CN101445265A - Method for preparing adulteration monocrystalline zinc oxide nanometer screwdriver by vapour deposition and device thereof - Google Patents
Method for preparing adulteration monocrystalline zinc oxide nanometer screwdriver by vapour deposition and device thereof Download PDFInfo
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Abstract
The invention belongs to the field of low dimensional nanophase material and nanotechnology, and discloses a method for preparing an adulteration monocrystalline zinc oxide nanometer screwdriver by vapour deposition and a device thereof. In the invention, zinc nitrate and metal nitrate used for adulteration are mixed and dissolved in deionized water to form solution, then the solution is mixed with citric acid and glycol, heated and stirred to form sol-gel, precursor is obtained by cracking, then the precursor is put in a ceramic boat and heated up in a tube type resistance furnace, heating, reaction, transport and cooling are carried out, inert gas is used as transport gas, a silicon chip is used as a base, and a large number of adulteration monocrystalline zinc oxide nanometer screwdrivers are generated on the silicon chip. The invention has simple technique, low requirements for equipment and high degree of controllability, and provides a good method for preparing an adulteration monocrystalline zinc oxide nanometer screwdriver and a good device thereof.
Description
Technical field
The invention belongs to low-dimension nano material and field of nanometer technology, be specifically related to a kind of method and device thereof that combines and prepare adulteration monocrystalline zinc oxide nanometer screwdriver by sol-gel method and chemical vapour deposition.
Background technology
Semiconductor doping is the approach of very effective its performance of improvement, and this is not only because be difficult to be avoided sneaking into of impurity in the crystalline preparation process, and main is in order to control semi-conductive character, artificially and controlledly to add some impurity.Therefore, start with, further investigate, the performance of possible improved semiconductor device with regard to the great basic problem that influences material property from the character of improving nano material itself.
Existing preparation doping techniques comprises ionic fluid implantttion technique, metal organic chemical vapor deposition technology (MOCVD), and its equipment and raw material are all expensive, and processing condition complexity and operant level require high, so the required cost height of product.The method that is used in air evaporation in Chinese patent CN1099816 " preparation method of ZnOw and device thereof " obtains the zinc peroxide nano whisker.In addition, in Chinese patent CN1772625 " a kind of method for preparing high yield indium doped nanometer zinc oxide disc ", must be the adulterated nanometer zinc oxide disc of metallic cation by the high temperature chemical vapor deposition method.So it is low to study a kind of cost, the preparation method of the single-crystal doped zinc-oxide nano laminate structure that controllability is good and device thereof have very significant meaning.
Summary of the invention
The method and the device thereof that the purpose of this invention is to provide the preparing adulteration monocrystalline zinc oxide nanometer screwdriver by vapour deposition that a kind of cost is low, controllability is good.
Technical scheme provided by the invention is: combining by sol-gel method and chemical vapour deposition prepares doped single crystal zinc oxide screwdriver-like nanostructure, and its concrete grammar step is:
(1) with zinc nitrate and be used for adulterated metal nitrate powder mixes, the amount of adulterated metal nitrate is 0.2～10%mol of zinc nitrate, and mixed powder dissolution is made the zinc nitrate solution of 0.1～1.0mol/l in deionized water; In this zinc nitrate solution of every 50ml, add 5～7g citric acid and 6～9ml ethylene glycol respectively; The mixing solutions of preparation obtains colloidal sol 50～100 ℃ of stirrings, and next constant temperature obtains gel under 120～180 ℃ of conditions; The gel of preparation obtains unbodied C-Zn-O-M composite precursor 200～500 ℃ of constant temperature cracking, and it is standby to be ground into powder, and wherein M is a doping metals;
(2) the composite precursor powder that step (1) is obtained heats up with the speed of 3～40 ℃/min, be heated to 600～1000 ℃, simultaneously with rare gas element as carrier gas, constant temperature 1～3h is cooled to 350～550 ℃ and can collects and obtain adulteration monocrystalline zinc oxide nanometer screwdriver.
As preferably, the purity of described zinc nitrate〉98%, be used for the purity of adulterated metal nitrate〉98%, the purity of citric acid is 99.9%, the purity of ethylene glycol is 99.9%.
As preferably, described to be used for adulterated metal nitrate be to be selected from any of cerous nitrate, Silver Nitrate and magnesium nitrate.
