CN106587148B - A kind of preparation method of the spherical yttrium stable zirconium oxide nano-powder of size uniform - Google Patents
A kind of preparation method of the spherical yttrium stable zirconium oxide nano-powder of size uniform Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of the spherical yttrium stable zirconium oxide nano-powder of size uniform, it is characterised in that it includes the following steps：Solution is made in zirconium source and yttrium source, adds precipitating reagent in the solution, dispersant is added after being sufficiently stirred, above-mentioned mixed solution is placed in reaction kettle, is first stirred at room temperature, product is obtained after reheating reaction a period of time；The product obtains semi-stability nanoscale yttrium stabilised zirconia by washing and ethyl alcohol washing, freeze-drying；Spherical yttrium stable zirconium oxide nano-powder is prepared after then carrying out thermostabilization processing again.The advantage of the invention is that：Yttrium stable zirconium oxide nano-powder even size distribution prepared by this method, pattern is spherical in shape, and crystallinity is high, the advantages that being stabilized at ambient temperature with tetragonal phase.
Description
Technical field：
The present invention relates to nano material production fields, are specifically exactly a kind of spherical yttrium stable zirconium oxide of size uniform
The preparation method of nano-powder.
Background technology：
Zirconium oxide（ZrO2）It is a kind of very important structural and functional material, there is chemical stability, it is wear-resistant, it leads
Hot coefficient is low, high temperature resistant, the characteristics such as corrosion resistance, thermal stability and impact resistance, is fire resistant covering material, thermal structure material
The important source material of material, biomaterial and electronic material, is widely applied in fields such as energy, material, electronics and environment.
Pure ZrO at room temperature2For white crystal, fusing point is 2680 DEG C, and boiling point is 4275 DEG C.Zirconium dioxide is more than one
Crystal system can be divided into three kinds of crystal forms：Monoclinic system（Monoclinic, m-ZrO2）, tetragonal crystal system（Tetragonal, t-ZrO2）
And cubic system（Cubic, c-ZrO2）.Monoclinic phase is stable phase at room temperature, and tetragonal phase and cubic phase are metastable phases.These are brilliant
Reversible phase transition can occur between type, while causing great bulk effect, be such as heated under the conditions of 1150 DEG C, zirconium dioxide
It is changed into tetragonal phase, volume contraction from monoclinic phase；When cooling, the opposite monoclinic phase transformation in four directions is answered along with about 6% ~ 8% shearing
Become the volume expansion with 3% ~ 5%, to which the material prepared easy tos produce crackle, or even rupture, therefore without great engineering value.
In recent years, by adulterating particle ionic radius and valence number and Zr4+Similar metal ion, such as Ca2+、Mg2+With
Y3+Deng.When introducing Y in zirconium oxide crystals3+When metal ion, they replace the position of zirconium ion in lattice, in order to ensure grain
The electroneutral of son will produce oxygen vacancies, and the Lacking oxygen being distributed in around zirconium ion reduces the repulsive force between oxygen oxygen so that matches
Position layer generates larger distortion, to promote the stabilization of tetragonal phase or cubic phase zirconium dioxide under room temperature.
Prepare nanometer Y2O3-ZrO2The method of powder is more, mainly has：Chemical precipitation method, Emulsions method, collosol and gel
Method and hydro-thermal method etc..The powder that usual chemical precipitation method is prepared needs high-temperature calcination, particle bad dispersibility, and agglomeration is tight
Weight.Sol-gal process length reaction time, process conditions are harsh, and cost of material is high, and organic solvent is hazardous to the human body, and are unsuitable for big
Technical scale metaplasia is produced.The powder that hydro-thermal method is prepared is with crystal property is good, purity is high, even size distribution, reunion journey
The advantages that degree is smaller and does not need high-temperature calcination process.
In recent years, also there are some new technologies, as Chinese invention patent 201310043645.9 uses overcritical hydro-thermal
Nano zirconium oxide powder is synthesized, the crystallinity that nano-particle is prepared is poor, and consersion unit requires high, chlorion after simultaneous reactions
Handle cumbersome, the problems such as production cost is big.
