CN111116199A - Preparation of Gd by vacuum pressureless sintering2Zr2O7Method for making transparent ceramics - Google Patents
Preparation of Gd by vacuum pressureless sintering2Zr2O7Method for making transparent ceramics Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 87
- 238000005245 sintering Methods 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 46
- 238000000498 ball milling Methods 0.000 claims abstract description 27
- 238000001272 pressureless sintering Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims abstract 4
- 239000000203 mixture Substances 0.000 claims abstract 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 28
- 238000001816 cooling Methods 0.000 claims description 21
- 239000002612 dispersion medium Substances 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 15
- 238000003825 pressing Methods 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 15
- 238000009694 cold isostatic pressing Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 12
- 238000005498 polishing Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 abstract description 11
- 238000002834 transmittance Methods 0.000 abstract description 10
- 230000003287 optical effect Effects 0.000 abstract description 6
- 239000002131 composite material Substances 0.000 abstract description 2
- 229910002609 Gd2Zr2O7 Inorganic materials 0.000 description 28
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 23
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 23
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 22
- 235000015895 biscuits Nutrition 0.000 description 14
- 238000005303 weighing Methods 0.000 description 12
- 238000000465 moulding Methods 0.000 description 11
- 230000006872 improvement Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
- 238000002490 spark plasma sintering Methods 0.000 description 2
- 229910026161 MgAl2O4 Inorganic materials 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005658 nuclear physics Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种真空无压烧结制备Gd2Zr2O7透明陶瓷的方法，特别是指采用复合烧结助剂，通过真空无压单步烧结的方法，在相对较低温度下实现Gd2Zr2O7透明陶瓷制备的一种方法。本发明是采用Gd2Zr2O7粉作为原料粉，并添加少量(≤2.5％)的Y2O3、La2O3、HfO2混合物作为烧结助剂，通过球磨混合后制成素坯，再通过相对较低温度下(1650℃－1750℃)真空无压单步烧结，即可获得具有良好的光学透过率Gd2Zr2O7透明陶瓷。
The invention discloses a method for preparing Gd 2 Zr 2 O 7 transparent ceramics by vacuum pressureless sintering, in particular to a method of vacuum pressureless single-step sintering by using a composite sintering aid to realize Gd 2 Zr 2 O 7 at a relatively low temperature A method for the preparation of Zr 2 O 7 transparent ceramics. In the present invention, Gd 2 Zr 2 O 7 powder is used as raw material powder, and a small amount (≤2.5%) of Y 2 O 3 , La 2 O 3 and HfO 2 mixture is added as sintering aid, and the green body is made by ball milling and mixing. , and then through vacuum pressureless single-step sintering at a relatively low temperature (1650℃-1750℃), Gd 2 Zr 2 O 7 transparent ceramics with good optical transmittance can be obtained.
Description
The technical field is as follows:
the invention relates to the field of ceramic materials, in particular to a method for preparing Gd2Zr2O7A method of making a transparent ceramic.
Background art:
the transparent ceramic is an optical material with wide application prospect, and has wide application prospect in the fields of high temperature resistant windows, optical fairings, light high-strength transparent armors, high-power illumination, medical detection, nuclear physics and the like. Gd of cubic structure2Zr2O7Has isotropic optical performance, and can be sintered and densified to obtain optically transparent ceramic. In addition, Gd is present2Zr2O7Has high density and atomic number, and is compatible with conventional MgAl2O4、Al2O3Compared with transparent ceramics, the ceramic is especially suitable for being used as a transparent scintillator for intercepting X rays and gamma rays, thereby having obvious application advantages in the fields of high-energy physics, medical detection and the like.
