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CN112939603A - Method for sintering yttrium oxide ceramic crucible at low temperature - Google Patents

Method for sintering yttrium oxide ceramic crucible at low temperature Download PDF

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CN112939603A
CN112939603A CN202110388155.7A CN202110388155A CN112939603A CN 112939603 A CN112939603 A CN 112939603A CN 202110388155 A CN202110388155 A CN 202110388155A CN 112939603 A CN112939603 A CN 112939603A
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powder
sintering
yttrium oxide
crucible
magnesium
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CN112939603B (en
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刘岩
李浩然
刘学建
黄政仁
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Jiangsu Institute Of Advanced Inorganic Materials
Shanghai Institute of Ceramics of CAS
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Suzhou Research Institute Shanghai Institute Of Ceramics Chinese Academy Of Sciences
Shanghai Institute of Ceramics of CAS
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Abstract

本发明涉及一种低温烧结氧化钇陶瓷坩埚的方法，选用氧化镁粉体和氧化钛粉体作为烧结助剂，直接与氧化钇粉体混合后压制成坩埚素坯，再进行烧结致密化，得到致密的氧化钇陶瓷坩埚；优选地，所述烧结助剂的含量为10～25wt%。

Figure 202110388155

The invention relates to a method for sintering yttrium oxide ceramic crucible at low temperature. Magnesium oxide powder and titanium oxide powder are selected as sintering aids, directly mixed with yttrium oxide powder and pressed into a crucible green body, and then sintered and densified to obtain A dense yttrium oxide ceramic crucible; preferably, the content of the sintering aid is 10-25wt%.

Figure 202110388155

Description

Method for sintering yttrium oxide ceramic crucible at low temperature
Technical Field
The invention relates to a preparation method of a ceramic crucible for titanium alloy vacuum induction melting, in particular to a method for sintering an yttrium oxide ceramic crucible at a low temperature by taking magnesium metatitanate or/and magnesium dititanate as a sintering aid, belonging to the field of erosion-resistant ceramics.
Background
The titanium alloy has the advantages of low density, high specific modulus, high-temperature strength, high-temperature creep resistance, high oxidation resistance, high melting point and the like, and is one of the indispensable alloys in the fields of aerospace, automobile manufacturing, biomedical engineering and the like. At present, a vacuum consumable electrode (VAR) smelting method is mainly used in the smelting process of the titanium alloy, and the titanium alloy smelted by the method has low overheating temperature, so that the smelted alloy has uneven microstructure and chemical components, large brittleness and poor hot-working performance; in addition, the process adopts a water-cooled copper crucible for forced cooling, so that the smelting cost is greatly improved. In view of the limitation of vacuum consumable electrode (VAR), in recent years, the vacuum induction melting technology of ceramic crucible is adopted as a new titanium alloy preparation process to reflect the eye curtain of people, compared with the traditional vacuum consumable electrode melting method, the method has the advantages of higher superheat degree, less volatilization of alloy elements, less component segregation and the like, and the problems of thick skull generation, high energy consumption and the like are avoided because of no adoption of forced water cooling measures, so the method is a novel technology for melting high-quality titanium alloy. The most important equipment in the vacuum induction melting technology of the ceramic crucible is the ceramic crucible, because titanium is an extremely active metal element, the titanium can almost have chemical reactions with most refractory materials at different degrees at high temperature, so that the pollution of the titanium alloy material is increased, the service performance of the titanium alloy material is reduced, and the service life of the refractory materials is also reduced. Therefore, there is a need for a ceramic crucible that is resistant to high temperatures, thermal shock, and chemical reactions with the alloy melt during alloy melting. Therefore, the search for a low cost, erosion resistant and long life ceramic crucible has become a major factor affecting the quality and cost of titanium alloys.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a method for preparing a yttria-based ceramic crucible for titanium alloy smelting, low temperature sintering, corrosion resistance and long service life.
In the first aspect, the invention provides a method for sintering an yttrium oxide ceramic crucible at a low temperature, which comprises the steps of selecting magnesium oxide powder and titanium oxide powder as sintering aids, directly mixing the magnesium oxide powder and the titanium oxide powder with yttrium oxide powder, pressing the mixture into a crucible blank, and sintering and densifying the crucible to obtain a dense yttrium oxide ceramic crucible; preferably, the content of the sintering aid is 10-25 wt%, and preferably 15-20 wt%.
Preferably, the molar ratio of the titanium oxide powder to the magnesium oxide powder is 1: 1-2: 1; the purity of the titanium oxide powder and the magnesium oxide powder is 95-99.99%, and the particle size range is 1-10 μm.
Preferably, the sintering densification temperature is not less than 1610 ℃, preferably 1610 to 1650 ℃, and more preferably 1645 to 1650 ℃; and the sintering densification time is 1-8 hours.
