CN107382326B - Method for improving sintering activity of micron zirconia powder - Google Patents
Method for improving sintering activity of micron zirconia powder Download PDFInfo
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- CN107382326B CN107382326B CN201710732490.8A CN201710732490A CN107382326B CN 107382326 B CN107382326 B CN 107382326B CN 201710732490 A CN201710732490 A CN 201710732490A CN 107382326 B CN107382326 B CN 107382326B
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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Abstract
The invention relates to a method for improving sintering activity of micron zirconia powder, which comprises the following steps: 1) adding water and a mineralizer into micron zirconia powder to prepare slurry; wherein, the content of the zirconia powder in the slurry is (5-45)%, the content of the mineralizer is (0.5-5)%, and the balance is water; 2) placing the prepared slurry into a reaction kettle, heating to 100-300 ℃ under the condition of continuous stirring, keeping the pressure (0.5-5) MPa of the reaction kettle, and keeping the temperature for 1-10 hours; 3) after the heat preservation is finished, naturally cooling to room temperature; 4) taking out the treated slurry, and repeatedly washing until the powder does not contain mineralizer cations; 5) washing the powder with an aqueous ethanol solution for 2-3 times, wherein the ratio of ethanol to deionized water is (2-3): 1; 6) and drying the washed powder at 100-120 ℃.
Description
Technical Field
The invention relates to a method, in particular to a method for improving sintering activity of micron zirconia powder, and belongs to the technical field of zirconia powder processing technologies.
Background
The zirconia ceramics are widely used for structural ceramics, high-temperature heat-insulating coatings, oxygen sensors, artificial teeth, joints and the like due to unique phase change toughening effect, excellent mechanical, thermal and electrical properties, good biocompatibility and the like. Zirconia has three different phase structures, monoclinic, tetragonal and cubic, depending on the temperature. Zirconia is monoclinic phase at room temperature, and is converted into tetragonal phase at about 1100 ℃, and the tetragonal phase is converted into cubic phase at about 2300 ℃. Because the tetragonal phase has the best mechanical property, a certain amount of phase stabilizer is usually added into zirconia to enable the tetragonal phase to stably exist at room temperature, and the commonly used phase stabilizer is yttria.
Because of high melting point and high brittleness, zirconia ceramics are mostly formed by preparing blanks from zirconia powder and then performing solid-phase sintering. To obtain the best performance, the density of the finished product needs to be sintered close to the theoretical value. The sintering activity of the powder is a central factor in determining the sinterability and final properties of the ceramic article. When the sintering activity of the powder is low, the product needs to be sintered at a higher temperature, so that the production cost is high, and the high sintering temperature can cause local over-sintering of the product and scrap. At present, the improvement of the sintering activity of zirconia powder is a main technical approach for reducing the production cost and improving the qualification rate of products.
The prior technical method for improving the sintering activity of the zirconia powder mainly reduces the grain size of the powder. When the powder does not contain hard agglomerates or the hard agglomerates are small in size, the smaller the crystal grain size of the powder is, the larger the specific surface area thereof is, and the higher the sintering activity is. Studies have shown that the sintering temperature of zirconia ceramics can be reduced from 1650 ℃ to 1200 ℃ or below when the grain size of the zirconia powder is reduced to within 100nm and there is no hard agglomeration or small hard agglomeration size in the powder. However, the disadvantages of using this technology are mainly the following: (1) as the grain size of the powder is reduced, particularly to the nanometer scale, the powder is highly susceptible to agglomeration to form hard agglomerates. When the blank contains hard aggregates, the sintering temperature cannot be effectively reduced, and the defects in the aggregates cannot be completely eliminated in the sintering process, so that the defects exist in the final product; (2) when the grain size of the powder is reduced, the flowability of the powder is deteriorated, resulting in difficulty in molding a green body. For example, higher pressures are required for dry-pressing; during injection molding, the mold cannot be sealed, so that the product has flash. Although the hard agglomeration of the powder can be reduced by adopting methods such as adding a surfactant, washing with alcohol and the like, the powder cost is obviously increased; (3) the cost of the powder is high. The low-agglomeration nano zirconia powder generally has a selling price at least three times that of micron powder.