At present Gd2Zr2O7The transparent ceramic is mainly prepared by high-temperature vacuum pressureless sintering (pressureless means no additional loading pressure except vacuum), spark plasma sintering and other methods. Gui et al (Ceramics International, Volume 44, Pages 7006->70% LaGdZr2O7A transparent ceramic. The high-temperature vacuum sintering is generally higher in preparation temperature and higher in equipment energy consumption; in addition, the high temperature vacuum environment brings many process control problems to the manufacturing process, such as: with the increase of temperature, when graphite is used as a heating element, the graphite has higher saturated vapor pressure under high-temperature vacuum. According to the thermodynamic equilibrium theory, the graphite saturated vapor pressure P (unit Pa) and the temperature T (unit K) are in exponential change rule as shown in formula (1), wherein P0Is at atmospheric pressure. For example, when the temperature is increased from 1700 ℃ to 1800 ℃, the saturated vapor pressure of graphite immediately increases to about 9 times that at 1750 ℃. Therefore, the sample is easily polluted by high-temperature volatilization, and the repeatability of the process is inevitably influenced.
In order to lower the sintering temperature, Zhou et al (Journal of the European Ceramic Society, Volume 37, Pages 1059-2O7The ceramic, however, cannot be transparent since 7% of residual pores still exist to cause light scattering. In order to both reduce the sintering temperature and increaseThe densification is achieved by adopting a spark plasma sintering method by Qi et al (Journal of the European ceramic society, Volume 38, Pages 2256-2Zr2O7The transparent ceramic is prepared at low temperature and quickly, but the transmittance needs to be further improved, and the method has the advantages that the sintering temperature is low, the preparation speed is high, but the manufacturing cost of the discharge plasma equipment is high, and the large-scale popularization and application are difficult; moreover, the discharge plasma equipment is characterized in that the temperature rise and fall speed is too fast, and obvious temperature gradient is inevitably caused, so that the discharge plasma equipment is not suitable for preparing ceramic high-brittleness materials, especially large-size ceramic samples. In the preparation process for obtaining transparent ceramics, there are also reports that: the sintering process adopts multiple steps and combines a sintering aid (such as patent CN201010139771.0), and the formed biscuit is sequentially processed by: short sintering (oxidizing atmosphere), main sintering (vacuum, H)2Or He in a non-oxidizing atmosphere) or pressure sintering (10MPa to 198MPa), polycrystalline transparent ceramics can be obtained. However, the multi-step sintering (especially by means of different equipment and atmosphere conditions, combination of pressureless and pressurized, etc.) leads to complicated experimental operation process, virtually increases development cost, and brings great test on process stability.
The invention content is as follows:
in order to solve the problems, the invention aims to provide a method for preparing Gd by vacuum pressureless single-step sintering at a relatively low temperature (1650-1750 ℃)2Zr2O7The method for preparing transparent ceramics is characterized by that it adds a proper sintering adjuvant to effectively reduce Gd2Zr2O7The sintering temperature of the transparent ceramic is high, and meanwhile, the high optical transmittance is obtained, and the method is also suitable for preparing large-size samples.
To achieve the above object, the method of the present invention is as follows:
preparation of Gd by vacuum pressureless sintering2Zr2O7A method of making a transparent ceramic, comprising the steps of:
the method comprises the following steps: weighing Gd2Zr2O7The powder is used as a raw material for standby; weighing powder A as sintering aid, powder A and Gd2Zr2O7The mass ratio of the powder is 0.5: 100-2.5: 100, respectively; the powder A comprises La2O3、Y2O3And HfO2；Y2O3、La2O3And HfO2The mass fractions in the powder A are respectively 30-60%, 20-40% and 15-35%;
step two: adding the powder A into a ball milling tank filled with high-purity zirconia balls, adding an organic solvent as a dispersion medium, and mixing by planetary ball milling to obtain slurry B;
step three: taking the slurry B, and removing a dispersion medium through low-temperature low-pressure evaporation to obtain powder C;
step four: taking the powder C, carrying out axial dry pressing molding, and then carrying out cold isostatic pressing to obtain a biscuit D;
step five: taking the biscuit D, placing the biscuit D in a sintering furnace, and carrying out single-step sintering in a vacuum atmosphere furnace, namely: heating to 1650-1750 deg.C, keeping the temperature for 5-10 h, cooling to 300 deg.C, naturally cooling, taking out, and polishing to obtain Gd2Zr2O7And a transparent ceramic E.