In the sintering densification process, partial titanium oxide powder and magnesium oxide powder in the sintering aid firstly form magnesium metatitanate powder (with a melting point of 1610 ℃) or/and magnesium dititanate powder (with a melting point of 1645 ℃) so as to form a liquid phase at a sintering densification temperature of more than or equal to 1610 ℃, so that the particle rearrangement and mass transfer processes are greatly promoted, and finally, the sintering densification of the yttrium oxide is realized.
Preferably, the sintering aid, the yttrium oxide powder, the grinding balls, the solvent and the binder are mixed to obtain suspension slurry, and the suspension slurry is subjected to ball milling, drying, grinding and sieving to obtain mixed powder.
Preferably, the mass of the sintering aid is 3-10 wt% of the weight of the yttrium oxide powder.
Preferably, the sieving is a sieve with 800 meshes to 400 meshes (18 mu m to 38 mu m).
Preferably, the solvent is a mixed solution of 2-butanone and/or ethanol, wherein the mass ratio of the 2-butanone to the ethanol is (0-20) to (80-100); the binder is at least one of polyvinyl butyral, epoxy resin, phenolic resin and dextrin, and the addition amount of the binder is not more than 0-6% of the total mass of the yttrium oxide powder and the sintering aid.
Preferably, the solid content of the suspension slurry is 50-65 wt%.
Through further research by the inventor, the following results are found: only by increasing the addition of magnesium oxide and titanium oxide can the probability of forming magnesium metatitanate or/and magnesium dititanate in the system be increased, and the density increase can be realized. However, magnesium oxide and titanium oxide which are not completely reacted in the sintering system still remain in the system in the form of a third phase, which not only results in the waste of raw materials, but also causes the reduction of the mechanical properties of the crucible due to the excessive remaining magnesium oxide and titanium oxide.
On the basis, the inventor also creatively provides a method for sintering the yttrium oxide ceramic crucible at low temperature, magnesium metatitanate powder or/and magnesium dititanate powder is directly selected as a sintering aid, is mixed with yttrium oxide powder and then is pressed into a crucible blank, and then is sintered and densified to obtain the dense yttrium oxide ceramic crucible.
In the invention, the magnesium metatitanate powder or/and magnesium dititanate powder and yttrium oxide powder are mixed and pressed into a crucible biscuit, and in the subsequent sintering process, the sintering aid can generate a proper liquid phase, which can greatly promote the particle rearrangement and mass transfer processes. The mechanism of action of the sintering aid is to produce a liquid phase at a relatively low temperature to promote sintering. Specifically, the melting point of the magnesium metatitanate powder is 1610 ℃, the magnesium metatitanate powder is melted to generate a liquid phase in the process of sintering and densifying the yttrium oxide, and the diffusion coefficient of the yttrium oxide in the liquid phase is increased. Compared with solid-phase sintering, the yttrium oxide is more favorable for diffusion in liquid-phase sintering, so that the yttrium oxide is sintered and compacted at low temperature, and the compacted yttrium oxide ceramic crucible is finally obtained. Likewise, MgTi2O5Has a melting point of 1645 ℃ and can also be densified at temperatures much lower than the conventional densification temperature (at least 2000 ℃) of yttria.
Preferably, titanium oxide powder and magnesium oxide powder are mixed and then subjected to solid-phase synthesis to obtain magnesium metatitanate or magnesium dititanate; preferably, the purity of the titanium oxide powder and the magnesium oxide powder is 95-99.99%, and the particle size range is 1-10 μm; the molar ratio of the titanium oxide powder to the magnesium oxide powder is 1:1 or 2: 1; the temperature of the solid phase synthesis is 1300-1400 ℃, and the synthesis atmosphere is air atmosphere.
Preferably, the sintering aid, the yttrium oxide powder, the grinding balls, the solvent and the binder are mixed to obtain suspension slurry, and the suspension slurry is subjected to ball milling, drying, grinding and sieving to obtain mixed powder.
Preferably, the mass of the sintering aid is 3-10 wt% of the weight of the yttrium oxide powder.
Preferably, the sieving is a sieve with 800 meshes to 400 meshes (18 mu m to 38 mu m).
Preferably, the solvent is a mixed solution of 2-butanone and/or ethanol, wherein the mass ratio of the 2-butanone to the ethanol is (0-20) to (80-100); the binder is at least one of polyvinyl butyral, epoxy resin, phenolic resin and dextrin, and the addition amount of the binder is not more than 0-6% of the total mass of the yttrium oxide powder and the sintering aid.
Preferably, the solid content of the suspension slurry is 50-65 wt%.
Preferably, the sintering densification temperature is not lower than the melting point of the sintering aid, preferably 1610 to 1650 ℃, and the time is 1 to 8 hours; more preferably, the sintering aid is magnesium metatitanate powder, and the densification temperature is 1610 ℃ to 1650 ℃; the sintering aid contains magnesium dititanate powder, and the densification temperature is 1645-1650 ℃. Preferably, the sintering aid is magnesium metatitanate powder, and the densification temperature is 1610 ℃ to 1650 ℃; the sintering aid contains magnesium dititanate powder, and the densification temperature is 1645-1650 ℃.
