CN109574073A - A kind of preparation method of high dispersion nanometer oxide zirconium powder - Google Patents
A kind of preparation method of high dispersion nanometer oxide zirconium powder Download PDFInfo
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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Abstract
The invention belongs to ceramic powders preparation technical field more particularly to a kind of preparation methods of high dispersion nanometer oxide zirconium.The present invention is metal-modified by doping yttrium, presoma is prepared using coprecipitation combines the nano zirconium oxide powder for obtaining a kind of high-purity high dispersive with hydrothermal crystallizing, also pass through ultrafiltration composite membrane technology simultaneously, remove the foreign ion in presoma, the more effective effect for playing mineralizer and controlling crystal form and particle dispersion in hydro-thermal reaction, concentration of the Zirconium powder in presoma is improved, the nano-powder of purity high yield is obtained.The stable nano zirconium oxide powder of yttrium prepared by the method for the present invention, its grain shape is the excellent properties such as spherical, particle diameter distribution is narrow, good dispersion, purity is high, soilless sticking, it can be widely applied to high-end bioceramic material, current zirconia material is solved in the material fragility caused by crystal transfer process, keeps zirconia ceramics flexible in application, extensive.
Description
Technical field
The invention belongs to ceramic powders preparation technical field more particularly to a kind of preparations of high-purity high dispersion nanometer oxide zirconium
Method.
Background technique
Zirconia ceramic have excellent physical and chemical properties, can resist rotten, wear-resistant, shock resistance, it is heat-insulated, every porcelain,
It is resistant to high temperatures and every characteristics such as electricity, it is widely used in catalysis, oxygen sensitive sensor, high-temperature solid fuel cell, fire proofed wood
Expect chemically inert surface's material, decorative appearance material and biomaterial etc., becomes one of the hot spot researched and developed now.
Zirconium dioxide (ZrO2) has a kind of special property --- martensitic traoformation, with the variation of temperature, ZrO2 structure
It can change, low temperature is monoclinic zro2 (m-ZrO2), and high temperature is completely reformed into cubic ZrO2 (t-ZrO2) to 1170 DEG C, then
It is warming up to 2370 DEG C to be changed into cubic ZrO 2 (c- ZrO2), while this is a reversible phase transition process again, and transition process
In along with shear strain and volume change, so that the thermal shock resistance of zirconia material is substantially reduced and is led to material cracks, sternly
The application of zirconia ceramic is limited again.Therefore, in order to reduce the influence of phase transformation, can be made by adding yttrium oxide (Y2O3)
T-ZrO2 is stable at room temperature.From 1975, the first discoveries such as Australian Scientists Gavie mixed yttrium type zirconium oxide phase transformation increasing
Since tough mechanism, currently, advanced Zirconium powder manufacturer both at home and abroad, such as Japanese Tosoh, domestic tricyclic group, special
Sharp CN102803180A, EP0140638B1, CN201510309285 etc. are all made of doped yttrium and obtain stable cubic phase oxidation
Zirconium.
Meanwhile the good zirconium dioxide of processability, the average particle size that powder requirement further includes powder is less than
100nm, shape are spherical shape, hard aggregation-free, purity is high, chemical composition are uniform, narrow particle size distribution, therefore the pottery of high-purity high dispersive
Porcelain powder is the key factor for determining powder characteristic, if powder reuniting seriously will affect the sintering of ceramics, increase sintering temperature
Deng.Currently, the method for preparing Zirconium powder has Hydrolyze method, the precipitation method, microemulsion method, hydro-thermal method, high-temperature spray pyrolysismethod, spray
Mist inductively coupled plasma method and freeze-drying, wherein coprecipitation process requires simply and readily to add other oxidations
Object is as stabilizer, but the method is readily incorporated other impurity elements and purity is caused to decline, the more difficult washing of colloidal precipitating of formation,
The rate of filtration is slow, and needs high-temperature calcination, is easy to appear blocking reunion in the drying process；And hydro-thermal method can be directly from molten
Crystalline oxides are obtained in liquid, avoid the calcine technology that traditional hydroxide is transformed into oxide, and its partial size and pattern
Controllably, the introducing of introduced contaminants is reduced, reduces the possibility for generating hard aggressiveness, but entire high process cost, yield are lower.