In a further improvement, in step one, Gd2Zr2O7The purity of the powder is not lower than 99 percent, and the average particle size is not higher than 80 nm; y is2O3、La2O3、HfO2The purity of the particles is not less than 99 percent, and the average particle size is not more than 100 nm.
In a further improvement, in the second step, the organic solvent is absolute ethyl alcohol;
in the second step, the purity of the zirconia balls is not lower than 99.5%; the rotation speed of the planetary ball milling is 100 r/m-350 r/m, and the ball milling time is 5 h-24 h.
In the second step, the mass ratio of the powder A to the dispersion medium is 1: 1-1: 5.
in the third step, the slurry B is taken out, sieved by a 200-mesh screen, and evaporated at low temperature and low pressure to remove a dispersion medium, so that powder C is obtained.
In a further improvement, in the third step, the low temperature means that the temperature is lower than 80 ℃, and the low pressure means that the pressure is lower than the standard atmospheric pressure, namely lower than 1.01 multiplied by 105Pa
In a further improvement, the low temperature is 40-70 ℃; low pressure means a pressure below 1000 Pa.
In the fourth step, the pressure of the axial dry pressing is 10 MPa-30 MPa; the pressure of the cold isostatic pressing is 150 MPa-300 MPa.
In the fifth step, the pressure of residual gas in the vacuum atmosphere sintering process is not higher than 5 multiplied by 10- 3Pa; the heating rate is controlled to be 2-10 ℃/min; the cooling rate is controlled within 15 ℃/min.
The invention has the beneficial effects that:
at present Gd2Zr2O7The transparent ceramic is mainly prepared by adopting methods such as high-temperature vacuum pressureless sintering, discharge plasma sintering and the like. The high-temperature vacuum environment brings many process control problems to the preparation process, volatile pollution is easily caused, the repeatability of the process is inevitably influenced, and long-term high-temperature (such as over 1800 ℃) operation has potential influence on equipment loss; the sintering aid is added in the vacuum pressureless sintering process to promote the sintering of the ceramic, however, the multi-step sintering reported in the prior art easily causes the experimental operation process to be complicated, and is not beneficial to reducing the development cost. The discharge plasma method can realize low-temperature and rapid sintering preparation, but is expensive in equipment, too rapid in temperature rise and fall, and not suitable for preparation of large-size samples and cost reduction. The invention provides a method for preparing Gd by composite auxiliary agent assisted vacuum pressureless single-step sintering2Zr2O7Transparent ceramic, its beneficial effect is: (1) gd can be effectively reduced by adding a proper sintering aid2Zr2O7The sintering temperature of the transparent ceramic is only 1650-1750 ℃, which is beneficial to reducing energy consumption and equipment loss and obtaining higher optical transmittance. (2) The vacuum pressureless sintering process only needs a single step, and the steps are simple and easy to operate; (3) the methodThe method only needs a conventional vacuum sintering furnace, does not need discharge plasma sintering equipment with high manufacturing cost, has low cost, is also suitable for preparing large-size samples, and has wide popularization and application prospects.
Drawings
FIG. 1 is Gd obtained in example 12Zr2O7Transmittance of a transparent ceramic sample;
FIG. 2 is Gd obtained in example 22Zr2O7Transmittance of a transparent ceramic sample;
FIG. 3 is Gd obtained in example 32Zr2O7Transmittance of a transparent ceramic sample;
FIG. 4 is Gd obtained in example 42Zr2O7Transmittance of a transparent ceramic sample;
FIG. 5 is Gd obtained in example 52Zr2O7Transmittance of transparent ceramic sample.
