CN1772599A - Process of preparing monodisperse nanometer semiconductor selenide particle - Google Patents
Process of preparing monodisperse nanometer semiconductor selenide particle Download PDFInfo
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- CN1772599A CN1772599A CN 200510109215 CN200510109215A CN1772599A CN 1772599 A CN1772599 A CN 1772599A CN 200510109215 CN200510109215 CN 200510109215 CN 200510109215 A CN200510109215 A CN 200510109215A CN 1772599 A CN1772599 A CN 1772599A
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- 239000002245 particle Substances 0.000 title claims abstract description 29
- 150000003346 selenoethers Chemical class 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000004065 semiconductor Substances 0.000 title claims abstract description 18
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 26
- 239000011669 selenium Substances 0.000 claims abstract description 26
- 239000002798 polar solvent Substances 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 229940091258 selenium supplement Drugs 0.000 claims description 24
- 239000012046 mixed solvent Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910021645 metal ion Inorganic materials 0.000 claims description 12
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 9
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 9
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 239000005642 Oleic acid Substances 0.000 claims description 9
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 9
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 9
- 150000002632 lipids Chemical class 0.000 claims description 9
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical group OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- BVTBRVFYZUCAKH-UHFFFAOYSA-L disodium selenite Chemical compound [Na+].[Na+].[O-][Se]([O-])=O BVTBRVFYZUCAKH-UHFFFAOYSA-L 0.000 claims description 7
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 7
- 230000002829 reductive effect Effects 0.000 claims description 7
- 229960001471 sodium selenite Drugs 0.000 claims description 7
- 239000011781 sodium selenite Substances 0.000 claims description 7
- 235000015921 sodium selenite Nutrition 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 claims description 6
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 5
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims description 4
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 4
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052793 cadmium Inorganic materials 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 239000011572 manganese Substances 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 12
- 239000000090 biomarker Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 229910000272 alkali metal oxide Inorganic materials 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 235000014113 dietary fatty acids Nutrition 0.000 abstract 1
- 229930195729 fatty acid Natural products 0.000 abstract 1
- 239000000194 fatty acid Substances 0.000 abstract 1
- 150000004665 fatty acids Chemical class 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 238000000634 powder X-ray diffraction Methods 0.000 description 12
- 239000002105 nanoparticle Substances 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 9
- 238000005119 centrifugation Methods 0.000 description 9
- 238000001035 drying Methods 0.000 description 9
- 229910001220 stainless steel Inorganic materials 0.000 description 9
- 239000010935 stainless steel Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 238000005406 washing Methods 0.000 description 9
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 7
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- GGYFMLJDMAMTAB-UHFFFAOYSA-N selanylidenelead Chemical compound [Pb]=[Se] GGYFMLJDMAMTAB-UHFFFAOYSA-N 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 2
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- UMUKXUYHMLVFLM-UHFFFAOYSA-N manganese(ii) selenide Chemical compound [Mn+2].[Se-2] UMUKXUYHMLVFLM-UHFFFAOYSA-N 0.000 description 2
- KNLQKHUBPCXPQD-UHFFFAOYSA-N manganese;sulfuric acid Chemical compound [Mn].OS(O)(=O)=O KNLQKHUBPCXPQD-UHFFFAOYSA-N 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 239000011592 zinc chloride Substances 0.000 description 2
- 235000005074 zinc chloride Nutrition 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 description 1
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 description 1
- LQWCJVQHKJHKDZ-UHFFFAOYSA-N cadmium sulfuric acid Chemical compound [Cd].S(O)(O)(=O)=O LQWCJVQHKJHKDZ-UHFFFAOYSA-N 0.000 description 1
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 description 1
- KDSXXMBJKHQCAA-UHFFFAOYSA-N disilver;selenium(2-) Chemical compound [Se-2].[Ag+].[Ag+] KDSXXMBJKHQCAA-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- -1 vitriol Chemical compound 0.000 description 1
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- Photovoltaic Devices (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The present invention discloses process of preparing monodisperse nanometer semiconductor selenide particle. The present invention prepares the monodisperse nanometer semiconductor selenide particle through reaction between metal ionic solution and selenium source inside the mixture system comprising alkali metal oxide, fatty acid and organic polar solvent. The selenium source is mixture system comprising selenide and reductant or metal selenium powder. The process of the present invention is simple, safe, low in cost, low in environmental pollution, and suitable for synthesis of several kinds of nanometer semiconductor selenide particle. The prepared nanometer semiconductor selenide particle may be applied widely in biological marker, analysis, solar cell and other fields.