Invention content：
The technology of the present invention is to overcome deficiency in the prior art, provides a kind of spherical yttrium stable zirconium oxide of size uniform and receives
Rice raw powder's production technology.
The present invention provides following technical scheme：
A kind of preparation method of the spherical yttrium stable zirconium oxide nano-powder of size uniform, main preparation process are：
（1）A certain amount of soluble zirconium source is weighed first and yttrium source is mixed with water, is made into the solution of 0 ~ 1 M；
（2）Precipitating reagent is added in the solution, the molar ratio of zirconium source and precipitating reagent is 1 in solution:1~6；
（3）0 ~ 5% dispersant is added in the solution again, mixed solution is formed after being sufficiently mixed；
（5）Above-mentioned mixed solution is placed in reaction kettle, control packed space is 60 ~ 85%, stirs 0 ~ 30 point at room temperature
Clock reacts 0 ~ 24 hour under the conditions of 150 ~ 210 DEG C；
（6）It is steady to obtain semi-stability nanoscale yttrium by washing and ethyl alcohol washing for the product that reaction is generated after freeze-drying
Determine zirconium powder body；
（7）Calcining in 0.5 ~ 2 hour, processing to be stabilized are carried out to the semi-stability nanoscale yttrium stabilised zirconia powder after drying
Afterwards and obtain spherical yttrium stable zirconium oxide nano-powder.
Based on the above technical solution, there can also be technical solution further below：
The zirconium source is zirconium sulfate or zirconium nitrate or zirconium oxychloride；The yttrium source is yttrium sulfate or yttrium nitrate or chlorination
Yttrium, stabilizer of the yttrium source as zirconium source, molar content 3%.
The precipitating reagent is urea.
The dispersant is the polyethylene glycol or glycerine that molecular weight is 4000.
The calcining is low temperature calcination mode stabilization processes, and calcination temperature is 400 ~ 800 DEG C.
Invention advantage：
The preparation method of the present invention is raw material as a result of soluble zirconium source and precipitating reagent urea, fills in a kettle
Divide reaction, obtains size uniform, pattern is the cubic phase nano yttrium stabilised zirconia of spherical shape, wherein main feature is as follows：
First, using urea as precipitating reagent, Urea, which slowly hydrolyzes, generates ammonium hydroxide so that cation is uniform to be precipitated
Adequately with precipitating reagent slow reaction can occur for precipitation, such metal ion, and obtained generation particle reaction is uniform；
Second, using hydro-thermal reaction equipment, by heating, pressurizeing to reaction system so that react high temperature, high pressure it is anti-
It being carried out under the conditions of answering, the indissoluble or insoluble substance in reaction can be dissolved and be recrystallized, high to the product purity of synthesis,
Growth defect is few, the crystal of favorable orientation；
Third is added Macrogol 4000 and keeps dispersibility so that particle is uniformly dispersed, and reunites less, simultaneously after reaction
Performance that is using Freeze Drying Technique so that interparticle well dispersed, keeping zirconium oxide excellent；
4th, oxide-stabilizing zirconia powder is prepared using doped yttrium oxide, yttrium stabilised zirconia can be under conditions of room temperature
Keep tetragonal phase crystal form so that ceramic material property prepared by nano-powder is significantly improved.
Due to the These characteristics that this preparation method has, make the present invention that yttrium stable zirconium oxide nano powder be prepared
Body has the advantages that good dispersion, size uniform, large specific surface area, crystallinity is preferable, while the object that zirconium dioxide itself is excellent
Reason and chemical characteristic（Such as fusing point is high, hardness is big, corrosion resistance, chemical stability preferably, resistance to acid and alkali and electrochemical performance
Deng）, so that can be applicable to catalyst, heat-barrier material, structural ceramics, solid fuel cell and sensing obtained by this preparation method
The extensive field such as device.
