CN1974485A - Process of preparing nanomter zinc oxide/sulfide core-shell structure - Google Patents
Process of preparing nanomter zinc oxide/sulfide core-shell structure Download PDFInfo
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- CN1974485A CN1974485A CN 200610154729 CN200610154729A CN1974485A CN 1974485 A CN1974485 A CN 1974485A CN 200610154729 CN200610154729 CN 200610154729 CN 200610154729 A CN200610154729 A CN 200610154729A CN 1974485 A CN1974485 A CN 1974485A
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- CN
- China
- Prior art keywords
- zinc oxide
- shell structure
- nanomter
- chloride
- tetrahydrofuran
- 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.)
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 39
- 239000011258 core-shell material Substances 0.000 title claims abstract description 25
- 239000005083 Zinc sulfide Substances 0.000 title claims abstract description 19
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical group [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052984 zinc sulfide Inorganic materials 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims abstract description 13
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 68
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001510 metal chloride Inorganic materials 0.000 claims abstract description 11
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 9
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 13
- 239000012279 sodium borohydride Substances 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 12
- 239000005864 Sulphur Substances 0.000 claims description 9
- 239000002073 nanorod Substances 0.000 claims description 9
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical group Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 8
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 8
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
- 239000011592 zinc chloride Substances 0.000 claims description 4
- 235000005074 zinc chloride Nutrition 0.000 claims description 4
- 229960003280 cupric chloride Drugs 0.000 claims description 2
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract 2
- 239000000203 mixture Substances 0.000 abstract 2
- 229910052708 sodium Inorganic materials 0.000 abstract 2
- 239000011734 sodium Substances 0.000 abstract 2
- 239000002086 nanomaterial Substances 0.000 description 12
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical group OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 6
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 230000005693 optoelectronics Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Luminescent Compositions (AREA)
Abstract
The present invention discloses process of preparing nanometer zinc oxide/sulfide core-shell structure. The process includes the following steps: 1. adding nanometer zinc oxide rod, sulfur powder and metal chloride simultaneously into tetrahydrofuran via ultrasonic dispersion to obtain mixture solution; and 2. ultrasonically dispersing sodium borahydride in tetrahydrofuran, dropping into the mixture solution to react for 0.5-3 hr, centrifuging, and drying. By means of the chemical reaction of sodium borahydride, sulfur powder and metal chloride, sulfide is adsorbed onto the surface of nanometer zinc oxide rod to obtain the nanometer zinc oxide/sulfide core-shell structure.
Description
Technical field
The present invention relates to prepare the method for nanomter zinc oxide/sulfide core-shell structure.
Background technology
Zinc oxide is a kind of important semiconductor material with wide forbidden band, and its nano material is widely used in optoelectronic areas such as photodiode, gas sensor, ultraviolet detector.In recent years, because the Zinc oxide-base matrix material is not only inherited the superior performance of zinc oxide itself, and shows many new performances in fields such as luminous and gas sensors, thereby be subjected to paying close attention to widely.As everyone knows, sulfide also is the important semiconductor material of a class, and they are widely used in optoelectronic areas such as solar cell, photodiode, detector.Therefore as the combination of two kinds of materials, the nanomter zinc oxide/sulfide core-shell structure expection can show that make new advances or superior performance.At present, the method for preparing nanomter zinc oxide/sulfide core-shell structure has high temperature vapour deposition harmony chemical method.But the temperature of reaction that above-mentioned two kinds of methods need be higher, comparatively complicated chemical reaction do not have ubiquity.
Summary of the invention
The purpose of this invention is to provide that a kind of technology is simple, prepare the methods of nanomter zinc oxide/sulfide core-shell structure under the room temperature in a large number.
The method for preparing nanomter zinc oxide/sulfide core-shell structure of the present invention may further comprise the steps:
1) zinc oxide nano rod, sulphur powder and metal chloride are joined in the tetrahydrofuran (THF) simultaneously, ultra-sonic dispersion obtains mixing solutions, and the mol ratio of zinc oxide nano rod, sulphur powder and metal chloride is 0.1～10: 0.1～10: 1;
2) with the sodium borohydride ultra-sonic dispersion in 100 milliliters of tetrahydrofuran (THF)s, the mol ratio of sodium borohydride and metal chloride is 0.1～10: 1;
3) with step 2) mixing solutions that makes splashes in the mixing solutions that step 1) makes, and reacts 0.5～3h;
4) reaction finishes, and is centrifugal, dry, obtains nanomter zinc oxide/sulfide core-shell structure.
