CN107059124A - A kind of method that utilization microwave synthesizes zinc oxide in large size crystal - Google Patents
A kind of method that utilization microwave synthesizes zinc oxide in large size crystal Download PDFInfo
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- CN107059124A CN107059124A CN201710208140.1A CN201710208140A CN107059124A CN 107059124 A CN107059124 A CN 107059124A CN 201710208140 A CN201710208140 A CN 201710208140A CN 107059124 A CN107059124 A CN 107059124A
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- 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
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- 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
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
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- 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
- C30B29/62—Whiskers or needles
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- 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
- C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
Abstract
The invention belongs to ceramic material field, it is related to a kind of method that utilization microwave synthesizes zinc oxide in large size crystal.Step is as follows：A certain amount of carbon source and Zinc oxide powder are weighed in mass ratio, and mixture I is obtained after being well mixed；The particulate adjunct of the mass 5 ~ 10% of mixture I is added into above-mentioned steps, mixture II is obtained after mixing；Mixture II is added in crucible, is placed in microwave reaction device and is heated at room temperature, after 0.5 ~ 1.5h of reaction, acicular crystal can be grown in crucible internal walls, the acicular crystal is zinc oxide in large size crystal.Zinc oxide will turn into wide bandgap semiconductor materials of future generation with its many excellent properties, growing large-size monocrystalline all has very important significance for basic research and practical application, this microwave-assisted synthesis is used to provide a new easy approach for the preparation of zinc oxide in large size monocrystal material, so as to promote its application and technology development.
Description
Technical field
The invention belongs to ceramic material field, it is related to the side that a kind of utilization microwave synthesizes zinc oxide in large size crystal
Method.
Background technology
Zinc oxide in large size crystal is a kind of important feature crystalline material, with excellent optics, electrology characteristic,
Many fields such as LED field, presentation of information and storage, optical communication and missile warning have broad application prospects.From current system
From the point of view of the present Research of standby zincite crystal, the growing technology of zinc oxide in large size monocrystalline is difficult.For example, using czochralski method
Developing zinc oxide monocrystalline, because the vapour pressure of zinc oxide is larger, it is necessary to need accurate control, skill in hyperbaric environment, growth course
Art difficulty is than larger.Hydrothermal Growth Zinc oxide single crystal is presently the most ripe method, but its growth rate is relatively low, it is necessary to high
Pressure ring border, growth cycle is long；Zinc oxide single crystal is prepared using chemical vapour deposition technique, the reaction time is still longer, up to one
Month or so, higher is required to testing equipment, cost is also higher.Recently, " one kind substitutes leaded fluxing agent and prepares large scale oxygen document
Change the research of zinc whisker method " use industrial zinc oxide（ZnO）Powder is raw material, and auxiliary agent is with potassium tetratitanate（K2Ti4O9）Based on, adopt
With flux growth metrhod, needle body length about 20mm ZnO whiskers are obtained.But this method is readily incorporated auxiliary agent impurity.
Recently, microwave-assisted synthesis has heating rate fast and the features such as the reaction time is short, and oxygen is prepared for by the technology
Change zinc crystalline material, have a good application prospect.Such as document " the microwave study on the synthesis of grade zincite crystal " is with oxygen
Change zinc powder is raw material, is heated using microwave and combines the zinc oxide that the method being vapor-deposited prepares 2.2 millimeters in a short time
Crystal.Document " technique of microwave synthesis ZnO whiskers is studied with electromagnetic performance " is by mixing μm level zinc oxide and a nanoscale
Zinc, the zinc oxide μm pipe and whisker of nearly 1 millimeter of length are prepared for using microwave heating technique.From the synthetically prepared oxidation of microwave current
For zinc single crystal technology, the Zinc oxide single crystal size of preparation is smaller, maximum only grade, can not also be referred to as large scale.
The content of the invention
The present invention prepares the not enough problem that just seems of zinc oxide in large size for the above-mentioned microwave-assisted synthesis of solution, and there is provided one
Plant the preparation method for preparing zinc oxide large-size crystals.Large scale Centimeter Level (1 ~ 2 centimetre) single-crystal zinc-oxide that the present invention is provided
The preparation method of crystal, is, using fine graphite powder and common zinc oxide powder as raw material, to add appropriate nickel or copper particulate adjunct, with
Synthesize large scale Centimeter Level (1 ~ 2 centimetre) zincite crystal material.
