimesic acid is conducive to the electric conductivity and active site quantity that improve composite material, and simple process is easy to operate, and reaction condition is mild, is suitable for industrialized production.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of Bi2Se3The preparation method of@C composite.
Background technique
Bismuth selenide (Bi2Se3) it is a kind of important semiconductor material, because it is with excellent light, heat, electricity, magnetic property,
There is high application value in the fields such as photocatalysis, sensor, metal-ion battery, thermo-electric device and photodetection.Currently,
Bi2Se3The preparation method of micro Nano material mainly have chemical vapour deposition technique, water (solvent) thermal method, wet chemistry method, magnetic sputtering method,
Electrochemical deposition, epitaxial growth and microwave method etc..But related Bi2Se3The report of/C composite is actually rare.
Chinese patent CN201810124872 discloses a kind of topological insulator heterojunction structure film Bi2Se3The preparation side of/C
Method, step mainly pass through control sputtering method and are initially formed carbon-based films, after treatment, then pass through magnetron sputtering on C film
Form one layer of Bi2Se3Film.Although this method easily forms heterojunction structure film, need using magnetron sputtering apparatus, production investment
Higher cost increases the financial burden of enterprise.
" Nano-Micro Letters " the 10th phase in 2018 discloses " a Bi2Se3/Cnanocomposite as a
new sodium-ion battery anodematerial".It with Bi, Se and graphite is that raw material is protected in argon gas reported in paper
Under shield, Bi is prepared by 48h ball milling2Se3/ C composite nano materials, and it is used as the negative electrode material of Na ion battery.Although should
The Bi of method preparation2Se3/ C composite nano materials show higher specific capacity and cyclical stability.But this method takes a long time,
Energy consumption is higher, increases production cost.
Summary of the invention
Invention broadly provides a kind of Bi2Se3The preparation method of@C composite, with selenium powder processing bismuth nitrate and
The bismuth metal-organic framework compound that benzenetricarboxylic acid is formed is conducive to the electric conductivity and active site quantity that improve composite material,
Simple process, easy to operate, mild condition are suitable for industrialized production.Its technical solution is as follows:
A kind of Bi2Se3The preparation method of@C composite, comprising the following steps:
(1) bismuth nitrate and trimesic acid are dissolved in solvent, obtains mixed liquor；
(2) mixed liquor is heated to reaction in reaction kettle, it is after the reaction was completed, reaction kettle is cooling, reaction product is carried out
Centrifuge separation washing, obtains bismuth metal-organic framework compound；
(3) bismuth metal-organic framework compound is mixed with selenium powder, grinds to obtain powder；
(4) under inert gas shielding, to powder selenization, Bi is obtained2Se3@C composite.
Preferably, solvent described in step (1) is the mixed solvent of n,N-Dimethylformamide and methanol.
Preferably, n,N-Dimethylformamide and the volume ratio of methanol are 1:(0.2-5).
Preferably, the molar ratio of bismuth nitrate and trimesic acid is 1:2 in step (1).
Preferably, the temperature heated in step (2) is 100-180 DEG C, reaction time 6-12h.
Preferably, washed product is distinguished using n,N-Dimethylformamide, methanol/ethanol in step (2), after the completion of washing
60-90 DEG C of vacuum drying.
Preferably, the mass ratio of bismuth metal-organic framework compound and selenium powder is 1.5: 1 in step (3).
Preferably, the condition of selenization is first in 280-320 DEG C of processing 2h, then again at 400-600 DEG C in step (4)
Handle 2h.
Using the above scheme, the invention has the following advantages that
Operation of the present invention is simple, and raw material resources are rich and easy to get, favorable repeatability.At high temperature, the activity of selenium is high, favorably
In obtaining high crystalline Bi2Se3Component.By pyrolysis organic ligand while selenizing, by nano-sized carbon and Bi2Se3Organically combine
Together, be conducive to the electric conductivity and stability for increasing active site, improving material, to further increase the property of composite material
Can, Bi2Se3@C composite has broad application prospects in fields such as photocatalysis, lithium ion battery and sodium-ion batteries.
