CN106587148A - Preparation method of uniform-size spherical yttrium-stabilized zirconia nano powder - Google Patents
Preparation method of uniform-size spherical yttrium-stabilized zirconia nano powder Download PDFInfo
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Abstract
The invention provides a preparation method of uniform-size spherical yttrium-stabilized zirconia nano powder. The method is characterized by comprising the following steps: making a zirconium source and a yttrium source into a solution; adding a precipitant into the solution; stirring sufficiently and adding a dispersing agent; putting the mixed solution into a reaction kettle; stirring at room temperature, and heating for reacting for a period of time to obtain a product; washing the product with water and ethanol; performing freeze drying to obtain semi-stable nano-scale yttrium-stabilized zirconium; and performing thermal stabilization treatment to obtain spherical yttrium-stabilized zirconia nano powder. The method provided by the invention has the following advantages: the prepared yttrium-stabilized zirconia nano powder is of uniform size distribution, spherical morphology and high crystallinity and exists stably in a tetragonal phase under a room-temperature condition.
Description
Technical field：
The present invention relates to nano material production field, is specifically exactly a kind of spherical yttrium stable zirconium oxide nanometer of size uniform
Raw powder's production technology.
Background technology：
Zirconium oxide（ZrO2）It is a kind of very important structural and functional material, wear-resistant with chemical stability, heat conduction system
The characteristics such as low, the high temperature resistant of number, corrosion resistance, heat stability and impact resistance, are fire resistant covering material, high-temperature structural material, life
The important source material of thing material 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 formations：Monoclinic system（Monoclinic, m-ZrO2）, tetragonal crystal system（Tetragonal, t-ZrO2）
And cubic system（Cubic, c-ZrO2）.Monoclinic phase is stable phase under room temperature, and Tetragonal and Emission in Cubic are metastable phases.These are brilliant
Reversible phase in version 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, volume contraction from monoclinic phase；During cooling, the opposite monoclinic phase transformation in four directions should along with about 6% ~ 8% shearing
Become the volumetric expansion with 3% ~ 5%, so as to the material for preparing easily is cracked, or even rupture, therefore without great construction value.
In recent years, by particle ionic radius and valence number and the Zr of adulterating4+Close metal ion, such as Ca2+、Mg2+With
Y3+Deng.When introducing Y in zirconium oxide crystals3+During metal ion, they replace the position of zirconium ion in lattice, in order to ensure grain
The electric neutrality of son can produce oxygen vacancies, and the Lacking oxygen being distributed in around zirconium ion reduces the repulsive force between oxygen oxygen so that match somebody with somebody
Position layer produces larger distortion, so as to promote room temperature condition under Tetragonal or Emission in Cubic zirconium dioxide stablize.
Prepare nanometer Y2O3-ZrO2The method of powder body is more, mainly has：Chemical precipitation method, Emulsions method, collosol and gel
Method and hydro-thermal method etc..The powder body that generally chemical precipitation method is prepared needs high-temperature calcination, and particle bad dispersibility, 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 body that hydro-thermal method is prepared has that crystal property is good, purity is high, even size distribution, reunion journey
The advantages of degree is less and does not need high-temperature calcination operation.
In recent years, some new techniques are also occurred in that, such as Chinese invention patent 201310043645.9 adopts supercritical hydro-thermal
Synthesis nano zirconium oxide powder, the degree of crystallinity for preparing nanoparticle is poor, and consersion unit has high demands, chloride ion after simultaneous reactions
The problems such as processing loaded down with trivial details, production cost is big.
The content of the invention：
The technology of the present invention is to overcome deficiency of the prior art, there is provided a kind of spherical yttrium stable zirconium oxide nano powder of size uniform
The preparation method of body.