The specific implementation mode is as follows:
in order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
The method comprises the following steps: weighing high-purity fine-granularity Gd2Zr2O7The powder is used as a raw material for standby; weighing La2O3、Y2O3、HfO2As a sintering aid. Mixing the four powders according to a certain proportion to obtain the standby powder A1.
Wherein, Gd2Zr2O7The purity of the powder is 99 percent, and the average particle size is 30 nm; y is2O3、La2O3、HfO2The purity of the powder is 99%, 99% and 99%, and the average particle size is 30nm, 30nm and 50 nm;
wherein, Y2O3、La2O3、HfO2Total mass of powder with Gd2Zr2O7The mass ratio of the powder is 0.5: 100, respectively; y is2O3、La2O3、HfO2The mass fractions of the powder, which account for the total mass of the three, are respectively 30%, 35% and 35%.
Step two: and adding the standby powder A1 into a ball milling tank filled with high-purity zirconia balls, adding a proper amount of absolute ethyl alcohol as a dispersion medium, and mixing by planetary ball milling to obtain slurry B1.
Wherein, the purity of the zirconia ball is 99.5%;
wherein the mass ratio of the powder A1 to the dispersion medium (absolute ethyl alcohol) is 1: 5;
wherein the rotation speed of the planetary ball milling is 100r/m, and the ball milling time is 5 h;
step three: and sieving the slurry B1 through a 200-mesh sieve, and evaporating at low temperature and low pressure to remove a dispersion medium to obtain powder C1.
Wherein the temperature here is 70 ℃;
wherein the pressure here is 1000 Pa;
step four: and taking the powder C1, carrying out axial dry pressing molding, and carrying out cold isostatic pressing to obtain a biscuit D1.
Wherein, the pressure of the axial dry pressing molding is 10 MPa;
wherein the cold isostatic pressing pressure is 150 MPa.
Step five: placing the biscuit D1 in a sintering furnace, heating to 1650 deg.C in vacuum atmosphere, keeping the temperature for 5h, cooling to 300 deg.C, naturally cooling, taking out, grinding and polishing to 1mm thickness to obtain Gd2Zr2O7Transparent ceramic E1.
Wherein, in the vacuum atmosphere sintering process, the residual gas pressure is (1.5 +/-0.5) multiplied by 10-3Pa；
Wherein the heating rate is controlled at 2 ℃/min; the cooling rate is controlled at 15 ℃/min.
Example 2
The method comprises the following steps: weighing high-purity fine-granularity Gd2Zr2O7The powder is used as a raw material for standby; weighing La2O3、Y2O3、HfO2As a sintering aid. Will be provided withThe four powders are mixed according to a certain proportion to obtain the standby powder A2.
Wherein, Gd2Zr2O7The purity of the powder is 99.5 percent, and the average particle size is 50 nm; y is2O3、La2O3、HfO2The purity of the powder is 99%, 99% and 99%, and the average particle size is 30nm, 30nm and 50 nm;
wherein, Y2O3、La2O3、HfO2Total mass of powder with Gd2Zr2O7The mass ratio of the powder is 1.0: 100, respectively; y is2O3、La2O3、HfO2The mass fraction of the powder accounts for 40 percent, 40 percent and 20 percent of the total mass of the powder;
step two: and adding the standby powder A2 into a ball milling tank filled with high-purity zirconia balls, adding a proper amount of absolute ethyl alcohol as a dispersion medium, and mixing by planetary ball milling to obtain slurry B2.
Wherein, the purity of the zirconia ball is 99.5%;
wherein the mass ratio of the powder A2 to the dispersion medium (absolute ethyl alcohol) is 1: 1;
wherein the rotation speed of the planetary ball milling is 130r/m, and the ball milling time is 24 h;
wherein the temperature here is 60 ℃;
wherein the pressure here is 500 Pa;
step four: and taking the powder C2, carrying out axial dry pressing molding, and carrying out cold isostatic pressing to obtain a biscuit D2.