Specific implementation mode：
Embodiment 1：
A kind of preparation method of the spherical yttrium stable zirconium oxide nano-powder of size uniform is using steps flow chart in detail below：
284g zirconium sulfates and 14g yttrium sulfate powder are weighed, a certain amount of water is added and is made into 1M solution.To it is above-mentioned prepare it is molten
Precipitating reagent urea is added in liquid, the wherein molar ratio of zirconium sulfate and urea is 1:6.Add 3% dispersant polyethylene glycol-
4000, it is sufficiently mixed.Above-mentioned solution is poured into hydrothermal reaction kettle, packed space 70%, stirs 30 minutes, stir at room temperature
It is 200 rpms to mix rate.
It is reacted under the conditions of 70 DEG C, completely rear reaction terminates.Product is taken out by washing and ethyl alcohol washing, freezing is dry
Calcining 1 hour is stabilized at dry processing, then 400 DEG C, and nanoscale semi-stability yttrium zirconium oxide is prepared after stabilization processes.
Powder crystallinity obtained by above-mentioned steps flow can be bad, and unformed, broken dispersion, particle morphology after dry is presented
Random, size is larger, is easy to happen reunion, and specific surface area is less than 5.0 m2/g。
Embodiment 2：
A kind of preparation method of the spherical yttrium stable zirconium oxide nano-powder of size uniform is using steps flow chart in detail below：
343g zirconium nitrates and 9g yttrium nitrate powder are weighed, a certain amount of water is added and is made into 1M solution.Into the solution prepared
Precipitating reagent urea is added, the wherein molar ratio of zirconium nitrate and urea is 1:4.The dispersant polyethylene glycol-4000 for adding 5%, fills
Divide mixing.
Above-mentioned solution is poured into hydrothermal reaction kettle, packed space 70%, is first stirred 30 minutes at ambient temperature,
Stir speed (S.S.) is 300 rpms.Reaction is reacted 4 hours under the conditions of temperature is 150 DEG C, is reacted and is terminated after precipitating completely.It takes
Go out product by washing and ethyl alcohol washing, freeze-drying obtains nanoscale semi-stability yttrium zirconium oxide.
Nanoscale yttrium stabilised zirconia after drying is stabilized to calcining 1 hour at 600 DEG C, is prepared after stabilization processes
Yttrium stable zirconium oxide nano-powder.Morphology microstructure is random, and Size Distribution is larger, and particle average size is about 100nm.
Monoclinic phase content is more in yttrium stable zirconium oxide nano-powder obtained by above-mentioned steps flow, and about 63.37%, four
The content of square phase is 36.63%, and specific surface area is 10 m2/g。
Embodiment 3：
A kind of preparation method of the spherical yttrium stable zirconium oxide nano-powder of size uniform is using steps flow chart in detail below：
284g zirconium sulfates and 14g yttrium sulfate powder are weighed, a certain amount of water is added and is made into 1 M solution.To the solution prepared
Middle addition precipitating reagent urea, the wherein molar ratio of zirconium sulfate and urea are 1:2.5.The dispersant polyethylene glycol for adding 2%, fills
Divide mixing.
Above-mentioned solution is poured into reaction kettle, packed space 80%, is stirred 30 minutes at room temperature.Reaction is in 200 DEG C of conditions
It is lower to carry out 4 hours.After reaction, natural cooling.Product is taken out by washing and ethyl alcohol washing, freeze-drying obtains nanometer
Grade semi-stability yttrium zirconium oxide.
Nanoscale yttrium stabilised zirconia after drying is stabilized to calcining 1 hour at 500 DEG C, is prepared after stabilization processes
The spherical yttrium stable zirconium oxide nano-powder of tetragonal phase.
Yttrium stable zirconium oxide nano-powder obtained by above-mentioned steps flow is presented tetragonal phase and is stabilized at room temperature, shape
Looks are spherical shape, and even size distribution, particle average size is about 30nm, and specific surface area is 21 m2/g。
The above described is only a preferred embodiment of the present invention, being not intended to limit the present invention in any form；Appoint
What those skilled in the art, without departing from the scope of the technical proposal of the invention, all using the side of the disclosure above
Method and technology contents make many possible changes and modifications to technical solution of the present invention, or are revised as the equivalent reality of equivalent variations
Apply example.Therefore, every content without departing from technical solution of the present invention, according to the technical essence of the invention does above example
Any simple modification, equivalent replacement, equivalence changes and modification, still fall within technical solution of the present invention protection in the range of.
