CN104646658A - Method for preparing hybridized nanocrystallines - Google Patents
Method for preparing hybridized nanocrystallines Download PDFInfo
- Publication number
- CN104646658A CN104646658A CN201310580975.1A CN201310580975A CN104646658A CN 104646658 A CN104646658 A CN 104646658A CN 201310580975 A CN201310580975 A CN 201310580975A CN 104646658 A CN104646658 A CN 104646658A
- Authority
- CN
- China
- Prior art keywords
- diphenyl ether
- solution
- preparation
- aucl
- hybridized
- 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
Abstract
A method for preparing hybridized nanocrystallines comprises the steps: adding zinc dioleate and triphenylphosphine sulfide of the same amounts to diphenyl ether containing gold nanoparticles; heating to be boiled, standing and centrifugally separating to obtain the hybridized nanocrystallines; with adoption of the method provided by the invention, the ZnSe-Au hybridized nanocrystallines can prepared; the prepared hybridized nanocrystallines are small in particle size and easy in dispersion; and the preparation process is stable and controllable.
Description
Technical field
The invention belongs to chemical technology field, particularly a kind of preparation method of hybridized nanometer crystal.
Background technology
Hybridized nanometer crystal combines the performance of several nano material, is a kind of new nano material.There is the material of some the type at present, its research has been had great importance.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of preparation method of hybridized nanometer crystal, ZnSe-Au hybridized nanometer crystal can be prepared.
To achieve these goals, the technical solution used in the present invention is:
A preparation method for hybridized nanometer crystal, is added to the zinc oleate of equivalent and triphenyl selenizing phosphine and comprises in the diphenyl ether of gold nano grain, after being heated to boiling, and standing centrifugation and get final product.
The preparation process of described triphenyl selenizing phosphine is as follows: be dissolved in the tetrahydrofuran solution of 3-5mL by 1mmol triphenylphosphine, then add 10-15mmol selenium powder, filters out unnecessary selenium powder, be recrystallized and obtain triphenyl selenizing phosphine after stirring 1d.
The preparation process of described zinc oleate is as follows: joined by 1mmol oxide powder and zinc in 1-3mmol oleic acid, stirring reaction at 110-120 DEG C, namely obtains zinc oleate after reaction terminates.
The described preparation process comprising the diphenyl ether of gold nano grain is as follows: the four octyl group ammonium bromide diphenyl ether solution be aqueous solution of chloraurate and the 1mL concentration of 3-5mmol/L by 1mL concentration being 3-5mmol/L mix, AuCl
4-be extracted in diphenyl ether; AuCl is comprised to isolated
4-diphenyl ether solution in add dialkyl group mercaptan, until comprise AuCl
4-diphenyl ether solution become white, add NaBH
4the aqueous solution, until diphenyl ether solution becomes purple, solution is separated the removal aqueous solution again, obtains and comprises the diphenyl ether solution of Au nano particle.
Method of the present invention can prepare ZnSe-Au hybridized nanometer crystal, and the product granularity prepared is little, easily disperses, and preparation process is stablized controlled.
Detailed description of the invention
Embodiments of the present invention are described in detail below in conjunction with embodiment.
Embodiment one
A preparation method for hybridized nanometer crystal, comprises the steps:
Step 1, is dissolved in 1mmol triphenylphosphine in the tetrahydrofuran solution of 3mL, then adds 15mmol selenium powder, filters out unnecessary selenium powder after stirring 1d, the obtained triphenyl selenizing phosphine of recrystallization.
Step 2, joins 1mmol oxide powder and zinc in 3mmol oleic acid, stirring reaction at 120 DEG C, and reaction terminates rear obtained zinc oleate.
The four octyl group ammonium bromide diphenyl ether solution that 1mL concentration is aqueous solution of chloraurate and the 1mL concentration of 5mmol/L by step 3 is 5mmol/L mix, AuCl
4-be extracted in diphenyl ether; AuCl is comprised to isolated
4-diphenyl ether solution in add dialkyl group mercaptan, until comprise AuCl
4-diphenyl ether solution become white, add NaBH
4the aqueous solution, until diphenyl ether solution becomes purple, solution is separated the removal aqueous solution again, obtains and comprises the diphenyl ether solution of Au nano particle.
