CN106591949A - Method and device for preparing monocrystal Ag-doped zinc oxide hexagonal micro tube by vapor deposition - Google Patents
Method and device for preparing monocrystal Ag-doped zinc oxide hexagonal micro tube by vapor deposition Download PDFInfo
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- CN106591949A CN106591949A CN201611036808.0A CN201611036808A CN106591949A CN 106591949 A CN106591949 A CN 106591949A CN 201611036808 A CN201611036808 A CN 201611036808A CN 106591949 A CN106591949 A CN 106591949A
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- tube
- zinc
- micron
- oxides
- doping
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000007740 vapor deposition Methods 0.000 title abstract 3
- 235000014692 zinc oxide Nutrition 0.000 claims description 31
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 20
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 claims description 17
- 239000003708 ampul Substances 0.000 claims description 15
- 239000010453 quartz Substances 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000000919 ceramic Substances 0.000 claims description 13
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- 239000010703 silicon Substances 0.000 claims description 13
- 229960001296 zinc oxide Drugs 0.000 claims description 12
- 230000008021 deposition Effects 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910001960 metal nitrate Inorganic materials 0.000 claims description 2
- 239000011812 mixed powder Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 4
- 239000007787 solid Substances 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 2
- 125000003821 2-(trimethylsilyl)ethoxymethyl group Chemical group [H]C([H])([H])[Si](C([H])([H])[H])(C([H])([H])[H])C([H])([H])C(OC([H])([H])[*])([H])[H] 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000001198 high resolution scanning electron microscopy Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002063 nanoring Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/66—Crystals of complex geometrical shape, e.g. tubes, cylinders
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Geometry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a method for preparing a monocrystal Ag-doped zinc oxide hexagonal micro tube at low cost and with good controllability by vapor deposition, and also aims at providing a device for preparing a monocrystal Ag-doped zinc oxide hexagonal micro tube by vapor deposition. The technical scheme provided by the invention is as follows: a monocrystal-doped zinc oxide tubular micro-nano structure is obtained by utilizing a tubular resistance furnace and applying a method with combination of vertical flow phase change reaction and gas-liquid-solid crystal growth mechanism, and the tube is characterized in that Ag is doped in the hexagonal micro tube and has the doping quantity accounting for 2%mol of zinc oxide, the hexagonal micro tube is of a monocrystal structure, the Ag-doped zinc oxide hexagonal micro tube has the length of a dozen micrometers, the length of each side of a hexagonal prism is 1.5 microns, and the tube diameter is 1 micron.
Description
Technical field：
The present invention relates to low-dimension nano material and nanotechnology, especially six side's micron of vapour deposition monocrystalline Ag doping zinc-oxides
The method and device of pipe.
Background technology：
Semiconductor nano material has on various photoelectric devices and is widely applied very much prospect due to its unique physical characteristic.Directly
Tape splicing gap semiconductor ZnO, band-gap energy are 3.37 eV, and big combination can be 60 meV, with important application prospect, are constructions
The material of hetero-junctions or superlattices, it is possible to obtain high performance laser diode and light emitting diode device, thus cause
It is extensive to pay close attention to.The ZnO of various patterns is successfully prepared out, such as：Nano wire, nano belt, nanotube, nano-rings etc.
Deng.As nano material has small yardstick, the features such as not easy to operate, cause the assembly cost of nano-device very high.
The content of the invention：
It is an object of the invention to provide six side's micron tube of vapour deposition monocrystalline Ag doping zinc-oxides that cost is relatively low, controllability is good
Method；It is a further object of the present invention to provide vapour deposition prepares the device of six side's micron tube of monocrystalline Ag doping zinc-oxides.
The present invention provide technical scheme be：Using a kind of tube type resistance furnace, with vertical rheological phase reaction and solution-air-
Gu the method that Crystal Growth Mechanism combines, obtains a kind of tubulose micro-nano structure of single-crystal doped Zinc Oxide, is characterized in this
Doped with silver in six side's micron tube, 2% mol of the doping for Zinc Oxide, six side's micron tube are mono-crystalline structures, and described Ag mixes
Six side's micron tube of miscellaneous Zinc Oxide, length of tube are more than ten micron, 1.5 μm of the hexagonal prism length of side, and caliber is 1 μm.
Method of the present invention step is：
The zinc nitrate of 0.01 mol and the silver nitrate mixing for doping, 5% mol of the combined amount for zinc nitrate are mixed by the first step
Powder after conjunction forms zinc nitrate solution in being dissolved into the deionized water of 50 ml, add the citric acid of 0.03 mol in the solution
With the ethylene glycol of 6.6 ml, the mixed solution of preparation obtains colloidal sol in 1 hour in 80 DEG C of stirrings, next permanent under the conditions of 150 DEG C
Temperature obtains gel in 8 hours；The gel of preparation is cracked in 400 DEG C of constant temperature for 1 hour, obtains unbodied C-Zn-O-Ag compound precursors
Body, is smashed with mortar standby.