On the other hand, the invention also provides a compact yttrium oxide ceramic crucible prepared by the method, and the compactness of the compact yttrium oxide ceramic crucible is 98-99.5% of the theoretical density.
Has the advantages that:
1. the invention provides a preparation method which is generally applicable to vacuum induction melting of titanium alloy crucibles and has strong application background;
2. the ceramic crucible provided by the invention has the advantages that the preparation process is simple, the operation and the control are easy, only a simple cold isostatic pressing process is adopted, the process steps are simplified, and the energy consumption is reduced;
3. the yttrium oxide-based ceramic crucible prepared by the invention has good erosion resistance, high thermal shock resistance and bending strength, and excellent service performance;
4. the crucible provided by the invention has the advantages of lower sintering temperature and longer service life, and can reduce the manufacturing cost of the crucible.
Drawings
FIG. 1 (a) is an external view of a low-temperature sintered yttria-based crucible prepared in example 1;
FIG. 1 (b) is a graph of the density of the low temperature sintered yttria-based crucible prepared in example 1;
FIG. 2 is a microscopic view of a low-temperature sintered yttrium oxide-based crucible prepared in example 1;
FIG. 3 is a graph of the flexural strength of the low temperature sintered yttria-based crucible prepared in example 1;
FIG. 4 (a) is an external view of a low-temperature sintered yttria-based crucible prepared in example 2;
FIG. 4 (b) is a microscopic view of a low-temperature sintered yttrium oxide-based crucible prepared in example 2;
FIG. 5 is a graph of the flexural strength of the low temperature sintered yttria-based crucible prepared in example 3.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
The invention provides a preparation method generally applicable to vacuum induction melting of titanium alloy crucibles, which realizes the preparation of yttrium oxide crucibles by low-temperature sintering and can overcome the defects of short service life and high titanium alloy melting cost of crucible preparation in the existing vacuum induction melting technology.
According to the invention, a small amount of sintering aid and binder are added, meanwhile, the organic matter of the yttrium oxide-based crucible is controlled not to exceed 6 wt% of the total mass of yttrium oxide ceramic powder and the sintering aid, the sintering aid is magnesium metatitanate (the melting point of which is 1610 ℃) or/and magnesium dititanate (the melting point of which is 1645 ℃) synthesized by titanium oxide and magnesium oxide through solid-phase reaction, and finally, the yttrium oxide-based crucible has good mechanical property, is uniform and compact in microstructure, and is very suitable for anti-erosion melting between ceramics and titanium alloy.
The following is an exemplary description of the preparation method of the yttrium oxide crucible sintered at low temperature by using magnesium metatitanate as a sintering aid.
And uniformly dispersing the magnesium oxide powder and the titanium dioxide powder in a solvent, drying and then preparing the sintering aid magnesium metatitanate in a muffle furnace.
Then, the yttrium oxide ceramic powder, the sintering aid (magnesium metatitanate powder), the grinding balls and the binder are uniformly dispersed in the solvent, and the slurry is obtained after ball milling. Wherein the mass ratio of the small balls to the total mass of the yttrium oxide ceramic powder and the sintering aid is 1: 1. The mass of the binder is not more than 6 wt% of the total mass of the ceramic powder and the sintering aid. Can avoid the defects of larger holes, cracks and the like in the later sintering process, and is favorable for improving the strength and the thermal shock resistance of the crucible. Specifically, the yttrium oxide ceramic powder, the sintering aid, the pellets, the binder and the like are gradually added in a step-by-step adding manner, so that the content of the sintering aid can reach 3-10 wt% of the total mass of the yttrium oxide ceramic powder. As an example, yttria ceramic powder and sintering aid are dissolved in a solvent, ball milled for 8 to 20 hours (for example, 14 hours), and then a binder is added, and ball milled for 4 to 20 hours (for example, 12 hours), so as to prepare slurry for low-temperature sintering.
And drying the slurry in an oven to obtain the yttrium oxide-based ceramic powder with low sintering temperature.
And (3) loading the yttrium oxide-based ceramic powder into a mold, and performing pressure forming by using a cold isostatic pressing method to obtain a crucible biscuit.
And placing the crucible biscuit in a muffle furnace for sintering and compacting to obtain a compact yttrium oxide-based crucible.
In the method, the mass percentage of the yttrium oxide ceramic powder can be 90-97% of the total mass of the yttrium oxide ceramic powder and the sintering aid. The sintering aid can be a mixture of two eutectic powder with a certain mixing ratio, and can also be a single powder with a low melting point. The mass percentage of the sintering aid powder can be 3-10% of the total mass of the ceramic powder and the sintering aid powder. When the yttrium oxide ceramic powder and the sintering aid powder are selected, the particle size range of the yttrium oxide ceramic powder can be 1-10 mu m, and the particle size range of the sintering aid powder can be 1-10 mu m.