As optimization, solution stirring 1～2h obtains colloidal sol in the described step (1), and the colloidal sol constant temperature 6～14h of preparation obtains gel, and the gel constant temperature cracking 1～5h of preparation obtains unbodied C-Zn-O-M composite precursor, and wherein M is a doping metals.
As optimization, the heat-up rate of described step (2) is 15～30 ℃/min, is heated to 900～1000 ℃.
As optimization, the flow velocity of described feeding rare gas element is per minute 450～550 standard cubic centimeters, and atmosphere pressures is 200～400 holders.
As preferably, described rare gas element is nitrogen, argon gas, neon.
The doping of described adulteration monocrystalline zinc oxide nanometer screwdriver is 0.1～3%mol of zinc oxide, and adulteration monocrystalline zinc oxide nanometer screwdriver handle length is 0.04～10 μ m, long 0.1～10 μ m of six side's handle ribs, and long 0.1～1.5 μ m in top, diameter is 5～500nm.
Method of the present invention can realize with following device of the present invention:
Device of the present invention is made up of tube type resistance furnace, ceramic boat, silicon chip and the silica tube of a heating source, and 750～1000 ℃ of warm areas of the silica tube in tube type resistance furnace are placed with ceramic boat, and 350～550 ℃ of warm areas of silica tube are placed with silicon chip.
The technical process of the inventive method comprises dosing, colloidal sol, gel, cracking, aftertreatment, easy and simple to handle, post-processed is selected conventional tube type resistance furnace for use, low for equipment requirements, cost is low, and because of tube type resistance furnace is the multiple spot temperature control, thermograde can be set as required, the controllable degree height is the good method of the adulteration monocrystalline zinc oxide nanometer screwdriver preparation device of becoming reconciled.
Description of drawings
Fig. 1 device synoptic diagram of the present invention.
Fig. 2 A, Fig. 2 B and Fig. 2 C are respectively the high resolution scanning Electronic Speculum figure (HRSEM) of the low power sem photograph (SEM) of embodiment 1 product, single nanometer screwdriver and the constituency composition on the single nanometer screwdriver can spectrogram (EDS).
Fig. 3 A, Fig. 3 B, and Fig. 3 C be respectively the x-ray diffraction pattern (XRD) of low power transmission electron microscope picture (TEM), selected area electron diffraction spectrogram (SAED) and a large amount of products of embodiment 1 product.
Embodiment
The present invention is further illustrated with specific embodiment below, but protection scope of the present invention is not limited to this:
Embodiment 1
(1) with 2.97gZn (NO
3)
26H
2O (purity 99.9%) and be used for adulterated cerous nitrate (Ce (NO
3)
36H
2O, 0.43g, purity 99.9%) mixed dissolution in the 50ml deionized water, in the solution of preparation, add citric acid (5.76g, purity 99.9%) and ethylene glycol (6.6ml, purity 99.9%) respectively;
(2) step (1) gained ingredients solution in the 150ml Erlenmeyer flask 80 ℃ of heating and stir 1h after obtain colloidal sol, next constant temperature 8h obtains gel under 150 ℃ of conditions; The gel of preparation obtains unbodied C-Zn-O-Ce composite precursor at 400 ℃ of constant temperature cracking 1h, and it is standby to be ground into powder with mortar;
(3) as shown in Figure 1, the C-Zn-O-Ce composite precursor powder 5 that step (2) is obtained moves in the ceramic boat 2, and ceramic boat 2 moved in 750～1000 ℃ of warm areas of the silica tube 4 of tube type resistance furnace 1, simultaneously silicon chip 3 is placed 350～550 ℃ of warm areas of silica tube 4, speed with 20 ℃/min heats up, be heated to 900 ℃, speed with per minute 530 standard cubic centimeters feeds nitrogen as carrier gas simultaneously, atmosphere pressures is 380 holders, constant temperature 1h is cooled to 350 ℃ of products of collecting preparation with silicon chip 3 as the base;
(4) gaseous products that obtains of step (3) is deposited on the silicon chip, can obtain the adulterated single-crystal zinc-oxide nano screwdriver of cerium.
