CN1304629C - Process for preparing nano tape and star shape nano material - Google Patents
Process for preparing nano tape and star shape nano material Download PDFInfo
- Publication number
- CN1304629C CN1304629C CNB2004100417514A CN200410041751A CN1304629C CN 1304629 C CN1304629 C CN 1304629C CN B2004100417514 A CNB2004100417514 A CN B2004100417514A CN 200410041751 A CN200410041751 A CN 200410041751A CN 1304629 C CN1304629 C CN 1304629C
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- Prior art keywords
- star
- nano
- zinc
- nano material
- wire netting
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 title abstract 2
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000005083 Zinc sulfide Substances 0.000 claims description 30
- 239000002127 nanobelt Substances 0.000 claims description 30
- 239000011701 zinc Substances 0.000 claims description 30
- 229910052725 zinc Inorganic materials 0.000 claims description 17
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 claims description 15
- 229910052980 cadmium sulfide Inorganic materials 0.000 claims description 15
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 10
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 7
- 239000005864 Sulphur Substances 0.000 claims 7
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims 1
- 239000003517 fume Substances 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 abstract description 11
- 239000002184 metal Substances 0.000 abstract description 11
- 230000035484 reaction time Effects 0.000 abstract description 3
- 230000001681 protective effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 4
- 238000000103 photoluminescence spectrum Methods 0.000 description 4
- 229910052793 cadmium Inorganic materials 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000004093 laser heating Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
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- Luminescent Compositions (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention discloses a process for rapidly preparing nano tapes and star-shaped nano material. Firstly, Zn is enwrapped in a reaction pipe by a metallic net; S is placed on one side of the Zn, and the metallic net is placed on the other side; the metallic net can be abutted with the Zn; then, protective gas is blown in from one end where the S is placed and is blown towards the metallic net; the reaction pipe is heated; heating temperature is from 750 to 1300 DEG C to make the S melt for generating steam; the metal Zn also generates the steam; after a reaction, a ZnS nano tape is obtained on the metallic net for enwrapping the Zn, and ZnS star-shaped nano material is obtained on the metallic net of the other side; when Cd is adopted for replacing the Zn, a CdS nano tape and CdS star-shaped nano material are obtained. Compared with the prior art, the present invention has the advantages of low reaction temperature, low cost and short reaction time. The present invention is the process for preparing nano tapes and star-shaped nano material, with the advantages of large economic value, practical value and wide market prospect.
Description
One, technical field
The present invention relates to a kind of method for preparing nano material, specifically a kind of quick method for preparing ZnS or CdS nano belt and star nano material.
Two, background technology
Along with the high speed development of electronics technology, the range of application of nano material more and more widely, wherein nano belt and star nano material are to make the critical material of nano-device.Generally utilize zinc sulphide (ZnS) at present, Cadmium Sulfide (CdS) powder pressing forming makes target through high-temperature calcination.Then target is put into crucible, integral body is put into the vacuum-evaporation chamber again, evaporation cavity is vacuumized, and sample is heated (electrically heated or LASER HEATING) to about 1200 ℃, and ZnS or CdS steam condense in substrate and forms nano belt, nanometer star material.For assurance obtains effect preferably, in experimentation, also need to add H sometimes
2Deng reducing gas.The shortcoming of this nano belt and star preparation of nanomaterials is: 1, with ZnS, the CdS powder is high temperature evaporation or laser splash in a vacuum, needs vacuum environment and high temperature (or laser), apparatus expensive; 2, long reaction time needs 1～4 hour usually.
Three, summary of the invention
The purpose of this invention is to provide the method for preparing ZnS or CdS nano belt and star nano material that a kind of speed of response is fast, cost is low.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method for preparing nano belt and star nano material is characterized in that it may further comprise the steps:
A) Zn or Cd are placed in the reaction tubes with the wire netting parcel, are sidelong at one of Zn or Cd and put S, place wire netting at the opposite side of Zn or Cd; Wire netting can be iron net or copper mesh; Reaction tubes can be silica tube, alundum tube or other high-temperature resistant tube; Wire netting can nestle up Zn and place.
