A method for producing a rare-earth silicate ceramic
Rare earth silicate ceramics were prepared by a low-temperature reactive melting infiltration method using rare earth oxides and rare earth microcrystalline glass. This method solved the problems of high-temperature damage and impurity residue in SiCf/SiC materials, improved the material's resistance to water and oxygen corrosion, and made it suitable for industrial production.
Patent Information
- Application Number
- CN202311810452.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-27
- Publication Date
- 2026-01-09
- Estimated Expiration
- 2043-12-27
AI Technical Summary
In the preparation of SiCf/SiC materials using existing technologies, the high-temperature reaction easily damages the fibers and leaves behind silicon or other impurities, affecting the material's resistance to water and oxygen and its high-temperature mechanical properties, thus shortening the service life of hot-end components of aero-engines.
Rare earth silicate ceramics are prepared by mixing rare earth oxides (RE2O3) and rare earth microcrystalline glass (RE-Al-Si-O) and using a low-temperature reaction melting infiltration method. This method solves the problems of high-temperature damage to fibers and impurity residues in traditional methods.
This method improves the high-temperature resistance to water and oxygen corrosion of the material, reduces the preparation temperature, simplifies the operation process, makes it suitable for industrial production, and provides a new method for preparing modified ceramic matrix composites.
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Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of silicate ceramic preparation, and particularly relates to a preparation method of rare earth silicate ceramic. BACKGROUND
[0002] As one of the most potential structural materials for the hot end components of the new generation of aero-engines, SiC f / SiC material is easy to react with water vapor (H2O) at high temperature to generate volatile substances such as H2SiO4, which causes the decrease of the mechanical properties such as bending strength and shear strength of the composite material, and even leads to material cracking, which seriously affects the service life of the hot end components of the aero-engine. The rare earth silicate has good high-temperature water vapor corrosion resistance, can keep the structure stable in the high-temperature gas environment, and its thermal expansion coefficient matches that of SiC f / SiC material, and is a candidate material for modifying the matrix of SiC f / SiC material.
[0003] At present, silicon or silicon-yttrium alloy is commonly used to prepare yttrium silicate by a reaction melt infiltration method (RMI) to modify SiC f / SiC material. However, the preparation temperature of this method is too high (≥ 1500℃), which is easy to damage the fibers, and there is often residual silicon or other impurities in the matrix of the obtained material, which seriously affects the water-oxygen resistance and high-temperature mechanical properties of the material, so it is urgent to develop a melt infiltration material with low melting point and complete reaction.
[0004] Document 1 "Formation mechanism of Si-Y-C ceramic matrix by reactive melt infiltration using Si-Y alloy and properties of C / Si-Y-C composites" uses reactive melt infiltration (RMI) to introduce Si-Y eutectic alloy into porous C / C preform to prepare C / Si-Y-C composites. The results show that there are four main regions in Si-Y-C matrix, namely amorphous carbon, polycrystalline SiC doped with YSi2, amorphous SiC and single crystal YSi2. Compared with traditional C / C-SiC, the mechanical properties and thermal conductivity of C / Si-Y-C composites are improved. Document 2 "Interaction between Y-Al-Si-O glass-ceramics for environmental barrier coating materials and Ca-Mg-Al-Si-O melts" studies the effect of composition on the properties of Y-Al-Si-O glass. The results show that the increase of Y2O3 content and the decrease of Al / Si ratio improve the nucleation rate, and the CMAS corrosion resistance of most Y2O3-Al2O3-SiO2 system glass-ceramics is better than that of Y2Si2O7. Document 3 "Microstructure and properties of SiC f / SiC joint brazed by Y-Al-Si-O glass" studies the effect of Y-Al-Si-O glass composition and brazing temperature on SiC f / SiC joint, in which Y30 (Y2O3 accounts for 30wt%) glass has good wettability with SiC f / SiC material and can be used for matrix modification of SiC f / SiC material. The invention introduces Y2O3-Al2O3-SiO2 system glass-ceramics into SiC f / SiC material, reacts with rare earth oxides, solves the problem of residual carbon (silicon) caused by traditional silicon infiltration or silicon-yttrium alloy, and rare earth oxides can promote the precipitation of crystals in Y2O3-Al2O3-SiO2 system glass-ceramics, causing glass-ceramic transformation in the material, with a conversion rate of more than 90%, avoiding the problem of softening and flowing out of Y2O3-Al2O3-SiO2 system glass-ceramics in water oxygen environment, and improving its water oxygen corrosion resistance. SUMMARY
[0005] The present application aims to provide a preparation method of rare earth silicate ceramic, which can replace the traditional infiltrant to prepare a rare earth silicate modified ceramic matrix composite and has innovation in method and idea.
