CN101323975B - Preparation of SnO2Method for preparing -ZnO heterogeneous nano branch structure - Google Patents
Preparation of SnO2Method for preparing -ZnO heterogeneous nano branch structure Download PDFInfo
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- CN101323975B CN101323975B CN2008101166244A CN200810116624A CN101323975B CN 101323975 B CN101323975 B CN 101323975B CN 2008101166244 A CN2008101166244 A CN 2008101166244A CN 200810116624 A CN200810116624 A CN 200810116624A CN 101323975 B CN101323975 B CN 101323975B
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- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 39
- 239000002070 nanowire Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000002086 nanomaterial Substances 0.000 claims abstract description 8
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 33
- 239000000843 powder Substances 0.000 claims description 32
- 239000002994 raw material Substances 0.000 claims description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 27
- 239000007789 gas Substances 0.000 claims description 19
- 230000012010 growth Effects 0.000 claims description 18
- 229910052573 porcelain Inorganic materials 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 15
- 239000012159 carrier gas Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 2
- 239000004065 semiconductor Substances 0.000 abstract description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 abstract description 3
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 238000002207 thermal evaporation Methods 0.000 abstract description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 238000007740 vapor deposition Methods 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 14
- 229910052786 argon Inorganic materials 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 238000001239 high-resolution electron microscopy Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000000739 chaotic effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000010897 surface acoustic wave method Methods 0.000 description 1
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Abstract
The invention belongs to the technical field of preparation of nano oxide semiconductor material heterostructure, and particularly relates to preparation of SnO with special morphology2-ZnO heterogeneous nanometer branch structure. The invention relates to a method for preparing a heterogeneous nano structure by adopting two-step vapor deposition. With Al2O3The substrate is a substrate, and Al is formed on the substrate by gas transmission and two-step thermal evaporation2O3Growing on a substrate to obtain SnO2-ZnO heterogeneous nano branch structure. The heterogeneous nano branch structure is SnO2The ZnO is taken as a branch in the radial direction, and the angle formed by two adjacent radial ZnO nanowires is 68-73 degrees. The obtained heterogeneous nano branch structure has stable shape and good quality, and has application prospect in the aspect of photoelectric devices.
Description
Technical field
The invention belongs to nanometer oxide semiconductor material heterojunction structure preparing technical field, particularly the SnO of preparation special appearance
2The method of-ZnO alloplasm nanobranch.
Background technology
ZnO is a kind of semi-conductor, piezoelectricity, photoconductive material of important broad stopband (3.37eV), has a wide range of applications in feds, solar cell, opto-electronic device and surface acoustic wave field such as lead.SnO
2Be a kind of typical semi-conductor type metal oxide, its energy gap is 3.16eV (300K).SnO
2One dimension Nano structures such as nano wire are little owing to its size on two dimensions, thereby have very high specific surface area, and its chemisorption power and catalytic capability all significantly strengthen, and its energy band structure also has more novel characteristics than its body material simultaneously.Both heterojunction structures, SnO
2The expection of-ZnO nano heterojunction can demonstrate some superior performances.Have unique photoelectric property and potential using value.Because the character of nano material depends on its microstructure sensitively, therefore in process of growth, control SnO better
2With the growth of ZnO monodimension nanometer material, good and have the one-dimensional nano heterogeneous knot material of ad hoc structure to obtain quality, in concrete application, having very important significance.
The existing SnO for preparing
2-ZnO heterojunction structure has shell structure (Weidong Yu, Xiaomin Li, Xiangdong Gao, and Feng Wu, J.Phys.Chem.B 2005,109,17078～17081), parallel nano belt structure (Jianwei Zhao, Changhui Ye, Xiaosheng Fang, Lirong Qin, andLide Zhang, Crystal Growth and Design, 2006,6,2643～2647) etc., these nanostructures do not have the fixed direction, chaotic has limited the application of material on nano-device.
Summary of the invention
The purpose of this invention is to provide a kind of SnO for preparing special appearance
2The method of-ZnO alloplasm nanobranch.