The powdered product that the first step is obtained by second step is moved in ceramic boat, is heated up in the quartz ampoule of tube type resistance furnace,
Programming rate is 15 DEG C/min, is heated to 950 DEG C, constant temperature 2 hours, then rapid to lower the temperature；Collected as substrate with silicon chip and prepared
Product, while being passed through nitrogen as carrier gas；The Ag doping zinc-oxide six side micron tube of three-dimensional is obtained on silicon chip,
2% mol of the Ag dopings of six side's micron tube of Ag doping zinc-oxides for Zinc Oxide.
The method of the present invention is realized with following device：
The device of the present invention is made up of tube type resistance furnace, ceramic boat, silicon chip and quartz ampoule, has stone in the centre of tube type resistance furnace
Ying Guan, the high-temperature region of quartz ampoule are placed with ceramic boat, and the relatively low warm area of quartz ampoule is placed with silicon chip；There is reaction precursor in ceramic boat
Body.
Described doped zinc oxide nano brush is monocrystalline state.
Method of the present invention process is simple, low for equipment requirements, controllable degree is high, is six side's micron of single-crystal doped Zinc Oxide
The standby good method of control is become reconciled device.
Description of the drawings：
Fig. 1 be the present invention schematic device, 1. tube type resistance furnace, 2. ceramic boat, 3. silicon chip, 4. quartz ampoule in figure
5. precursors.
Low power scanning electron microscope (SEM) photograph SEMs of the Fig. 2 for product.
Fig. 3 is high resolution scanning electron microscope HRSEM of single six sides micron tube.
Fig. 4 is constituency composition energy spectrum diagram EDS in single six sides micron tube.
Fig. 5 is the x-ray diffraction pattern XRD of the six side's micron tube of Ag doping zinc-oxides for preparing.
Specific embodiment：
The method that embodiment 1, vapour deposition prepares six side's micron tube of monocrystalline Ag doping zinc-oxides, the first step is by the nitre of 0.01 mol
Sour zinc and the silver nitrate mixing for doping, 5% mol of the combined amount for zinc nitrate, mixed powder are dissolved into 50 ml's
Zinc nitrate solution is formed in deionized water, the ethylene glycol of the citric acid and 6.6 ml of 0.03 mol is added in the solution, preparation
Mixed solution obtains colloidal sol in 1 hour in 80 DEG C of stirrings, and next under the conditions of 150 DEG C, constant temperature obtains gel in 8 hours；What is prepared is solidifying
Glue is cracked in 400 DEG C of constant temperature for 1 hour, is obtained unbodied C-Zn-O-Ag composite precursors, is smashed with mortar standby.
The powdered product that the first step is obtained by second step is moved in ceramic boat, middle in the quartz ampoule of tube type resistance furnace to rise
Temperature, programming rate are 15 DEG C/min, are heated to 950 DEG C, constant temperature 2 hours, then rapid to lower the temperature；With metal spraying silicon chip as substrate
The product for preparing is collected, while nitrogen is passed through as carrier gas；The Ag doping zinc-oxide six of three-dimensional is obtained on silicon chip
Square micron tube, the Ag dopings of six side's micron tube of Ag doping zinc-oxides are 2% mol of Zinc Oxide.
The purity of embodiment 2, zinc nitrate> 98%.
The purity of embodiment 3, metal nitrate silver> 98%.
Embodiment 4, six side's micron tube of Ag doping zinc-oxides, length of tube are more than ten micron, 1.5 μm of the hexagonal prism length of side,
Caliber is 1 μm.
Embodiment 5, six side's micron tube of Ag doping zinc-oxides are monocrystalline state.
Embodiment 6, the device of the present invention are made up of tube type resistance furnace 1, ceramic boat 2, silicon chip 3 and quartz ampoule 4, in tubular type
The high-temperature region that there is quartz ampoule 4, quartz ampoule 4 centre of resistance furnace 1 is placed with ceramic boat 2, and the relatively low warm area of quartz ampoule 4 is placed with silicon
Piece 3；There are precursors 5 in ceramic boat 2.
Claims (6)
1. the method for six side's micron tube of vapour deposition monocrystalline Ag doping zinc-oxides, is characterized in that：The first step is by 0.01 mol's
Zinc nitrate and the silver nitrate mixing for doping, 5% mol of the combined amount for zinc nitrate, mixed powder are dissolved into 50 ml
Deionized water in form zinc nitrate solution, add the ethylene glycol of the citric acid and 6.6 ml of 0.03 mol in the solution, prepare
Mixed solution obtain colloidal sol within 1 hour in 80 DEG C of stirrings, next under the conditions of 150 DEG C, constant temperature obtains gel in 8 hours；Prepare
Gel is cracked in 400 DEG C of constant temperature for 1 hour, is obtained unbodied C-Zn-O-Ag composite precursors, is smashed with mortar standby；
The powdered product that the first step is obtained by second step is moved in ceramic boat, middle in the quartz ampoule of tube type resistance furnace to heat up, and is risen
Warm speed is 15 DEG C/min, is heated to 950 DEG C, constant temperature 2 hours, then rapid to lower the temperature；Collected as substrate with metal spraying silicon chip and made
Standby product, while being passed through nitrogen as carrier gas；The Ag doping zinc-oxide six side micron of three-dimensional is obtained on silicon chip
Pipe, the Ag dopings of six side's micron tube of Ag doping zinc-oxides are 2% mol of Zinc Oxide.
