CN111348627A - Supercritical CO of ZnTe nano-particles2Synthesis method - Google Patents
Supercritical CO of ZnTe nano-particles2Synthesis method Download PDFInfo
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- CN111348627A CN111348627A CN201811654977.XA CN201811654977A CN111348627A CN 111348627 A CN111348627 A CN 111348627A CN 201811654977 A CN201811654977 A CN 201811654977A CN 111348627 A CN111348627 A CN 111348627A
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention provides supercritical CO of ZnTe nano particles2The synthesis method is characterized by comprising the following steps: adding zinc salt, strong base, a tellurium-containing compound and a reducing agent into deionized water in sequence, and dissolving to obtain a solution; pumping the solution into a high-pressure reaction kettle of a supercritical device; pumping out air and pumping in CO2Stopping ventilation after 20-30 minutes, heating to 50-70 ℃, and continuously pressurizing to enable CO2Pumping into an autoclave, and stabilizing at constant temperature and constant pressure for 1.5-2 hours when the pressure reaches 120-150 bar; and filtering and washing the precipitate after pressure relief to obtain ZnTe nano particles. The method adopts common raw materials, has high yield and uniform particle size of the synthesized ZnTe nano particles, and can be applied to the fields of optical compound batteries, ultraviolet light-emitting diodes, sensors and the like.
Description
Technical Field
The invention belongs to the technical field of material chemistry, and relates to supercritical CO of ZnTe nano particles2A synthetic method.
Background
The zinc telluride crystal has good electro-optic effect under the action of near infrared (800 nm) ultrashort pulse, is a common optically rectified THz radiation source and detection material, and has application in green light emitting devices, solar cells, waveguides, modulators and other photoelectric devices. The nano zinc telluride material has both semiconductor characteristics and nano scale effect, and has unique optical and electrical characteristics. ZnTe nano-scale is usually synthesized in an inert atmosphere of organic phase. The invention adopts supercritical CO2And synthesizing ZnTe nano particles by the process.
Disclosure of Invention
The invention aims to provide supercritical CO of ZnTe nano particles2The synthesis method is characterized by comprising the following steps: sequentially mixing zinc salt, strong base, tellurium-containing compound and reducing agentAdding into deionized water, and dissolving to obtain a solution; pumping the solution into a high-pressure reaction kettle of a supercritical device; pumping out air and pumping in CO2Stopping ventilation after 20-30 minutes, heating to 50-70 ℃, and continuously pressurizing to enable CO2Pumping into an autoclave, and stabilizing at constant temperature and constant pressure for 1.5-2 hours when the pressure reaches 120-150 bar; and filtering and washing the precipitate after pressure relief to obtain ZnTe nano particles.
The zinc salt comprises one of zinc chloride, zinc sulfate and zinc acetate, the concentration of the zinc salt in the solution is 1 mmol/L-5 mmol/L, and the strong base is sodium hydroxide or potassium hydroxide, and the concentration of the strong base is 0.1-0.5 mol/L.
The tellurium-containing compound comprises one of tellurium dioxide, sodium tellurite and potassium tellurite, the added molar weight of the tellurium-containing compound is the same as that of the zinc salt, the reducing agent comprises one of sodium borohydride, potassium borohydride and hydrazine hydrate, and the molar concentration of the reducing agent is 10-20 times that of the zinc salt.
The washing is alternately washing by using deionized water and ethanol, filtering is carried out by adopting a centrifuge precipitation or suction filtration device after each washing, a filtered product is dispersed in the deionized water or the ethanol again, the filtering is repeated until the pH value of the filtrate is 7, and the final washing by using the ethanol is convenient for drying; the drying is carried out in a vacuum oven at 50-80 ℃, and the vacuum degree is less than 133 Pa.
The method adopts common raw materials, has high yield and uniform particle size of the synthesized ZnTe nano particles, and can be applied to the fields of optical compound batteries, ultraviolet light-emitting diodes, sensors and the like.
While the invention has been disclosed in the foregoing description with reference to specific embodiments thereof, the foregoing description is directed to only certain specific embodiments of the invention and many more specific features of the invention may be employed than as disclosed herein. Therefore, the scope of the present invention should not be limited to the disclosure of the embodiments, but should include all combinations of the contents embodied in different parts, and various substitutions and modifications without departing from the present invention, and are covered by the claims of the present invention.
Drawings
FIG. 1 is a transmission electron micrograph of ZnTe nanoparticles synthesized using the present invention (example 1).
Detailed Description
Example 1
Sequentially adding 1mmol/L zinc chloride, 0.1mol/L sodium hydroxide, 1mmol/L tellurium dioxide and 0.02mol/L hydrazine hydrate into deionized water, and dissolving to obtain a solution; pumping the solution into a high-pressure reaction kettle of a supercritical device; pumping out air and pumping in CO2Stopping ventilation after 20 minutes, heating to 50 ℃, and continuously pressurizing to obtain CO2Pumping into a high-pressure kettle, and stabilizing at constant temperature and constant pressure for 1.5 hours when the pressure reaches 120 bar; and (3) filtering and washing the precipitate after pressure relief to obtain ZnTe nano particles shown in figure 1.
