CN110228819A - A kind of hydrothermal preparing process of nano zirconium oxide powder - Google Patents
A kind of hydrothermal preparing process of nano zirconium oxide powder Download PDFInfo
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- CN110228819A CN110228819A CN201910609573.7A CN201910609573A CN110228819A CN 110228819 A CN110228819 A CN 110228819A CN 201910609573 A CN201910609573 A CN 201910609573A CN 110228819 A CN110228819 A CN 110228819A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The present invention relates to function powder material preparation technical field more particularly to a kind of hydrothermal preparing process of nano zirconium oxide powder, and preparation method is with ZrOCl2·8H2O is raw material, obtains nano zirconium oxide powder after hydro-thermal reaction, then after washed, calcining, specially takes ZrOCl2·8H2O, which is dissolved in deionized water, obtains zirconyl chloride solution, hydrogen peroxide is added, it stirs and is placed in hydrothermal reaction kettle, and it is passed through oxygen and carries out hydro-thermal reaction, after the reaction was completed, it is cooled to room temperature discharging, is filtered, Washing of Filter Cake, without chloride ion, then obtains nano zirconium oxide powder to cleaning solution after calcining.A kind of hydrothermal preparing process of nano zirconium oxide powder of the invention, simplifies preparation process, reduces experimental facilities requirement, and the diameter of particle prepared is smaller, good dispersion, purity is high.
Description
Technical field
The present invention relates to function powder material preparation technical field more particularly to a kind of hydro-thermal systems of nano zirconium oxide powder
Preparation Method.
Background technique
Zirconia ceramics is shielded with no signal, high tenacity, high-flexural strength and high-wearing feature, excellent heat-proof quality etc.
Advantage has good application prospect in mobile phone backboard and frame field, has excellent biocompatibility and corrosion resistance, make
What it became that best full porcelain tooth is preced with prepares material, while sensitive unit for electrical property parameters, can be mainly used in lambda sensor,
The fields such as solid oxide fuel cell and high temperature exothermic body.But pure zirconia ceramics is at room temperature easily from tetragonal phase converting
At monoclinic phase, the cracking of ceramics is caused, and by stably-doped dose of yttrium oxide, the Zirconium powder of tetragonal phase can be made in room temperature
Exist in stable state down, changing pure zirconia ceramics leads to ceramic cracking at monoclinic phase from tetragonal phase converting at room temperature
Critical defect.
Currently, mobile phone backboard and frame material are mainly mainly made of metal materials, and with the arrival that 5G is communicated, metal material
Lead to declining to a great extent for signal and data transmission bauds due to the shielding action to signal, the development for being unable to satisfy 5G communication is wanted
It asks.Zirconia ceramics material has many advantages, such as that no signal shielding, intensity is big, hardness is high, toughness is strong, good drop resistant performance, is
The emphasis of current phone backboard and frame Materials, and adapt to current phone material high-endization, the effective measures of differentiation.
The performance quality of nano zirconium oxide powder has decisive role for the performance of zirconia ceramics.Therefore, it to mention
The performance of high zirconia ceramics, needs to solve the technology of preparing of high-performance nano Zirconium powder.Current nano zirconium oxide powder
Preparation method mainly use hydro-thermal method, the nano zirconium oxide powder partial size of hydro-thermal method preparation is small, with high purity, good dispersion, but
Its high requirements on the equipment, required technical difficulty is big, poor safety performance.
Summary of the invention
In view of this, simplifying system the object of the present invention is to provide a kind of hydrothermal preparing process of nano zirconium oxide powder
Standby technique reduces experimental facilities requirement, and the diameter of particle prepared is smaller, good dispersion, purity is high.
The present invention solves above-mentioned technical problem by following technological means:
A kind of hydrothermal preparing process of nano zirconium oxide powder, the preparation method is with ZrOCl2·8H2O is raw material, in acid
Property under the conditions of, after hydro-thermal reaction, then it is washed, calcining obtain nano zirconium oxide powder.
