CN102408101A - Preparation method of cadmium telluride quantum dot - Google Patents
Preparation method of cadmium telluride quantum dot Download PDFInfo
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- CN102408101A CN102408101A CN2010102892058A CN201010289205A CN102408101A CN 102408101 A CN102408101 A CN 102408101A CN 2010102892058 A CN2010102892058 A CN 2010102892058A CN 201010289205 A CN201010289205 A CN 201010289205A CN 102408101 A CN102408101 A CN 102408101A
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- tellurite
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Abstract
The invention provides a preparation method of a cadmium telluride quantum dot, and the method is suitable for the technical field of aqueous phase synthesis. The preparation method comprises the following steps: dissolving a source compound of cadmium, citrate and tellurite in water according to a predetermined sequence under a stirring condition; and adding sulfydryl ligand and alkali metal borohydride, stirring at the temperature of 10 DEG C to 30 DEG C and reacting for 1 minute to 10 minutes to obtain the cadmium telluride quantum dot, wherein the predetermined sequence is as follows: mixing one of the source compound of cadmium and tellurite with citric acid and then adding the other of the source compound of cadmium and tellurite into the mixture. The preparation method of the cadmium telluride quantum dot provided by the invention has the advantages of low cost, high synthetic efficiency, simplicity in operation and suitability for industrial production.
Description
Technical field
The invention belongs to the water synthesis technical field, relate in particular to a kind of preparation method of cadmium telluride quantum dot.
Background technology
Quantum dot is a kind of semiconductor nanocrystal or crystallite, is made up of II-VI, III-V or IV-VI period element, and diameter is at the spherical material of 1nm-100nm.What research was more at present is II-VI type quantum dots such as CdS, CdSe, CdTe, ZnS.These nanoparticles show the character different with macroscopic material, comprise high quantum emission productive rate, the size adjustable of emmission spectrum, narrow spectrum band etc.In addition, the controlling dimension size can be regulated the position of emmission spectrum.The unique character of quantum dot is based on it self quantum effect; When particle size reaches nanometer scale; Because the size confinement causes dimensional effect, quantum confined effect, macro quanta tunnel effect and surface effects; Have the normal sight system low dimension rerum natura different thereby derive nanometer system, show many electronics and optical characteristics that are different from macroscopic material, it is had broad application prospects at aspects such as photovoltaic material, luminescent material, photosensor, biomarkers with microsystem.
At present, the preparation of quantum dot mainly contains two kinds of approach, i.e. organic phase preparation and water preparation.The preparation quantum dot mainly adopts the organo-metallic method in organic phase; The organo-metallic method is the method that in high boiling organic solvent, prepares quantum dot through the presoma pyrolysis; Advantages such as the quantum dot of this method preparation has that kind is many, fluorescence quantum yield is high, excellent in optical properties, particle diameter are controlled; Therefore, become the main method of present preparation quantum dot.But it is that preparation condition is harsh that this method prepares the shortcoming of quantum dot, and reactions step is complicated, and processing safety is low, and reagent toxicity is strong, and experimental cost is high; For further application, need the quantum dot that the organic synthesis method makes be transferred to water, its complex steps, the quantum yield of the quantum dot aqueous solution that obtains after the processing and stability all reduce greatly.
In recent years, the direct quantum dot that in the aqueous solution, synthesizes excellent property became the research focus.The ultimate principle of aqueous phase synthesis method is in water, to add stablizer (like sulfhydryl compound etc.), obtains nanoparticle through the water ion exchange reaction.Water prepare quantum dot have the reaction conditions gentleness, simple to operate, toxicity is little, cost is low, favorable reproducibility, surface charge and surface properties is controlled easily, introduce advantages such as molecule of functional group easily; And, directly solved the water-soluble problem of nanoparticle because quantum dot is at the aqueous phase synthetic.But the prior art water all is with NaHTe or H when synthesizing cadmium telluride quantum dot (CdTe)
2Te is as the Te source, but these Te source presomas are unstable, needs synthetic in advance; Need oxygen free condition during reaction, and use Schlenk technology (technology that vacuum and rare gas element switch), this makes water synthesize the CdTe complicated operation, and equipment requirements is strict, is unfavorable for suitability for industrialized production, and the particle diameter of the CdTe of preparation is not easy control.These all become the difficult problem that the inhibition water prepares CdTe.