Above-mentioned metal chloride can be Cadmium chloride fine powder, zinc chloride, cupric chloride or lead chloride.
Beneficial effect of the present invention is:
Preparation technology is simple, and output is big, utilizes the chemical reaction of sodium borohydride, sulphur powder and metal chloride can make sulfide be adsorbed on the surface of zinc oxide nano rod, the core-shell nano structure that is easy to get, and quality is good; Adopt the inventive method can prepare multiple nanomter zinc oxide/sulfide core-shell structure.
Description of drawings
Fig. 1 is the stereoscan photograph of zinc oxide/Cadmium Sulfide core-shell nano structure;
Fig. 2 is the transmission electron microscope photo of zinc oxide/Cadmium Sulfide core-shell nano structure;
Fig. 3 is the stereoscan photograph of zinc oxide/zinc sulphide core-shell nano structure;
Fig. 4 is the transmission electron microscope photo of zinc oxide/zinc sulphide core-shell nano structure.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment 1
5 mmole zinc oxide nano rods, 5 mmole sulphur powder and 0.5 mmole Cadmium chloride fine powder are added in 100 milliliters of tetrahydrofuran (THF)s, and ultrasonic 1 hour.Then with 5 mmole sodium borohydride ultra-sonic dispersion in 100 milliliters of tetrahydrofuran (THF)s.Then the mixing solutions with sodium borohydride and tetrahydrofuran (THF) splashes in the above-mentioned solution, and reaction 0.5h.After finishing, reaction, obtains zinc oxide/Cadmium Sulfide core-shell nano structure with the solution centrifugal, the drying that obtain.Fig. 1 and Fig. 2 are respectively the scanning electron microscope and the transmission electron microscope photos of zinc oxide/Cadmium Sulfide core-shell nano structure.As seen from the figure, the diameter of zinc oxide nuclear is 30～50nm, and the thickness of Cadmium Sulfide shell is 5～10nm.
Embodiment 2
0.5 mmole zinc oxide nano rod, 0.5 mmole sulphur powder and 5 mmole Cadmium chloride fine powdeies are added in 100 milliliters of tetrahydrofuran (THF)s, and ultrasonic 1 hour.Then with 0.5 mmole sodium borohydride ultra-sonic dispersion in 100 milliliters of tetrahydrofuran (THF)s.Then the mixing solutions with sodium borohydride and tetrahydrofuran (THF) splashes in the above-mentioned solution, and reaction 3h.After finishing, reaction, obtains zinc oxide/Cadmium Sulfide core-shell nano structure with the solution centrifugal, the drying that obtain.Its result is similar with example 1.
Embodiment 3
2 mmole zinc oxide nano rods, 5 mmole sulphur powder and 0.5 mmole zinc chloride are added in 100 milliliters of tetrahydrofuran (THF)s, and ultrasonic 1 hour.Then with 2 mmole sodium borohydride ultra-sonic dispersion in 100 milliliters of tetrahydrofuran (THF)s.Then the mixing solutions with sodium borohydride and tetrahydrofuran (THF) splashes in the above-mentioned solution, and reaction 1h.After finishing, reaction, obtains zinc oxide/zinc sulphide core-shell nano structure with the solution centrifugal, the drying that obtain.Fig. 3 and Fig. 4 are respectively the scanning electron microscope and the transmission electron microscope photos of zinc oxide/zinc sulphide core-shell nano structure.As seen from the figure, the diameter of zinc oxide nuclear is 30～50nm, and the thickness of sulfuration cadmia is 5～10nm.
Embodiment 4
2 mmole zinc oxide nano rods, 5 mmole sulphur powder and 1 mmole zinc chloride are added in 100 milliliters of tetrahydrofuran (THF)s, and ultrasonic 1 hour.Then with 2 mmole sodium borohydride ultra-sonic dispersion in 100 milliliters of tetrahydrofuran (THF)s.Then the mixing solutions with sodium borohydride and tetrahydrofuran (THF) splashes in the above-mentioned solution, and reaction 2h.After finishing, reaction, obtains zinc oxide/zinc sulphide core-shell nano structure with the solution centrifugal, the drying that obtain.Its result is similar with example 3.