Preparation SnO of the present invention
2The method of-ZnO alloplasm nanobranch may further comprise the steps:
1) with raw material SnO
2Powder and raw material Graphite Powder 99 are to mix and ground in 1: 5～5: 1 by the mol ratio of material, are to mix and ground in 1: 5～5: 1 raw material ZnO powder and raw material Graphite Powder 99 by the mol ratio of material; Above-mentioned mole with raw material graphite is a benchmark;
2) the raw material SnO that step 1) is obtained
2The mixture of powder and raw material Graphite Powder 99 is put into porcelain boat, then porcelain boat is placed on the middle part of tube furnace;
3) with Al
2O
3Substrate is tiled in step 2) the tube furnace downstream far from middle part 5～20cm place, as SnO
2The substrate of nanostructure growth;
4) tube furnace with step 3) is heated to 800～1000 ℃, and heat-up rate is at 10～30 ℃/min;
5) rare gas element and air are fed in the tube furnace of step 4) as carrier gas, the flow of rare gas element is 10～100sccm, and the flow of air is 2～10sccm; Pressure in the tube furnace is 50～500Pa, keeps 30～60 minutes, and reaction naturally cools to room temperature after finishing, and takes out Al
2O
3Substrate;
6) the raw material ZnO powder that step 1) is obtained and the mixture of raw material Graphite Powder 99 are put into porcelain boat, then porcelain boat are placed on the middle part of tube furnace; Al with the step 5) taking-up
2O
3Substrate is tiled in the tube furnace downstream far from middle part 5～20cm place, as the substrate of ZnO nanostructure growth;
7) tube furnace with step 6) is heated to 900～1100 ℃, and heat-up rate is at 10～30 ℃/min;
8) rare gas element and air are fed in the tube furnace of step 7) as carrier gas, the flow of rare gas element is 10～100sccm, and the flow of air is 2～10sccm; Pressure in the tube furnace is 50～5000Pa, keeps 20～90 minutes, and reaction naturally cools to room temperature after finishing, and takes out Al
2O
3Substrate, Al
2O
3White lint shape product above the substrate is SnO
2-ZnO alloplasm nanobranch; Wherein said SnO
2The axial of the alloplasm nanobranch of-ZnO is SnO
2Nano wire radially is the ZnO nano wire.
The SnO that the present invention prepares
2The axial SnO of the alloplasm nanobranch of-ZnO
2The radius of nano wire is about 40nm～150nm, and (length is 1um～5um) to length in micron dimension; Radially the radius of ZnO nano wire is at 20nm～150nm, preferably at 20～100nm; Length is at 50nm～2um, preferably at 50nm～200nm, adjacent two radially ZnO nano wire angulation at 68 °～73 °.
Described raw material SnO
2The particle diameter of powder is 0.5um～100um, and purity is 99.99%.
The particle diameter of described raw material Graphite Powder 99 is 1um～30um, and purity is 99.99%.
The particle diameter of described raw material ZnO powder is 0.5um～100um, and purity is 99.99%.
Described rare gas element is an argon gas etc.
The present invention utilizes tube furnace, prepares SnO with two methods that go on foot thermal evaporations
2The alloplasm nanobranch of-ZnO, the preparation method is simple, obtains a kind of nano-heterogeneous structure of specific morphology, the pure and good stability of pattern.Characterize by high resolution and to verify that radially nano wire is a ZnO structure and along the growth of (0001) direction, the high resolution photo that obtains as shown in Figure 1, axially nano wire is SnO
2Structure and edge (101) direction growth, the high resolution photo that obtains as shown in Figure 2.
The SnO that the inventive method prepares
2There is application prospect emission on the scene of-ZnO alloplasm nanobranch and photoelectric device aspect.
Description of drawings
Fig. 1. the embodiment of the invention 1,2 and 3 SnO
2In-ZnO the alloplasm nanobranch radially the ZnO nano wire choose the high-resolution electron microscopy photo.
Fig. 2. the embodiment of the invention 1,2 and 3 SnO
2Axial SnO in the-ZnO alloplasm nanobranch
2Nano wire is chosen the high-resolution electron microscopy photo.
Fig. 3. the SnO of the embodiment of the invention 1
2The stereoscan photograph of-ZnO alloplasm nanobranch.