In an alternative embodiment, the beads are zirconia beads added in an amount of 100 wt.% of the total mass of the yttria ceramic powder and the sintering aid.
In an alternative embodiment, the binder is polyvinyl butyral or the like, and is added in an amount of not more than 6 wt.%, for example 3 wt.%, of the total mass of the yttria ceramic powder and the sintering aid.
In an alternative embodiment, the solvent can be 2-butanone and/or ethanol, wherein the mass ratio of the 2-butanone to the ethanol is (0-20): (80-100), such as 0: 100.
In an optional embodiment, the drying temperature is 70 to 100 ℃ and the drying time is 8 to 18 hours, for example, 80 ℃ for 12 hours.
In an alternative embodiment, the isostatic pressure is 200 to 250MPa, and the dwell time is 1 to 3 minutes, for example 200MPa for 2 minutes.
In an optional embodiment, the sintering temperature of the ceramic crucible is 1550-1650 ℃, and the heat preservation time is 1-8 hours. In the sintering process, the size of the crucible biscuit is reduced by about 20-40% due to volatilization of the binder and the appearance of a sintering aid liquid phase, and the proper sintering temperature and sintering time can avoid cracks caused by severe shrinkage of the crucible biscuit or density reduction caused by failure of the sintering temperature.
It should be noted that the above embodiment, while exemplified by magnesium metatitanate, is equally applicable to magnesium dititanate or a mixture of the two.
In the present disclosure, when the sintering aid is selected from titanium oxide powder and magnesium oxide powder, the molar ratio of the titanium oxide powder to the magnesium oxide powder may be 1:1 to 2: 1. The addition amount of the additive needs to meet 15-25 wt%. If the addition amount is insufficient, Y2O3The crucible performance is not significantly improved. If the amount of Y is too large, Y will be caused2O3The mechanical properties of the crucible are reduced.
In an optional embodiment, the sintering densification temperature is not less than 1610 ℃, preferably 1610 to 1650 ℃, and more preferably 1645 to 1650 ℃; and the sintering densification time is 1-8 hours.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
5 wt.% of MgTiO with the sintering temperature of 1650 ℃ and the heat preservation time of 2h is prepared3Powder sintering of Y2O3The crucible comprises the following steps:
(1) the sintering aid content of the yttrium oxide crucible forming slurry sintered at low temperature by taking magnesium metatitanate as the sintering aid is 5 wt.%, and MgTiO3The powder is prepared by solid-phase reaction, MgO and TiO21 mol.% to 1 mol.%; binder addition 3 wt.%;
(2) 160gY was prepared according to the above design ratio2O327.6g of MgO powder with the particle size of 1 μm and 27.6g of TiO powder are weighed respectively based on the crucible forming slurry252.4g of powder, ZrO2Ball: 80g, solvent: 48g of absolute ethanol and 1 mu m Y2O3160g of powder MgTiO3Powder (prepared by solid phase reaction) 8g, ZrO2Ball: 168g, binder: polyvinyl butyral (PVB)5.04g, solvent: 102g of absolute ethyl alcohol.
(3) Firstly, MgO powder and TiO are mixed2Placing the powder and solvent into polyethylene tank, sealing, adding ZrO2Ball milling is carried out, and materials are mixed for 14 hours on a planetary mixer; and (3) placing the slurry in a vacuum drying oven, drying at the temperature of 80 ℃ for 12h, and preserving the dried powder in a muffle furnace at the temperature of 1350 ℃ for 4h to obtain the sintering aid magnesium metatitanate.
(4) Will Y2O3Powder of MgTiO3Placing the powder and solvent into polyethylene tank, sealing, adding ZrO2Ball milling is carried out, and materials are mixed for 14 hours on a planetary mixer; then, a binder is added to the polymerAnd (3) in an ethylene tank, after sealing, mixing all the raw materials for 12h, placing the slurry in a vacuum drying oven, drying at the temperature of 80 ℃ for 12h, and drying to obtain the powder for low-temperature sintering.
(5) And (3) putting the powder into a mold, pressurizing to 200Mpa by using a cold isostatic pressing method, maintaining the pressure for 2min, and forming to finish the preparation of the crucible biscuit.
(6) And placing the obtained biscuit in a muffle furnace to be burnt to 1650 ℃, and keeping the temperature for 2h to finish the preparation of the yttrium oxide crucible.
Sintering Y2O3The basic crucible is taken out of the muffle furnace, Y2O3The density of the base crucible is very high, and can reach more than 98%, as shown in attached figures 1a and 1 b. The distribution of yttria and sintering aid in the yttria-based crucible was observed using a scanning electron microscope and a dramatic decrease in porosity was observed, as shown in fig. 2.