Further, the preparation method specifically: take ZrOCl2·8H2O is dissolved in deionized water that obtain zirconium oxychloride molten
Liquid is added hydrogen peroxide, stirs and be placed in hydrothermal reaction kettle, and is passed through oxygen and carries out hydro-thermal reaction, and reaction is completed
Afterwards, it is cooled to room temperature discharging, is filtered, Washing of Filter Cake to cleaning solution is without chloride ion, then obtains nano zirconium oxide powder after calcining.
Further, the concentration of the zirconyl chloride solution is 0.1~4mol/L.
Further, the temperature of the hydro-thermal reaction is 100~300 DEG C, and the reaction time is 2~72h.
Further, when the hydro-thermal reaction, the amount of fill of hydrothermal reaction kettle is not more than the 80% of reaction kettle dischargeable capacity.
Further, the volume ratio of the hydrogen peroxide and zirconyl chloride solution is (0.2~4): 10.
Further, the temperature of the calcining is 1000 DEG C, calcination time 2h.
Compared with the existing technology, the invention has the benefit that
1, it is usually that the precipitating reagents such as ammonium hydroxide are added in basic zirconium chloride that existing hydro-thermal method, which prepares the preparation method of zirconium oxide, makes it
It generates zirconium hydroxide and carries out hydro-thermal reaction again；And the present invention is directly directly coordinated using zirconium oxychloride with water under the high temperature conditions
Karyogenesis zirconium hydroxide, and on the one hand the oxygen in the zirconium hydroxide generated decomposes generation in water-heat process from basic zirconium chloride
Oxygen；On the other hand the oxygen released is decomposed in water-heat process from hydrogen peroxide, so that basic zirconium chloride total overall reaction generates
Zirconium hydroxide, entire reaction process when avoiding existing hydro-thermal method and preparing Zirconium powder, are first added it is not necessary that precipitating reagent is added
The big problem of nonhomogen-ous nucleation growth bring particle diameter distribution caused by precipitating reagent, therefore preparation method of the invention can be made
Standby uniform particle diameter, and mono-dispersed nano Zirconium powder out.
2, the hydrothermal preparing process of nano zirconium oxide powder of the invention effectively prevents the use of precipitating reagent, can be in acid
Property under the conditions of directly prepare Zirconium powder, saved material, simplified preparation process, reduced production cost, be suitble to
In the stable mass production of Zirconium powder.
Detailed description of the invention
The SEM for the nano zirconium oxide powder that Fig. 1 embodiment of the present invention one is prepared schemes；
The XRD diagram for the nano zirconium oxide powder that Fig. 2 embodiment of the present invention one is prepared；
The SEM figure for the zirconia ceramics that nano zirconium oxide powder sinters into is prepared using embodiment one by Fig. 3.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in detail:
The hydrothermal preparing process of a kind of nano zirconium oxide powder of the invention, with ZrOCl2·8H2O is raw material, in acid item
Under part, nano zirconium oxide powder is obtained after hydro-thermal reaction, then after washed, calcining.
Embodiment one
(1) ZrOCl is taken2·8H2O is dissolved in deionized water, and it is molten that preparation obtains the zirconium oxychloride that concentration is 0.5mol/L
The volume ratio of liquid, addition hydrogen peroxide, hydrogen peroxide and zirconyl chloride solution is 1:10.
(2) after stirring, configured solution is fitted into hydrothermal reaction kettle, and be passed through oxygen, control loads
Amount is not more than the 80% of reaction kettle dischargeable capacity, and reacts 12h under the conditions of 180 DEG C.
(3) after the reaction was completed, it discharges, filters after reaction kettle is cooled to room temperature, filter cake is washed with deionized to washing
Liquid is without chloride ion.
(4) product after above-mentioned washing is put into crucible, through 1000 DEG C of calcining 2h, obtains nano zirconium oxide powder.
The SEM for the nano zirconium oxide powder being prepared schemes as shown in Figure 1, XRD diagram is as shown in Fig. 2, Fig. 3 is to utilize preparation
The SEM for the zirconia ceramics that obtained nano zirconium oxide powder sinters into schemes.
Embodiment two
(1) ZrOCl is taken2·8H2O is dissolved in deionized water, and it is molten that preparation obtains the zirconium oxychloride that concentration is 1.0mol/L
The volume ratio of liquid, addition hydrogen peroxide, hydrogen peroxide and zirconyl chloride solution is 2:10.