The present invention provides technical scheme below：
A kind of preparation method of the spherical yttrium stable zirconium oxide nano-powder of size uniform, its main preparation process is：
（1）A certain amount of soluble zirconium source is weighed first and yttrium source mixes with water, be made into the solution of 0 ~ 1 M；
（2）Precipitant is added in the solution, the mol ratio of zirconium source and precipitant is 1 in solution:1~6；
（3）Add 0 ~ 5% dispersant in the solution again, mixed solution is formed after being sufficiently mixed；
（5）Above-mentioned mixed solution is inserted in reactor, it is 60 ~ 85% to control packed space, is stirred 0 ~ 30 minute under room temperature,
React 0 ~ 24 hour under the conditions of 150 ~ 210 DEG C；
（6）The product that reaction is generated obtains semi-stability nanoscale yttrium stabilised zirconia through washing and washing with alcohol after lyophilization
Powder body；
（7）The calcining of 0.5 ~ 2 hour is carried out to dried semi-stability nanoscale yttrium stabilised zirconia powder body, after process to be stabilized and
Obtain spherical yttrium stable zirconium oxide nano-powder.
On the basis of above-mentioned technical proposal, there can also be technical scheme further below：
Described zirconium source is Disulfatozirconic acid. or zirconium nitrate or zirconium oxychloride；Described yttrium source is Yttrium sesquisulfate or Yttrium trinitrate or Yttrium chloride(Y2Cl6),
Used as the stabilizer in zirconium source, its molar content is 3% in described yttrium source.
The precipitant is carbamide.
The dispersant is Polyethylene Glycol that molecular weight is 4000 or glycerol.
The calcining is low temperature calcination mode stabilizing treatment, and calcining heat 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 precipitant carbamide, fully anti-in a kettle.
Should, obtain size uniform, pattern is spherical cubic phase nano yttrium stabilised zirconia, wherein it is main the characteristics of it is as follows：
First, using carbamide as precipitant, Urea slowly hydrolyzes generation ammonia so that it is heavy that cation is uniformly separated out
Form sediment, such metal ion sufficiently can occur slow reaction with precipitant, and the generation particle reaction for obtaining is uniform；
Second, using hydro-thermal reaction equipment, by heating to reaction system, pressurizeing so that reaction is in high temperature, the reaction bar of high pressure
Carry out under part, the indissoluble or insoluble material in reaction can dissolve and recrystallization, so as to the product purity of synthesis is high, growth
Defect is few, the crystal of favorable orientation；
3rd, add Macrogol 4000 to keep dispersibility after reaction so that granule is uniformly dispersed, and reunites less, while using
Freeze Drying Technique causes interparticle well dispersed, to keep zirconium oxide excellent performance；
4th, oxide-stabilizing zirconia powder is prepared using doped yttrium oxide, yttrium stabilised zirconia can keep under conditions of room temperature
Tetragonal crystal formation so that ceramic material property prepared by nano-powder is significantly improved.
Due to the These characteristics that this preparation method possesses, therefore the present invention is set to prepare yttrium stable zirconium oxide nano powder
Body, with good dispersion, size uniform, specific surface area is big, the advantages of degree of crystallinity is preferable, while the excellent thing of zirconium dioxide itself
Reason and chemical characteristic（As fusing point is high, hardness is big, corrosion resistance, chemical stability preferably, resistance to acids and bases and electrochemical performance
Deng）, so that this preparation method gained can be applicable to catalyst, heat-barrier material, structural ceramicss, solid fuel cell and sensing
The extensive field such as device.
Specific embodiment：
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 Disulfatozirconic acid .s and 14g Yttrium sesquisulfate powder are weighed, adds a certain amount of water to be made into 1M solution.To in the above-mentioned solution for preparing
Precipitant carbamide is added, the wherein mol ratio of Disulfatozirconic acid. and carbamide is 1:6.3% dispersant PEG-4000 is added, is filled
Divide mixing.Above-mentioned solution is poured in hydrothermal reaction kettle, packed space is 70%, is stirred 30 minutes under room temperature, stir speed (S.S.) is
200 rpms.
Reacted under the conditions of 70 DEG C, completely rear reaction terminates.Product is taken out through washing and washing with alcohol, freezing is dry
Stabilisation is calcined 1 hour at dry process, then 400 DEG C, and nanoscale semi-stability yttrium zirconium oxide is prepared after stabilizing treatment.
Powder crystallinity obtained by above-mentioned steps flow process can be bad, is presented unformed, and dispersion, particle morphology are crushed after being dried
Random, size is larger, is susceptible to reunite, 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 trinitrate powder are weighed, adds a certain amount of water to be made into 1M solution.Add in the solution for preparing
The mol ratio of precipitant carbamide, wherein zirconium nitrate and carbamide is 1:4.5% dispersant PEG-4000 is added, it is fully mixed
Close.