2. the method for six side's micron tube of vapour deposition monocrystalline Ag doping zinc-oxides according to claim 1, is characterized in that：
The purity of zinc nitrate> 98%.
3. the method for six side's micron tube of vapour deposition monocrystalline Ag doping zinc-oxides according to claim 1, is characterized in that：
The purity of metal nitrate silver> 98%.
4. the method for six side's micron tube of vapour deposition monocrystalline Ag doping zinc-oxides according to claim 1, is characterized in that：Ag
Six side's micron tube of doping zinc-oxide, length of tube are more than ten micron, 1.5 μm of the hexagonal prism length of side, and caliber is 1 μm.
5. according to claim 1 or 4 six side's micron tube of vapour deposition monocrystalline Ag doping zinc-oxides method, its feature
It is：Six side's micron tube of Ag doping zinc-oxides is monocrystalline state.
6. a kind of device of such as Claims 1 to 5 any one methods described, is characterized in that：By tube type resistance furnace（1）, ceramic boat
（2）, silicon chip（3）And quartz ampoule（4）Composition, in tube type resistance furnace（1）Centre have quartz ampoule（4）, quartz ampoule（4）High-temperature region
It is placed with ceramic boat（2）, quartz ampoule（4）Relatively low warm area is placed with silicon chip（3）；Ceramic boat（2）Inside there are precursors（5）.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611036808.0A CN106591949A (en) | 2016-11-23 | 2016-11-23 | Method and device for preparing monocrystal Ag-doped zinc oxide hexagonal micro tube by vapor deposition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611036808.0A CN106591949A (en) | 2016-11-23 | 2016-11-23 | Method and device for preparing monocrystal Ag-doped zinc oxide hexagonal micro tube by vapor deposition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106591949A true CN106591949A (en) | 2017-04-26 |
Family
ID=58592699
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611036808.0A Pending CN106591949A (en) | 2016-11-23 | 2016-11-23 | Method and device for preparing monocrystal Ag-doped zinc oxide hexagonal micro tube by vapor deposition |
Country Status (1)
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| CN (1) | CN106591949A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594670A (en) * | 2003-09-09 | 2005-03-16 | 电子科技大学 | Preparation method for C-axis preferred orientation single crystal ZnO hexagonus microtubule |
| CN101445960A (en) * | 2008-09-23 | 2009-06-03 | 河南大学 | Method for preparing adulteration monocrystalline zinc oxide nanometer brush by vapour deposition and device thereof |
| CN101445265A (en) * | 2008-09-23 | 2009-06-03 | 河南大学 | Method for preparing adulteration monocrystalline zinc oxide nanometer screwdriver by vapour deposition and device thereof |
| US20120314726A1 (en) * | 2009-12-23 | 2012-12-13 | Dongguk University Industry-Academic Cooperation Foundation | Laser diode using zinc oxide nanorods and manufacturing method thereof |
| CN105220229A (en) * | 2015-11-06 | 2016-01-06 | 中国科学院理化技术研究所 | A kind of preparation method of TiO2 monocrystal nano pipe array |
-
2016
- 2016-11-23 CN CN201611036808.0A patent/CN106591949A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594670A (en) * | 2003-09-09 | 2005-03-16 | 电子科技大学 | Preparation method for C-axis preferred orientation single crystal ZnO hexagonus microtubule |
| CN101445960A (en) * | 2008-09-23 | 2009-06-03 | 河南大学 | Method for preparing adulteration monocrystalline zinc oxide nanometer brush by vapour deposition and device thereof |
| CN101445265A (en) * | 2008-09-23 | 2009-06-03 | 河南大学 | Method for preparing adulteration monocrystalline zinc oxide nanometer screwdriver by vapour deposition and device thereof |
| US20120314726A1 (en) * | 2009-12-23 | 2012-12-13 | Dongguk University Industry-Academic Cooperation Foundation | Laser diode using zinc oxide nanorods and manufacturing method thereof |
| CN105220229A (en) * | 2015-11-06 | 2016-01-06 | 中国科学院理化技术研究所 | A kind of preparation method of TiO2 monocrystal nano pipe array |
Non-Patent Citations (1)
| Title |
|---|
| 巩合春: "铈或银掺杂氧化锌微纳材料制备及发光性质研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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