Therefore, it is necessary to provide a kind of effective preparation method, the nano oxidized zirconium powder of high-purity high dispersive high yield is obtained
Body.
Summary of the invention
In view of the above problems, the present invention is metal-modified by doping yttrium, prepare presoma using coprecipitation and hydro-thermal is brilliant
Change and combine the preparation method of the nano zirconium oxide powder for obtaining high-purity high dispersive a kind of, in order to improve powder purity and
The yield of product, the present invention also pass through ultrafiltration composite membrane technology, remove the foreign ion in presoma, improve Zirconium powder and exist
The yield of concentration and final powder in presoma；And the method that mineralizer is added in water-heat process, it is received with reaching raising
The dispersibility of rice corpuscles in the solution, avoids the reunion of particle.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of high-purity high dispersion nanometer oxide zirconium raw powder's production technology, which is characterized in that this method includes following step
It is rapid:
A. inorganic zirconium salts and inorganic yttrium salts are placed in container by mole 100:2~4, add deionized water, with
Zirconium ion concentration is configured in 0.2~1mol/L, uniform stirring to clear solution；
B. 1~5% dispersing agent (with weighed zirconates in step A and yttrium salt quality summation meter) is weighed, and step A is added
In the clear solution of preparation, it is stirred at room temperature；
C. the mixing speed in rate-determining steps B, is slowly added dropwise precipitating reagent in the solution, until solution ph is at 8~14
Reaction terminates；
D. at normal temperature by precipitated liquid made from step C, after being aged 12~72 hours, Ceramic Composite membrane separation plant is added
In, ultrafiltration is carried out with deionized water to precipitating reagent and is cleaned, the foreign ion in filtrate is removed, until using 0.1mol/L silver nitrate
Solution is tested, and chloride ion-containing, obtained hydronium(ion) do not aoxidize zirconium precursor body in filtrate, and controlled concentration is 5~10%；
E. precursor solution made from a certain amount of step D is taken to be added in hydrothermal reaction kettle, and the mineralizer being added is molten
In 0.1mol/L~0.5mol/L, hydrothermal temperature is 180~220 DEG C for concentration control in liquid, and the hydro-thermal time is 6~18 hours,
Then it cools down at room temperature, completes hydro-thermal reaction；
F. step E solution after cooling is poured out into reaction kettle, Ceramic Composite membrane separation plant is added herein, uses deionized water
It is dehydrated after carrying out cleaning 1 hour, then natural air drying at room temperature, last 70~120 DEG C of dryings 3 hours nano oxidized to get arriving
Zirconium powder body；
Inorganic zirconium salts in step (A) are selected from one or both of zirconium oxychloride, zirconium nitrate；
Inorganic yttrium salts described in step (A) are selected from one or both of yttrium nitrate, yttrium chloride.
Dispersing agent in step (B) is selected from Liquid Macrogol, polyethylene glycol 400, polyethylene glycol 500, Macrogol 600
One of；
Precipitating reagent in step (C) can be selected from one of ammonium hydroxide, sodium hydroxide, urea, potassium hydroxide, sodium carbonate；
Mineralizer in step (E) be selected from ethanol amine, diethanol amine, triethanolamine, glycerine, ethylene glycol monomethyl ether one kind
Or two kinds.
The last Zirconium oxide nano grain obtained of the present invention, grain diameter 20~30nm and particle diameter distribution it is narrow, point
Scattered property is good, and the purity for mixing yttrium Zirconium powder reaches 99.0% or more, is calculated by the mass percent of zirconium ion, final 90%
Above zirconium oxychloride is prepared into Zirconium powder.And the zirconium ion presoma of high concentration, after adding mineralizer, hydro-thermal reaction
Powder dispersity obtained is good, without agglomeration.The Zirconium powder of good performance can be applied to high-end biology pottery
Ceramic material, finished product are related to mobile fingerprint identification piece, wireless charging wearing wrist-watch appearance member, engine components, bioscience component
(such as Dental Erosion, joint repair) field.