[0006] The present application is achieved by the following technical scheme: a preparation method of rare earth silicate ceramic, which specifically comprises the following steps:
[0007] S1, preparing a rare earth glass-ceramic block: mixing raw material powders of the rare earth glass-ceramic block to obtain mixed slurry, drying the mixed slurry to obtain mixed powders, and heating the mixed powders to obtain the rare earth glass-ceramic block through high-temperature holding treatment;
[0008] S2, preparing a rare earth glass-ceramic powder: wet ball milling the rare earth glass-ceramic block obtained in step S1 to obtain slurry, drying the slurry and sieving to obtain the rare earth glass-ceramic powder;
[0009] S3, preparing a rare earth silicate ceramic: mixing the rare earth glass-ceramic powder obtained in step S2 with rare earth oxides, wet ball milling to obtain rare earth silicate ceramic slurry, drying the slurry and pressing into a rare earth silicate ceramic block, and heating and then performing high-temperature holding treatment to obtain the rare earth silicate ceramic.
[0010] Preferably, in step S1, the raw material of the rare earth glass-ceramic block comprises the following components in mass percentage: RE2O3: 20-40wt%, Al2O3: 10-20wt%, SiO2: 50-60wt%, and the particle size of the RE2O3, Al2O3 and SiO2 is 1-5μm. The above mass percentage is suitable for large-scale production, and the rare earth glass-ceramic prepared in this range is uniform in composition, has high crystallinity after sintering at 1400℃, and it is difficult to prepare uniform glass body when the particle size is too small or too large, so the particle size in the above range is adopted in the present application.
[0011] Preferably, the RE is selected from at least one of Y, Yb, Ho, Er, Ho, Dy, Sc, and Lu. In the present application, the bond energy of RE-O is not much different, and the properties of the glass-ceramic formed are similar.
[0012] Preferably, B2O3 is further included, and the addition amount of B2O3 is 5-10% of the mass of the rare earth glass-ceramic block.
[0013] Preferably, in step S1, the parameters of wet ball milling are as follows: a drum ball mill is used, wet ball mixing is performed for 24h, and the rotating speed of the drum ball mill is 250-350r / min.
[0014] As preferred, in the step S1, the parameters of drying are as follows: the drying time is 5-10h, and the drying temperature is 80-120℃.
[0015] As preferred, in the step S1, the parameters of high-temperature holding treatment are as follows: the holding temperature is 1600-1700℃, the holding time is 2-3h, and the heating rate is 5℃ / min.
[0016] As preferred, in the step S2, the parameters of wet ball milling are as follows: a planetary ball mill is adopted, the wet ball milling time is 24h, and the rotation speed of the planetary ball mill is 250-350r / min.
[0017] As preferred, in the step S2, the parameters of drying are as follows: the drying time is 5-10h, and the drying temperature is 80-120℃.
[0018] As preferred, in the step S2, the mesh number of sieving is 200.