Wherein, the pressure of the axial dry pressing molding is 10 MPa;
wherein the cold isostatic pressing pressure is 300 MPa.
Step five: placing the biscuit D2 in a sintering furnace, heating to 1650 deg.C in vacuum atmosphere, keeping the temperature for 10h, cooling to 300 deg.C, naturally cooling, taking out, grinding and polishing to 1mm thickness to obtain Gd2Zr2O7Transparent ceramic E2.
Wherein, in the vacuum atmosphere sintering process, the residual gas pressure is(4.5±0.5)×10-3Pa；
Wherein the heating rate is controlled at 10 ℃/min; the cooling rate is controlled at 5 ℃/min.
Example 3
The method comprises the following steps: weighing high-purity fine-granularity Gd2Zr2O7The powder is used as a raw material for standby; weighing La2O3、Y2O3、HfO2As a sintering aid. Mixing the four powders according to a certain proportion to obtain the standby powder A3.
Wherein, Gd2Zr2O7The purity of the powder is 99.9 percent, and the average particle size is 50 nm; y is2O3、La2O3、HfO2The purity of the powder is 99.5 percent, 99.5 percent and 99.5 percent respectively, and the average particle size is 60nm, 55nm and 70nm respectively;
wherein, Y2O3、La2O3、HfO2Total mass of powder with Gd2Zr2O7The mass ratio of the powder is 1.5: 100, respectively; y is2O3、La2O3、HfO2The mass fraction of the powder accounts for 40 percent, 30 percent and 30 percent of the total mass of the powder;
step two: and adding the standby powder A3 into a ball milling tank filled with high-purity zirconia balls, adding a proper amount of absolute ethyl alcohol as a dispersion medium, and mixing by planetary ball milling to obtain slurry B3.
Wherein, the purity of the zirconia ball is 99.5%;
wherein the mass ratio of the powder A3 to the dispersion medium (absolute ethyl alcohol) is 1: 2;
wherein the rotation speed of the planetary ball milling is 320r/m, and the ball milling time is 10 h;
wherein the temperature here is 40 ℃;
wherein the pressure here is 500 Pa;
step four: and taking the powder C3, carrying out axial dry pressing molding, and carrying out cold isostatic pressing to obtain a biscuit D3.
Wherein, the pressure of the axial dry pressing molding is 30 MPa;
wherein the cold isostatic pressing pressure is 200 MPa.
Step five: placing the biscuit D3 in a sintering furnace, heating to 1700 ℃ in vacuum atmosphere, keeping the temperature for 8h, cooling to 300 ℃, naturally cooling, taking out, and grinding and polishing to 1mm thickness to obtain Gd2Zr2O7Transparent ceramic E3.
Wherein, in the vacuum atmosphere sintering process, the residual gas pressure is (3.5 +/-0.5) multiplied by 10-3Pa；
Wherein the heating rate is controlled at 7 ℃/min; the cooling rate is controlled at 8 ℃/min.
Example 4
The method comprises the following steps: weighing high-purity fine-granularity Gd2Zr2O7The powder is used as a raw material for standby; weighing La2O3、Y2O3、HfO2As a sintering aid. Mixing the four powders according to a certain proportion to obtain the standby powder A4.
Wherein, Gd2Zr2O7The purity of the powder is 99 percent, and the average particle size is 80 nm; y is2O3、La2O3、HfO2The purity of the powder is 99.9 percent, 99.9 percent and 99.5 percent respectively, and the average particle size is 60nm, 55nm and 70nm respectively;
wherein, Y2O3、La2O3、HfO2Total mass of powder with Gd2Zr2O7The mass ratio of the powder is 2.5: 100, respectively; y is2O3、La2O3、HfO2The mass fraction of the powder accounts for 60 percent, 25 percent and 15 percent of the total mass of the powder;
step two: and adding the standby powder A4 into a ball milling tank filled with high-purity zirconia balls, adding a proper amount of absolute ethyl alcohol as a dispersion medium, and mixing by planetary ball milling to obtain slurry B4.
