CN102849784A - Method and apparatus used for producing nano-grade zinc oxide through plasma gas-phase reaction - Google Patents
Method and apparatus used for producing nano-grade zinc oxide through plasma gas-phase reaction Download PDFInfo
- Publication number
- CN102849784A CN102849784A CN2012101441981A CN201210144198A CN102849784A CN 102849784 A CN102849784 A CN 102849784A CN 2012101441981 A CN2012101441981 A CN 2012101441981A CN 201210144198 A CN201210144198 A CN 201210144198A CN 102849784 A CN102849784 A CN 102849784A
- Authority
- CN
- China
- Prior art keywords
- plasma
- temperature
- zinc oxide
- reaction
- zinc
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000010574 gas phase reaction Methods 0.000 title claims abstract description 13
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 26
- 239000011701 zinc Substances 0.000 claims abstract description 26
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 239000000047 product Substances 0.000 claims abstract description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000001301 oxygen Substances 0.000 claims abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 8
- 238000000859 sublimation Methods 0.000 claims abstract description 6
- 230000008022 sublimation Effects 0.000 claims abstract description 6
- 230000003647 oxidation Effects 0.000 claims description 19
- 238000007254 oxidation reaction Methods 0.000 claims description 19
- 239000003517 fume Substances 0.000 claims description 15
- 238000004821 distillation Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 7
- 230000001590 oxidative effect Effects 0.000 claims description 6
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 4
- 229910001882 dioxygen Inorganic materials 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 238000005272 metallurgy Methods 0.000 abstract 1
- 229960001296 zinc oxide Drugs 0.000 description 22
- 238000005516 engineering process Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Images
Abstract
The invention relates to a method and an apparatus used for producing nano-grade zinc oxide through a plasma gas-phase reaction. The invention belongs to metallurgy and chemical-engineering nano-grade novel materials. According to the invention, high-frequency oxygen plasma or air plasma is delivered into a reactor; metal zinc vapor is delivered into the reactor; in the reactor, zinc vapor is subjected to a reaction with oxygen in the plasma, such that zinc oxide is produced; the reaction temperature is controlled above a zinc oxide sublimation temperature, such that a high-temperature reaction product composed of sublimation-state zinc oxide and plasma tail-flame is obtained; the high-temperature reaction product is delivered into an air cooling device, and is rapidly cooled to a temperature below 423K, such that nano-grade zinc oxide powder is formed; the powder is collected by a filter bag, such that nano-grade zinc oxide finished product with particle size of 15-50nm and specific surface area of 40-80m<2>/g is obtained. With the method and the apparatus provided by the invention, no three-waste is caused during a production process. The production method is simple, and production cost is low. The product has good dispersity, and is prevented from agglomerate after long-time storage. The surface of the powder is not modified, such that characteristics of original-state nano-grade particles are maintained.
Description
Technical field:
The present invention relates to a kind of plasma (orifice) gas phase reaction and produce the method and apparatus of nano zine oxide, belong to metallurgical, chemical industry nanometer field of new.
Background technology:
Zinc oxide is the inorganic functional material that a kind of quilt is extensive and widely apply, total consumption of the annual various zinc oxide of China is about more than 1,200,000 tons, because production technology, quality product, the reasons such as production cost, wherein the consumption of nano zine oxide seldom, only account for about 1% of total consumption, nano zine oxide refers to that particle size is less than the Zinc oxide powder of 100 nanometers (nm), because utmost point granular and the high-specific surface area of nanometer powder crystal grain, make it have the surface and interface effect, quantum size effect, volume effect and macro quanta tunnel effect, thereby make nano zine oxide at chemical industry, electronics, pottery, space flight, optics, it is special that many fields such as medicine have obtained, important using value, along with the progress of science and technology, the application percentage of expectation nano zine oxide in the total consumption of zinc oxide will be brought up to 3-5%.
The preparation method of nano zine oxide can be divided into the methods such as liquid phase method, solid phase method, vapor phase process, comprehensive crossover substantially, the overwhelming majority's in the market nano zine oxide industrialization product, the method of producing all is attended by single or many production links such as liquid phase reaction and precipitation, drying, calcining, its production process is wayward, production cost is high, and quality product is difficult to satisfy the requirement of some special applications.