To solve the above problems, the present invention uses following technical scheme：
A kind of method that utilization microwave synthesizes zinc oxide in large size crystal, step is as follows：
（1）A certain amount of carbon source and Zinc oxide powder are weighed in mass ratio, and mixture I is obtained after being well mixed；
（2）To step（1）The middle particulate adjunct for adding the mass 5 ~ 10% of mixture I, obtains mixture II after mixing；
（3）Mixture II is added in crucible, is placed in microwave reaction device and is heated at room temperature, after 0.5 ~ 1.5h of reaction,
Acicular crystal can be grown in crucible internal walls, the acicular crystal is zinc oxide in large size crystal.
The step（1）Middle carbon source is graphite composite powder or activated carbon, and the mass ratio of the carbon source and Zinc oxide powder is 1：
（1~2）.
The step（2）Middle particulate adjunct is nickel particle or copper particle, and the granularity of particulate adjunct is 0.1 ~ 1mm.
The granularity of the graphite composite powder or activated carbon is 1 ~ 3 μm.
The Zinc oxide powder granularity is 1 μm, and purity is 99%.
The step（3）In microwave reaction device be microwave Muffle furnace, the condition of reaction is：Heating rate is 10 ~ 30
DEG C/min, final temperature is 1050 ~ 1100 DEG C, and the time for keeping final temperature is 0.5 ~ 1.5h.
The beneficial effects of the present invention are：
（1）Using the microwave synthesis method of the zinc oxide in large size crystal of above-mentioned technical proposal, its operation principle：Sharp reduction with carbon
Zinc oxide, is allowed to form Zn steam, by the effect of nickel or copper particulate adjunct, occurs following reduction reaction, generates zinc oxide material
Material；
C+ZnO=Zn+CO
Zn+O2=ZnO。
（2）Zinc oxide will turn into wide bandgap semiconductor materials of future generation, growing large-size monocrystalline with its many excellent properties
All have very important significance for basic research and practical application, use this microwave-assisted synthesis for zinc oxide in large size
The preparation of monocrystal material provides a new easy approach, so that promote its application and technology development, can from Fig. 3 and Fig. 4
It was observed that, by modulation process, can on zinc oxide trunk surface can also epitaxial growth reduced size different-shape oxygen
Change zinc crystal, such as sheet, cone and pectination, it is clear that also can be as GaN, the ideal substrate of the novel optoelectronic materials such as SiC.
Brief description of the drawings
Fig. 1 is the schematic diagram for the zincite crystal product that example 1 is obtained.
Fig. 2 is the XRD for the zincite crystal product that example 1 is obtained.
Fig. 3 is the FE-SEM shape appearance figures for the zincite crystal product part that example 1 is obtained.
Fig. 4 is the FE-SEM shape appearance figures for the zincite crystal its surface that example 2 is obtained.
Embodiment
A kind of method that utilization microwave synthesizes zinc oxide in large size crystal, step is as follows：
（1）A certain amount of carbon source and Zinc oxide powder are weighed in mass ratio, and mixture I is obtained after being well mixed；
（2）To step（1）The middle particulate adjunct for adding the mass 5 ~ 10% of mixture I, obtains mixture II after mixing；
（3）Mixture II is added in crucible, is placed in microwave reaction device and is heated at room temperature, after 0.5 ~ 1.5h of reaction,
Acicular crystal can be grown in crucible internal walls, the acicular crystal is zinc oxide in large size crystal.
The step（1）Middle carbon source is graphite composite powder or activated carbon, and the mass ratio of the carbon source and Zinc oxide powder is 1：
（1~2）.
The step（2）Middle particulate adjunct is nickel or copper particle, and the granularity of particle is 0.1 ~ 1mm.
The granularity of the graphite composite powder or activated carbon is 1 ~ 3 μm.
The Zinc oxide powder granularity is 1 μm, and purity is 99%.
The step（3）In microwave reaction device be microwave Muffle furnace, the condition of reaction is：Heating rate is 10 ~ 30
DEG C/min, final temperature is 1050 ~ 1100 DEG C, and the time for keeping final temperature is 0.5 ~ 1.5h.
Explanation is further explained to the present invention with reference to specific embodiment：
Embodiment 1
It is 1mm copper from the powdered graphite that particle mean size is 2 μm, the high-purity zinc oxide that particle mean size is 1 μm and particle mean size
Grain makees raw material, by C：ZnO：The quality of copper particle is 2.25 grams, 4.5 grams and 0.475 gram and weighs powder, is then mixed in mortar
30 minutes, it is well mixed it.The raw material of preparation is put into the silica crucible that internal diameter is 45mm, is placed in microwave Muffle furnace
Row reaction synthesis, heating rate is 30 DEG C/min, and synthesis temperature is 1100 DEG C, is incubated 1h.In crucible internal walls institute after furnace cooling
It is zinc oxide acicular crystal to obtain product as white needles, and length is 1 ~ 2 centimetre, product as white needles is detected, as a result such as
Shown in Fig. 1-3.