Compared with nano zirconia powder, the micron zirconia powder has the advantages of low price, good fluidity, easy blank forming and the like, and has better technical significance for improving the application if the sintering activity of the micron zirconia powder can be improved.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides the method for improving the sintering activity of the micron zirconia powder, and the powder treated by the method has the advantages of easy blank forming, low cost, high sintering activity and the like.
In order to achieve the above object, the present invention provides a method for improving sintering activity of a micro zirconia powder, comprising:
1) adding water and a mineralizer into micron zirconia powder to prepare slurry, wherein the content of the zirconia powder in the slurry is 5-45 wt%, the weight content of the mineralizer is 0.5-5 wt%, and the balance is deionized water;
2) placing the prepared slurry into a pressure reaction kettle, heating to 100-300 ℃ under the condition of continuous stirring, keeping the pressure of the reaction kettle at 0.5-5 MPa, and preserving heat for 1-10 hours;
3) after the heat preservation is finished, naturally cooling to room temperature;
4) taking out the treated slurry, and repeatedly washing the slurry by using deionized water until the powder does not contain mineralizer cations;
5) washing the powder with an aqueous ethanol solution for 2-3 times, wherein the ratio of ethanol to deionized water is (2-3): 1;
6) and drying the washed powder at 100-120 ℃ to obtain the required powder.
As a modification of the invention, in the step 1, the mineralizer is Na2CO3、NaOH、K2CO3And one or a combination of more of KOH.
As an improvement of the invention, the content of the zirconia powder in the slurry in the step 1) is 25-35 wt%.
As an improvement of the invention, the heating temperature in the step 2) is 180-210 ℃.
Compared with the prior art, the invention has the following advantages: under the conditions of temperature, pressure and mineralizer selected by the technical scheme, micron zirconia powder particles are eroded by water, a thin nano zirconia covering layer is generated on the surface, and the sintering activity of the powder is improved through the nano layer; the sintering temperature can be obviously reduced. Meanwhile, because the interior of the powder particles is compact, hard aggregates similar to those in the nano zirconia powder cannot be formed, so that the powder has better fluidity and is easy to form blanks, and meanwhile, the defect of difficult removal cannot be formed in the sintering process. Compared with the preparation process of the nano zirconia powder, the whole cost is about half of that of the preparation process because the dispersing agent and the ball milling procedure are not used for improving the dispersibility, so that the product cost is greatly reduced; the invention also widens the application of the micron zirconia powder such as the electric melting zirconia powder, and can be used in the field of fine ceramics with higher added value.
The specific implementation mode is as follows:
for the purpose of enhancing an understanding of the present invention, the following detailed description is given in conjunction with examples.
Example 1:
with a commercially available micron 3mol% Y2O3Stabilized zirconia powder and NaOH as mineralizers, according to the ratio zirconia powder: preparing slurry from water =30:2:68, adding the slurry into a reaction kettle, treating for 2 hours at 180 ℃ under 1MPa, repeatedly washing for 5 times, and then adopting a reaction condition of 3: washing with ethanol aqueous solution of 1 for 2 times, and drying at 120 deg.C to obtain powder. The processed powder and the original powder are adopted to prepare a green body under the same process conditions, the performance of a sintered product is shown in the following table 1, and the processed powder not only reduces the sintering temperature, but also obviously improves the performance of the product.
Example 2:
with a commercially available micron 3mol% Y2O3Stabilized zirconia powder and a NaOH, KOH combination mineralizer, wherein NaOH: KOH = 1: 1. according to the weight ratio of zirconia powder to mineralizer: preparing slurry from water =35:3:62, adding the slurry into a reaction kettle, treating for 10 hours at 220 ℃ and 2MPa, repeatedly washing for 5 times, and then adopting a reaction condition of 2.5: washing with ethanol aqueous solution of 1 for 2 times, and drying at 120 deg.C to obtain powder. The processed powder and the original powder are used for preparing a green body under the same process conditions, and the properties of a sintered product are shown in the following table 1. The treated powder has low sintering temperature and obviously raised product performance.