Detailed description of the invention
Fig. 1 is the Bi prepared in embodiment 12Se3The XRD diagram of@C composite.
Specific embodiment
Experimental method in following embodiment is conventional method unless otherwise required, related experiment reagent and material
Material is conventional chemical reagent and material unless otherwise required.
Embodiment 1
The present embodiment Bi2Se3The preparation step of@C composite is as follows:
(1) 2mmol bismuth nitrate, 4mmol trimesic acid are weighed, and is dissolved in 10.0mL N, N- dimethyl formyl
The in the mixed solvent that amine and 20.0mL methanol are formed；
(2) by reaction mixture obtained by step (1) be transferred to polytetrafluoroethyllining lining, be sealed in stainless steel cauldron carry out it is molten
Agent thermal response, reaction temperature are 120 DEG C, reaction time 12h, after reaction, cooled to room temperature, centrifuge separation, and
Precipitating is successively washed with n,N-Dimethylformamide and methanol, is deposited in 60 DEG C of vacuum drying, obtaining white powder is bismuth metal-
Organic frame compound；
(3) 1.5g bismuth metal-organic framework compound is mixed with 1.0g selenium powder, is finely ground, be then charged into porcelain boat, be put into pipe
In formula furnace, under protection of argon gas, with the heating rate of 2 DEG C/min, 300 DEG C are first warming up to, and keep the temperature 2h；Then again with 5 DEG C/
The heating rate of min is warming up to 600 DEG C, and keeps the temperature 2h, and Bi can be obtained after reaction2Se3@C composite.
Bi2Se3The XRD of@C composite is as shown in Figure 1.
Embodiment 2
The present embodiment Bi2Se3The preparation step of@C composite is as follows:
(1) 2mmol bismuth nitrate, 4mmol trimesic acid are weighed, and is dissolved in 15.0mL N, N- dimethyl formyl
The in the mixed solvent that amine and 15.0mL methanol are formed；
(2) by reaction mixture obtained by step (1) be transferred to polytetrafluoroethyllining lining, be sealed in stainless steel cauldron carry out it is molten
Agent thermal response, reaction temperature are 140 DEG C, reaction time 8h, and after reaction, cooled to room temperature, centrifuge separation is used in combination
N,N-Dimethylformamide and methanol washing precipitating, are deposited in 60 DEG C of vacuum drying, obtaining white powder is that bismuth metal-has machine frame
Frame compound；
(3) 1.5g bismuth metal-organic framework compound is mixed with 1.0g selenium powder, is finely ground, be then charged into quartz boat, be put into
In tube furnace, under nitrogen protection, with the heating rate of 2 DEG C/min, be first warming up to 300 DEG C, and keep the temperature 2h, then again with 5 DEG C/
The heating rate of min is warming up to 500 DEG C, and keeps the temperature 2h, and Bi can be obtained after reaction2Se3@C composite.
Embodiment 3
In the present embodiment, as follows with the difference of embodiment 1:
Solvent thermal reaction temperature is 140 DEG C in step (2), reaction time 12h；
In step (3) under protection of argon gas, with the heating rate of 5 DEG C/min, 300 DEG C are first raised to, and keep the temperature 2h, then again
With the heating rate of 5 DEG C/min, 400 DEG C are raised to, and keeps the temperature 2h.
Embodiment 4
In the present embodiment, as follows with the difference of embodiment 1:
In step (3) under nitrogen protection, with the heating rate of 2 DEG C/min, 300 DEG C are first raised to, and keep the temperature 2h, then again
With the heating rate of 5 DEG C/min, 500 DEG C are raised to, and keeps the temperature 2h.
Embodiment 5
In the present embodiment, as follows with the difference of embodiment 2:
20.0mL N,N-dimethylformamide is used in step (1) and 10.0mL ethyl alcohol is mixed solvent.