Summary of the invention
Based on above problem, the embodiment of the invention provides a kind of with low cost, cadmium telluride quantum dot preparation method that combined coefficient is high.
The present invention realizes like this; A kind of cadmium telluride quantum dot preparation method comprises the steps: under the agitation condition, and is according to predefined procedure that source compound, Citrate trianion and the tellurite of cadmium is soluble in water; Add the sulfydryl part; Add alkali metal borohydride again, stirring reaction is 1 minute-10 minutes under 10 ℃ of-30 ℃ of conditions, obtains cadmium telluride quantum dot; Said predefined procedure be meant with one in the source compound of cadmium and the tellurite with after Hydrocerol A mixes, add among both another again.
The cadmium telluride quantum dot preparation method of the embodiment of the invention; Through selecting tellurite stable in the air tellurium source for use as cadmium telluride quantum dot; Make that cadmium telluride quantum dot preparation method equipment requirements provided by the invention is low, with low cost, combined coefficient is high; Simple to operate, be applicable to suitability for industrialized production.
Description of drawings
Fig. 1 is the fluorescence emission spectrogram of the CdTe that provides of the embodiment of the invention;
Fig. 2 is the electron-microscope scanning figure of the CdTe that provides of the embodiment of the invention.
Embodiment
In order to make the object of the invention, technical scheme and advantage clearer,, the present invention is further elaborated below in conjunction with accompanying drawing and embodiment.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
The embodiment of the invention provides a kind of cadmium telluride quantum dot preparation method, comprises the steps: under the agitation condition, and is according to predefined procedure that source compound, Citrate trianion and the tellurite of cadmium is soluble in water; Add the sulfydryl part; Add alkali metal borohydride again, stirring reaction is 1 minute-10 minutes under 10 ℃ of-30 ℃ of conditions, obtains cadmium telluride quantum dot; Said predefined procedure be meant with one in the source compound of cadmium and the tellurite with after Hydrocerol A mixes, add among both another again.
Among the preparation method of the embodiment of the invention, source compound, Citrate trianion and the tellurite of cadmium is soluble in water, said predefined procedure be meant with one in the source compound of cadmium and the tellurite with after Hydrocerol A mixes, add among both another again.This predefined procedure is specific as follows: earlier the source compound of cadmium is put into reactor drum and mix with Citrate trianion, add tellurite again; Perhaps, earlier tellurite is put into reactor drum and mix, add the source compound of cadmium again with Citrate trianion; Perhaps, earlier Citrate trianion is put into reactor drum and mix the source compound that adds cadmium again with tellurite; Perhaps earlier Citrate trianion being put into reactor drum mixes with the source compound of cadmium and adds tellurite again.Add according to above-mentioned predefined procedure, make tellurite can not directly contact, thereby suppress to generate tellurous acid cadmium deposition with the source compound of cadmium.Add source compound or the tellurite that adds cadmium after the Citrate trianion, can directly add the source compound or the tellurite of solid-state cadmium, also can add the source compound of cadmium or the aqueous solution of tellurite.
Wherein, Citrate trianion is meant one or more in Tripotassium Citrate, Trisodium Citrate, hydration Trisodium Citrate or the hydration Tripotassium Citrate.Citrate trianion plays dissemination in embodiments of the present invention, and the source compound of avoiding cadmium directly contacts with tellurite and generates tellurous acid cadmium deposition.
The source compound of cadmium is meant, in the aqueous solution, can dissolve the compound that ionization goes out cadmium ion, for example one or more in Cadmium chloride fine powder, cadmium bromide, cadmium iodide, cadmium nitrate, cadmium chlorate, cadmium acetate, cadmium perchlorate, Cadmium Sulphate or the cadmium carbonate.
Tellurite is the tellurium source of embodiment of the invention preparation method cadmium telluride.Tellurite is meant in the aqueous solution compound that can ionization goes out the tellurous acid radical ion, and tellurite includes but not limited to one or more in potassium tellurite, sodium tellurite, the tellurous acid lithium.Embodiment of the invention preparing method's tellurite, highly stable in air, can be not oxidized, make the preparation method of the embodiment of the invention solve needs employing specific installation and method in the prior art, stablize the problem in tellurium source.Embodiment of the invention preparation method is low for equipment requirements, and reaction conditions is gentle, need not carry out anaerobic control to reaction conditions, simplifies preparation procedure greatly, has practiced thrift cost.