B) shielding gas is blown in the reaction tubes from an end of placing S, and blows to wire netting; Shielding gas can be nitrogen or rare gas element.
C) reaction tubes is heated, make the S fusing, produce steam, Metal Zn also produces steam; With heating unit reaction tubes is heated, Heating temperature is 750～1300 ℃; When adopting metal Cd, Heating temperature is 300～1300 ℃.
D) through after the reaction, on the wire netting of parcel zinc, obtain the ZnS nano belt, on the opposite side wire netting, obtain ZnS star nano material; When adopting metal Cd, on the wire netting of parcel Cd, obtain the CdS nano belt, on the opposite side wire netting, obtain CdS star nano material.
In the present invention, Metal Zn also can be placed in the different reaction tubess with S, to Zn and S heating, obtains Zn steam and S steam respectively, Zn steam and S steam is mixed again, and obtains zinc sulfide nano-belt and zinc sulphide star nano material.Can directly S steam be blown in the reaction tubes at Metal Zn place during mixing, obtain nano belt and star nano material; Also S steam and Zn steam can be blown in the 3rd reaction tubes jointly, in the 3rd reaction tubes, mix, obtain nano belt and star nano material on the metallic matrix in the 3rd pipe.
The present invention utilizes S and Metal Zn; Cd makes raw material; in steam, react; temperature of reaction is 750～1300 ℃ (ZnS); 300～1300 ℃ (CdS); adopt nitrogen or protection of inert gas simultaneously and, after about 1～10 minute, obtain ZnS (CdS) nano belt and ZnS (CdS) star nano material as carrier gas.Compared with prior art, advantage of the present invention is: 1, do not need vacuum environment and high temperature, cost is low; 2, the reaction times weak point only needs the several minutes time usually.
Four, description of drawings
Fig. 1 is a synoptic diagram of the present invention;
Fig. 2 is the ZnS nano belt sem photograph that the present invention makes;
Fig. 3 is the photoluminescence spectrum of ZnS nano belt, excitation wavelength 325 nanometers;
Fig. 4 is the transmission electron microscope picture of the ZnS star nano material that makes of the present invention;
Fig. 5 is the photoluminescence spectrum of ZnS star nano material, excitation wavelength 325 nanometers.
Five, embodiment
A kind of method for preparing ZnS nano belt and star nano material of the present invention, preparation process is finished in reaction tubes, and reaction tubes is a silica tube, also can be alundum tube or other high-temperature resistant tube, may further comprise the steps:
A) an amount of S is placed on A place in the reaction tubes, Zn is placed on B place in the reaction tubes with the wire netting parcel, place wire netting at the opposite side C place of Zn; Wire netting can be the iron net; Wire netting can nestle up Zn and place.
B) with shielding gas N
2Blow to the C place of placing wire netting from the A that places S; Shielding gas also can be a rare gas element.
C) with heating unit reaction tubes is heated, Heating temperature is 1000 ℃, makes the S fusing, produces steam, and Metal Zn also produces steam; Regulate the temperature at A place, make that the quantity of steam of the steam of S and Metal Zn is suitable.When adopting metal Cd, Heating temperature is 800 ℃ and gets final product.
D) after reaction after a while (about 5 minutes) obtain a large amount of ZnS nano belt on the wire netting at B place, obtain a large amount of ZnS star nano materials on the wire netting at C place.When adopting metal Cd, on the wire netting of parcel Cd, obtain the CdS nano belt, on the opposite side wire netting, obtain CdS star nano material.
The sem photograph of the ZnS nano belt that is obtained by above preparation method is seen accompanying drawing 2, and the photoluminescence spectrum of this ZnS nano belt is seen accompanying drawing 3.The ZnS star nano material that obtains transmission electron microscope picture see accompanying drawing 4, the photoluminescence spectrum of this ZnS star nano material is seen accompanying drawing 5.ZnS nano belt and ZnS star nano material are to make the critical material of nano-device, are widely used in making fluorescent material simultaneously.