[0019] As preferred, in the step S3, the rare earth oxide is selected from at least one of Y2O3, Yb2O3, Ho2O3, Er2O3, Dy2O3, Dy2O3, Sc2O3 and Lu2O3, and the mass ratio of the rare earth microcrystalline glass powder and the rare earth oxide is 1:(1-2).
[0020] As preferred, in the step S3, the parameters of wet ball milling are as follows: a planetary ball mill is adopted, the wet ball milling time is 24h, and the rotation speed of the planetary ball mill is 250-350r / min.
[0021] As preferred, the parameters of drying are as follows: the drying time is 5-10h, and the drying temperature is 80-120℃.
[0022] As preferred, in the step S3, the parameters of high-temperature holding treatment are as follows: the holding temperature is 1400℃, the holding time is 3h, and the heating rate is 5℃ / min.
[0023] As preferred, in the step S3, the parameters of pressing are as follows: the pressing stress is 10-20MPa, and the pressing time is 5-10min.
[0024] Compared with the prior art, the present application has the following advantages:
[0025] 1. The present application firstly proposes to realize the preparation of rare earth silicate ceramics by using rare earth oxide (RE2O3) and rare earth microcrystalline glass (RE-Al-Si-O), which provides a new idea for the preparation of rare earth silicate ceramics and the transformation of rare earth microcrystalline glass to ceramics.
[0026] 2, Si-Y alloy reaction melting depth preparation of SiC in document 1 f Compared with the SiC material, the application solves the problem of excessive residual carbon or residual silicon, and can effectively improve the high-temperature water-oxygen corrosion resistance of the material; compared with the rare earth silicate (≥ 1500 DEG C) prepared by SiO2 pressureless sintering in document 4 "Watervapour corrosion of rare earth monosilicates for environmental barrier coating application", the preparation temperature of the application is low (1300-1400 DEG C), and the problem of fiber and matrix damage caused by excessively high preparation temperature can be solved.
[0027] 3, The method provided by the patent has low cost, simple preparation process, short preparation period, strong repeatability, no special requirement for equipment, and can realize industrial production, and provides a new method for preparing rare earth silicate modified ceramic matrix composite by reaction infiltration method;
[0028] 4, The application provides a method for preparing rare earth silicate ceramic by using rare earth glass-ceramics, wherein rare earth oxides (RE2O3) and rare earth glass-ceramics (RE-Al-Si-O) are mixed and pressed into tablets, and the rare earth silicate ceramic is formed by reaction at a high temperature of 1300-1400 DEG C in a vacuum furnace, which can be used for preparing rare earth silicate ceramic powder, and can also be used for preparing rare earth silicate modified ceramic matrix composite and rare earth silicate ceramic coating. BRIEF DESCRIPTION OF DRAWINGS
[0029] Figure 1 The XRD pattern of Yb2Si2O7 ceramic powder prepared in example 1 of the application;
[0030] Figure 2 The SEM pattern and energy spectrum area scanning result of Yb2Si2O7 ceramic powder prepared in example 1 of the application;
[0031] Figure 3 Yb2Si2O7 modified SiC prepared in example 4 of the application f The scanning photo of the / SiC composite material. DETAILED DESCRIPTION
[0032] In order to make the above-mentioned purposes, features and advantages of the application more obvious and easy to understand, the specific embodiments of the application will be described in detail below with reference to the drawings.
[0033] It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the present application. Additionally, for a range of values of, for example, the upper limit and lower limit of a range of values are included in the range. Each intermediate value of the stated range and each smaller range between any two intermediate values in the stated range and each stated value in the stated range are also included in the present application. The upper and lower limits of these smaller ranges can independently be included or excluded in the ranges.
[0034] Many modifications and variations of the present application described herein will be apparent to those of ordinary skill in the art from the foregoing description. Accordingly, the scope of the present application should be determined by reference to the appended claims and their equivalents rather than by reference to the foregoing description, which is by way of example only.