Plasma body is the 4th attitude of material, a kind of by molecule, atom, ion, the molecular ionized gas of electronics and light, it presents the labile state that highly excites, the present invention utilizes the oxygen that is plasma state in the plasma body and the zinc fume of gaseous state to carry out oxidizing reaction, under the condition that is higher than the zinc oxide sublimation temperature, obtain distillation attitude zinc oxide, distillation attitude zinc oxide not yet is completed in temperature-fall period in the situation that solid crystal or nucleus not yet grow up, thereby sharply cooled off the superfine little state that has kept the zinc oxide nucleus by freezing air, final acquisition granularity is superfine, active high nano zine oxide, compared with the prior art, the present invention has: the production process three-waste free pollution; Production method is easy, without the production cycle, namely produce and get final product; Industrial production cost is low; The plasma heat utilization efficiency is high; Quality product is high, purposes wide, good dispersity, long-term storage are not reunited; The powder that obtains without any finishing and modification, the characteristics such as characteristic that kept the ecosystem nanoparticle to have.
With the similar technology of the present invention publication number being arranged is the Chinese patent of CN1083538A " preparing zinc-oxide by use of plasma method Processes and apparatus ", disclosed is to adopt high-frequency plasma generator that zinc subcarbonate is carried out roasting pyrolysis, pulverizing, refinement, thereby obtains nano level zinc oxide.Famous U.S. Tekna Plasma Systems Inc. (Tekna Plasma Systems Inc) provide plasma technique and equipment, prepared sizes are at nano-powder and spherical powders such as the titanium oxide of 20～100 nanometers, zirconium white, aluminum oxide, silicon oxide, but have no technology and the Product Report similar to the present invention.
Summary of the invention:
An object of the present invention is, provide a kind of plasma (orifice) gas phase reaction to produce the method for nano zine oxide; Another object of the present invention is to provide a kind of plasma (orifice) gas phase reaction to produce the device of nano zine oxide.
The technical scheme of invention:
The method of nano zine oxide is produced in the plasma (orifice) gas phase reaction, it is characterized in that: the method is in a reactor, a kind of in input high frequency oxygen gas plasma or the air plasma, input temp is the metallic zinc steam of 1130～1230K simultaneously, oxygen generation oxidizing reaction in zinc fume and the plasma body generates zinc oxide ZnO, the zinc oxide that generates and flame passes and a small amount of unreacted zinc fume enter the abundant oxidation in assisted oxidation chamber through the outlet of reactor reaction thing, the control temperature of reaction is on the sublimation temperature of zinc oxide, acquisition is the high-temperature reaction product of 1973～2273K by the temperature that distillation attitude zinc oxide and plasma tail flame form, this high-temperature reaction product enters air-cooler from the assisted oxidation chamber, the amount of being transfused to is that the cooling air of 20～50 times of high-temperature reaction product tolerance sharply is cooled under the 423K temperature, form the primary mixture of nano zine oxide powder and cooling air, primary mixture is received powder through filter bag again and is obtained the nano zine oxide finished product through the outlet of air-cooler.
The production equipment of nano zine oxide is produced in the plasma (orifice) gas phase reaction, comprises reactor, air-cooler, it is characterized in that: plasma body input aperture, zinc fume input aperture, reactant outlet are arranged on the described reactor structure; Air-cooler is textural an assisted oxidation chamber, cooling air intake, cooler outlet.The reactant outlet of reactor is terminal to be connected with the assisted oxidation chamber of air-cooler.
Description of drawings:
Accompanying drawing is production equipment structural representation of the present invention.
Be labeled as the 1-reactor in the accompanying drawing, manufactured by high-temperature refractory and metal cools water jacket; 2-plasma body input aperture; , 3-zinc fume input aperture; The outlet of 4-reactor reaction thing; 5-high-temperature refractory lining; The 6-watercooling jacket, the 7-air-cooler; , 8-assisted oxidation chamber; The 9-cooling air intake; The 10-cooler outlet.