Wherein, the purity of the zirconia ball is 99.9%;
wherein the mass ratio of the powder A4 to the dispersion medium (absolute ethyl alcohol) is 1: 3;
wherein the rotation speed of the planetary ball milling is 350r/m, and the ball milling time is 20 h;
wherein the temperature here is 40 ℃;
wherein the pressure here is 700 Pa;
step four: and taking the powder C4, carrying out axial dry pressing molding, and carrying out cold isostatic pressing to obtain a biscuit D4.
Wherein, the pressure of the axial dry pressing molding is 20 MPa;
wherein the cold isostatic pressing pressure is 300 MPa.
Step five: placing the biscuit D4 in a sintering furnace, heating to 1750 ℃ in a vacuum atmosphere, preserving heat for 10h, cooling to 300 ℃, naturally cooling, taking out, and grinding and polishing to 1mm thickness to obtain Gd2Zr2O7Transparent ceramic E4.
Wherein, in the vacuum atmosphere sintering process, the residual gas pressure is (4.5 +/-0.5) multiplied by 10-3Pa；
Wherein the heating rate is controlled at 5 ℃/min; the cooling rate is controlled at 8 ℃/min.
Example 5
The method comprises the following steps: weighing high-purity fine-granularity Gd2Zr2O7The powder is used as a raw material for standby; weighing La2O3、Y2O3、HfO2As a sintering aid. Mixing the four powders according to a certain proportion to obtain the standby powder A5.
Wherein, Gd2Zr2O7The purity of the powder is 99.9 percent, and the average particle size is 80 nm; y is2O3、La2O3、HfO2The purity of the powder is 99.9%, 99.9% and 99.9%, and the average particle size is 100nm, 80nm and 96 nm;
wherein, Y2O3、La2O3、HfO2Total mass of powder with Gd2Zr2O7The mass ratio of the powder is 2.5: 100, respectively; y is2O3、La2O3、HfO2The mass fraction of the powder accounts for the proportion of the total mass of the powder, the powder and the powder60%, 20% and 20% respectively;
step two: and adding the standby powder A5 into a ball milling tank filled with high-purity zirconia balls, adding a proper amount of absolute ethyl alcohol as a dispersion medium, and mixing by planetary ball milling to obtain slurry B5.
Wherein, the purity of the zirconia ball is 99.9%;
wherein the mass ratio of the powder A5 to the dispersion medium (absolute ethyl alcohol) is 1: 4;
wherein the rotation speed of the planetary ball milling is 200r/m, and the ball milling time is 16 h;
wherein the temperature here is 50 ℃;
wherein the pressure here is 700 Pa;
step four: and taking the powder C5, carrying out axial dry pressing molding, and carrying out cold isostatic pressing to obtain a biscuit D5.
Wherein, the pressure of the axial dry pressing molding is 20 MPa;
wherein the cold isostatic pressing pressure is 250 MPa.
Step five: placing the biscuit D5 in a sintering furnace, heating to 1730 deg.C under vacuum atmosphere, keeping the temperature for 15h, cooling to 300 deg.C, naturally cooling, taking out, grinding and polishing to 1mm thickness to obtain Gd2Zr2O7Transparent ceramic E5.
Wherein, in the vacuum atmosphere sintering process, the residual gas pressure is (2.5 +/-0.5) multiplied by 10-3Pa；
Wherein the heating rate is controlled at 3 ℃/min; the cooling rate is controlled at 10 ℃/min.
FIGS. 1 to 5 show Gd prepared in examples 1 to 5, respectively2Zr2O7Transmittance of transparent ceramic sample.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
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