The sintered yttria crucible was cut according to the standard sample size required for mechanical properties, and the flexural strength was measured using a DDL-20 electronic universal tester from catharanthus mechanical science research institute, ltd. Y prepared as described above2O3The mechanical properties of the base crucible are shown in FIG. 3, and it can be found that 10 wt.% MgTiO is added3Y as a sintering aid2O3The three-point bending strength of the crucible can reach 102 +/-10 MPa.
Example 2
10 wt.% of MgTiO with the sintering temperature of 1650 ℃ and the heat preservation time of 2h is prepared3Powder sintering of Y2O3The crucible comprises the following steps:
(1) the sintering aid content of the yttrium oxide crucible forming slurry sintered at low temperature by taking magnesium metatitanate as the sintering aid is 10 wt.%, and MgTiO3The powder is prepared by solid-phase reaction, MgO and TiO21 mol.% to 1 mol.%; binder addition 3 wt.%;
(2) 160gY was prepared according to the above design ratio2O35.52g of MgO powder with the particle size of 1 μm and TiO powder are respectively weighed based on the crucible forming slurry2Powder 10.48g, ZrO2Ball: 16g, solvent: 10g of absolute ethanol and 1 mu m Y2O3160g of powder MgTiO3Powder (prepared by solid phase reaction) 16g, ZrO2Ball: 176g, binder: polyvinyl butyral (PVB)5.28g, solvent: 108g of absolute ethyl alcohol.
(3) Firstly, MgO powder and TiO are mixed2Placing the powder and solvent into polyethylene tank, sealing, adding ZrO2Ball milling is carried out, and materials are mixed for 14 hours on a planetary mixer; and (3) placing the slurry in a vacuum drying oven, drying at the temperature of 80 ℃ for 12h, and preserving the dried powder in a muffle furnace at the temperature of 1350 ℃ for 4h to obtain the sintering aid magnesium metatitanate.
(4) Will Y2O3Powder of MgTiO3Placing the powder and solvent into polyethylene tank, sealing, adding ZrO2Ball milling is carried out, and materials are mixed for 14 hours on a planetary mixer; then, adding the binder into a polyethylene tank, sealing, mixing all the raw materials for 12 hours, placing the slurry in a vacuum drying oven, drying at 80 ℃ for 12 hours, and drying to obtain the powder for low-temperature sintering.
(5) And (3) putting the composite powder into a mold, pressurizing to 200Mpa by using a cold isostatic pressing method, maintaining the pressure for 2min, and forming to finish the preparation of the crucible biscuit.
(6) And placing the obtained biscuit in a muffle furnace to be burnt to 1650 ℃, and keeping the temperature for 2h to finish the preparation of the yttrium oxide crucible.
And taking the sintered yttrium oxide crucible out of the muffle furnace, wherein the compactness of the crucible is very high and can reach more than 98 percent, as shown in the attached figures 4a and 1 b. By observing the distribution of yttria and sintering aid in the yttria-based crucible using a scanning electron microscope, a dramatic decrease in porosity was observed, as shown in FIG. 4 b.
Sintering Y2O3The crucible was cut in accordance with the standard sample size required for mechanical properties, and the flexural strength was measured using a DDL-20 electronic universal tester from changchun mechanical science research institute, ltd. Y prepared as described above2O3The mechanical properties of the base crucible are shown in FIG. 3, and it can be found that 10 wt.% MgTiO is added3Y as a sintering aid2O3The three-point bending strength of the crucible can reach 111 +/-10 MPa.
Example 3
10 wt.% of MgTiO with the sintering temperature of 1650 ℃ and the heat preservation time of 4h is prepared3Powder sintering of Y2O3The crucible comprises the following steps:
(1) the sintering aid content of the yttrium oxide crucible forming slurry sintered at low temperature by taking magnesium metatitanate as the sintering aid is 10 wt.%, and MgTiO3The powder is prepared by solid-phase reaction, MgO and TiO21 mol.% to 1 mol.%; binder addition 3 wt.%;
(2) 160gY was prepared according to the above design ratio2O35.52g of MgO powder with the particle size of 1 μm and TiO powder were weighed respectively to prepare a slurry for forming a suspension in a crucible2Powder 10.48g, ZrO2Ball: 16g, solvent: 10g of absolute ethanol and 1 mu m Y2O3160g of powder MgTiO3Powder (prepared by solid phase reaction) 16g, ZrO2Ball: 176g, binder: polyvinyl butyral (PVB)5.28g, solvent: 108g of absolute ethyl alcohol.
(3) Firstly, MgO powder and TiO are mixed2Placing the powder and solvent into polyethylene tank, sealing, adding ZrO2Ball milling is carried out, and materials are mixed for 14 hours on a planetary mixer; and (3) placing the slurry in a vacuum drying oven, drying at the temperature of 80 ℃ for 12h, and preserving the dried powder in a muffle furnace at the temperature of 1350 ℃ for 4h to obtain the sintering aid magnesium metatitanate.