Analytical test shows (seeing accompanying drawing 2A～Fig. 3 C), and product mainly is made up of the adulterated zinc oxide nanometer screwdriver of cerium; According to electronic spectrum EDS, see Fig. 2 C, be that doped with cerium is approximately 1.1%mol as can be known; The nanometer screwdriver handle length for preparing as can be known according to scanning electron microscope sem (seeing Fig. 2 A and Fig. 2 B) and transmission electron microscope TEM (seeing Fig. 3 A) is 4 μ m, the long 1 μ m of six side's handle ribs, and the long 1.5 μ m in top, diameter is 200nm; According to selected area electron diffraction SAED (seeing Fig. 3 B) and X-ray diffraction XRD (seeing Fig. 3 C) as can be known the structure of nanometer screwdriver be six side's monocrystalline kenels.
(1) with 3.29g Zn (NO
3)
26H
2O (purity 99.9%) and be used for adulterated Silver Nitrate (AgNO
3, 0.17g, purity 99.99%) mixed dissolution in the 50ml deionized water, the preparation solution in add citric acid (5.99g, purity 99.9%) and ethylene glycol (7.6ml, purity 99.9%) respectively;
(2) step (1) gained ingredients solution in the 150ml Erlenmeyer flask 90 ℃ of heating and stir 1.5h after obtain colloidal sol, next constant temperature 7h obtains gel under 170 ℃ of conditions, the gel of preparation is at 350 ℃ of constant temperature cracking 1.5h, obtain unbodied C-Zn-O-Ag composite precursor, it is standby to be ground into powder with mortar;
(3) as shown in Figure 1, the C-Zn-O-Ag composite precursor powder 5 that step (2) is obtained moves in the ceramic boat 2, and ceramic boat 2 moved in 750～1000 ℃ of warm areas of the silica tube 4 of tube type resistance furnace 1, simultaneously silicon chip 3 is placed 350～550 ℃ of warm areas of silica tube 4, speed with 15 ℃/min heats up, be heated to 950 ℃, speed with per minute 500 standard cubic centimeters feeds nitrogen as carrier gas simultaneously, atmosphere pressures is 300 holders, constant temperature 2h, be cooled to 400 ℃, collect the product of preparation with silicon chip 3 as the base;
(4) gaseous products that obtains of step (3) is deposited on the silicon chip, can obtain silver-colored adulterated single-crystal zinc-oxide nano screwdriver.
Analytical test shows: product mainly is made up of the adulterated zinc oxide nanometer screwdriver of silver, according to electronic spectrum EDS, is that doping Ag is approximately 0.9%mol as can be known; According to scanning electron microscope sem and transmission electron microscope TEM as can be known screwdriver handle length be 6 μ m, the long 3 μ m of six side's handle ribs; The long 1.0 μ m in top, diameter is 100nm; According to selected area electron diffraction SAED and X-ray diffraction XRD as can be known the structure of nanometer screwdriver be six side's monocrystalline kenels; Figure slightly.
Embodiment 3
(1) with 4.82g Zn (NO
3)
26H
2O (purity 99.9%) and be used for adulterated magnesium nitrate (Mg (NO
3)
26H
2O, 0.39g, purity 99.99%) mixed dissolution in the 50ml deionized water, in the solution of preparation, add citric acid (6.15g, purity 99.9%) and ethylene glycol (8.3ml, purity 99.9%);
(2) step (1) gained ingredients solution in the 150ml Erlenmeyer flask 50 ℃ of heating and stir 2h after obtain colloidal sol, next constant temperature 14h obtains gel under 120 ℃ of conditions, the gel of preparation is at 200 ℃ of constant temperature cracking 5h, obtain unbodied C-Zn-O-Mg composite precursor, with mortar that its grinding powder is standby;
(3) as shown in Figure 1, the C-Zn-O-Mg composite precursor powder 5 that step (2) is obtained moves in the ceramic boat 2, and ceramic boat 2 moved in 750～1000 ℃ of warm areas of the silica tube 4 of tube type resistance furnace 1, simultaneously silicon chip 3 is placed 350～550 ℃ of warm areas of silica tube 4, speed with 3 ℃/min heats up, be heated to 600 ℃, speed with per minute 450 standard cubic centimeters feeds nitrogen as carrier gas simultaneously, atmosphere pressures is 200 holders, constant temperature 3h, be cooled to 450 ℃, collect the product of preparation with silicon chip 3 as the base;
(4) gaseous products that obtains of step (3) is deposited on the silicon chip, can obtain magnesium doped zinc oxide nano screwdriver.