Beneficial effects of the present invention are as follows:
1) present invention is easy pH value, the concentration of organic mineralizer, hydro-thermal by inquiring into presoma on the basis of many experiments
The influence of temperature, hydro-thermal time to powder crystallinity energy obtains dispersed good, particle diameter distribution to obtain optimal experiment condition
Narrow mixes yttrium nm-class powder of zirconium oxide；
2) Ceramic Composite membrane separation plant is used, the foreign ion in precursor solution is effectively removed, improves zirconium ion
Purity, it is often more important that eliminate influence of the foreign ion in hydro-thermal reaction for ion crystal form, obtain the oxygen of tetragonal phase
Change zirconium crystal；
3) preparation improves the yield of nano zircite, while preparing under High Concentration Situation, and hydro-thermal reaction remains to point
It is good to dissipate property, the Zirconium powder that do not reunite.
Detailed description of the invention
Fig. 1 is the XRD diagram of products obtained therefrom in the embodiment of the present invention 1
Fig. 2 is the TEM figure of products obtained therefrom in the embodiment of the present invention 1
Specific embodiment
After now specific embodiments of the present invention are described in.
Embodiment 1
A kind of high-purity high dispersion nanometer oxide zirconium raw powder's production technology, method includes the following steps:
A. drug 131g ZrOCl28H2O and 3.88gYCl36H2O are weighed, is placed in container, deionization is added
Water is to 1L, to configure zirconium ion concentration in 0.4mol/L, uniform stirring to clear solution；
B. 2g polyethylene glycol 400 is weighed, and is added in the clear solution of step A preparation, is stirred at room temperature；
C. the mixing speed in rate-determining steps B, is slowly added dropwise the NaOH solution of 1mol/L in the solution, until solution ph
Reacting at 10 terminates；
D. at normal temperature by precipitated liquid made from step C, after being aged 24 hours, it is added in Ceramic Composite membrane separation plant,
Ultrafiltration is carried out with deionized water to precipitating reagent to clean, removes the foreign ion in filtrate, until molten using 0.1mol/L silver nitrate
Liquid is tested, and chloride ion-containing, obtained hydronium(ion) do not aoxidize zirconium precursor body in filtrate, and controlled concentration is 6%；
E. tri- ethyl alcohol of 30g for taking precursor solution made from a certain amount of step D to be added in hydrothermal reaction kettle, and being added
In the solution, hydrothermal temperature is 180 DEG C to amine, and the hydro-thermal time is 18 hours, is then cooled down at room temperature, and hydro-thermal reaction is completed；
F. step E solution after cooling is poured out into reaction kettle, Ceramic Composite membrane separation plant is added herein, uses deionized water
It is dehydrated after carrying out cleaning 1 hour, then natural air drying at room temperature, last 70 DEG C of drying 3 hours are to get to nano oxidized zirconium powder
Body；
Sample manufactured in the present embodiment, by XRD diagram 1 it can be seen that is obtained is tetragonal phase zirconium oxide crystal, partial size is logical
The calculating of xrd half-peak breadth and scanning transmission electron microscope are crossed, the zirconia powder for obtaining that primary particle size mean value is 25nm or so can be calculated
Body.Grain shape can be observed as spherical, particle diameter distribution is narrow, good dispersion by TEM Fig. 2, soilless sticking phenomenon, and finally mix yttrium oxygen
Change zirconium powder purity and reaches 99% or more.