Above-mentioned solution is poured in hydrothermal reaction kettle, packed space is 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 for 150 DEG C, is reacted after precipitation is complete and is terminated.Take
Go out product through washing and washing with alcohol, lyophilization, obtain nanoscale semi-stability yttrium zirconium oxide.
By dried nanoscale yttrium stabilised zirconia, stabilisation is calcined 1 hour at 600 DEG C, is prepared after stabilizing treatment
Yttrium stable zirconium oxide nano-powder.Morphology microstructure is random, and distribution of sizes 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 process, 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 Disulfatozirconic acid .s and 14g Yttrium sesquisulfate powder are weighed, adds a certain amount of water to be made into 1 M solution.Add in the solution for preparing
Enter precipitant carbamide, the wherein mol ratio of Disulfatozirconic acid. and carbamide is 1:2.5.2% dispersant Polyethylene Glycol is added, it is fully mixed
Close.
Above-mentioned solution is poured in reactor, packed space is 80%, stirred 30 minutes under room temperature.Reaction is in 200 DEG C of conditions
Under carry out 4 hours.After reaction terminates, natural cooling.Product is taken out through washing and washing with alcohol, lyophilization, nanometer is obtained
Level semi-stability yttrium zirconium oxide.
By dried nanoscale yttrium stabilised zirconia, stabilisation is calcined 1 hour at 500 DEG C, is prepared after stabilizing treatment
The spherical yttrium stable zirconium oxide nano-powder of Tetragonal.
Yttrium stable zirconium oxide nano-powder obtained by above-mentioned steps flow process is presented at room temperature Tetragonal stable existence, its shape
Looks are spherical, even size distribution, and particle average size is about 30nm, and specific surface area is 21 m2/g。
The above, is only presently preferred embodiments of the present invention, and any pro forma restriction is not made to the present invention；Appoint
What those of ordinary skill in the art, under without departing from technical solution of the present invention ambit, all using the side of the disclosure above
Method and technology contents make many possible variations and modification, or the equivalent reality for being revised as equivalent variations to technical solution of the present invention
Apply example.Therefore, every content without departing from technical solution of the present invention, is done according to the technical spirit of the present invention to above example
Any simple modification, equivalent, equivalence changes and modification, still fall within the range of technical solution of the present invention protection.
Claims (5)
1. the preparation method of the spherical yttrium stable zirconium oxide nano-powder of a kind of size uniform, its main preparation process is：
（1）A certain amount of soluble zirconium source is weighed first and yttrium source mixes with water, be made into the solution of 0 ~ 1 M；
（2）Precipitant is added in the solution, the mol ratio of zirconium source and precipitant is 1 in solution:1~6；
（3）Add 0 ~ 5% dispersant in the solution again, mixed solution is formed after being sufficiently mixed；
（5）Above-mentioned mixed solution is inserted in reactor, it is 60 ~ 85% to control packed space, is stirred 0 ~ 30 minute under room temperature,
React 0 ~ 24 hour under the conditions of 150 ~ 210 DEG C；
（6）The product that reaction is generated obtains semi-stability nanoscale yttrium stabilised zirconia through washing and washing with alcohol after lyophilization
Powder body；
（7）The calcining of 0.5 ~ 2 hour is carried out to dried semi-stability nanoscale yttrium stabilised zirconia powder body, after process to be stabilized and
Obtain spherical yttrium stable zirconium oxide nano-powder.
2. a kind of preparation method of the spherical yttrium stable zirconium oxide nano-powder of described size uniform is required according to right 1, its
It is characterised by：Described zirconium source is Disulfatozirconic acid. or zirconium nitrate or zirconium oxychloride；Described yttrium source is Yttrium sesquisulfate or Yttrium trinitrate or chlorine
Change yttrium, used as the stabilizer in zirconium source, its molar content is 3% for described yttrium source.
3. a kind of preparation method of the spherical yttrium stable zirconium oxide nano-powder of described size uniform is required according to right 1, its
It is characterised by：The precipitant is carbamide.