Example 2
Sequentially adding 2mmol/L zinc sulfate, 0.3mol/L potassium hydroxide, 2mmol/L potassium tellurite and 0.03mol/L potassium borohydride into deionized water, and dissolving to obtain a solution; pumping the solution into a high-pressure reaction kettle of a supercritical device; pumping out air and pumping in CO2After 30 minutes, the ventilation is stopped, the temperature is raised to 60 ℃, and the pressurization is continued to lead CO2Pumping into a high-pressure kettle, and stabilizing at constant temperature and constant pressure for 2 hours when the pressure reaches 130 bar; and filtering and washing the precipitate after pressure relief to obtain ZnTe nano particles.
Example 3
Sequentially adding 5mmol/L zinc acetate, 0.5mol/L sodium hydroxide, 5mmol/L sodium tellurite and 0.05mol/L sodium borohydride into deionized water, and dissolving to obtain a solution; pumping the solution into a high-pressure reaction kettle of a supercritical device; pumping out air and pumping in CO2After 30 minutes, the ventilation is stopped, the temperature is raised to 70 ℃, and the CO is continuously pressurized2Pumping into a high-pressure kettle, and stabilizing at constant temperature and constant pressure for 1.5 hours when the pressure reaches 150 bar; and filtering and washing the precipitate after pressure relief to obtain ZnTe nano particles.
Claims (5)
1. Supercritical CO of ZnTe nano-particles2The synthesis method is characterized by comprising the following steps: adding zinc salt, strong base, a tellurium-containing compound and a reducing agent into deionized water in sequence, and dissolving to obtain a solution; pumping the solution into a high-pressure reaction kettle of a supercritical device; pumping out air and pumping in CO2Stopping ventilation after 20-30 minutes, heating to 50-70 ℃, and thenContinuously pressurizing to remove CO2Pumping into an autoclave, and stabilizing at constant temperature and constant pressure for 1.5-2 hours when the pressure reaches 120-150 bar; and filtering and washing the precipitate after pressure relief to obtain ZnTe nano particles.
2. Supercritical CO of ZnTe nanoparticles according to claim 12The synthesis method is characterized by comprising the following steps: the zinc salt comprises one of zinc chloride, zinc sulfate and zinc acetate, the concentration of the zinc salt in the solution is 1 mmol/L-5 mmol/L, and the strong base is sodium hydroxide or potassium hydroxide, and the concentration of the strong base is 0.1-0.5 mol/L.
3. Supercritical CO of ZnTe nanoparticles according to claim 12The synthesis method is characterized by comprising the following steps: the tellurium-containing compound comprises one of tellurium dioxide, sodium tellurite and potassium tellurite, the added molar weight of the tellurium-containing compound is the same as that of the zinc salt, the reducing agent comprises one of sodium borohydride, potassium borohydride and hydrazine hydrate, and the molar concentration of the reducing agent is 10-20 times that of the zinc salt.
4. Supercritical CO of ZnTe nanoparticles according to claim 12The synthesis method is characterized by comprising the following steps: the washing is alternately washing by using deionized water and ethanol, filtering is carried out by adopting a centrifuge precipitation or suction filtration device after each washing, a filtered product is dispersed in the deionized water or the ethanol again, the filtering is repeated until the pH value of the filtrate is 7, and the final washing by using the ethanol is convenient for drying; the drying is carried out in a vacuum oven at 50-80 ℃, and the vacuum degree is less than 133 Pa.
5. Supercritical CO of ZnTe nanoparticles as defined in any one of claims 1 to 42ZnTe nano-particles prepared by the synthetic method.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811654977.XA CN111348627A (en) | 2018-12-24 | 2018-12-24 | Supercritical CO of ZnTe nano-particles2Synthesis method |
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| CN201811654977.XA CN111348627A (en) | 2018-12-24 | 2018-12-24 | Supercritical CO of ZnTe nano-particles2Synthesis method |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7758843B1 (en) * | 2009-04-01 | 2010-07-20 | U.S. Department Of Energy | Inclusion free cadmium zinc tellurium and cadmium tellurium crystals and associated growth method |
| CN103000890A (en) * | 2012-12-13 | 2013-03-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of cathode material Li2Mn1-x-yCoxNiySiO4 for lithium ion battery |
| CN105460903A (en) * | 2015-09-22 | 2016-04-06 | 苏州星烁纳米科技有限公司 | Nanocrystal preparation method, nanocrystal, and preparation and preservation apparatus of gas solution |
| US9314777B2 (en) * | 2012-07-27 | 2016-04-19 | Lawrence Livermore National Security, Llc | High surface area graphene-supported metal chalcogenide assembly |
-
2018
- 2018-12-24 CN CN201811654977.XA patent/CN111348627A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7758843B1 (en) * | 2009-04-01 | 2010-07-20 | U.S. Department Of Energy | Inclusion free cadmium zinc tellurium and cadmium tellurium crystals and associated growth method |
| US9314777B2 (en) * | 2012-07-27 | 2016-04-19 | Lawrence Livermore National Security, Llc | High surface area graphene-supported metal chalcogenide assembly |
| CN103000890A (en) * | 2012-12-13 | 2013-03-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of cathode material Li2Mn1-x-yCoxNiySiO4 for lithium ion battery |
| CN105460903A (en) * | 2015-09-22 | 2016-04-06 | 苏州星烁纳米科技有限公司 | Nanocrystal preparation method, nanocrystal, and preparation and preservation apparatus of gas solution |
Non-Patent Citations (1)
| Title |
|---|
| JIQING JIAO 等: "Biomolecule-assisted synthesis of ZnS nanocorals and open-benzene ring in supercritical carbon dioxide", 《MATERIALS RESEARCH BULLETIN》 * |
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Application publication date: 20200630 |