Embodiment 6
In the present embodiment, as follows with the difference of embodiment 2:
Step (1) uses 25.0mL N,N-dimethylformamide and 5.0mL methanol；Under protection of argon gas, with 2 DEG C/min
Heating rate, be first raised to 300 DEG C, and keep the temperature 2h, be then raised to 600 DEG C again with the heating rate of 5 DEG C/min, and keep the temperature 2h.
Embodiment 7
In the present embodiment, as follows with the difference of embodiment 1:
Step (1) uses 5.0mL N,N-dimethylformamide and 25.0mL ethyl alcohol.
Embodiment 8
In the present embodiment, as follows with the difference of embodiment 2:
Solvent thermal reaction temperature is 160 DEG C in step (2), reaction time 6h.
It will be apparent to those skilled in the art that can make various other according to the above description of the technical scheme and ideas
Corresponding change and deformation, and all these changes and deformation all should belong to the protection scope of the claims in the present invention
Within.
Claims (8)
1. a kind of Bi2Se3The preparation method of@C composite, it is characterised in that: the following steps are included:
(1) bismuth nitrate and trimesic acid are dissolved in solvent, obtains mixed liquor；
(2) mixed liquor is heated to reaction in reaction kettle, it is after the reaction was completed, reaction kettle is cooling, reaction product is centrifuged
Separating, washing obtains bismuth metal-organic framework compound；
(3) bismuth metal-organic framework compound is mixed with selenium powder, grinds to obtain powder；
(4) under inert gas shielding, to powder selenization, Bi is obtained2Se3@C composite.
2. Bi according to claim 12Se3The preparation method of@C composite, it is characterised in that: molten described in step (1)
Agent is the mixed solvent of N,N-dimethylformamide and methanol.
3. Bi according to claim 22Se3The preparation method of@C composite, it is characterised in that: N, N- dimethyl formyl
The volume ratio of amine and methanol is 1:(0.2-5).
4. Bi according to claim 12Se3The preparation method of@C composite, it is characterised in that: bismuth nitrate in step (1)
Molar ratio with trimesic acid is 1:2.
5. Bi according to claim 12Se3The preparation method of@C composite, it is characterised in that: heated in step (2)
Temperature is 100-180 DEG C, reaction time 6-12h.
6. Bi according to claim 12Se3The preparation method of@C composite, it is characterised in that: N is used in step (2),
Dinethylformamide, methanol/ethanol distinguish washed product, 60-90 DEG C of vacuum drying after the completion of washing.
7. Bi according to claim 12Se3The preparation method of@C composite, it is characterised in that: bismuth gold in step (3)
The mass ratio of category-organic frame compound and selenium powder is 1.5:1.
8. Bi according to claim 12Se3The preparation method of@C composite, it is characterised in that: in step (4) at selenizing
The condition of reason is first in 280-320 DEG C of processing 2h, then again in 400-600 DEG C of processing 2h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811564018.9A CN109573962A (en) | 2018-12-20 | 2018-12-20 | A kind of Bi2Se3The preparation method of@C composite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811564018.9A CN109573962A (en) | 2018-12-20 | 2018-12-20 | A kind of Bi2Se3The preparation method of@C composite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109573962A true CN109573962A (en) | 2019-04-05 |
Family
ID=65930227
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811564018.9A Pending CN109573962A (en) | 2018-12-20 | 2018-12-20 | A kind of Bi2Se3The preparation method of@C composite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109573962A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111420668A (en) * | 2020-04-08 | 2020-07-17 | 西安交通大学 | In-situ synthesis of α -Bi2O3/CuBi2O4Preparation method and application of heterojunction photocatalytic material |
| CN114759188A (en) * | 2022-06-16 | 2022-07-15 | 暨南大学 | Potassium ion battery negative electrode material and preparation method and application thereof |
| CN116598489A (en) * | 2023-07-17 | 2023-08-15 | 帕瓦(长沙)新能源科技有限公司 | Negative electrode material of sodium ion battery and preparation method and application thereof |
-
2018