Fig. 4. the SnO of the embodiment of the invention 2
2The stereoscan photograph of-ZnO alloplasm nanobranch.
Fig. 5. the SnO of the embodiment of the invention 3
2The transmission electron microscope photo of-ZnO alloplasm nanobranch.
Embodiment
Embodiment 1.
Raw materials used purity is 99.99%; SnO
2The particle diameter of powder is 0.5um～100um, and the particle diameter of Graphite Powder 99 is 1um～30um, and the particle diameter of ZnO powder is 0.5um～100um.With 0.1mol SnO
2Powder and 0.5mol Graphite Powder 99 mix and also grind evenly, 0.1mol ZnO powder and 0.5mol Graphite Powder 99 are mixed and grind evenly, put into two porcelain boats respectively, with porcelain boat one (0.1mol SnO
2Powder and 0.5mol Graphite Powder 99 mix) put into the tube furnace middle part, with Al
2O
3Substrate is tiled in the tube furnace downstream apart from 5～20cm place, stove middle part, as the substrate of nanowire growth; Feed flow and be the argon gas of 100sccm and air that flow is 10sccm as carrier gas, keep air pressure at 500Pa, keeping heat-up rate is 10 ℃/min, keeps cooling naturally after 60 minutes, taking-up Al to 800 ℃
2O
3Substrate.The porcelain boat two that ZnO powder and Graphite Powder 99 are housed is placed on the tube furnace middle part, with the Al that takes out
2O
3Substrate is placed on the tube furnace downstream apart from the growth substrate of 5～20cm place, stove middle part as the reaction of second step, feed flow and be the argon gas of 100sccm and air that flow is 10sccm as carrier gas, keep the stove internal gas pressure at 50Pa, the speed that with heat-up rate is 10 ℃/min is warmed up to 900 ℃ of growths 20 minutes with temperature, treats that system cooling back takes out Al
2O
3Substrate is at Al
2O
3Obtain SnO above the substrate
2-ZnO heterojunction nanowire structure, the product electromicroscopic photograph as shown in Figure 3.The product pattern is illustrated in figure 3 as branch structure, SnO
2Axial SnO2 nano wire radius in the-ZnO alloplasm nanobranch is at 100～150nm, length 2～5um, radially the radius of ZnO nano wire is at 100～150nm, and length is 50～150nm, adjacent two radially ZnO nano wire angulation at 68 °～73 °, as shown in Figure 3.
Raw materials used purity is 99.99%; SnO
2The particle diameter of powder is 0.5um～100um, and the particle diameter of Graphite Powder 99 is 1um～30um, and the particle diameter of ZnO powder is 0.5um～100um, with 0.5mol SnO
2Powder and 0.1mol Graphite Powder 99 mix and also grind evenly, 0.5mol ZnO powder and 0.1mol Graphite Powder 99 are mixed and grind evenly, put into two porcelain boats respectively, with porcelain boat one (0.1mol SnO
2Powder and 0.5mol Graphite Powder 99 mix) put into the tube furnace middle part, with Al
2O
3Substrate is tiled in the tube furnace downstream apart from 5～20cm place, stove middle part, as the substrate of nanowire growth; Feed flow and be the argon gas of 50sccm and air that flow is 5sccm as carrier gas, keep air pressure at 50Pa, keeping heat-up rate is 30 ℃/min, keeps cooling naturally after 30 minutes, taking-up Al to 1000 ℃
2O
3Substrate.The porcelain boat two that ZnO powder and Graphite Powder 99 are housed is pushed into the tube furnace middle part, with the Al that takes out
2O
3Substrate is placed on the tube furnace downstream apart from the growth substrate of 5～20cm place, stove middle part as the reaction of second step, feed flow and be the argon gas of 50sccm and air that flow is 5sccm as carrier gas, keep the stove internal gas pressure at 100Pa, the speed that with heat-up rate is 20 ℃/min is warmed up to 950 ℃ of growths 90 minutes with temperature, treats that system cooling back takes out Al
2O
3Substrate is at Al
2O
3Obtain SnO above the substrate
2-ZnO heterojunction nanowire structure, the product electromicroscopic photograph as shown in Figure 4.The product pattern is illustrated in figure 4 as branch structure, SnO
2Axial SnO in the-ZnO alloplasm nanobranch
2The nano wire radius is at 40～60nm, length 2～5um, radially ZnO nano wire radius is at 20～50nm, length is 1～2um, adjacent two radially ZnO nano wire angulation at 70 °, as shown in Figure 4.