Claims (3)
1. a kind of preparation method of the spherical yttrium stable zirconium oxide nano-powder of size uniform, main preparation process are：
（1）A certain amount of soluble zirconium source is weighed first and yttrium source is mixed with water, is made into the solution of 1 M；
（2）It is added precipitating reagent in the solution, the precipitating reagent is urea, and the molar ratio of zirconium source and precipitating reagent is 1 in solution:
2.5；
（3）2% dispersant is added in the solution again, the dispersant is the polyethylene glycol that molecular weight is 4000, fully mixed
Mixed solution is formed after conjunction；
（5）Above-mentioned mixed solution is placed in reaction kettle, control packed space is 80%, is stirred 30 minutes at room temperature, at 200 DEG C
Under the conditions of react 4 hours；
（6）The product that reaction is generated obtains semi-stability nanoscale yttrium stabilised zirconia by washing and ethyl alcohol washing after freeze-drying
Powder；
（7）The calcining that 1 hour is carried out to the semi-stability nanoscale yttrium stabilised zirconia powder after drying, after processing to be stabilized and obtains
Spherical yttrium stable zirconium oxide nano-powder.
2. a kind of preparation method of the spherical yttrium stable zirconium oxide nano-powder of size uniform according to claim 1,
It is characterized in that：The zirconium source is zirconium sulfate or zirconium nitrate or zirconium oxychloride；The yttrium source is yttrium sulfate or yttrium nitrate or chlorine
Change yttrium, stabilizer of the yttrium source as zirconium source, molar content 3%.
3. a kind of preparation method of the spherical yttrium stable zirconium oxide nano-powder of size uniform according to claim 1,
It is characterized in that：The calcining is low temperature calcination mode stabilization processes, and calcination temperature is 400 ~ 800 DEG C.
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| CN114890467B (en) * | 2022-06-30 | 2023-08-08 | 北京大学口腔医学院 | Low-crystallinity yttrium-stabilized cubic phase zirconia powder and preparation method thereof |
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Address after: 233000 28 yuan yuan Road, Huaihe Industrial Park, Huaishang District, Bengbu, Anhui Applicant after: ANHUI ZHONGCHUANG ELECTRONIC INFORMATION MATERIAL CO., LTD. Applicant after: Bengbu Zhongheng New Materials Scientific and Technological Co., Ltd. Applicant after: Bengbu design Institute of Glass Industry Address before: 233010 east side of Long Jin Road, long Zi Lake District, Bengbu City, Anhui province (Kasen glass new material science and Technology Industrial Park) Applicant before: Bengbu Zhongheng New Materials Scientific and Technological Co., Ltd. Applicant before: ANHUI ZHONGCHUANG ELECTRONIC INFORMATION MATERIAL CO., LTD. Applicant before: Bengbu design Institute of Glass Industry |
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Address after: 233000 28 yuan yuan Road, Huaihe Industrial Park, Huaishang District, Bengbu, Anhui Patentee after: Anhui Kaisheng Applied Materials Co.,Ltd. Patentee after: BENGBU ZHONGHENG NEW MATERIALS SCIENTIFIC AND TECHNOLOGICAL Co.,Ltd. Patentee after: BENGBU DESIGN & Research Institute FOR GLASS INDUSTRY Address before: 233000 28 yuan yuan Road, Huaihe Industrial Park, Huaishang District, Bengbu, Anhui Patentee before: ANHUI ZHONGCHUANG ELECTRONIC INFORMATION MATERIAL Co.,Ltd. Patentee before: BENGBU ZHONGHENG NEW MATERIALS SCIENTIFIC AND TECHNOLOGICAL Co.,Ltd. Patentee before: BENGBU DESIGN & Research Institute FOR GLASS INDUSTRY |
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