(4) Will Y2O3Powder of MgTiO3Placing the powder and solvent into polyethylene tank, sealing, adding ZrO2Ball milling is carried out, and materials are mixed for 14 hours on a planetary mixer; then, adding the binder into a polyethylene tank, sealing, mixing all the raw materials for 12 hours, placing the slurry in a vacuum drying oven, drying at 80 ℃ for 12 hours, and drying to obtain the powder for low-temperature sintering.
(5) And (3) putting the composite powder into a mold, pressurizing to 200Mpa by using a cold isostatic pressing method, maintaining the pressure for 2min, and forming to finish the preparation of the crucible biscuit.
(6) And placing the obtained biscuit in a muffle furnace to be burnt to 1650 ℃, and keeping the temperature for 4 hours to finish the preparation of the yttrium oxide crucible.
The sintered yttrium oxide crucible is subjected to standardization according to the mechanical property requirementThe specimens were cut in size, and the flexural strength was measured using a DDL-20 electronic universal tester available from Changchun mechanical science research institute, Ltd. Y prepared as described above2O3The mechanical properties of the base crucible are shown in FIG. 5, and it can be found that 10 wt.% MgTiO is added3Y as a sintering aid2O3The three-point bending strength of the crucible can reach 137 +/-15 MPa.
Example 4
10 wt.% MgTiO with the sintering temperature of 1620 ℃ and the holding time of 2h is prepared3Powder sintering of Y2O3The crucible comprises the following steps:
(1) the sintering aid content of the magnesium metatitanate reinforced yttrium oxide crucible forming slurry is 10 wt.%, and MgTiO3The powder is prepared by solid-phase reaction, MgO and TiO21 mol.% to 1 mol.%; binder addition 3 wt.%;
(2) 160gY was prepared according to the above design ratio2O35.52g of MgO powder with the particle size of 1 μm and TiO powder were weighed respectively to prepare a slurry for forming a suspension in a crucible2Powder 10.48g, ZrO2Ball: 16g, solvent: 10g of absolute ethanol and 1 mu m Y2O3160g of powder MgTiO3Powder (prepared by solid phase reaction) 16g, ZrO2Ball: 176g, binder: polyvinyl butyral (PVB)5.28g, solvent: 108g of absolute ethyl alcohol.
(3) Firstly, MgO powder and TiO are mixed2Placing the powder and solvent into polyethylene tank, sealing, adding ZrO2Ball milling is carried out, and materials are mixed for 14 hours on a planetary mixer; and (3) placing the slurry in a vacuum drying oven, drying at the temperature of 80 ℃ for 12h, and preserving the dried powder in a muffle furnace at the temperature of 1350 ℃ for 4h to obtain the sintering aid magnesium metatitanate.
(4) Will Y2O3Powder of MgTiO3Placing the powder and solvent into polyethylene tank, sealing, adding ZrO2Ball milling is carried out, and materials are mixed for 14 hours on a planetary mixer; then, adding the binder into a polyethylene tank, sealing, mixing all the raw materials for 12 hours, placing the slurry in a vacuum drying oven, drying at 80 ℃ for 12 hours, and drying to obtain the powder for low-temperature sintering.
(5) And (3) putting the composite powder into a mold, pressurizing to 200Mpa by using a cold isostatic pressing method, maintaining the pressure for 2min, and forming to finish the preparation of the crucible biscuit.
(6) And placing the obtained biscuit in a muffle furnace to be burnt to 1620 ℃, and keeping the temperature for 2 hours to finish the preparation of the yttrium oxide crucible.
Example 5
The preparation of the yttria crucible of example 5 is described with reference to example 1, except that: MgTiO 23The addition amount is 3 wt% of the yttrium oxide ceramic powder.
Example 6
The preparation of the yttria crucible of example 6 is described with reference to example 1, except that: selected from MgO and TiO2The molar ratio is 1:1, and the magnesium metatitanate is synthesized by solid-phase reaction at 1350 ℃. The obtained magnesium metatitanate is taken as a sintering aid and then mixed with yttrium oxide powder, and the addition amount of the sintering aid is 5wt% of the yttrium oxide ceramic powder.
Example 7
The preparation of the yttria crucible of example 7 is described with reference to example 1, except that: no binder was added.
Example 8
The preparation of the yttria crucible of example 8 is described with reference to example 1, except that: the sintering aid is magnesium dititanate powder, and the addition amount is 3wt percent of the yttrium oxide ceramic powder.
Example 9
The preparation of the yttria crucible of example 9 is described with reference to example 1, except that: the sintering aid is magnesium dititanate powder, and the addition amount is 5wt percent of the yttrium oxide ceramic powder.
Example 10
The preparation of the yttria crucible of this example 10 is described with reference to example 1, except that: the sintering aid is magnesium dititanate powder, and the addition amount is 10wt percent of the yttrium oxide ceramic powder.