Step 4, is added to the zinc oleate of equivalent and triphenyl selenizing phosphine and comprises in the diphenyl ether of gold nano grain, after being heated to boiling, and standing centrifugation and get final product.
Embodiment two
A preparation method for hybridized nanometer crystal, comprises the steps:
Step 1, is dissolved in 1mmol triphenylphosphine in the tetrahydrofuran solution of 5mL, then adds 10mmol selenium powder, filters out unnecessary selenium powder after stirring 1d, the obtained triphenyl selenizing phosphine of recrystallization.
Step 2, joins 1mmol oxide powder and zinc in 1mmol oleic acid, stirring reaction at 110 DEG C, and reaction terminates rear obtained zinc oleate.
The four octyl group ammonium bromide diphenyl ether solution that 1mL concentration is aqueous solution of chloraurate and the 1mL concentration of 3mmol/L by step 3 is 3mmol/L mix, AuCl
4-be extracted in diphenyl ether; AuCl is comprised to isolated
4-diphenyl ether solution in add dialkyl group mercaptan, until comprise AuCl
4-diphenyl ether solution become white, add NaBH
4the aqueous solution, until diphenyl ether solution becomes purple, solution is separated the removal aqueous solution again, obtains and comprises the diphenyl ether solution of Au nano particle.
Step 4, is added to the zinc oleate of equivalent and triphenyl selenizing phosphine and comprises in the diphenyl ether of gold nano grain, after being heated to boiling, and standing centrifugation and get final product.
Embodiment three
A preparation method for hybridized nanometer crystal, comprises the steps:
Step 1, is dissolved in 1mmol triphenylphosphine in the tetrahydrofuran solution of 4mL, then adds 12mmol selenium powder, filters out unnecessary selenium powder after stirring 1d, the obtained triphenyl selenizing phosphine of recrystallization.
Step 2, joins 1mmol oxide powder and zinc in 2mmol oleic acid, stirring reaction at 112 DEG C, and reaction terminates rear obtained zinc oleate.
The four octyl group ammonium bromide diphenyl ether solution that 1mL concentration is aqueous solution of chloraurate and the 1mL concentration of 4mmol/L by step 3 is 4mmol/L mix, AuCl
4-be extracted in diphenyl ether; AuCl is comprised to isolated
4-diphenyl ether solution in add dialkyl group mercaptan, until comprise AuCl
4-diphenyl ether solution become white, add NaBH
4the aqueous solution, until diphenyl ether solution becomes purple, solution is separated the removal aqueous solution again, obtains and comprises the diphenyl ether solution of Au nano particle.
Step 4, is added to the zinc oleate of equivalent and triphenyl selenizing phosphine and comprises in the diphenyl ether of gold nano grain, after being heated to boiling, and standing centrifugation and get final product.
Claims (4)
1. a preparation method for hybridized nanometer crystal, is characterized in that, the zinc oleate of equivalent and triphenyl selenizing phosphine is added to and comprises in the diphenyl ether of gold nano grain, after being heated to boiling, and standing centrifugation and get final product.
2. the preparation method of hybridized nanometer crystal according to claim 1, it is characterized in that, the preparation process of described triphenyl selenizing phosphine is as follows: be dissolved in the tetrahydrofuran solution of 3-5mL by 1mmol triphenylphosphine, add 10-15mmol selenium powder again, filter out unnecessary selenium powder after stirring 1d, be recrystallized and obtain triphenyl selenizing phosphine.
3. the preparation method of hybridized nanometer crystal according to claim 1, is characterized in that, the preparation process of described zinc oleate is as follows: joined by 1mmol oxide powder and zinc in 1-3mmol oleic acid, stirring reaction at 110-120 DEG C, namely obtains zinc oleate after reaction terminates.