Embodiment 3.
Raw materials used purity is 99.99%; SnO
2The particle diameter of powder is 0.5um～100um, and the particle diameter of Graphite Powder 99 is 1um～30um, and the particle diameter of ZnO powder is 0.5um～100um, with 0.1mol SnO
2Powder and 0.5mol Graphite Powder 99 mix and also grind evenly, 0.1mol ZnO powder and 0.4mol Graphite Powder 99 are mixed and grind evenly, put into two porcelain boats respectively, with porcelain boat one (0.1mol SnO
2Powder and 0.5mol Graphite Powder 99 mix) put into the tube furnace middle part, with Al
2O
3Substrate is tiled in the tube furnace downstream apart from 5～20cm place, stove middle part, as the substrate of nanowire growth; Feed flow and be the argon gas of 10sccm and air that flow is 2sccm as carrier gas, keep air pressure at 50Pa, keeping heat-up rate is 20 ℃/min, keeps cooling naturally after 60 minutes, taking-up Al to 1000 ℃
2O
3Substrate.The porcelain boat two that ZnO powder and Graphite Powder 99 are housed is pushed into the tube furnace middle part, with the Al that takes out
2O
3Substrate is placed on the tube furnace downstream apart from the growth substrate of 5～20cm place, stove middle part as the reaction of second step, feed flow and be the argon gas of 10sccm and air that flow is 2sccm as carrier gas, keep the stove internal gas pressure at 5000Pa, the speed that with heat-up rate is 30 ℃/min is warmed up to 1100 ℃ of growths 30 minutes with temperature, treats that system cooling back takes out Al
2O
3Substrate is at Al
2O
3Obtain SnO above the substrate
2-ZnO heterojunction nanowire structure, the product electromicroscopic photograph as shown in Figure 5.The product pattern is the branch structure as shown in Figure 5, SnO
2Axial SnO in the-ZnO alloplasm nanobranch
2The nano wire radius is at 40～60nm, length 2～5um, radially the radius of ZnO nano wire is at 30～50nm, length is 100～200nm, adjacent two radially ZnO nano wire angulation at 68 °～73 °, as shown in Figure 5.
Claims (10)
1. one kind prepares SnO
2The method of-ZnO alloplasm nanobranch is characterized in that, this method may further comprise the steps:
1) with raw material SnO
2Powder and raw material Graphite Powder 99 are to mix and ground in 1: 5～5: 1 by the mol ratio of material, are to mix and ground in 1: 5～5: 1 raw material ZnO powder and raw material Graphite Powder 99 by the mol ratio of material; Above-mentioned mole with raw material graphite is a benchmark;
2) the raw material SnO that step 1) is obtained
2The mixture of powder and raw material Graphite Powder 99 is put into porcelain boat, then porcelain boat is placed on the middle part of tube furnace;
3) with Al
2O
3Substrate is tiled in step 2) the tube furnace downstream far from middle part 5～20cm place, as SnO
2The substrate of nanostructure growth;
4) tube furnace with step 3) is heated to 800～1000 ℃, and heat-up rate is at 10～30 ℃/min;
5) rare gas element and air are fed in the tube furnace of step 4) as carrier gas, the flow of rare gas element is 10～100sccm, and the flow of air is 2～10sccm; Pressure in the tube furnace is 50～500Pa, and reaction naturally cools to room temperature after finishing, and takes out Al
2O
3Substrate;
6) the raw material ZnO powder that step 1) is obtained and the mixture of raw material Graphite Powder 99 are put into porcelain boat, then porcelain boat are placed on the middle part of tube furnace; Al with the step 5) taking-up
2O
3Substrate is tiled in the tube furnace downstream far from middle part 5～20cm place, as the substrate of ZnO nanostructure growth;
7) tube furnace with step 6) is heated to 900～1100 ℃, and heat-up rate is at 10～30 ℃/min;
8) rare gas element and air are fed in the tube furnace of step 7) as carrier gas, the flow of rare gas element is 10～100sccm, and the flow of air is 2～10sccm; Pressure in the tube furnace is 50～5000Pa, and reaction naturally cools to room temperature after finishing, and takes out Al
2O
3Substrate, Al
2O
3Product above the substrate is SnO
2-ZnO alloplasm nanobranch; Wherein said SnO
2The axial of the alloplasm nanobranch of-ZnO is SnO
2Nano wire radially is the ZnO nano wire.