Analytical test shows: product mainly is made up of the adulterated zinc oxide nanometer screwdriver of magnesium; According to electronic spectrum EDS, be that doped with Mg is approximately 1.6%mol as can be known; The nanometer screwdriver handle length for preparing as can be known according to scanning electron microscope sem and transmission electron microscope TEM is 8 μ m, the long 6 μ m of six side's handle ribs, and the long 1.3 μ m in top, diameter is 400nm; According to selected area electron diffraction SAED and X-ray diffraction XRD as can be known the structure of nanometer screwdriver be six side's monocrystalline kenels; Figure slightly.
(1) with 11.88gZn (NO
3)
26H
2O (purity 99.9%) and be used for adulterated cerous nitrate (Ce (NO
3)
36H
2O, 0.53g, purity 99.9%) mixed dissolution in the 50ml deionized water, in the solution of preparation, add citric acid (6.65g, purity 99.9%) and ethylene glycol (8.7ml, purity 99.9%) respectively;
(2) step (1) gained ingredients solution in the 150ml Erlenmeyer flask 60 ℃ of heating and stir 2h after obtain colloidal sol, next constant temperature 12h obtains gel under 135 ℃ of conditions; The gel of preparation obtains unbodied C-Zn-O-Ce composite precursor at 300 ℃ of constant temperature cracking 3.5h, and it is standby to be ground into powder with mortar;
(3) as shown in Figure 1, the C-Zn-O-Ce composite precursor powder 5 that step (2) is obtained moves in the ceramic boat 2, and ceramic boat 2 moved in 750～1000 ℃ of warm areas of the silica tube 4 of tube type resistance furnace 1, simultaneously silicon chip 3 is placed 350～550 ℃ of warm areas of silica tube 4, speed with 10 ℃/min heats up, be heated to 700 ℃, speed with per minute 480 standard cubic centimeters feeds neon as carrier gas simultaneously, atmosphere pressures is 250 holders, constant temperature 3h, be cooled to 480 ℃, collect the product of preparation with silicon chip 3 as the base;
(4) gaseous products that obtains of step (3) is deposited on the silicon chip, can obtain the adulterated single-crystal zinc-oxide nano screwdriver of cerium.
Analytical test shows that product mainly is made up of the adulterated zinc oxide nanometer screwdriver of cerium; According to electronic spectrum EDS, be that doped with cerium is approximately 2.3%mol as can be known; The nanometer screwdriver handle length for preparing as can be known according to scanning electron microscope sem and transmission electron microscope TEM is 1 μ m, the long 0.6 μ m of six side's handle ribs, and the long 0.7 μ m in top, diameter is 60nm; According to selected area electron diffraction SAED and X-ray diffraction XRD as can be known the structure of nanometer screwdriver be six side's monocrystalline kenels.
Embodiment 5
(1) with 1.50gZn (NO
3)
26H
2O (purity 99.9%) and be used for adulterated Silver Nitrate (AgNO
3, 0.01g, purity 99.99%) mixed dissolution in the 50ml deionized water, the preparation solution in add citric acid (5.03g, purity 99.9%) and ethylene glycol (6.1ml, purity 99.9%) respectively;
(2) step (1) gained ingredients solution in the 150ml Erlenmeyer flask 70 ℃ of heating and stir 1.5h after obtain colloidal sol, next constant temperature 10h obtains gel under 160 ℃ of conditions, the gel of preparation is at 500 ℃ of constant temperature cracking 2h, obtain unbodied C-Zn-O-Ag composite precursor, it is standby to be ground into powder with mortar;
(3) as shown in Figure 1, the C-Zn-O-Ag composite precursor powder 5 that step (2) is obtained moves in the ceramic boat 2, and ceramic boat 2 moved in 750～1000 ℃ of warm areas of the silica tube 4 of tube type resistance furnace 1, simultaneously silicon chip 3 is placed 350～550 ℃ of warm areas of silica tube 4, speed with 30 ℃/min heats up, be heated to 800 ℃, speed with per minute 520 standard cubic centimeters feeds argon gas as carrier gas simultaneously, atmosphere pressures is 350 holders, constant temperature 2h, be cooled to 500 ℃, collect the product of preparation with silicon chip 3 as the base;
(4) gaseous products that obtains of step (3) is deposited on the silicon chip, can obtain silver-colored adulterated single-crystal zinc-oxide nano screwdriver.