Sulfydryl part (L) forms coordination through the surface effects of its sulphur with cadmium telluride, can play stabilization to reaction product CdTe.Sulfydryl part (L) includes but not limited to one or more in halfcystine, Gelucystine, Thiovanic acid, thiohydracrylic acid, sulfydryl butyric acid, thioglycolate salt, mercapto propionate, sulfydryl butyrates, mercaptoethanol, mercaptoethylamine, Methyl Thioglycolate, Thiovanic acid second fat, mercapto-propionate or the gsh.
Alkali metal borohydride as reductive agent, can be reduced to tellurium ion (Te with positive tetravalence tellurium in the tellurious acid group in the preparation method of the embodiment of the invention
2-).Alkali metal borohydride includes but not limited to one or more in lithium borohydride, Peng Qinghuana or the POTASSIUM BOROHYDRIDE 97MIN.
Particularly, among the embodiment of the invention preparation method, add alkali metal borohydride after, the reaction times is restriction not, reacts to be green to solution and get final product, is roughly 1 minute-10 minutes, reacts to solution to be green, explains that the CdTe nucleus forms in the reaction solution.
Further; Embodiment of the invention preparation method is after the adding alkali metal borohydride reacts; Further may further comprise the steps; Be specially and temperature is adjusted to 70 ℃-100 ℃ down continued stirring reactions 45 minutes-12 hours, the mode through heating in water bath or reflux keeps temperature of reaction at 70 ℃-100 ℃, is preferably the reflux mode.The purpose of this reaction be before on the nucleus basis that generates of reaction, let the nucleus continued growth, make its particle diameter become big, the not concrete restriction of the time of reaction comes controlling reaction time according to the concentration of reaction soln, desired particle diameter.The time range that the present invention implements is 45 minutes-12 hours.The preparation method of the embodiment of the invention, the particle diameter of the cadmium telluride quantum dot of preparation is between 2nm-60nm, because the dimensional effect of cadmium telluride quantum dot, the fluorescent emission wavelength of this cadmium telluride quantum dot is between 520nm-700nm.
Particularly; Among the embodiment of the invention preparation method; The source compound of cadmium and the mol ratio of tellurite are 5: 1-1: 5; The mol ratio of tellurite and alkali metal borohydride is 1: 50-1: 100, and the mol ratio of Citrate trianion and tellurite is 1: 5-1: 20, the mol ratio of sulfydryl part (L) and tellurite is 1: 5-1: 20.
The preparation method of the embodiment of the invention in the water-soluble solution of source compound, Citrate trianion and tellurite with cadmium, because the dissemination of Citrate trianion, makes can not react between source compound and the tellurite of cadmium to generate tellurous acid cadmium deposition; Add alkali-metal hydroborate, the strong reducing property of alkali metal borohydride is with tellurious acid group (TeO
3 2-) middle Te
4+Be reduced to Te
2-, the reaction formula of this step is expressed as: 4TeO
3 2-+ 3BH
4 -→ 4Te
2-+ 3BO
2 -+ 6H
2O; Owing in mixing solutions, there is cadmium ion, cadmium ion and tellurium ionic reaction generate cadmium telluride quantum dot deposition (CdTe), and reaction formula is expressed as Cd
2+← L+Te
2--CdTe ← L, wherein, L is meant the sulfydryl part, through forming coordination between sulfydryl part and the cadmium telluride, realizes the provide protection of sulfydryl part to cadmium telluride, makes that the cadmium telluride quantum dot of embodiment of the invention preparation is stable, can not decompose.
Embodiment of the invention preparation method is placed on all reactants in the reactor drum and reacts, alkali metal borohydride reduction tellurious acid group at first, and secondly tellurium ion and cadmium ion reaction generation cadmium telluride, step is simple, has improved combined coefficient.Therefore also realized " one kettle way " preparation cadmium telluride quantum dot.
The cadmium telluride quantum dot preparation method of the embodiment of the invention, reaction conditions is gentle, to equipment require lowly, the reactant chemical property is stable; Greatly reduce cost, can generate the quantum dot of multiple nanometer particle size simultaneously, combined coefficient is high; Simple to operate, be applicable to suitability for industrialized production.
Below in conjunction with specific embodiment and accompanying drawing embodiment of the present invention is specified.