Description
Technical field
The present invention relates to preparation of nanomaterials, particularly relate to a kind of method for preparing nanometer semiconductor selenide particle.
Background technology
Nanometer semiconductor selenide particle has in fields such as biomarker, analysis, solar cells widely to be used.Developed at present the method for multiple synthetic selenide nanometer particle, on " nature " magazine, reported to be stablizer and style control agent in 2000, be raw material as people such as Peng XG with organic cadmium of metal and selenium powder with TOPO-HPA, the method of synthesizing cadmium selenide nano-crystal (2000,404 volume 59-61 pages or leaves); Subsequently calendar year 2001 in " American Chemical Society can will ", have reported again with TOPO-HPA be stablizer, Cadmium oxide be the raw material synthesizing cadmium selenide nano-crystal method (J.Am.Chem.Soc., 2001,123:183); People such as Li Yadong have reported on U.S.'s " inorganic chemistry " magazine with the reaction at aqueous phase direct reaction synthesizing CdSe and zinc selenide of cadmium metal powder, zinc powder and selenium powder calendar year 2001, but this method is difficult to realize the control (calendar year 2001,40 volume 3840-3841 pages or leaves) to the product size.
In sum, at present the synthetic method of the domestic and international nanometer semiconductor selenide particle of reporting has generally all used a large amount of organic solvents to be liquid-phase system, still lacks at present based on the water liquid-phase system, applicable to the report of multiple semiconductor selenide monodisperse nanoparticle synthetic method.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing monodisperse nanometer semiconductor selenide particle.
The method for preparing monodisperse nanometer semiconductor selenide particle provided by the present invention, be that metal ion solution and selenium source are reacted in the mixed system of alkali metal hydroxide, lipid acid and organic polar solvent, obtain described monodisperse nanometer semiconductor selenide particle; Described selenium source is the system that selenium-containing compound and reductive agent are formed, and perhaps is the metal selenium powder.
The step of above-mentioned reaction is: earlier solid alkali metal oxyhydroxide is joined in the mixed solvent of lipid acid and organic polar solvent, add metal ion solution and selenium source after the mixing again, 20-300 ℃ of reaction down, obtain described monodisperse nano metal oxide particle then.
Wherein, selenium-containing compound commonly used is a Sodium Selenite in the selenium source of above-mentioned selenium-containing compound and reductive agent composition, and reductive agent is a hydrazine hydrate N2H4 H2O-100, and the mol ratio of reductive agent and described selenium-containing compound is 5-10: 1.
In the reaction system, the volume ratio of lipid acid and organic polar solvent is 1: 0.5-10; The concentration of metal ion solution is 0.01-0.5mol/L, and the mol ratio of selenium element and metal ion is 0.1-6 in the selenium source: 1; The mol ratio of alkali metal hydroxide and described metal ion is 1-10: 1.
Metal ion is zinc, silver, cadmium, manganese or lead ion etc., can its soluble salt, and waiting as nitrate, vitriol, acetate or hydrochloride provides; Lipid acid is oleic acid, stearic acid or capric acid etc.; Organic polar solvent is ethanol, acetone, ethylene glycol, quadrol or glycerol etc.
The present invention constitutes mixed solvent system with lipid acid and polar solvent, is raw material with soluble metallic salt, selenium source and alkali metal hydroxide, prepares monodisperse nanometer semiconductor selenide particle.The inventive method is easy, safety, cost is low, suitability is wide, be applicable to the synthetic of multiple nanometer semiconductor selenide particle simultaneously, overcome and adopted cost and the problem of environmental pollution that a large amount of organic solvent brought in the existing synthetic route, the nanometer semiconductor selenide particle that is obtained can be widely used in fields such as biomarker, analysis, solar cell.