Embodiment 2
It is 0.1mm from the activated carbon powder that particle mean size is 3 μm, the high-purity zinc oxide that particle mean size is 1 μm and particle mean size
Copper size particles for feed stock material, by C：ZnO：The quality of copper particle is 2.25 grams, 2.25 grams and 0.25 gram and weighs powder, then in mortar
Mixing 40 minutes, is well mixed it.The raw material of preparation is put into the silica crucible that internal diameter is 45mm, is placed in microwave Muffle furnace
Middle progress reaction synthesis, heating rate is 10 DEG C/min, and synthesis temperature is 1050 DEG C, is incubated 1.5h.In crucible after furnace cooling
White spicule obtained by inwall is zinc oxide acicular crystal, as shown in Figure 4.
Embodiment 3
It is 0.5mm copper from the powdered graphite that particle mean size is 3 μm, the high-purity zinc oxide that particle mean size is 1 μm and particle mean size
Size particles for feed stock material, by C：ZnO：The quality of copper particle is 2.25 grams, 3.25 grams and 0.275 gram and weighs powder, then in mortar
Mixing 30 minutes, is well mixed it.The raw material of preparation is put into the silica crucible that internal diameter is 45mm, is placed in microwave Muffle furnace
Middle progress reaction synthesis, heating rate is 20 DEG C/min, and synthesis temperature is 1100 DEG C, is incubated 0.5h.In crucible after furnace cooling
Product as white needles obtained by inwall is zinc oxide acicular crystal.
Embodiment 4
It is 0.1mm nickel from the powdered graphite that particle mean size is 2 μm, the high-purity zinc oxide that particle mean size is 1 μm and particle mean size
Size particles for feed stock material, by C：ZnO：The quality of nickel particle is 2.25 grams, 4 grams and 0.5 gram and weighs powder, and 30 are then mixed in mortar
Minute, it is well mixed it.The raw material of preparation is put into the silica crucible that internal diameter is 45mm, is placed in microwave Muffle furnace and carries out
Reaction synthesis, heating rate is 10 DEG C/min, and synthesis temperature is 1100 DEG C, is incubated 0.5h.In crucible internal walls institute after furnace cooling
It is zinc oxide acicular crystal to obtain product as white needles.
Embodiment 5
It is 0.5mm nickel from the powdered graphite that particle mean size is 1 μm, the high-purity zinc oxide that particle mean size is 1 μm and particle mean size
Size particles for feed stock material, by C：ZnO：The quality of nickel particle is 2.25 grams, 4.5 grams and 0.435 gram and weighs powder, is then mixed in mortar
Close 30 minutes, be well mixed it.The raw material of preparation is put into the silica crucible that internal diameter is 45mm, be placed in microwave Muffle furnace
Reaction synthesis is carried out, heating rate is 25 DEG C/min, and synthesis temperature is 1050 DEG C, is incubated 1h.In crucible internal walls after furnace cooling
Gained product as white needles is zinc oxide acicular crystal.
Embodiment 6
It is 0.5mm from the active carbon powder that particle mean size is 2 μm, the high-purity zinc oxide that particle mean size is 1 μm and particle mean size
Nickel particle makees raw material, by C：ZnO：The quality of nickel particle is 2.25 grams, 4.5 grams and 0.435 gram and weighs powder, then in mortar
Mixing 30 minutes, is well mixed it.The raw material of preparation is put into the silica crucible that internal diameter is 45mm, is placed in microwave Muffle furnace
Middle progress reaction synthesis, heating rate is 30 DEG C/min, and synthesis temperature is 1050 DEG C, is incubated 1.5h.In crucible after furnace cooling
Product as white needles obtained by inwall is zinc oxide acicular crystal.
Embodiment 7
It is 0.1mm from the activated carbon powder that particle mean size is 1 μm, the high-purity zinc oxide that particle mean size is 1 μm and particle mean size
Copper size particles for feed stock material, by C：ZnO：The quality of copper particle is 2.25 grams, 2.25 grams and 0.45 gram and weighs powder, then in mortar
Mixing 40 minutes, is well mixed it.The raw material of preparation is put into the silica crucible that internal diameter is 45mm, is placed in microwave Muffle furnace
Middle progress reaction synthesis, heating rate is 10 DEG C/min, and synthesis temperature is 1080 DEG C, is incubated 1h.After furnace cooling in crucible
White spicule obtained by wall is zinc oxide acicular crystal.