Embodiment one
The preparation method of cadmium telluride quantum dot, concrete steps are following:
I) under the agitation condition, in deionized water, adds CdCl
2Being made into 50ml concentration is 3 * 10
-3The solution of mol/L;
II) adds 100mg two hydration disodium citrates;
III) adding 4ml concentration is 10 * 10
-3The sodium tellurite aqueous solution of mol/L;
IV) adds L-halfcystine 50mg;
V) adds NaBH
450mg continues to stir under 15 ℃ of temperature, when solution colour becomes green, makes reaction soln at 100 ℃ of refluxed reaction 1h.
See also Fig. 1, Fig. 1 shows the cadmium telluride quantum dot fluorescence emission spectrogram of embodiment of the invention preparation, and as can be seen from Figure 1, the fluorescent emission intensity of cadmium telluride quantum dot between 500nm-600nm of embodiment of the invention preparation is the strongest.
See also Fig. 2, Fig. 2 shows the cadmium telluride quantum dot transmission electron microscope picture of embodiment of the invention preparation, among the figure; Representative is cadmium telluride quantum dot in the black circles; Its particle diameter is about 5nm, is sulfydryl part (L) at the shallow slightly coating substances of the peripheral color of this quantum dot, works to stablize CdTe.
Embodiment two
I) under the agitation condition, in deionized water, add potassium tellurite, preparation 5ml concentration is 10 * 10
-3The tellurite deionized water solution of mol/L;
II) adds Trisodium Citrate;
III) adding 100ml concentration is 4 * 10
-3Mol/L cadmium nitrate deionized water solution;
IV) adds Thiovanic acid 100mg;
V) adds POTASSIUM BOROHYDRIDE 97MIN 80mg, continue to stir down, when solution colour becomes green, use heating in water bath to keep 100 ℃ of reaction 4h, obtain cadmium telluride quantum dot at 20 ℃.
The prepared cadmium telluride quantum dot of embodiment of the invention preparation method has identical character with embodiment one prepared cadmium telluride quantum dot, does not do detailed elaboration at this.
The above is merely preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of within spirit of the present invention and principle, being done, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a cadmium telluride quantum dot preparation method comprises the steps: under the agitation condition, and is according to predefined procedure that source compound, Citrate trianion and the tellurite of cadmium is soluble in water; Add the sulfydryl part; Add alkali metal borohydride again, stirring reaction is 1 minute-10 minutes under 10 ℃ of-30 ℃ of conditions, obtains cadmium telluride quantum dot; Said predefined procedure be meant with one in the source compound of cadmium and the tellurite with after Hydrocerol A mixes, add among both another again.
2. cadmium telluride quantum dot preparation method as claimed in claim 1 is characterized in that, said Citrate trianion is selected from one or more in Tripotassium Citrate, Trisodium Citrate, hydration Trisodium Citrate or the hydration Tripotassium Citrate.
3. cadmium telluride quantum dot preparation method as claimed in claim 1 is characterized in that the source compound of said cadmium is selected from one or more in Cadmium chloride fine powder, cadmium bromide, cadmium iodide, cadmium nitrate, cadmium chlorate, cadmium acetate, cadmium perchlorate, Cadmium Sulphate or the cadmium carbonate.
4. cadmium telluride quantum dot preparation method as claimed in claim 1 is characterized in that, said tellurite is selected from one or more in potassium tellurite, sodium tellurite or the tellurous acid lithium.
5. cadmium telluride quantum dot preparation method as claimed in claim 1; It is characterized in that the sulfydryl part is selected from one or more in halfcystine, Gelucystine, Thiovanic acid, thiohydracrylic acid, sulfydryl butyric acid, thioglycolate salt, mercapto propionate, sulfydryl butyrates, mercaptoethanol, mercaptoethylamine, Methyl Thioglycolate, Thiovanic acid second fat, mercapto-propionate or the gsh.
6. cadmium telluride quantum dot preparation method as claimed in claim 1 is characterized in that alkali metal borohydride is selected from one or more in lithium borohydride, Peng Qinghuana or the POTASSIUM BOROHYDRIDE 97MIN.
7. cadmium telluride quantum dot preparation method as claimed in claim 1 is characterized in that, described reaction further may further comprise the steps: behind said stirring reaction, temperature is adjusted to 70 ℃ of-100 ℃ of stirring reactions 45 minutes-12 hours.