[0035] The specific embodiment of the present application aims to provide a preparation method of rare earth silicate ceramics, which specifically comprises the following steps:
[0036] S1, preparing a rare earth glass-ceramic block: mixing raw material powders of the rare earth glass-ceramic block to obtain a mixed slurry, drying the mixed slurry to obtain a mixed powder, and heating the mixed powder to obtain the rare earth glass-ceramic block through high-temperature holding treatment;
[0037] S2, preparing a rare earth glass-ceramic powder: wet ball-milling the rare earth glass-ceramic block prepared in step S1 to obtain a slurry, drying the slurry, and sieving to obtain the rare earth glass-ceramic powder;
[0038] S3, preparing a rare earth silicate ceramic: mixing the rare earth glass-ceramic powder prepared in step S2 with a rare earth oxide, wet ball-milling to obtain a rare earth silicate ceramic slurry, drying the slurry, pressing into a rare earth silicate ceramic block, and heating to obtain the rare earth silicate ceramic through high-temperature holding treatment.
[0039] In the specific embodiment, in step S1, the raw material of the rare earth glass-ceramic block comprises the following components in mass percentage: RE2O3: 20-40 wt%, Al2O3: 10-20 wt%, SiO2: 50-60 wt%, and the particle size of the RE2O3, Al2O3 and SiO2 is 1-5 μm.
[0040] In the specific embodiment, RE is selected from at least one of Y, Yb, Ho, Er, Ho, Dy, Sc, and Lu.
[0041] In the specific embodiment, B2O3 is further included, and the addition amount of the B2O3 is 5-10% of the mass of the rare earth glass-ceramic block.
[0042] In the specific embodiment, in step S1, the parameters of wet ball milling are as follows: a drum ball mill is used, wet ball mixing is performed for 24 h, and the rotating speed of the drum ball mill is 250-350 r / min.
[0043] In the specific embodiment, in step S1, the parameters of drying are as follows: the drying time is 5-10 h, and the drying temperature is 80-120 DEG C.
[0044] In the specific embodiment, in step S1, the parameters of high-temperature heat preservation treatment are as follows: the heat preservation temperature is 1600-1700 DEG C, the heat preservation time is 2-3 h, and the temperature rising rate is 5 DEG C / min.
[0045] In the specific embodiment, in step S2, the parameters of wet ball milling are as follows: a planetary ball mill is used, wet ball milling is performed for 24 h, and the rotating speed of the planetary ball mill is 250-350 r / min.
[0046] In the specific embodiment, in step S2, the parameters of drying are as follows: the drying time is 5-10 h, and the drying temperature is 80-120 DEG C.
[0047] In the specific embodiment, in step S2, the mesh number of sieving is 200.
[0048] In the specific embodiment, in step S3, the rare earth oxide is selected from at least one of Y2O3, Yb2O3, Ho2O3, Er2O3, Dy2O3, Dy2O3, Sc2O3 and Lu2O3, and the mass ratio of the rare earth microcrystalline glass powder to the rare earth oxide is 1:(1-2).
[0049] In the specific embodiment, in step S3, the parameters of wet ball milling are as follows: a planetary ball mill is used, wet ball milling is performed for 24 h, and the rotating speed of the planetary ball mill is 250-350 r / min.
[0050] In the specific embodiment, in step S3, the parameters of drying are as follows: the drying time is 5-10 h, and the drying temperature is 80-120 DEG C.
[0051] In the specific embodiment, in step S3, the parameters of high-temperature heat preservation treatment are as follows: the heat preservation temperature is 1400 DEG C, the heat preservation time is 3 h, and the temperature rising rate is 5 DEG C / min.
[0052] In the specific embodiment, in step S3, the parameters of pressing are as follows: the pressing stress is 10-20 MPa, and the pressing time is 5-10 min.
[0053] The technical effects of the present application are described below in combination with specific embodiments.