- 2018-12-20 CN CN201811564018.9A patent/CN109573962A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| GUANZHI WANG ET AL.: "A novel metal–organic framework based on bismuth and trimesic acid: synthesis,structure and properties", 《DALTON TRANSACTIONS》 * |
| 顾翼东: "《化学词典》", 30 September 1989, 上海辞书出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111420668A (en) * | 2020-04-08 | 2020-07-17 | 西安交通大学 | In-situ synthesis of α -Bi2O3/CuBi2O4Preparation method and application of heterojunction photocatalytic material |
| CN114759188A (en) * | 2022-06-16 | 2022-07-15 | 暨南大学 | Potassium ion battery negative electrode material and preparation method and application thereof |
| CN114759188B (en) * | 2022-06-16 | 2022-09-06 | 暨南大学 | Potassium ion battery negative electrode material and preparation method and application thereof |
| CN116598489A (en) * | 2023-07-17 | 2023-08-15 | 帕瓦(长沙)新能源科技有限公司 | Negative electrode material of sodium ion battery and preparation method and application thereof |
| CN116598489B (en) * | 2023-07-17 | 2023-10-24 | 帕瓦(长沙)新能源科技有限公司 | Negative electrode material of sodium ion battery and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109573962A (en) | A kind of Bi2Se3The preparation method of@C composite | |
| WO2022032743A1 (en) | Cote2/mxene composite material and preparation method therefor | |
| CN109888206B (en) | Lithium ion battery cathode material Bi/Bi2O3C, preparation and application thereof | |
| CN109326784B (en) | Phosphorus doped MoS2Preparation method and application of loaded graphene nanosheet | |
| CN105140471B (en) | A kind of MoS2/ C composite cathode material of lithium ion battery and preparation method thereof | |
| CN108658119B (en) | Method for preparing copper sulfide nanosheet and compound thereof by low-temperature vulcanization technology and application | |
| CN105226187A (en) | Film crystal silicon perovskite heterojunction solar cell and preparation method thereof | |
| CN109301204B (en) | Preparation method of hollow sphere structure tin sulfide/tin oxide lithium ion battery anode material | |
| CN107739053B (en) | A kind of three-phase system molybdenum oxide MoO3/Mo4O11/MoO2Nano-electrode material and preparation method thereof | |
| CN110790262B (en) | Preparation method for preparing nitrogen-sulfur double-doped graphene negative electrode material by low-temperature molten salt method | |
| CN110246917A (en) | A kind of inorganic perovskite solar battery and preparation method | |
| CN107475694B (en) | A kind of method and its application preparing two tungsten selenide semiconductive thin films on FTO substrate | |
| CN104310421A (en) | Preparation method of high-purity lithium tetrafluoroborate | |
| CN113173936B (en) | Non-doped hole transport material based on condensed ring electron-withdrawing parent nucleus and synthesis method and application thereof | |
| CN108047246A (en) | Saddle-shaped hole transport material, synthesis method thereof and perovskite solar cell | |
| CN109962229A (en) | A kind of two cobaltous selenides of molybdenum doping sheet/graphene combination electrode material preparation method | |
| CN112490438A (en) | Magnesium ion battery positive electrode material Mo-VS4N-GNTs and uses thereof | |
| CN108249428B (en) | Method for preparing single-layer graphene based on electrolyte solvent hot-insertion lithium stripping | |
| CN106115785B (en) | A kind of pure phase MoO2Anode material of lithium-ion battery and preparation method thereof | |
| WO2022032747A1 (en) | Method for preparing sulfur-doped rese2/mxene composite material | |
| CN105489885B (en) | A kind of rodlike cobaltosic oxide of multi-pore micron and the preparation method and application thereof | |
| CN108400298A (en) | A kind of method and its application preparing the graphene-supported antimony nanotube negative material of sodium-ion battery | |
| CN109438415A (en) | A kind of non-condensed electron acceptor material, preparation method and its organic solar batteries constructed | |
| CN109187671B (en) | Preparation method of selenium and sulfur doped graphene quantum dot modified metalloporphyrin nanotube photosensitive sensing material | |
| CN102315288A (en) | Thin film solar cell and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190405 |
|
| RJ01 | Rejection of invention patent application after publication |