Description of drawings
Fig. 1 is the prepared zinc selenide X-ray powder diffraction figure of embodiment 2.
Fig. 2 is that embodiment 2 prepared zinc selenide TEM Electronic Speculum detect figure.
Fig. 3 is the prepared cadmium selenide X-ray powder diffraction figure of embodiment 4.
Fig. 4 is that embodiment 4 prepared cadmium selenide TEM Electronic Speculum detect figure.
Fig. 5 is the prepared lead selenide X-ray powder diffraction figure of embodiment 8.
Fig. 6 is that embodiment 8 prepared lead selenide TEM Electronic Speculum detect figure.
Fig. 7 is that embodiment 9 prepared lead selenide TEM Electronic Speculum detect figure.
Embodiment
Embodiment 1,
Taking by weighing 0.7gNaOH adds in the mixed solvent of 10ml oleic acid, 15ml ethylene glycol, fully behind the about 30mins of reaction, taking by weighing 0.8g analytical pure Silver Nitrate again is dissolved in the 20mL water, take by weighing 0.4g analytical pure selenium powder, silver ion solution and the selenium powder that is made into added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 140 ℃ of reaction 24h, gained precipitates after centrifugation, washing, drying, obtains black powder.Product is accredited as silver selenide through X-ray powder diffraction; (TEM) carries out morphology analysis to it with transmission electron microscope, and observing its pattern is the dispersed nano particle, and particle diameter is about 20nm.
Embodiment 2:
Taking by weighing 0.5gNaOH adds in 5ml oleic acid, the 10ml ethanol mixed solvent, fully behind the about 30mins of reaction, taking by weighing 1g analytical pure zinc chloride again is dissolved in the 20mL water, take by weighing 0.8g analytical pure selenium powder, and with in the zine ion solution and selenium powder adding mixed solvent that are made into, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 180 ℃ of reaction 24h, gained precipitates through centrifugation, 1molL
-1After NaOH solution washing, deionized water wash, the drying, obtain yellow powder.Product is accredited as zinc selenide through X-ray powder diffraction as shown in Figure 1; (TEM) carries out morphology analysis to it with transmission electron microscope, and as can be seen from Figure 2 its pattern is the dispersed nano particle, and particle diameter is between 15-20nm.
Embodiment 3:
Taking by weighing 0.4gKOH adds in the mixed solvent of 10ml oleic acid, 10ml acetone, fully behind the about 30mins of reaction, taking by weighing 0.5g analytical pure zinc chloride again is dissolved in the 5mL water, taking by weighing 0.3g analytical pure Sodium Selenite is dissolved in the 5mL water, zine ion, plasma selenium solution and the 10ml analytical pure hydrazine hydrate N2H4 H2O-100 (volumetric concentration 80%) that is made into added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 160 ℃ of reaction 24h, the gained precipitation obtains yellow powder after centrifugation, washing, drying.Product is accredited as zinc selenide through X-ray powder diffraction; (TEM) carries out morphology analysis to it with transmission electron microscope, and observing its pattern is the dispersed nano particle, and particle diameter is between 10-20nm.
Embodiment 4:
Taking by weighing 1gNaOH adds in 10ml oleic acid, the 8ml ethanol mixed solvent, fully behind the about 30mins of reaction, taking by weighing 0.8g analytical pure sulfuric acid cadmium again heats in 20mL water and makes its dissolving, and with in the cadmium-ion solution and 1.0g analytical pure selenium powder adding mixed solvent that are made into, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 180 ℃ of reaction 24h, gained precipitates through centrifugation, 1molL
-1After NaOH solution washing, deionized water wash, the drying, obtain black powder.Product is accredited as cadmium selenide through X-ray powder diffraction as shown in Figure 3; (TEM) carries out morphology analysis to it with transmission electron microscope, and as can be seen from Figure 4 its pattern is the dispersed nano particle, and particle diameter is between 4 ~ 5nm.