[0054] Embodiment 1
[0055] Step 1: Preparation of the rare earth glass-ceramic powder: Y2O3, Al2O3, SiO2 powders are mixed in a mass ratio of 30:15:55, 5wt% B2O3 powder is added as fluxing agent, then wet ball mixing is performed in a drum ball mill for 24h, the ball milling speed is 250-350r / min, the obtained slurry is placed in an oven and dried at 80℃ for 10h. The dried powder is heated at 1600℃ for 3h, the heating rate is 5℃ / min, then water quenching is performed, and a rare earth glass-ceramic Y2O3-Al2O3-SiO2 block is obtained. The rare earth glass-ceramic Y2O3-Al2O3-SiO2 block is wet ball milled in a planetary ball mill for 24h, the obtained slurry is placed in an oven and dried at 80℃ for 10h, and then the rare earth glass-ceramic Y2O3-Al2O3-SiO2 powder is obtained by sieving through a 200 mesh sieve.
[0056] Step 2: Preparation of the rare earth silicate ceramic: the rare earth glass-ceramic Y2O3-Al2O3-SiO2 powder and Yb2O3 powder are mixed in a mass ratio of 2:1 in a ball mill for 24h, the obtained slurry is placed in an oven and dried at 80℃ for 10h, and then the dried powder is pressed into a ceramic block, which is heated at 1400℃ for 3h, the heating rate is 5℃ / min, and a Yb2Si2O7 ceramic block is prepared.
[0057] The prepared product is detected, and the detection results are shown in Figure 1 and Figure 2 Figure 1 is an XRD pattern of the Yb2Si2O7 ceramic powder prepared in Example 1 of the present application, Figure 2 is an SEM pattern and energy spectrum area scanning result of the Yb2Si2O7 ceramic powder prepared in Example 1 of the present application.
[0058] Further detection shows that the main crystal phase of the ceramic generated under the condition is Yb2Si2O7, the mass gain is 0.11% after corrosion in a water-oxygen environment of 1250℃, 50% H2O-50% O2 for 100h, and the ceramic exhibits good water-oxygen resistance. A small amount of Y2SiO5 is precipitated on the surface of the material after water-oxygen corrosion.
[0059] Example 2
[0060] Step 1: Preparation of rare earth glass-ceramic powder: Y2O3, Al2O3, SiO2powder was mixed according to the mass ratio of 25:15:60, 5wt% B2O3 powder was added to flux, then wet ball mixing in a roller ball mill for 24h, the ball milling speed was 250-350r / min, the obtained slurry was placed in an oven and dried at 80℃ for 10h. The dried powder was heat treated at 1600℃ for 3h with a heating rate of 5℃ / min, and then water quenching, to obtain rare earth glass-ceramic Y2O3-Al2O3-SiO2 block. The rare earth glass-ceramic Y2O3-Al2O3-SiO2 block was wet ball milled in a planetary ball mill for 24h, the obtained slurry was placed in an oven and dried at 80℃ for 10h, and then sieved through a 200 mesh sieve to obtain rare earth glass-ceramic Y2O3-Al2O3-SiO2 powder.
[0061] Step 2: Preparation of rare earth silicate ceramic: The rare earth glass-ceramic Y2O3-Al2O3-SiO2 powder and Yb2O3 powder were mixed according to the mass ratio of 1:1 in a ball mill for 24h, the obtained slurry was placed in an oven and dried at 80℃ for 10h, and then the dried powder was pressed into a ceramic block, which was heat treated at 1400℃ for 3h with a heating rate of 5℃ / min, to obtain ytterbia ceramic block.
[0062] It was found through testing that, with the increase of Yb2O3 content, the diffraction peak intensity of Yb2Si2O7 increased, the yield of ytterbia increased, and the mass increased by 0.14% after corrosion in a water-oxygen environment of 1250℃, 50% H2O-50% O2 for 100h.