Embodiment:
Embodiment 1: shown in accompanying drawing 1, the temperature that high-frequency plasma generator is produced is that the high frequency oxygen gas plasma of 4273～9273K is by plasma body input aperture 2 inputs of reactor, to come from zinc evaporator crucible or zinc re-distillation furnace temperature and be the metallic zinc steam of 1130～1230K by 3 inputs of zinc fume input aperture, zinc oxide 2Zn+O will occur to generate in reactor this moment
2The thermopositive reaction of=2ZnO, according to reaction formula, the actual input of oxygen is by 1.1～1.2 times of inpuies of controlling respectively oxygen gas plasma and zinc fume of theoretical requirement, temperature of reaction is controlled on the sublimation temperature of 1973～2373K scope zinc oxide, the zinc fume of the zinc oxide that reaction generates and flame passes and a small amount of not complete reaction is after reactor reaction thing outlet 4 enters the assisted oxidation chamber 8 abundant oxidations of air-cooler, formation is the high-temperature reaction product of 1973～2273K by the temperature that distillation attitude zinc oxide and plasma tail flame form, this high-temperature reaction product enters air-cooler from the assisted oxidation chamber under the centrifugal induced draught fan effect, distillation attitude zinc oxide not yet is completed in temperature-fall period in the situation that solid crystal or nucleus not yet grow up, be that the cooling air of 20～50 times of high-temperature reaction product tolerance sharply is cooled under the 423K temperature by the input that is entered by cooling air intake 9, thereby the superfine little state that has kept the zinc oxide nucleus, form the primary mixture of nano zine oxide powder and cooling air, primary mixture is through after the outlet 10 of air-cooler, enter traditional powder collecting system through connecting tube, by centrifugal induced draught fan, receive powder through filter bag again and obtain the nano zine oxide finished product.The finished product grain size scope is that 15～50 nanometers, specific surface area are 40～80 meters
2/ gram, loose density 0.22～0.25 gram per centimeter
3
Embodiment 2: shown in accompanying drawing 1, the temperature that high-frequency plasma generator is produced is that the air plasma of 4273～8273K is by plasma body input aperture 2 inputs of reactor, to come from zinc evaporator crucible or zinc re-distillation furnace temperature and be the metallic zinc steam of 1130～1230K by 3 inputs of zinc fume input aperture, zinc oxide 2Zn+O will occur to generate in reactor this moment
2The thermopositive reaction of=2ZnO, according to reaction formula, the actual input of oxygen is by 1.1～1.3 times of inpuies of controlling respectively air plasma and zinc fume of theoretical requirement, temperature of reaction is controlled on the sublimation temperature of 1973～2293K scope zinc oxide, the zinc oxide that reaction generates and flame passes and a small amount of not zinc fume of complete reaction, enter the assisted oxidation chamber 8 abundant oxidations of air-cooler through reactor outlet 4 after, formation is the high-temperature reaction product of 1973～2193K by the temperature that distillation attitude zinc oxide and plasma tail flame form, this high-temperature reaction product enters air-cooler from the assisted oxidation chamber, distillation attitude zinc oxide not yet is completed in temperature-fall period in the situation that solid crystal or nucleus not yet grow up, be that the cooling air of 20～50 times of high-temperature reaction product tolerance sharply is cooled under the 423K temperature by the input that is entered by cooling air intake 9, thereby the superfine little state that has kept the zinc oxide nucleus, form the primary mixture of nano zine oxide powder and cooling air, primary mixture is through after the outlet 10 of air-cooler, enter traditional powder collecting system through connecting tube, by centrifugal induced draught fan, receive powder through filter bag again and obtain the nano zine oxide finished product.The finished product grain size scope is that 20～50 nanometers, specific surface area are 40～75 meters
2/ gram, loose density 0.23～0.25 gram per centimeter
3
Reactor of the present invention, water cooler are provided with cleaning eye, temperature measurer, and temperature of reaction can be by the operational condition of control plasma generator, and coefficient of excess and the watercooling jacket water temperature of oxygen realize in the control oxidizing reaction.Cooling air can be provided by centrifugal induced draught fan, gas blower or other gas transportation facilities.