Embodiment 5:
Taking by weighing 1gKOH adds in the mixed solvent of 5ml capric acid, 5ml glycerol, fully behind the about 30mins of reaction, taking by weighing 1g analytical pure cadmium nitrate again is dissolved in the 10mL water, taking by weighing 1g analytical pure Sodium Selenite is dissolved in the 10mL water, cadmium ion, plasma selenium solution and the 10mL analytical pure hydrazine hydrate N2H4 H2O-100 (volumetric concentration 80%) that is made into added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 250 ℃ of reaction 24h, the gained precipitation obtains black powder after centrifugation, washing, drying.Product is accredited as cadmium selenide through X-ray powder diffraction; (TEM) carries out morphology analysis to it with transmission electron microscope, and observing its pattern is the dispersed nano particle, and particle diameter is between 20-30nm.
Embodiment 6:
Taking by weighing 0.5gNaOH adds in 8ml oleic acid, the 15ml ethanol mixed solvent, fully behind the about 30mins of reaction, taking by weighing 0.5g analytical pure sulfuric acid manganese again is dissolved in the 17mL water, the mn ion solution and the 0.5g analytical pure selenium powder that are made into are added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 50 ℃ of reaction 24h, gained precipitates through centrifugation, 1molL
-1After NaOH solution washing, deionized water wash, the drying, obtain black powder.Product is accredited as manganese selenide through X-ray powder diffraction as shown in Figure 5; (TEM) carries out morphology analysis to it with transmission electron microscope, and as can be seen from Figure 6 its pattern is the dispersed nano particle, and particle diameter is between 5-6nm.
Embodiment 7:
Take by weighing in 0.5gNaOH, the 3g analytical pure stearic acid adding 20ml ethanol, fully behind the about 30mins of reaction, taking by weighing 0.5g analytical pure sulfuric acid manganese again is dissolved in the 6mL water, taking by weighing 0.3g analytical pure Sodium Selenite is dissolved in the 4mL water, mn ion, selenium solution and the 10mL analytical pure hydrazine hydrate N2H4 H2O-100 (volumetric concentration 80%) that is made into added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 70 ℃ of reaction 24h, the gained precipitation obtains black powder after centrifugation, washing, drying.Product is accredited as manganese selenide through X-ray powder diffraction; (TEM) carries out morphology analysis to it with transmission electron microscope, and can observe its pattern is the dispersed nano particle, and particle diameter is between 40-50nm.
Embodiment 8:
Taking by weighing 0.4gNaOH adds in the mixed solvent of 10ml oleic acid, 10ml quadrol, fully behind the about 30mins of reaction, taking by weighing 1g analytical pure lead nitrate again is dissolved in the 5mL water, taking by weighing 0.5g analytical pure Sodium Selenite is dissolved in the 5mL water, lead ion, plasma selenium solution and the 8mL analytical pure hydrazine hydrate N2H4 H2O-100 (volumetric concentration 80%) that is made into added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 20 ℃ of reaction 24h, the gained precipitation obtains black powder after centrifugation, washing, drying.Product is accredited as lead selenide through X-ray powder diffraction as shown in Figure 7; (TEM) carries out morphology analysis to it with transmission electron microscope, and as can be seen from Figure 8 its pattern is the dispersed nano particle, and particle diameter is between 4-5nm.
Embodiment 9:
Taking by weighing 1gNaOH adds in the mixed solvent of 10ml oleic acid, 10ml quadrol, fully behind the about 30mins of reaction, taking by weighing 1g analytical pure lead nitrate again is dissolved in the 5mL water, taking by weighing 0.5g analytical pure Sodium Selenite is dissolved in the 5mL water, lead ion, plasma selenium solution and the 8mL analytical pure hydrazine hydrate N2H4 H2O-100 (volumetric concentration 80%) that is made into added in the mixed solvent, stir, place the withstand voltage reactor of stainless steel of 40ml, behind 20 ℃ of reaction 24h, the gained precipitation obtains black powder after centrifugation, washing, drying.Product is accredited as lead selenide through X-ray powder diffraction as shown in Figure 7; (TEM) carries out morphology analysis to it with transmission electron microscope, and as can be seen from Figure 8 its pattern is the dispersed nano particle, and particle diameter is between 7-8nm.