Claims (2)
1. method for preparing nanomter zinc oxide/sulfide core-shell structure is characterized in that may further comprise the steps:
1) zinc oxide nano rod, sulphur powder and metal chloride are joined in the tetrahydrofuran (THF) simultaneously, ultra-sonic dispersion obtains mixing solutions, and the mol ratio of zinc oxide nano rod, sulphur powder and metal chloride is 0.1～10: 0.1～10: 1;
2) with the sodium borohydride ultra-sonic dispersion in 100 milliliters of tetrahydrofuran (THF)s, the mol ratio of sodium borohydride and metal chloride is 0.1～10: 1;
3) with step 2) mixing solutions that makes splashes in the mixing solutions that step 1) makes, and reacts 0.5～3h;
4) reaction finishes, and is centrifugal, dry, obtains nanomter zinc oxide/sulfide core-shell structure.
2. the method for preparing nanomter zinc oxide/sulfide core-shell structure according to claim 1 is characterized in that said metal chloride is Cadmium chloride fine powder, zinc chloride, cupric chloride or lead chloride.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610154729XA CN100500617C (en) | 2006-11-21 | 2006-11-21 | Process of preparing nanomter zinc oxide/sulfide core-shell structure |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610154729XA CN100500617C (en) | 2006-11-21 | 2006-11-21 | Process of preparing nanomter zinc oxide/sulfide core-shell structure |
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| Publication Number | Publication Date |
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| CN1974485A true CN1974485A (en) | 2007-06-06 |
| CN100500617C CN100500617C (en) | 2009-06-17 |
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| CNB200610154729XA Expired - Fee Related CN100500617C (en) | 2006-11-21 | 2006-11-21 | Process of preparing nanomter zinc oxide/sulfide core-shell structure |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102104079A (en) * | 2010-12-21 | 2011-06-22 | 中国科学院理化技术研究所 | Preparation method of one-dimensional ZnO/ZnS core-shell structure nano array and single crystal ZnS nano tube array |
| CN102104078A (en) * | 2010-12-21 | 2011-06-22 | 中国科学院理化技术研究所 | Preparation method of ZnO/ZnS core-shell structure one-dimensional nano material and single crystal ZnS nanotube |
| CN101665883B (en) * | 2009-10-19 | 2011-08-10 | 浙江大学 | Method for preparing nano-porous block of Fe-Sn intermetallic compound |
| CN106966443A (en) * | 2017-03-24 | 2017-07-21 | 福州大学 | A kind of preparation method of transition metal oxide/sulfide nano composite material |
-
2006
- 2006-11-21 CN CNB200610154729XA patent/CN100500617C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665883B (en) * | 2009-10-19 | 2011-08-10 | 浙江大学 | Method for preparing nano-porous block of Fe-Sn intermetallic compound |
| CN102104079A (en) * | 2010-12-21 | 2011-06-22 | 中国科学院理化技术研究所 | Preparation method of one-dimensional ZnO/ZnS core-shell structure nano array and single crystal ZnS nano tube array |
| CN102104078A (en) * | 2010-12-21 | 2011-06-22 | 中国科学院理化技术研究所 | Preparation method of ZnO/ZnS core-shell structure one-dimensional nano material and single crystal ZnS nanotube |
| CN102104078B (en) * | 2010-12-21 | 2012-03-28 | 中国科学院理化技术研究所 | Preparation method of ZnO/ZnS core-shell structure one-dimensional nano material and single crystal ZnS nanotube |
| CN102104079B (en) * | 2010-12-21 | 2012-05-23 | 中国科学院理化技术研究所 | Preparation method of one-dimensional ZnO/ZnS core-shell structure nano array and single crystal ZnS nano tube array |
| CN106966443A (en) * | 2017-03-24 | 2017-07-21 | 福州大学 | A kind of preparation method of transition metal oxide/sulfide nano composite material |
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| Publication number | Publication date |
|---|---|
| CN100500617C (en) | 2009-06-17 |
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Granted publication date: 20090617 Termination date: 20121121 |