Assisted oxidation chamber in the accompanying drawing of the present invention and water cooler are made as one, oxidizing chamber outlet downwards, so that clear up fast fouling or maintenance, also reactor and assisted oxidation chamber can be made as a whole or change oxidizing chamber Way out, its using method is described consistent with specification sheets with the result.Because all being existing mature technology the present invention, the preparation of Radio-frequency plasma torch and zinc fume no longer describes in detail.
Claims (5)
1. the method for nano zine oxide is produced in the plasma (orifice) gas phase reaction, it is characterized in that: the method is in a reactor, a kind of in input high frequency oxygen gas plasma or the air plasma, input simultaneously the metallic zinc steam, oxygen generation oxidizing reaction in zinc fume and the plasma body generates zinc oxide ZnO, the zinc oxide that generates and flame passes and a small amount of unreacted zinc fume enter the abundant oxidation in assisted oxidation chamber through the outlet of reactor reaction thing, the control temperature of reaction is on the sublimation temperature of zinc oxide, the high-temperature reaction product that acquisition is comprised of distillation attitude zinc oxide and plasma tail flame, this high-temperature reaction product enters in the air-cooler from the assisted oxidation chamber, the air that is cooled sharply is cooled under the 423K temperature, form the primary mixture of nano zine oxide powder and cooling air, receive powder through filter bag again and obtain the nano zine oxide finished product.
2. the method for nano zine oxide is produced in plasma (orifice) gas phase reaction according to claim 1, and it is characterized in that: the control temperature of the metallic zinc steam of described input is 1130～1230K.
3. the method for nano zine oxide is produced in plasma (orifice) gas phase reaction according to claim 1 and 2, it is characterized in that: by the high-temperature reaction product that distillation attitude zinc oxide and plasma tail flame form, be that temperature is the reaction product of 1973～2273K scope.
4. according to claim 1 or the 3 described plasma (orifice) gas phase reactions method of producing nano zine oxides, it is characterized in that: the cooling air input is 20～50 times of high-temperature reaction product tolerance.
5. the production equipment of nano zine oxide is produced in the plasma (orifice) gas phase reaction, comprises reactor, air-cooler, it is characterized in that: plasma body input aperture, zinc fume input aperture, reactant outlet are arranged on the described reactor structure; Air-cooler is textural an assisted oxidation chamber, cooling air intake, cooler outlet; The reactant outlet of reactor is terminal to be connected with the assisted oxidation chamber of air-cooler.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210144198.1A CN102849784B (en) | 2012-05-10 | 2012-05-10 | Plasma (orifice) gas phase reaction produces the method and apparatus of nano zine oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210144198.1A CN102849784B (en) | 2012-05-10 | 2012-05-10 | Plasma (orifice) gas phase reaction produces the method and apparatus of nano zine oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102849784A true CN102849784A (en) | 2013-01-02 |
| CN102849784B CN102849784B (en) | 2016-08-31 |
Family
ID=47396834
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210144198.1A Expired - Fee Related CN102849784B (en) | 2012-05-10 | 2012-05-10 | Plasma (orifice) gas phase reaction produces the method and apparatus of nano zine oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102849784B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939060A (en) * | 2021-02-05 | 2021-06-11 | 中国人民解放军战略支援部队航天系统部装备部装备保障队 | Zinc oxide nano material and preparation method and application thereof |
| CN115863851A (en) * | 2022-12-01 | 2023-03-28 | 西藏康盛能源开发有限公司 | Energy storage device based on zinc sublimation and oxidation and control method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1083538A (en) * | 1992-08-29 | 1994-03-09 | 中国科学院化工冶金研究所 | The preparing zinc-oxide by use of plasma method Processes and apparatus |
| CN101151214A (en) * | 2004-12-28 | 2008-03-26 | 纳米科技创造私人有限公司 | Nanostructured zinc oxide and a method of producing the same |