4. the preparation method of hybridized nanometer crystal according to claim 1, it is characterized in that, the described preparation process comprising the diphenyl ether of gold nano grain is as follows: the four octyl group ammonium bromide diphenyl ether solution be aqueous solution of chloraurate and the 1mL concentration of 3-5mmol/L by 1mL concentration being 3-5mmol/L mix, AuCl
4-be extracted in diphenyl ether; AuCl is comprised to isolated
4-diphenyl ether solution in add dialkyl group mercaptan, until comprise AuCl
4-diphenyl ether solution become white, add NaBH
4the aqueous solution, until diphenyl ether solution becomes purple, solution is separated the removal aqueous solution again, obtains and comprises the diphenyl ether solution of Au nano particle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310580975.1A CN104646658A (en) | 2013-11-16 | 2013-11-16 | Method for preparing hybridized nanocrystallines |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310580975.1A CN104646658A (en) | 2013-11-16 | 2013-11-16 | Method for preparing hybridized nanocrystallines |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104646658A true CN104646658A (en) | 2015-05-27 |
Family
ID=53238581
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310580975.1A Pending CN104646658A (en) | 2013-11-16 | 2013-11-16 | Method for preparing hybridized nanocrystallines |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104646658A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105642910A (en) * | 2016-01-25 | 2016-06-08 | 中国科学技术大学 | Au nanoparticle composite nanosheets and preparation method thereof |
| CN112710704A (en) * | 2020-12-04 | 2021-04-27 | 安徽大学 | Au nanoparticle loaded porous ZnO nanobelt and preparation method and application thereof |
-
2013
- 2013-11-16 CN CN201310580975.1A patent/CN104646658A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105642910A (en) * | 2016-01-25 | 2016-06-08 | 中国科学技术大学 | Au nanoparticle composite nanosheets and preparation method thereof |
| CN112710704A (en) * | 2020-12-04 | 2021-04-27 | 安徽大学 | Au nanoparticle loaded porous ZnO nanobelt and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104477900B (en) | A kind of microwave method prepares the method for multicolor fluorescence graphene quantum dot | |
| Maisang et al. | Enhanced photocatalytic performance of visible-light-driven BiOBr/BiPO4 composites | |
| CN105670633B (en) | A kind of method that micro passage reaction continuously prepares quantum dot | |
| CN102807209A (en) | Method for preparing graphene quantum dots | |
| TWI462990B (en) | Preparation of red fluorescent gold nanometer material | |
| CN108892130A (en) | The green synthesis method of graphene quantum dot is prepared using starch | |
| CN103531363B (en) | The preparation method of dye sensibilization solar cell nanometer TiO2 film light anode slurries | |
| CN103864137B (en) | Flower shape zinc oxide nano material and preparation method thereof | |
| CN102816567A (en) | Method for preparing high-yield carbon quantum dots | |
| CN105665737A (en) | Biosynthesis method of nano Ag | |
| CN103980893A (en) | One-step preparation method of multicolor fluorescent functionalized graphene quantum dots | |
| Sabet et al. | Synthesis and characterization of CuInSe2 nanocrystals via facile microwave approach and study of their behavior in solar cell | |
| CN105565379B (en) | Cu3SbS4The controllable method for preparing of nanocrystalline material | |
| CN104646658A (en) | Method for preparing hybridized nanocrystallines | |
| CN105905882B (en) | Derived from the high yield N doping fluorescent carbon nano dot synthetic method containing unsaturated double-bond chitosan | |
| CN102502610A (en) | Simple method for preparing a large amount of graphene | |
| CN105060346B (en) | The self-stabilization dispersion molybdenum trioxide nano preparation method with colloid in a kind of water | |
| CN104084089B (en) | The preparation method of rosin emulsifying agent | |
| CN104690293A (en) | Preparation method for silver nanowires of different length-diameter ratios | |
| CN106629664A (en) | Method for synthesizing carbon quantum dots from water chestnuts and application of carbon quantum dots | |
| CN102660258A (en) | Method for preparing water-soluble CdS quantum dot | |
| CN102373507A (en) | Method for hydrothermally synthesizing Bi2WO6 material under assistance of imidazole ionic liquids | |
| CN108213460B (en) | Microwave preparation method of monodisperse gold-silver alloy nanoparticles | |
| CN104587995A (en) | Method for preparing porous spherical titanium dioxide | |
| CN103934473B (en) | A kind of method utilizing waste agronomic crop to prepare water-soluble precious metal nano particle |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150527 |