Example 11
The preparation of the yttria crucible of example 11 is described with reference to example 1, except that: MgO and TiO with the molar ratio of 1:1 are directly added2As a sintering aid, the total addition amount is 15 wt% of the yttrium oxide ceramic powder.
Example 12
The preparation of the yttria crucible of example 12 is described with reference to example 1, except that: MgO and TiO with the molar ratio of 1:1 are directly added2As a sintering aid, the total addition amount is 25wt% of the yttrium oxide ceramic powder.
Example 13
The preparation of the yttria crucible of example 13 is described with reference to example 1, except that: MgO and TiO with the molar ratio of 1:1 are directly added2As a sintering aid, the total addition amount is 20 wt% of the yttrium oxide ceramic powder.
Example 14
The preparation of the yttria crucible of example 14 is described with reference to example 12, except that: MgO and TiO with the molar ratio of 1:2 are directly added2As a sintering aid, the total addition amount is 25wt% of the yttrium oxide ceramic powder.
Example 15
The preparation of the yttria crucible of this example 15 is referred to example 11 with the difference that: MgO and TiO with the molar ratio of 1:1 are directly added2As a sintering aid, the total addition amount is 10wt% of the yttrium oxide ceramic powder. Due to MgO and TiO2The addition amount is low, the dispersion is high, even if magnesium metatitanate is formed in the sintering and compacting process, the formation amount is low, the sintering and compacting are not facilitated, and the performance improvement is limited.
Comparative example 1
The preparation of the yttria crucible of this comparative example 1 is referred to example 1, except that: MgTiO 23The amount added was 0.
Comparative example 2
The preparation of the yttria crucible of 1 of this comparative example 2 is referred to example 1 with the difference that: MgTiO 23The addition amount is 12 wt% of the yttrium oxide ceramic powder.
Comparative example 3
The preparation of the yttria crucible of 1 of this comparative example 3 is referred to example 1, except that: the sintering aid is magnesium dititanate powder, and the addition amount is 12wt percent of the yttrium oxide ceramic powder.
Comparative example 4
The preparation of the yttria crucible of this comparative example 4 is referred to example 1, except that: MgO and TiO with the molar ratio of 1:1 are directly added2As a sintering aid, the total addition amount is 5wt% of the yttrium oxide ceramic powder. Due to MgO and TiO2The addition amount is low, the dispersion is large, even if magnesium metatitanate is formed in the sintering and densification process, the formation amount is very low, and the sintering and densification are not facilitated.
Comparative example 5
The preparation of the yttria crucible of this comparative example 5 is referred to example 1, except that: the sintering temperature is 1550 ℃ and the time is 2 h. Because the sintering temperature is lower than the melting point of the sintering aid, no liquid phase appears in the system at the moment, and the sintering densification is also not facilitated.
Comparative example 6
The preparation of the yttria crucible of this comparative example 6 is referred to example 11, except that: MgO and TiO with the molar ratio of 1:1 are directly added2As a sintering aid, the total addition amount is 30 wt% of the yttrium oxide ceramic powder. Due to MgO and TiO2The addition amount is too high, so that excessive liquid phase generated by excessive sintering aids can be generated, yttrium oxide grains grow up, and residual MgO and TiO2Too much third phase results in a decrease in mechanical properties.
Table 1 shows the preparation and performance parameters of the yttria crucible:
Figure BDA0003015769950000101
Figure BDA0003015769950000111

Claims (11)