Claims (7)
1, a kind of method for preparing nano belt and star nano material is characterized in that it may further comprise the steps:
A) metallic zinc is placed in the reaction tubes with the wire netting parcel, is sidelong at one of zinc and puts sulphur, place wire netting at the opposite side of zinc;
B) shielding gas is blown in the reaction tubes from an end of placing sulphur, and blows to wire netting;
C) reaction tubes is heated, make the sulphur fusing, produce steam, metallic zinc also produces steam;
D) through after the reaction, on the wire netting of parcel zinc, obtain zinc sulfide nano-belt, on the opposite side wire netting, obtain zinc sulphide star nano material.
2, the method for preparing nano belt and star nano material according to claim 1 is characterized in that: in steps A) in, wire netting can be iron net or copper mesh; Reaction tubes can be silica tube, alundum tube or other high-temperature resistant tube.
3, the method for preparing nano belt and star nano material according to claim 1 is characterized in that: in steps A) in, the wire netting of opposite side nestles up zinc and places.
4, the method for preparing nano belt and star nano material according to claim 1 is characterized in that: step B), shielding gas can be nitrogen or rare gas element.
5, the method for preparing nano belt and star nano material according to claim 1 is characterized in that: at step C) in, with heating unit reaction tubes being heated, Heating temperature is 750～1300 ℃.
6, the method for preparing nano belt and star nano material according to claim 1 is characterized in that: in steps A) in, metallic zinc can replace with cadmium metal; At step C) in Heating temperature be 300～1300 ℃; At step D) in obtain the cadmium sulfide nano band, on the opposite side wire netting, obtain Cadmium Sulfide star nano material.
7, the method for preparing nano belt and star nano material according to claim 1 is characterized in that: in steps A) in, metallic zinc and wire netting are placed in the reaction tubes, and sulphur is placed in another reaction tubes; At step C) in, respectively metallic zinc and sulphur are heated, produce zinc and sulphur steam, and sulphur steam is blown in the reaction tubes at metallic zinc place and mixes with zinc fume; At step D) in obtain zinc sulfide nano-belt and zinc sulphide star nano material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100417514A CN1304629C (en) | 2004-08-20 | 2004-08-20 | Process for preparing nano tape and star shape nano material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100417514A CN1304629C (en) | 2004-08-20 | 2004-08-20 | Process for preparing nano tape and star shape nano material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1598043A CN1598043A (en) | 2005-03-23 |
| CN1304629C true CN1304629C (en) | 2007-03-14 |
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|---|---|---|---|
| CNB2004100417514A Expired - Fee Related CN1304629C (en) | 2004-08-20 | 2004-08-20 | Process for preparing nano tape and star shape nano material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104659652B (en) * | 2015-02-13 | 2017-11-10 | 湖南大学 | A kind of wavy nanobelt and the nano laser array preparation method based on wavy nanobelt |
| CN105177499B (en) * | 2015-05-22 | 2018-02-06 | 许昌学院 | A kind of quantum dot is the thermal evaporation that forerunner prepares near-stoichiometric CdS film |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1256170A (en) * | 1998-12-04 | 2000-06-14 | 中国科学院大连化学物理研究所 | Nanometer-level TiO2 photocatalyst carried by metal net and its preparation |
| US20040000266A1 (en) * | 2002-06-27 | 2004-01-01 | D'evelyn Mark Philip | Method for reducing defect concentrations in crystals |
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- 2004-08-20 CN CNB2004100417514A patent/CN1304629C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1256170A (en) * | 1998-12-04 | 2000-06-14 | 中国科学院大连化学物理研究所 | Nanometer-level TiO2 photocatalyst carried by metal net and its preparation |
| US20040000266A1 (en) * | 2002-06-27 | 2004-01-01 | D'evelyn Mark Philip | Method for reducing defect concentrations in crystals |
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| Publication number | Publication date |
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| CN1598043A (en) | 2005-03-23 |
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