[0063] Example 3
[0064] Step 1: Preparation of rare earth glass-ceramic powder: Y2O3, Al2O3, SiO2powder was mixed according to the mass ratio of 25:15:60, 5wt% B2O3 powder was added to flux, then wet ball mixing in a roller ball mill for 24h, the ball milling speed was 250-350r / min, the obtained slurry was placed in an oven and dried at 80℃ for 10h. The dried powder was heat treated at 1600℃ for 3h with a heating rate of 5℃ / min, and then water quenching, to obtain rare earth glass-ceramic Y2O3-Al2O3-SiO2 block. The rare earth glass-ceramic Y2O3-Al2O3-SiO2 block was wet ball milled in a planetary ball mill for 24h, the obtained slurry was placed in an oven and dried at 80℃ for 10h, and then sieved through a 200 mesh sieve to obtain rare earth glass-ceramic Y2O3-Al2O3-SiO2 powder.
[0065] Step 2: Preparation of rare earth silicate ceramic: Rare earth glass-ceramics Y2O3-Al2O3-SiO2 powder and Yb2O3 powder were mixed in a ball mill for 24 h at a mass ratio of 1:2. The mixed slurry was placed in an oven and dried at 80℃ for 10 h. The dried powder was pressed into a ceramic block, which was heat treated at 1400℃ for 3 h at a heating rate of 5℃ / min to prepare Yb2Si2O7 ceramic block.
[0066] It was found through testing that the strength of Yb2Si2O7 increased with further increase of Yb2O3 content. The mass gain was 0.097% after corrosion in a 1250℃, 50% H2O-50% O2 water-oxygen environment for 100 h.
[0067] Example 4
[0068] Step 1: Preparation of rare earth glass-ceramics powder: Y2O3, Al2O3 and SiO2 powders were mixed at a mass ratio of 30:15:55, and 5wt% B2O3 powder was added as flux. The mixture was then wet ball mixed in a drum ball mill for 24 h. The mixed slurry was placed in an oven and dried at 80℃ for 10 h. The dried powder was heat treated at 1600℃ for 3 h at a heating rate of 5℃ / min, followed by water quenching to obtain a rare earth glass-ceramics Y2O3-Al2O3-SiO2 block. The rare earth glass-ceramics Y2O3-Al2O3-SiO2 block was wet ball milled in a planetary ball mill for 24 h. The obtained slurry was placed in an oven and dried at 80℃ for 10 h, and then sieved through a 200 mesh sieve to obtain rare earth glass-ceramics Y2O3-Al2O3-SiO2 powder.
[0069] Step 2: Slurry preparation and impregnation: 80wt% water and 1wt% ammonium lithium polyacrylate were mixed and magnetically stirred for 30 min at a stirring rate of 100 r / min. 15wt% Yb2O3 was added to the mixed liquid and ball milled at a drum rotation speed of 120 r / min for 12 h to obtain a mixed Yb2O3 slurry. The semi-dense SiC f / SiC material was vacuum and pressure impregnated with the Yb2O3 slurry and dried at 80℃ for 10 h.
[0070] Step 3: Preparation of Yb2Si2O7 modified SiC f / SiC material by glass melt reaction infiltration: The dried SiC f / SiC material was embedded in Y2O3-Al2O3-SiO2 powder and placed in a vacuum sintering furnace and heated to 1400℃ for 3 h at a heating rate of 5℃ / min under vacuum protection to obtain Yb2Si2O7 modified SiC f / SiC composite material.
[0071] Yb2Si2O7 modified SiC prepared in Example 4 of the present application f The Yb2Si2O7 modified SiC composite material prepared in Example 4 of the present application was detected, and the detection results are shown in Figure 3 Figure 3 Yb2Si2O7 modified SiC prepared in Example 4 of the present application f The scanning photograph of the Yb2Si2O7 modified SiC composite material prepared in Example 4 of the present application.
[0072] Although the present application has been disclosed as above, the protection scope of the present application is not limited to this. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present application, and these changes and modifications shall fall within the protection scope of the present application.