4. a kind of preparation method of the spherical yttrium stable zirconium oxide nano-powder of described size uniform is required according to right 1, its
It is characterised by：The dispersant is Polyethylene Glycol that molecular weight is 4000 or glycerol.
5. a kind of preparation method of the spherical yttrium stable zirconium oxide nano-powder of described size uniform is required according to right 1, its
It is characterised by：The calcining is low temperature calcination mode stabilizing treatment, and calcining heat is 400 ~ 800 DEG C.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108059186A (en) * | 2017-12-25 | 2018-05-22 | 山东磊宝锆业科技股份有限公司 | It is given up the method that zirconium prepares Zirconium powder as raw material hydro-thermal method using solid |
| CN108640151A (en) * | 2018-06-11 | 2018-10-12 | 东南大学 | Zirconia hollow microsphere containing aluminium and preparation method thereof |
| 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 |
| 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 |
| CN113149071A (en) * | 2021-04-19 | 2021-07-23 | 中民驰远实业有限公司 | Synthetic nano ZrO2Method for preparing powder |
| CN113753949A (en) * | 2021-09-29 | 2021-12-07 | 湖南皓志科技股份有限公司 | Preparation method of porous mesoporous nano zirconia |
| CN113979770A (en) * | 2021-12-01 | 2022-01-28 | 安徽中创电子信息材料有限公司 | Preparation method of enhanced yttrium-stabilized nano composite zirconia ceramic powder |
| CN114408968A (en) * | 2022-01-25 | 2022-04-29 | 山东理工大学 | Rare earth stabilized zirconia nano powder and preparation method thereof |
| CN114890467A (en) * | 2022-06-30 | 2022-08-12 | 北京大学口腔医学院 | Low-crystallinity yttrium-stabilized cubic-phase zirconia powder and preparation method thereof |
| CN115124074A (en) * | 2022-07-26 | 2022-09-30 | 宣城市晶纳环保科技有限公司 | Preparation method of high-dispersion composite nano zirconium dioxide |
| 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 |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108059186A (en) * | 2017-12-25 | 2018-05-22 | 山东磊宝锆业科技股份有限公司 | It is given up the method that zirconium prepares Zirconium powder as raw material hydro-thermal method using solid |
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| CN108640151B (en) * | 2018-06-11 | 2020-07-14 | 东南大学 | Aluminum-containing zirconium oxide hollow microsphere and preparation method thereof |
| 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 |
| CN111320479B (en) * | 2020-03-06 | 2022-05-31 | 山东国瓷功能材料股份有限公司 | Nano zirconium oxide material, preparation method and application thereof |
| 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 |
| CN113149071A (en) * | 2021-04-19 | 2021-07-23 | 中民驰远实业有限公司 | Synthetic nano ZrO2Method for preparing powder |
| CN113753949A (en) * | 2021-09-29 | 2021-12-07 | 湖南皓志科技股份有限公司 | Preparation method of porous mesoporous nano zirconia |
| CN113979770B (en) * | 2021-12-01 | 2022-08-19 | 安徽凯盛应用材料有限公司 | Preparation method of enhanced yttrium-stabilized nano composite zirconia ceramic powder |
| CN113979770A (en) * | 2021-12-01 | 2022-01-28 | 安徽中创电子信息材料有限公司 | Preparation method of enhanced yttrium-stabilized nano composite zirconia ceramic 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 |
| CN114408968A (en) * | 2022-01-25 | 2022-04-29 | 山东理工大学 | Rare earth stabilized zirconia nano powder and preparation method thereof |
| CN114890467A (en) * | 2022-06-30 | 2022-08-12 | 北京大学口腔医学院 | Low-crystallinity yttrium-stabilized cubic-phase zirconia powder and preparation method thereof |
| 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 |
| CN115124074A (en) * | 2022-07-26 | 2022-09-30 | 宣城市晶纳环保科技有限公司 | Preparation method of high-dispersion composite nano zirconium dioxide |
| CN115124074B (en) * | 2022-07-26 | 2024-02-06 | 宣城市晶纳环保科技有限公司 | Preparation method of high-dispersion composite nano zirconium dioxide |
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