Claims (7)
1, a kind of method for preparing monodisperse nanometer semiconductor selenide particle, be that metal ion solution and selenium source are reacted in the mixed system of alkali metal hydroxide, lipid acid and organic polar solvent, obtain described monodisperse nanometer semiconductor selenide particle; Described selenium source is the system that selenium-containing compound and reductive agent are formed, and perhaps is the metal selenium powder.
2, method according to claim 1, it is characterized in that: the step of described reaction is: earlier solid alkali metal oxyhydroxide is joined in the mixed solvent of lipid acid and organic polar solvent, add metal ion solution and selenium source after the mixing again, 20-300 ℃ of reaction down, obtain described monodisperse nano metal oxide particle then.
3, method according to claim 1 is characterized in that: described selenium-containing compound is a Sodium Selenite; Described reductive agent is a hydrazine hydrate N2H4 H2O-100, and the mol ratio of described reductive agent and described selenium-containing compound is 5-10: 1.
4, according to claim 1 or 2 or 3 described methods, it is characterized in that: the volume ratio of described lipid acid and organic polar solvent is 1: 0.5-10; The concentration of described metal ion solution is 0.01-0.5mol/L, and the mol ratio of selenium element and metal ion is 0.1-6 in the described selenium source: 1; The mol ratio of described alkali metal hydroxide and described metal ion is 1-10: 1.
5, according to claim 1 or 2 or 3 described methods, it is characterized in that: described metal ion is zinc, silver, cadmium, manganese or lead ion.
6, according to claim 1 or 2 or 3 described methods, it is characterized in that: described lipid acid is oleic acid, stearic acid or capric acid.
7, according to claim 1 or 2 or 3 described methods, it is characterized in that: described organic polar solvent is ethanol, acetone, ethylene glycol, quadrol or glycerol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101092158A CN100344531C (en) | 2005-10-19 | 2005-10-19 | Process of preparing monodisperse nanometer semiconductor selenide particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101092158A CN100344531C (en) | 2005-10-19 | 2005-10-19 | Process of preparing monodisperse nanometer semiconductor selenide particle |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1772599A true CN1772599A (en) | 2006-05-17 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102086043A (en) * | 2009-12-08 | 2011-06-08 | 中国科学院福建物质结构研究所 | Preparation method for metal chalcogenide crystalline microporous material |
| CN105036092A (en) * | 2015-08-07 | 2015-11-11 | 中南大学 | Preparation method of spherical silver selenide particles |
| CN109036863A (en) * | 2018-07-23 | 2018-12-18 | 浙江大学 | A kind of selenides@carbon based fibers electrode material for super capacitor and preparation method thereof |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1159211C (en) * | 2002-06-07 | 2004-07-28 | 清华大学 | Synthesis of several metal selenides and tellurides as semiconductor material |
| CN1191193C (en) * | 2003-01-10 | 2005-03-02 | 清华大学 | Synthesis of nano hollow balls of zinc selenide |
| JP4445716B2 (en) * | 2003-05-30 | 2010-04-07 | 日立ソフトウエアエンジニアリング株式会社 | Nanoparticle production method |
| CN1526637A (en) * | 2003-09-25 | 2004-09-08 | 浙江大学 | Prepn of Bi2Te3-base compound nanotube |
| CN1268013C (en) * | 2004-05-13 | 2006-08-02 | 浙江大学 | Method for preparing transition metal distibide |
| CN1299998C (en) * | 2004-11-05 | 2007-02-14 | 中国科学院长春应用化学研究所 | Synthesis method for cadmium selenide and cadmium telluride quantum dot |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102086043A (en) * | 2009-12-08 | 2011-06-08 | 中国科学院福建物质结构研究所 | Preparation method for metal chalcogenide crystalline microporous material |
| CN105036092A (en) * | 2015-08-07 | 2015-11-11 | 中南大学 | Preparation method of spherical silver selenide particles |
| CN109036863A (en) * | 2018-07-23 | 2018-12-18 | 浙江大学 | A kind of selenides@carbon based fibers electrode material for super capacitor and preparation method thereof |
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