Analytical test shows: product mainly is made up of the adulterated zinc oxide nanometer screwdriver of silver, according to electronic spectrum EDS, is that doping Ag is approximately 0.1%mol as can be known; According to scanning electron microscope sem and transmission electron microscope TEM as can be known screwdriver handle length be 0.04 μ m, the long 0.1 μ m of six side's handle ribs; The long 0.3 μ m in top, diameter is 6nm; According to selected area electron diffraction SAED and X-ray diffraction XRD as can be known the structure of nanometer screwdriver be six side's monocrystalline kenels; Figure slightly.
Embodiment 6
(1) with 14.92gZn (NO
3)
26H
2O (purity 99.9%) and be used for adulterated magnesium nitrate (Mg (NO
3)
26H
2O, 0.64g, purity 99.99%) mixed dissolution in the 50ml deionized water, in the solution of preparation, add citric acid (6.97g, purity 99.9%) and ethylene glycol (9.1ml, purity 99.9%);
(2) step (1) gained ingredients solution in the 150ml Erlenmeyer flask 100 ℃ of heating and stir 1h after obtain colloidal sol, next constant temperature 6h obtains gel under 180 ℃ of conditions, the gel of preparation is at 500 ℃ of constant temperature cracking 1h, obtain unbodied C-Zn-O-Mg composite precursor, with mortar that its grinding powder is standby;
(3) as shown in Figure 1, the C-Zn-O-Mg composite precursor powder 5 that step (2) is obtained moves in the ceramic boat 2, and ceramic boat 2 moved in 750～1000 ℃ of warm areas of the silica tube 4 of tube type resistance furnace 1, simultaneously silicon chip 3 is placed 350～550 ℃ of warm areas of silica tube 4, speed with 40 ℃/min heats up, be heated to 1000 ℃, speed with per minute 550 standard cubic centimeters feeds nitrogen as carrier gas simultaneously, atmosphere pressures is 400 holders, constant temperature 1h, be cooled to 550 ℃, collect the product of preparation with silicon chip 3 as the base;
(4) gaseous products that obtains of step (3) is deposited on the silicon chip, can obtain magnesium doped zinc oxide nano screwdriver.
Analytical test shows: product mainly is made up of the adulterated zinc oxide nanometer screwdriver of magnesium; According to electronic spectrum EDS, be that doped with Mg is approximately 3% mol as can be known; The nanometer screwdriver handle length for preparing as can be known according to scanning electron microscope sem and transmission electron microscope TEM is 10 μ m, the long 10 μ m of six side's handle ribs, and the long 1.5 μ m in top, diameter is 500nm; According to selected area electron diffraction SAED and X-ray diffraction XRD as can be known the structure of nanometer screwdriver be six side's monocrystalline kenels; Figure slightly.
Claims (9)
1. the method for preparing adulteration monocrystalline zinc oxide nanometer screwdriver by vapour deposition is characterized in that the step of described method is:
(1) with zinc nitrate and be used for adulterated metal nitrate powder mixes, the amount of adulterated metal nitrate is 0.2～10%mol of zinc nitrate, and mixed powder dissolution is made the zinc nitrate solution of 0.1～1.0mol/l in deionized water; In this zinc nitrate solution of every 50ml, add 5～7g citric acid and 6～9ml ethylene glycol respectively; The mixing solutions of preparation obtains colloidal sol 50～100 ℃ of stirrings, and next constant temperature obtains gel under 120～180 ℃ of conditions; The gel of preparation obtains unbodied C-Zn-O-M composite precursor 200～500 ℃ of constant temperature cracking, and it is standby to be ground into powder, and wherein M is a doping metals;
(2) the composite precursor powder that step (1) is obtained heats up with the speed of 3～40 ℃/min, be heated to 600～1000 ℃, simultaneously with rare gas element as carrier gas, constant temperature 1～3h is cooled to 350～550 ℃ and can collects and obtain adulteration monocrystalline zinc oxide nanometer screwdriver.
2. the method for preparing adulteration monocrystalline zinc oxide nanometer screwdriver by vapour deposition as claimed in claim 1, the purity that it is characterized in that described zinc nitrate〉98%, the purity that is used for adulterated metal nitrate〉98%, the purity of citric acid is 99.9%, the purity of ethylene glycol is 99.9%.