Claims
1. A method for producing a rare-earth silicate ceramic, characterized by, The preparation method specifically comprises the following steps: S1, preparing a rare earth glass-ceramic bulk: mixing raw material powders of the rare earth glass-ceramic bulk to obtain a mixed slurry, drying the mixed slurry to obtain a mixed powder, and heating the mixed powder to obtain the rare earth glass-ceramic bulk through high-temperature heat preservation treatment; S2, preparing a rare earth glass-ceramic powder: wet ball milling the rare earth glass-ceramic bulk obtained in step S1 to obtain a slurry, drying the slurry, and sieving to obtain the rare earth glass-ceramic powder; S3, preparing a rare earth silicate ceramic: mixing the rare earth glass-ceramic powder obtained in step S2 with a rare earth oxide, wet ball milling to obtain a rare earth silicate ceramic slurry, drying the slurry, and pressing into a rare earth silicate ceramic bulk, and heating to obtain the rare earth silicate ceramic through high-temperature heat preservation treatment; In step S1, the raw material of the rare earth glass-ceramic bulk comprises the following components in mass percentage: RE2O3: 20-40 wt%, Al2O3: 10-20 wt%, SiO2: 50-60 wt%, and the particle size of the RE2O3, Al2O3 and SiO2 is 1-5 μm; B2O3 is further included, and the addition amount of the B2O3 is 5-10% of the mass of the rare earth glass-ceramic bulk, and the RE is selected from at least one of Y, Yb, Er, Ho, Dy, Sc, and Lu.
2. The method for producing a rare-earth silicate ceramic according to claim 1, characterized by, In step S1, the parameters of wet ball milling are as follows: a drum ball mill is used, wet ball mixing is performed for 24 h, and the rotating speed of the drum ball mill is 250-350 r / min; and / or, In step S1, the parameters of drying are as follows: the drying time is 5-10 h, and the drying temperature is 80-120 °C; and / or, In step S1, the parameters of high-temperature heat preservation treatment are as follows: the heat preservation temperature is 1600-1700 °C, the heat preservation time is 2-3 h, and the heating rate is 5 °C / min.
3. The method for producing a rare-earth silicate ceramic according to claim 1, wherein In step S2, the parameters of wet ball milling are as follows: a planetary ball mill is used, wet ball milling is performed for 24 h, and the rotating speed of the planetary ball mill is 250-350 r / min; and / or, In step S2, the parameters of drying are as follows: the drying time is 5-10 h, and the drying temperature is 80-120 °C; and / or, In step S2, the mesh number of sieving is 200.
4. The method for producing a rare-earth silicate ceramic according to claim 1, wherein In step S3, the rare earth oxide is selected from at least one of Y2O3, Yb2O3, Ho2O3, Er2O3, Dy2O3, Sc2O3, and Lu2O3, and the mass ratio of the rare earth glass-ceramic powder to the rare earth oxide is 1:(1-2).
5. The method for producing a rare-earth silicate ceramic according to claim 1, wherein In step S3, the parameters of wet ball milling are as follows: a planetary ball mill is used, wet ball milling is performed for 24 h, and the rotating speed of the planetary ball mill is 250-350 r / min; and / or, The parameters of drying are as follows: the drying time is 5-10 h, and the drying temperature is 80-120 °C.
6. The method for producing a rare-earth silicate ceramic according to claim 1, wherein In step S3, the parameters of high-temperature heat preservation treatment are as follows: the heat preservation temperature is 1400 °C, the heat preservation time is 3 h, and the heating rate is 5 °C / min.
7. The method for producing a rare-earth silicate ceramic according to claim 1, wherein In step S3, the parameters of pressing are as follows: the pressing stress is 10-20 MPa, and the pressing time is 5-10 min.
Citation Information
Patent Citations
Ceramic material of microcrystalline glass, and preparation method
CN1872753A