Embodiment 2
A kind of high-purity high dispersion nanometer oxide zirconium raw powder's production technology, method includes the following steps:
A. it weighs drug 131g ZrOCl28H2O to be placed in container, adds deionized water to 0.5L, to configure zirconium ion
Concentration is in 0.8mol/L, then weighs 1.5g yttrium oxide and be dissolved in concentrated nitric acid, is added in zirconium solution after dissolution to be mixed, uniformly stirs
It mixes to clear solution；
B. 2g polyethylene glycol 400 is weighed, and is added in the clear solution of step A preparation, is stirred at room temperature；
C. the mixing speed in rate-determining steps B, is slowly added dropwise the ammonia spirit of 25% mass percent concentration in the solution,
Until solution ph is reacted at 9 and is terminated；
D. at normal temperature by precipitated liquid made from step C, after being aged 18 hours, it is added in Ceramic Composite membrane separation plant,
Ultrafiltration is carried out with deionized water to precipitating reagent to clean, removes the foreign ion in filtrate, until molten using 0.1mol/L silver nitrate
Liquid is tested, and chloride ion-containing, obtained hydronium(ion) do not aoxidize zirconium precursor body in filtrate, and controlled concentration is 8%；
E. the 35g glycerine for taking precursor solution made from a certain amount of step D to be added in hydrothermal reaction kettle, and being added
In the solution, hydrothermal temperature is 200 DEG C, and the hydro-thermal time is 18 hours, is then cooled down at room temperature, completes hydro-thermal reaction；
F. step E solution after cooling is poured out into reaction kettle, Ceramic Composite membrane separation plant is added herein, uses deionized water
It is dehydrated after carrying out cleaning 1 hour, then natural air drying at room temperature, last 110 DEG C of drying 3 hours are to get to nano oxidized zirconium powder
Body；
Sample manufactured in the present embodiment obtains the Zirconium powder that primary particle size mean value is 20nm or so, grain diameter point
Cloth is narrow, good dispersion, soilless sticking phenomenon, and finally mixing yttrium Zirconium powder purity reaches 99% or more.
Although the present invention has already been described in detail in the embodiment, itself is simultaneously not considered as to limit of the invention
System.The invention is not limited to above embodiment, using same as the previously described embodiments or similar raw material and preparation method or
All changes, equivalents and the improved preparation method within the context described in it are chased after, in protection model of the invention
Within enclosing.
Claims (5)
1. high dispersion nanometer oxide zirconium raw powder's production technology, which is characterized in that method includes the following steps:
A. inorganic zirconium salts and inorganic yttrium salts are placed in container by mole 100:2~4, add deionized water, with configuration
Zirconium ion concentration is in 0.2~1mol/L, uniform stirring to clear solution；
B. 1~5% dispersing agent (with weighed zirconates in step A and yttrium salt quality summation meter) is weighed, and step A preparation is added
Clear solution in, be stirred at room temperature；
C. the mixing speed in rate-determining steps B, is slowly added dropwise precipitating reagent in the solution, until solution ph is reacted at 8~14
Terminate；
D. at normal temperature by precipitated liquid made from step C, after being aged 12~72 hours, it is added in Ceramic Composite membrane separation plant,
Ultrafiltration is carried out with deionized water to precipitating reagent to clean, removes the foreign ion in filtrate, until molten using 0.1mol/L silver nitrate
Liquid is tested, and chloride ion-containing, obtained hydronium(ion) do not aoxidize zirconium precursor body in filtrate, and controlled concentration is 5~10%；
E. precursor solution made from a certain amount of step D is taken to be added in hydrothermal reaction kettle, the mineralizer of addition is in the solution
In 0.1mol/L~0.5mol/L, hydrothermal temperature is 180~220 DEG C for concentration control, and the hydro-thermal time is 6~18 hours, is then existed
It cools down at room temperature, completes hydro-thermal reaction；
F. step E solution after cooling is poured out into reaction kettle, Ceramic Composite membrane separation plant is added herein, is carried out with deionized water
Cleaning is dehydrated after 1 hour, and last 70~120 DEG C of drying 3 hours are to get to nano zirconium oxide powder；
Inorganic zirconium salts in step (A) are selected from one or both of zirconium oxychloride, zirconium nitrate；
Inorganic yttrium salts described in step (A) are selected from one or both of yttrium nitrate, yttrium chloride；
Dispersing agent in step (B) is in Liquid Macrogol, polyethylene glycol 400, polyethylene glycol 500, Macrogol 600
It is a kind of；
Precipitating reagent in step (C) can be selected from one of ammonium hydroxide, sodium hydroxide, urea, potassium hydroxide, sodium carbonate；
Mineralizer in step (E) be selected from one of ethanol amine, diethanol amine, triethanolamine, glycerine, ethylene glycol monomethyl ether or
Two kinds.