8. cadmium telluride quantum dot preparation method as claimed in claim 7 is characterized in that, the mol ratio of said tellurite and said alkali metal borohydride is 1: 50-1: 100.
9. cadmium telluride quantum dot preparation method as claimed in claim 1 is characterized in that, the source compound of said cadmium and the mol ratio of said tellurite are 5: 1-1: 5.
10. cadmium telluride quantum dot preparation method as claimed in claim 1 is characterized in that, the mol ratio of said Citrate trianion and said tellurite is 1: 5-1: 20, and the mol ratio of said sulfydryl part and said tellurite is 1: 5-1: 20.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786037A (en) * | 2012-06-05 | 2012-11-21 | 大连理工大学 | CdX quantum dot and preparation method thereof |
| CN103525424A (en) * | 2013-10-21 | 2014-01-22 | 山东交通学院 | CdTe quantum dots, preparation method therefor and applications in detection of trace explosives |
| CN104059670A (en) * | 2014-06-11 | 2014-09-24 | 武汉大学 | Water phase preparation method of CdTeSeS alloy quantum dot |
| CN105694893A (en) * | 2016-04-12 | 2016-06-22 | 北京化工大学 | Langmiur-Blodgett composite lighting film of cadmium telluride quantum dots and layered double hydroxide and manufacturing method thereof |
| CN106467294A (en) * | 2016-10-17 | 2017-03-01 | 浙江和谱生物科技有限公司 | The aqueous phase preparation method of suppression tumor cell nanometer cadmium telluride |
| CN109721036A (en) * | 2019-01-02 | 2019-05-07 | 北京科技大学 | A kind of method of chemical liquid phase reaction preparation selenizing thin film lead |
| CN111518543A (en) * | 2019-02-01 | 2020-08-11 | 苏州星烁纳米科技有限公司 | Quantum dot dispersion system, color film and display device |
| CN113428842A (en) * | 2021-06-08 | 2021-09-24 | 长安大学 | Cadmium manganese telluride nano powder and preparation method thereof |
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| CN1858149A (en) * | 2006-06-02 | 2006-11-08 | 中国科学院长春应用化学研究所 | Process for preparing cadmium telluride quantum spot |
| CN101698889A (en) * | 2009-10-21 | 2010-04-28 | 江南大学 | Method for detecting DNA base number based on quantum dot and PCR technology |
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2010
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1858149A (en) * | 2006-06-02 | 2006-11-08 | 中国科学院长春应用化学研究所 | Process for preparing cadmium telluride quantum spot |
| CN101698889A (en) * | 2009-10-21 | 2010-04-28 | 江南大学 | Method for detecting DNA base number based on quantum dot and PCR technology |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786037A (en) * | 2012-06-05 | 2012-11-21 | 大连理工大学 | CdX quantum dot and preparation method thereof |
| CN103525424A (en) * | 2013-10-21 | 2014-01-22 | 山东交通学院 | CdTe quantum dots, preparation method therefor and applications in detection of trace explosives |
| CN104059670A (en) * | 2014-06-11 | 2014-09-24 | 武汉大学 | Water phase preparation method of CdTeSeS alloy quantum dot |
| CN105694893A (en) * | 2016-04-12 | 2016-06-22 | 北京化工大学 | Langmiur-Blodgett composite lighting film of cadmium telluride quantum dots and layered double hydroxide and manufacturing method thereof |
| CN106467294A (en) * | 2016-10-17 | 2017-03-01 | 浙江和谱生物科技有限公司 | The aqueous phase preparation method of suppression tumor cell nanometer cadmium telluride |
| CN106467294B (en) * | 2016-10-17 | 2018-08-24 | 浙江和谱生物科技有限公司 | Inhibit the aqueous phase preparation method of tumour cell nanometer cadmium telluride |
| CN109721036A (en) * | 2019-01-02 | 2019-05-07 | 北京科技大学 | A kind of method of chemical liquid phase reaction preparation selenizing thin film lead |
| CN111518543A (en) * | 2019-02-01 | 2020-08-11 | 苏州星烁纳米科技有限公司 | Quantum dot dispersion system, color film and display device |
| CN113428842A (en) * | 2021-06-08 | 2021-09-24 | 长安大学 | Cadmium manganese telluride nano powder and preparation method thereof |
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Application publication date: 20120411 |