1.一种低温烧结氧化钇陶瓷坩埚的方法，其特征在于，选用氧化镁粉体和氧化钛粉体作为烧结助剂，直接与氧化钇粉体混合后压制成坩埚素坯，再进行烧结致密化，得到致密的氧化钇陶瓷坩埚；优选地，所述烧结助剂的含量为10～25wt%。1. a method for low-temperature sintering yttrium oxide ceramic crucible, is characterized in that, select magnesium oxide powder and titanium oxide powder as sintering aid, directly mix with yttrium oxide powder and press into crucible green body, then carry out sintering dense to obtain a dense yttrium oxide ceramic crucible; preferably, the content of the sintering aid is 10-25wt%. 2.根据权利要求1所述的方法，其特征在于，所述氧化钛粉体和氧化镁粉体的摩尔比为1:1～2:1；所述氧化钛粉体和氧化镁粉体的纯度为95～99.99%，粒度范围为1μm～10μm。2. The method according to claim 1, wherein the molar ratio of the titanium oxide powder and the magnesium oxide powder is 1:1 to 2:1; The purity is 95～99.99%, and the particle size range is 1μm～10μm. 3.根据权利要求1或2所述的方法，其特征在于，所述烧结致密化的温度≥1610℃，优选为1610～1650℃，更优选为1645℃～1650℃；所述烧结致密化的时间为1～8小时。3. The method according to claim 1 or 2, wherein the temperature of the sintering and densification is ≥1610°C, preferably 1610-1650°C, more preferably 1645°C-1650°C; The time is 1 to 8 hours. 4.一种低温烧结氧化钇陶瓷坩埚的方法，其特征在于，选用偏钛酸镁粉体或/和二钛酸镁粉体作为烧结助剂，与氧化钇粉体混合后压制成坩埚素坯，再进行烧结致密化，得到致密的氧化钇陶瓷坩埚；优选地，所述烧结助剂的质量为氧化钇粉体重量的3～10wt%。4. a method for sintering yttrium oxide ceramic crucible at low temperature, it is characterized in that, select magnesium metatitanate powder or/and magnesium dititanate powder as sintering aid, after mixing with yttrium oxide powder, press into crucible green body , and then sintered and densified to obtain a dense yttrium oxide ceramic crucible; preferably, the mass of the sintering aid is 3-10wt% of the weight of the yttrium oxide powder. 5.根据权利要求4所述的方法，其特征在于，将氧化钛粉体和氧化镁粉体混合后进行固相合成，得到偏钛酸镁或二钛酸镁；优选地，所述氧化钛粉体和氧化镁粉体的摩尔比为1:1或2:1；所述氧化钛粉体和氧化镁粉体的纯度为95～99.99%，粒度范围为1μm～10μm；所述固相合成的温度为1300～1400℃，合成气氛为空气气氛。5. The method according to claim 4, wherein the titanium oxide powder and the magnesium oxide powder are mixed and then subjected to solid-phase synthesis to obtain magnesium metatitanate or magnesium dititanate; preferably, the titanium oxide The molar ratio of the powder to the magnesium oxide powder is 1:1 or 2:1; the purity of the titanium oxide powder and the magnesium oxide powder is 95 to 99.99%, and the particle size range is 1 μm to 10 μm; the solid phase synthesis The temperature is 1300～1400℃, and the synthesis atmosphere is air atmosphere. 6.根据权利要求4或5所述的方法，其特征在于，所述烧结致密化的温度≥烧结助剂的熔点、优选为1610～1650℃，时间为1～8小时；更优选地，烧结助剂为偏钛酸镁粉体，所述致密化温度为1610℃～1650℃；所述烧结助剂含有二钛酸镁粉体，所述致密化温度为1645℃～1650℃。6. The method according to claim 4 or 5, wherein the temperature of the sintering and densification is greater than or equal to the melting point of the sintering aid, preferably 1610-1650°C, and the time is 1-8 hours; more preferably, the sintering The auxiliary agent is magnesium metatitanate powder, and the densification temperature is 1610°C to 1650°C; the sintering aid contains magnesium dititanate powder, and the densification temperature is 1645°C to 1650°C. 7.根据权利要求1-6中任一项所述的方法，其特征在于，将烧结助剂、氧化钇粉体、研磨球、溶剂和粘结剂混合得到悬浮液浆料，并且进行球磨处理、干燥、研磨、过筛，得到混合粉体。7. The method according to any one of claims 1-6, characterized in that sintering aid, yttrium oxide powder, grinding balls, solvent and binder are mixed to obtain suspension slurry, and ball milling is performed , drying, grinding and sieving to obtain mixed powder. 8.根据权利要求6所述的方法，其特征在于，所述过筛为过800目～400目筛网。8 . The method according to claim 6 , wherein the sieving is to pass through a 800-mesh to 400-mesh sieve. 9 . 9.根据权利要6所述的方法，其特征在于，所述溶剂为2-丁酮或/和乙醇的混合溶液，其中2-丁酮和乙醇的质量比为（0～20）:（80～100）；所述粘结剂为聚乙烯缩丁醛、环氧树脂、酚醛树脂和糊精中的至少一种，加入量为氧化钇粉体和烧结助剂总质量的0%～6%。9. The method according to claim 6, wherein the solvent is a mixed solution of 2-butanone or/and ethanol, wherein the mass ratio of 2-butanone and ethanol is (0～20):(80 ~100); the binder is at least one of polyvinyl butyral, epoxy resin, phenolic resin and dextrin, and the addition amount is 0% to 6% of the total mass of yttrium oxide powder and sintering aid . 10.根据权利要求6所述的方法，其特征在于，所述悬浮液浆料的固含量为50～65wt%。10 . The method according to claim 6 , wherein the solid content of the suspension slurry is 50-65 wt %. 11 . 11.一种根据权利要求1-10中任一项所述的方法制备的致密的氧化钇陶瓷坩埚，其特征在于，所述致密的氧化钇陶瓷坩埚的致密度为理论密度的98%～99.5%。11. A dense yttrium oxide ceramic crucible prepared by the method according to any one of claims 1-10, wherein the dense yttrium oxide ceramic crucible has a density of 98% to 99.5 of the theoretical density %.
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