2. a kind of preparation method of the nano zircite of high-purity high dispersive according to claim 1, which is characterized in that institute
Stating Zirconium powder is tetragonal phase zirconium oxide, and grain diameter is in 20~30nm and particle diameter distribution is narrow, good dispersion.
3. a kind of preparation method of the nano zircite of high-purity high dispersive according to claim 1, characteristic are, most
90% or more zirconium oxychloride is prepared into Zirconium powder eventually, and the loss late of raw material is lower in preparation process.
4. a kind of preparation method of the nano zircite of high-purity high dispersive according to claim 1, characteristic are, pottery
The compound membrane separation plant of porcelain can efficiently remove the foreign ion in reaction solution, retain hydronium(ion) zirconium oxide sediment, make final
The purity for mixing yttrium Zirconium powder reaches 99.0% or more.
5. a kind of preparation method of the nano zircite of high-purity high dispersive according to claim 1, characteristic are, root
It, can according to different mineralizers and mineralizer concentration, control presoma pH value, the hydro-thermal reaction time and hydrothermal temperature is selected
Under the conditions of the zirconium ion presoma of high concentration, still obtainable good dispersion after hydro-thermal reaction, the not no nanometer of agglomeration
Zirconium powder.
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Cited By (18)
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|---|---|---|---|---|
| CN110203969A (en) * | 2019-06-28 | 2019-09-06 | 河南科技大学 | A kind of high dispersive cubic phase nano zirconium oxide and preparation method thereof |
| CN110586058A (en) * | 2019-10-10 | 2019-12-20 | 河南科技大学 | Preparation method of nano titanium dioxide/zirconium oxide composite photocatalyst |
| CN111205088A (en) * | 2020-01-15 | 2020-05-29 | 中国恩菲工程技术有限公司 | Method for preparing scandia-stabilized zirconia powder by hydrothermal method and scandia-stabilized zirconia powder prepared by method |
| CN111320479A (en) * | 2020-03-06 | 2020-06-23 | 山东国瓷功能材料股份有限公司 | Nano zirconium oxide material, preparation method and application thereof |
| CN111646506A (en) * | 2020-07-21 | 2020-09-11 | 宁德三祥纳米新材料有限公司 | Method for preparing nano zirconium oxide by internal gel method |
| CN111825450A (en) * | 2020-07-21 | 2020-10-27 | 宁德三祥纳米新材料有限公司 | Method for preparing nano zirconia by gel-hydrothermal process |
| CN111848161A (en) * | 2020-08-05 | 2020-10-30 | 上海大学(浙江·嘉兴)新兴产业研究院 | Preparation method of nano zirconia powder |
| CN111960466A (en) * | 2020-08-20 | 2020-11-20 | 苏州锦艺新材料科技有限公司 | Preparation method of nano zirconia hollow sphere |
| CN112125663A (en) * | 2020-08-14 | 2020-12-25 | 广东省科学院稀有金属研究所 | Preparation method of monodisperse yttria-stabilized zirconia nano powder |
| CN112266244A (en) * | 2020-10-14 | 2021-01-26 | 安徽元琛环保科技股份有限公司 | Preparation method of high-sintering-activity zirconium oxide powder |
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| CN112624191A (en) * | 2020-09-25 | 2021-04-09 | 无锡晟源泰新材料科技有限公司 | Precursor ingredient for preparing tetragonal nano zirconia and method for producing tetragonal nano zirconia under low temperature condition |
| 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) |
| CN116102350A (en) * | 2022-12-27 | 2023-05-12 | 中铝广西有色稀土开发有限公司 | Preparation method of spherical composite zirconia powder |
| CN116161958A (en) * | 2022-12-27 | 2023-05-26 | 中铝广西有色稀土开发有限公司 | Preparation method of yttrium-stabilized zirconia nano-powder |
| CN116262662A (en) * | 2021-12-14 | 2023-06-16 | 东莞市陶陶新材料科技有限公司 | Submicron spherical zirconia powder and preparation method thereof, and zirconia ceramic |
| CN117228715A (en) * | 2023-11-10 | 2023-12-15 | 琥崧科技集团股份有限公司 | Preparation method of zirconium dioxide sintered body |
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