Claims (6)
1. a kind of method that utilization microwave synthesizes zinc oxide in large size crystal, it is characterised in that step is as follows：
（1）A certain amount of carbon source and Zinc oxide powder are weighed in mass ratio, and mixture I is obtained after being well mixed；
（2）To step（1）The middle particulate adjunct for adding the mass 5 ~ 10% of mixture I, obtains mixture II after mixing；
（3）Mixture II is added in crucible, is placed in microwave reaction device and is heated at room temperature, after reaction 0.5h ~ 1.5h,
Acicular crystal can be grown in crucible internal walls, the acicular crystal is zinc oxide in large size crystal.
2. the method for zinc oxide in large size crystal is synthesized using microwave as claimed in claim 1, it is characterised in that：The step
（1）Middle carbon source is graphite composite powder or activated carbon, and the mass ratio of the carbon source and Zinc oxide powder is 1：（1~2）.
3. the method for zinc oxide in large size crystal is synthesized using microwave as claimed in claim 1, it is characterised in that：The step
（2）Middle particulate adjunct is nickel particle or copper particle, and the particle mean size of particulate adjunct is 0.1 ~ 1mm.
4. the method for zinc oxide in large size crystal is synthesized using microwave as claimed in claim 2, it is characterised in that：The graphite
The granularity of powder or activated carbon is 1 ~ 3 μm.
5. the method for zinc oxide in large size crystal is synthesized using microwave as claimed in claim 1 or 2, it is characterised in that：It is described
Zinc oxide powder granularity is 1 μm, and purity is 99%.
6. the method for zinc oxide in large size crystal is synthesized using microwave as claimed in claim 1, it is characterised in that：The step
（3）In microwave reaction device be microwave Muffle furnace, the condition of reaction is：Heating rate is 10 ~ 30 DEG C/min, and final temperature is
1050 ~ 1100 DEG C, the time for keeping final temperature is 0.5 ~ 1.5h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114150380A (en) * | 2021-10-29 | 2022-03-08 | 中广核研究院有限公司 | Zinc oxide crystal and preparation method thereof |
| CN115504501A (en) * | 2021-06-22 | 2022-12-23 | 中国科学院理化技术研究所 | Microwave heating body zinc oxide and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS642608A (en) * | 1987-06-25 | 1989-01-06 | Oji Paper Co Ltd | Heating promotion material for microwave cooking |
| CN1986909A (en) * | 2006-11-07 | 2007-06-27 | 北京矿冶研究总院 | Technology for preparing tetrapod-like zinc oxide whisker by normal pressure zinc vapour oxidation method |
| CN105755541A (en) * | 2016-03-22 | 2016-07-13 | 中原工学院 | Method for synthesizing zinc oxide whiskers by using microwave-induced combustion synthesis reaction |
| CN105926029A (en) * | 2016-05-09 | 2016-09-07 | 郑州云江科技有限公司 | Method for quick synthesis of zinc oxide whiskers by means of microwaves |
-
2017
- 2017-03-31 CN CN201710208140.1A patent/CN107059124B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS642608A (en) * | 1987-06-25 | 1989-01-06 | Oji Paper Co Ltd | Heating promotion material for microwave cooking |
| CN1986909A (en) * | 2006-11-07 | 2007-06-27 | 北京矿冶研究总院 | Technology for preparing tetrapod-like zinc oxide whisker by normal pressure zinc vapour oxidation method |
| CN105755541A (en) * | 2016-03-22 | 2016-07-13 | 中原工学院 | Method for synthesizing zinc oxide whiskers by using microwave-induced combustion synthesis reaction |
| CN105926029A (en) * | 2016-05-09 | 2016-09-07 | 郑州云江科技有限公司 | Method for quick synthesis of zinc oxide whiskers by means of microwaves |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115504501A (en) * | 2021-06-22 | 2022-12-23 | 中国科学院理化技术研究所 | Microwave heating body zinc oxide and preparation method and application thereof |
| CN115504501B (en) * | 2021-06-22 | 2023-10-24 | 中国科学院理化技术研究所 | Microwave heating element zinc oxide and preparation method and application thereof |
| CN114150380A (en) * | 2021-10-29 | 2022-03-08 | 中广核研究院有限公司 | Zinc oxide crystal and preparation method thereof |
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