3. the method for preparing adulteration monocrystalline zinc oxide nanometer screwdriver by vapour deposition as claimed in claim 1 is characterized in that described to be used for adulterated metal nitrate be to be selected from any of cerous nitrate, Silver Nitrate and magnesium nitrate.
4. the method for preparing adulteration monocrystalline zinc oxide nanometer screwdriver by vapour deposition as claimed in claim 1, it is characterized in that solution stirring 1～2h obtains colloidal sol in the described step (1), the colloidal sol constant temperature 6～14h of preparation obtains gel, the gel constant temperature cracking 1～5h of preparation obtains unbodied C-Zn-O-M composite precursor, and wherein M is a doping metals.
5. the method for preparing adulteration monocrystalline zinc oxide nanometer screwdriver by vapour deposition as claimed in claim 1 is characterized in that the heat-up rate in the described step (2) is 15～30 ℃/min, is heated to 900～1000 ℃.
6. the method for preparing adulteration monocrystalline zinc oxide nanometer screwdriver by vapour deposition as claimed in claim 1 is characterized in that described rare gas element flow velocity is per minute 450～550 standard cubic centimeters, and atmosphere pressures is 200～400 holders.
7. the method for preparing adulteration monocrystalline zinc oxide nanometer screwdriver by vapour deposition as claimed in claim 6 is characterized in that described rare gas element is nitrogen, argon gas, neon.
8. the method for preparing adulteration monocrystalline zinc oxide nanometer screwdriver by vapour deposition as claimed in claim 1, the doping that it is characterized in that described adulteration monocrystalline zinc oxide nanometer screwdriver is 0.1～3%mol of zinc oxide, adulteration monocrystalline zinc oxide nanometer screwdriver handle length is 0.04～10 μ m, long 0.1～10 μ m of six side's handle ribs, long 0.1～1.5 μ m in top, diameter is 5～500nm.
9. the device of preparing adulteration monocrystalline zinc oxide nanometer screwdriver by vapour deposition, this device is made up of tube type resistance furnace (1), ceramic boat (2), silicon chip (3) and silica tube (4), it is characterized in that: 750～1000 ℃ of warm areas of the silica tube (4) in tube type resistance furnace (1) are placed with ceramic boat (2), and 350～550 ℃ of warm areas of silica tube (4) are placed with silicon chip (3).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103739002A (en) * | 2013-07-29 | 2014-04-23 | 南昌大学 | Preparation method of one-dimensional nanostructured material |
| CN106591949A (en) * | 2016-11-23 | 2017-04-26 | 濮阳市质量技术监督检验测试中心 | Method and device for preparing monocrystal Ag-doped zinc oxide hexagonal micro tube by vapor deposition |
| MD4455C1 (en) * | 2015-11-27 | 2017-07-31 | Государственный Университет Молд0 | Process for unseeded vapor production of ZnO single crystals |
| MD4500C1 (en) * | 2015-07-23 | 2018-02-28 | Государственный Университет Молд0 | Process for gaseous-phase production of ZnO single crystals |
| MD4517C1 (en) * | 2016-10-11 | 2018-04-30 | Государственный Университет Молд0 | Method for gaseous-phase production of ZnO single crystals without seed |
-
2008
- 2008-09-23 CN CNA2008101414225A patent/CN101445265A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103739002A (en) * | 2013-07-29 | 2014-04-23 | 南昌大学 | Preparation method of one-dimensional nanostructured material |
| MD4500C1 (en) * | 2015-07-23 | 2018-02-28 | Государственный Университет Молд0 | Process for gaseous-phase production of ZnO single crystals |
| MD4455C1 (en) * | 2015-11-27 | 2017-07-31 | Государственный Университет Молд0 | Process for unseeded vapor production of ZnO single crystals |
| MD4517C1 (en) * | 2016-10-11 | 2018-04-30 | Государственный Университет Молд0 | Method for gaseous-phase production of ZnO single crystals without seed |
| CN106591949A (en) * | 2016-11-23 | 2017-04-26 | 濮阳市质量技术监督检验测试中心 | Method and device for preparing monocrystal Ag-doped zinc oxide hexagonal micro tube by vapor deposition |
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