(2) after stirring, configured solution is fitted into hydrothermal reaction kettle, and be passed through oxygen, control loads
Amount is not more than the 80% of reaction kettle dischargeable capacity, and reacts 8h under the conditions of 220 DEG C.
(3) after the reaction was completed, it discharges, filters after reaction kettle is cooled to room temperature, filter cake is washed with deionized to washing
Liquid is without chloride ion.
(4) product after above-mentioned washing is put into crucible, through 1000 DEG C of calcining 2h, obtains nano zirconium oxide powder.
Embodiment three
(1) ZrOCl is taken2·8H2O is dissolved in deionized water, is prepared and is obtained the zirconyl chloride solution that concentration is 4mol/L,
The volume ratio of addition hydrogen peroxide, hydrogen peroxide and zirconyl chloride solution is 4:10.
(2) after stirring, configured solution is fitted into hydrothermal reaction kettle, and be passed through oxygen, control loads
Amount is not more than the 80% of reaction kettle dischargeable capacity, and reacts 2h under the conditions of 300 DEG C.
(3) after the reaction was completed, it discharges, filters after reaction kettle is cooled to room temperature, filter cake is washed with deionized to washing
Liquid is without chloride ion.
(4) product after above-mentioned washing is put into crucible, through 1000 DEG C of calcining 2h, obtains nano zirconium oxide powder.
Example IV
(1) ZrOCl is taken2·8H2O is dissolved in deionized water, and it is molten that preparation obtains the zirconium oxychloride that concentration is 0.1mol/L
The volume ratio of liquid, addition hydrogen peroxide, hydrogen peroxide and zirconyl chloride solution is 0.2:10.
(2) after stirring, configured solution is fitted into hydrothermal reaction kettle, and be passed through oxygen, control loads
Amount is not more than the 80% of reaction kettle dischargeable capacity, and reacts 72h under the conditions of 100 DEG C.
(3) after the reaction was completed, it discharges, filters after reaction kettle is cooled to room temperature, filter cake is washed with deionized to washing
Liquid is without chloride ion.
(4) product after above-mentioned washing is put into crucible, through 1000 DEG C of calcining 2h, obtains nano zirconium oxide powder.
Embodiment five
(1) ZrOCl is taken2·8H2O is dissolved in deionized water, and it is molten that preparation obtains the zirconium oxychloride that concentration is 2.5mol/L
The volume ratio of liquid, addition hydrogen peroxide, hydrogen peroxide and zirconyl chloride solution is 2.5:10.
(2) after stirring, configured solution is fitted into hydrothermal reaction kettle, and be passed through oxygen, control loads
Amount is not more than the 80% of reaction kettle dischargeable capacity, and reacts 48h under the conditions of 200 DEG C.
(3) after the reaction was completed, it discharges, filters after reaction kettle is cooled to room temperature, filter cake is washed with deionized to washing
Liquid is without chloride ion.
(4) product after above-mentioned washing is put into crucible, through 1000 DEG C of calcining 2h, obtains nano zirconium oxide powder
Obviously, the above embodiment of the present invention only to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.Here all embodiments can not be exhaustive.It is all to belong to this hair
The obvious changes or variations that bright technical solution is extended out are still in the scope of protection of the present invention.
Claims (7)
1. a kind of hydrothermal preparing process of nano zirconium oxide powder, which is characterized in that the preparation method is with ZrOCl2·8H2O is
Raw material, in acid condition, after hydro-thermal reaction, then washed, calcining obtains nano zirconium oxide powder.
2. a kind of hydrothermal preparing process of nano zirconium oxide powder according to claim 1, which is characterized in that the preparation
Method specifically: take ZrOCl2·8H2O, which is dissolved in deionized water, obtains zirconyl chloride solution, and hydrogen peroxide is added, is sufficiently stirred
It is uniformly placed in hydrothermal reaction kettle, and is passed through oxygen progress hydro-thermal reaction and is cooled to room temperature discharging after the reaction was completed, filter,
Washing of Filter Cake, without chloride ion, then obtains nano zirconium oxide powder to cleaning solution after calcining.