Example 3:
with a commercially available micron 3mol% Y2O3Stabilized zirconia powder and NaOH, KOH combined mineralizer, where K2CO3: KOH = 1: 2. according to the weight ratio of zirconia powder to mineralizer: preparing slurry from water =25:5:70, adding the slurry into a reaction kettle, treating for 4 hours at 280 ℃ under 3MPa, repeatedly washing for 6 times, and then adopting a ratio of 3: washing with ethanol aqueous solution of 1 for 2 times, and drying at 120 deg.C to obtain powder. Preparing a blank by adopting the treated powder and the original powder under the same process condition, and sinteringThe properties of the finished article are shown in table 1 below; the treated powder has low sintering temperature and obviously raised product performance.
TABLE 1 comparison of ceramic article Properties before and after powder treatment
It should be noted that the above-mentioned embodiments are not intended to limit the scope of the present invention, and all equivalent modifications and substitutions based on the above-mentioned technical solutions are within the scope of the present invention as defined in the claims.
Claims (3)
1. A method for increasing the sintering activity of a micron zirconia powder, comprising the steps of:
1) adding water and a mineralizer into micron zirconia powder to prepare slurry, wherein the weight content of the zirconia powder in the slurry is 5-45%, the weight content of the mineralizer is 0.5-5%, and the balance is deionized water;
2) placing the prepared slurry into a pressure reaction kettle, heating to 100-300 ℃ under the condition of continuous stirring, keeping the pressure of the reaction kettle at 0.5-5 MPa, and preserving heat for 1-10 hours;
3) after the heat preservation is finished, naturally cooling to room temperature;
4) taking out the treated slurry, and repeatedly washing the slurry by using deionized water until the powder does not contain mineralizer cations;
5) washing the powder for 2-3 times by adopting an aqueous ethanol solution, wherein the ratio of ethanol to deionized water is 2-3: 1;
6) drying the washed powder at 100-120 ℃ to obtain the required powder;
in the step 1, the mineralizer is Na2CO3、NaOH、K2CO3And one or a combination of more of KOH.
2. The method for improving sintering activity of micron zirconia powder according to claim 1, wherein the content of zirconia powder in the slurry in step 1) is 25-35%.
3. The method for improving sintering activity of micron zirconia powder according to claim 2, wherein the heating temperature in step 2) is 180-210 ℃.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0130480A2 (en) * | 1983-07-05 | 1985-01-09 | Norton Company | Process for the preparation of ceramic powders |
| CN101550001A (en) * | 2009-04-09 | 2009-10-07 | 上海交通大学 | Yttrium zirconium composite nano-ceramic powder |
| CN101618351A (en) * | 2009-08-06 | 2010-01-06 | 上海理工大学 | Nanometer or micrometer structure composite material and preparation method thereof |
| CN104129990A (en) * | 2014-07-23 | 2014-11-05 | 西安航天复合材料研究所 | Preparation method of hollow spherical YSZ powder for plasma spraying |
| CN105967687A (en) * | 2016-07-14 | 2016-09-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Grain-composition zirconia powder preparation and ceramic sintering method |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0130480A2 (en) * | 1983-07-05 | 1985-01-09 | Norton Company | Process for the preparation of ceramic powders |
| CN101550001A (en) * | 2009-04-09 | 2009-10-07 | 上海交通大学 | Yttrium zirconium composite nano-ceramic powder |
| CN101618351A (en) * | 2009-08-06 | 2010-01-06 | 上海理工大学 | Nanometer or micrometer structure composite material and preparation method thereof |
| CN104129990A (en) * | 2014-07-23 | 2014-11-05 | 西安航天复合材料研究所 | Preparation method of hollow spherical YSZ powder for plasma spraying |
| CN105967687A (en) * | 2016-07-14 | 2016-09-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Grain-composition zirconia powder preparation and ceramic sintering method |
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