| EP1215174B1 (en) * | 1999-08-25 | 2009-09-30 | Showa Denko K.K. | Highly white zinc oxide fine particles and method for preparation thereof |
-
2012
- 2012-05-10 CN CN201210144198.1A patent/CN102849784B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1083538A (en) * | 1992-08-29 | 1994-03-09 | 中国科学院化工冶金研究所 | The preparing zinc-oxide by use of plasma method Processes and apparatus |
| EP1215174B1 (en) * | 1999-08-25 | 2009-09-30 | Showa Denko K.K. | Highly white zinc oxide fine particles and method for preparation thereof |
| CN101151214A (en) * | 2004-12-28 | 2008-03-26 | 纳米科技创造私人有限公司 | Nanostructured zinc oxide and a method of producing the same |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939060A (en) * | 2021-02-05 | 2021-06-11 | 中国人民解放军战略支援部队航天系统部装备部装备保障队 | Zinc oxide nano material and preparation method and application thereof |
| CN115863851A (en) * | 2022-12-01 | 2023-03-28 | 西藏康盛能源开发有限公司 | Energy storage device based on zinc sublimation and oxidation and control method thereof |
| CN115863851B (en) * | 2022-12-01 | 2023-10-10 | 茂炜能源股份有限公司 | Energy storage device based on zinc sublimation and oxidation and control method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102849784B (en) | 2016-08-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109455728B (en) | Device and method for producing high-purity superfine spherical silicon micro powder by heating gas | |
| CN101497432B (en) | Method for preparing single or composite metal oxide by atomizing and oxidizing solution | |
| Hirano et al. | Synthesis of highly crystalline hexagonal cesium tungsten bronze nanoparticles by flame-assisted spray pyrolysis | |
| Liu et al. | Controlled fabrication and characterization of microspherical FeCO3 and α-Fe2O3 | |
| CN101293674A (en) | Method for preparing spindle shaped alpha-Fe2O3 powder | |
| Ozcelik et al. | Synthesis and characterization of iron oxide particles using spray pyrolysis technique | |
| Gholamrezaei et al. | Novel precursors for synthesis of dendrite-like PbTe nanostructures and investigation of photoluminescence behavior | |
| Zhou et al. | Morphology-controlled synthesis of Co3O4 by one step template-free hydrothermal method | |
| Xu et al. | Ethylene glycol assisted spray pyrolysis for the synthesis of hollow BaFe12O19 spheres | |
| CN106830051A (en) | A kind of method for preparing nanometer Zinc oxide powder as raw material with industrial zinc oxide | |
| Cardillo et al. | Highly porous hematite nanorods prepared via direct spray precipitation method | |
| Sun et al. | Preparation of high purity MoO3 through volatilization of technical-grade Mo calcine in water vapor atmosphere | |
| CN101993111A (en) | Method for preparing nanometer vanadous oxide | |
| CN105621485A (en) | Preparation method of vanadium trioxide powder | |
| CN102849784A (en) | Method and apparatus used for producing nano-grade zinc oxide through plasma gas-phase reaction | |
| CN103482681A (en) | Method for preparing monodisperse spherical nano ZnO | |
| Katsuki et al. | Controlled synthesis of hexagonal α-Fe2O3 crystals for ceramic colors by hydrothermal reaction of FeCl3 and NaOH solutions | |
| JP2014019617A (en) | Lithium titanate fine particle and method for manufacturing the same | |
| Rajendran et al. | Preparation and characterization of nanocrystalline CuO powders with the different surfactants and complexing agent mediated precipitation method | |
| CN108083334A (en) | A kind of preparation method of monodisperse spherical nano zirconium dioxide powder body material | |
| CN107759210A (en) | A kind of Yb2SiO5The preparation method of spraying powder | |
| CN104308170A (en) | Superfine iron powder preparation method | |
| CN108640144B (en) | Yttrium oxide double-stage nanosphere and preparation method thereof | |
| CN102990075A (en) | Method for preparing carbon-coated iron nano particles | |
| CN101343043A (en) | Amphoteric metal compound nano-material and method of preparing the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| DD01 | Delivery of document by public notice |
Addressee: Fan Youyu Document name: the First Notification of an Office Action |
|
| DD01 | Delivery of document by public notice |
Addressee: Fan Youyu Document name: Notification to Make Formalities Rectification |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160831 |