3. a kind of hydrothermal preparing process of nano zirconium oxide powder according to claim 2, which is characterized in that the oxygen chlorine
The concentration for changing zirconium solution is 0.1~4mol/L.
4. a kind of hydrothermal preparing process of nano zirconium oxide powder according to claim 3, which is characterized in that the hydro-thermal
The temperature of reaction is 100~300 DEG C, and the reaction time is 2~72h.
5. a kind of hydrothermal preparing process of nano zirconium oxide powder according to claim 2, which is characterized in that the hydro-thermal
When reaction, the amount of fill of hydrothermal reaction kettle is not more than the 80% of reaction kettle dischargeable capacity.
6. a kind of hydrothermal preparing process of nano zirconium oxide powder according to claim 2, which is characterized in that the dioxygen
The volume ratio of water and zirconyl chloride solution is (0.2~4): 10.
7. a kind of hydrothermal preparing process of nano zirconium oxide powder according to any claim from 1 to 6, special
Sign is that the temperature of the calcining is 1000 DEG C, calcination time 2h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111439782A (en) * | 2020-03-04 | 2020-07-24 | 山西新华化工有限责任公司 | Synchronous protection NH3/SO2Preparation method of zirconium hydroxide protective material |
| CN113624835A (en) * | 2020-05-07 | 2021-11-09 | 崔学晨 | Preparation method and application of zirconia particles for detecting atomized DMMP (dimethyl formamide MP) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1524794A (en) * | 2003-02-28 | 2004-09-01 | 中国石油化工股份有限公司 | Hydrothermal synthesis method of zirconia |
| CN101239823A (en) * | 2008-03-03 | 2008-08-13 | 景德镇和川粉体技术有限公司 | Method for preparing nano zirconium oxide powder used for optical communication device by water decomposition method |
| CN101696033A (en) * | 2009-10-23 | 2010-04-21 | 山东理工大学 | Preparation method for synthesizing sheeted zirconia by using hydrothermal method |
| CN109553129A (en) * | 2018-11-23 | 2019-04-02 | 中科合成油技术有限公司 | Nanoscale high dispersive zirconium oxide and preparation method thereof prepares the application in aromatic hydrocarbons in synthesis gas |
-
2019
- 2019-07-08 CN CN201910609573.7A patent/CN110228819A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1524794A (en) * | 2003-02-28 | 2004-09-01 | 中国石油化工股份有限公司 | Hydrothermal synthesis method of zirconia |
| CN101239823A (en) * | 2008-03-03 | 2008-08-13 | 景德镇和川粉体技术有限公司 | Method for preparing nano zirconium oxide powder used for optical communication device by water decomposition method |
| CN101696033A (en) * | 2009-10-23 | 2010-04-21 | 山东理工大学 | Preparation method for synthesizing sheeted zirconia by using hydrothermal method |
| CN109553129A (en) * | 2018-11-23 | 2019-04-02 | 中科合成油技术有限公司 | Nanoscale high dispersive zirconium oxide and preparation method thereof prepares the application in aromatic hydrocarbons in synthesis gas |
Non-Patent Citations (4)
| Title |
|---|
| J.M.E. MATOS等: "Reflux synthesis and hydrothermal processing of ZrO2 nanopowders at low temperature", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
| TATIANE M等: "Stable colloidal suspensions of nanostructured zirconium oxide synthesized by hydrothermal process", 《J NANOPART RES》 * |
| 朱洪法等: "《催化剂手册》", 31 August 2008, 金盾出版社 * |
| 李飞等: "水热法制备纳米氧化锆煅烧过程中晶粒生长特性研究", 《RARE METAL MATERIALS AND ENGINEERING》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111439782A (en) * | 2020-03-04 | 2020-07-24 | 山西新华化工有限责任公司 | Synchronous protection NH3/SO2Preparation method of zirconium hydroxide protective material |
| CN111439782B (en) * | 2020-03-04 | 2022-07-29 | 山西新华防化装备研究院有限公司 | Synchronous protection NH 3 /SO 2 Preparation method of zirconium hydroxide protective material |
| CN113624835A (en) * | 2020-05-07 | 2021-11-09 | 崔学晨 | Preparation method and application of zirconia particles for detecting atomized DMMP (dimethyl formamide MP) |
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