2. method according to claim 1 is characterized in that: when the pressure in the step 5) tube furnace is 50～500Pa, keep 30～60 minutes reaction times.
3. method according to claim 1 is characterized in that: when the pressure in the step 8) tube furnace is 50～5000Pa, keep 20～90 minutes reaction times.
4. method according to claim 1 is characterized in that: described axial SnO
2The radius of nano wire is at 40nm～150nm, and length is 1 μ m～5 μ m.
5. method according to claim 1 is characterized in that: the radius of described radially ZnO nano wire is at 20～150nm, and length is at 50nm～2 μ m.
6. method according to claim 1 or 5 is characterized in that: SnO
2In-ZnO the alloplasm nanobranch adjacent two radially ZnO nano wire angulation at 68 °～73 °.
7. method according to claim 1 is characterized in that: axial SnO
2The radius of nano wire is at 40nm～150nm, and length is 1 μ m～5 μ m; Radially the radius of ZnO nano wire is at 20～150nm, and length is at 50nm～2 μ m, adjacent two radially ZnO nano wire angulation at 68 °～73 °.
8. method according to claim 1 is characterized in that: described raw material SnO
2The particle diameter of powder is 0.5 μ m～100 μ m; The particle diameter of described raw material ZnO powder is 0.5 μ m～100 μ m.
9. method according to claim 1 is characterized in that: the particle diameter of described raw material Graphite Powder 99 is 1 μ m～30 μ m, and purity is 99.99%.
10. according to claim 1 or 8 described methods, it is characterized in that: described raw material SnO
2The purity of powder or raw material ZnO powder is 99.99%.
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| CN102504816B (en) * | 2011-11-08 | 2014-05-07 | 浙江天旭科技有限公司 | Method for preparing nano luminescent material ZnO/SnO2 heterostructure |
| CN102618849B (en) * | 2012-03-15 | 2013-07-10 | 中国科学院理化技术研究所 | One-dimensional ZnO/SnO2Preparation method of core-shell structure nano heterojunction semiconductor material |
| CN106082314B (en) * | 2016-06-08 | 2017-08-25 | 济南大学 | A kind of method that porous SnO 2 nanotube is grown in conductive substrates |
| CN109119511B (en) * | 2018-07-24 | 2020-04-24 | 大连理工大学 | Preparation method of ultraviolet light detector with nanorod array heterojunction structure |
| CN109382087B (en) * | 2018-11-23 | 2021-06-25 | 西南交通大学 | Tin dioxide-zinc stannate core-shell nanowire and preparation method thereof |
| CN109950519B (en) * | 2019-03-13 | 2022-04-19 | 河源广工大协同创新研究院 | Positive electrode material of lithium-sulfur primary battery and preparation method of positive electrode material |
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Non-Patent Citations (4)
| Title |
|---|
| s.h.sun等.Large-scale synthesis of SnO2 nanobelts.《Applied Physics A –Materials Science & Processing》.2003,第76卷287-289. * |
| Shuhui Sun等.Controlled Growth and Optical Properties of One-Dimensional ZnO Nanostructures on SnO2 Nanobelts.《Crystal Growth & Design》.2007,第7卷(第10期),1988-1991. * |
| Shuhui Sun等.Controlled Growth of SnO2 Hierarchical Nanostructures by a Multistep Thermal Vapor Deposition Process.《Chem. Eur. J》.2007,第13卷9087-9092. * |
| Tianjun Sun等.Controllable Fabrication and Photocatalytic Activity of ZnO Nanobelt Arrays.《J. Phys. Chem. C》.2007,第112卷715-721. * |
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