CN109608173B - Al (aluminum)2O3Complex phase ceramic sintered sample and shape control method - Google Patents
Al (aluminum)2O3Complex phase ceramic sintered sample and shape control method Download PDFInfo
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Abstract
The invention belongs to the technical field of ceramic sintering and discloses Al2O3A complex phase ceramic sintered sample and a shape control method. Taking certain mass of Al2O3Placing the powder and SiC powder in a ball mill, and adding trace ZrO into the ball mill2Adding a small amount of absolute ethyl alcohol after the powder is added, mixing and ball milling for 10-15h to obtain Al2O3Base complex phase powder; placing the complex phase powder into a steel mould and forming by cold isostatic pressing under certain pressure; preheating the blank formed by cold isostatic pressing in vacuum to remove water and volatile substances in the blank; and setting a corresponding temperature-raising system for the ceramic sintering equipment, and sintering the ceramic material. In the invention, Al2O3Adding trace ZrO into-SiC complex phase powder2Powder of effectively inhibiting Al2O3The deformation of the-SiC ceramic body in the sintering process promotes the normal use of the material, and the defective rate of the ceramic material can be greatly reduced.
Description
Technical Field
The invention belongs to the technical field of ceramic sintering, and particularly relates to Al2O3The shape control method of the complex phase ceramic sintered sample is based on.
Background
Currently, the current state of the art commonly used in the industry is such that:
ceramic materials have found wide application in many fields. However, its most fatal weakness is high brittleness and low reliability, especially Al2O3Ceramics are brittle and have poor thermal shock resistance, limiting their use in many applications. Furthermore, the recrystallization of the grains necessarily occurring during the high-temperature sintering of the ceramic material brings obstacles to the preparation of the single-phase ceramic material, and therefore, the idea of the complex-phase ceramic comes into force. The nano-scale second phase exists in the structure interior or crystal boundary of the micron-scale or submicron-scale matrix, so that the effects of strengthening and toughening the material can be simultaneously achieved, andthe thermal shock resistance can be improved. In addition, it is a good target for material design. Therefore, the complex phase ceramic becomes the ceramic material with the most practical significance.
Al2O3The base complex phase ceramic is a very important and basic engineering ceramic material in practical application and scientific research, and the system comprises Al2O3-SiC、Al2O3-ZrO2And so on. The most common sintering method for preparing these ceramics is atmospheric sintering under air atmosphere. However, this preparation method is to sinter Al2O3When the-SiC complex phase ceramic is used, a small amount of SiC on the surface and in the sample can be oxidized and converted into SiO2Therefore, the specimen may be deformed and bent, resulting in failure of the material to be normally used.
In summary, the problems of the prior art are as follows:
ceramic materials cannot be machined like metals after sintering, and therefore require a high dimensional stability of the green body. For Al2O3The sintering of the-SiC complex phase ceramic usually needs the protection of inert gas, not only the equipment investment is large, but also the production cost is higher. Using common heating equipment to heat Al2O3The equipment and production cost can be reduced by sintering the-SiC complex phase ceramic, but the formed body is deformed due to the oxidation of SiC, so that the shape stability of the ceramic body is poor.
At present, more Al is applied2O3The base complex phase ceramic system comprises Al2O3-SiC、Al2O3-ZrO2During sintering to prepare Al2O3When the-SiC complex phase ceramic is used, a small amount of SiC on the surface and in the sample can be oxidized and converted into SiO2Therefore, the specimen may be deformed and bent, resulting in failure of the material to be normally used.
The difficulty and significance for solving the technical problems are as follows:
for Al in air atmosphere2O3When the-SiC complex phase ceramic is sintered under normal pressure, how to inhibit the shape deformation of a blank under the high-temperature condition is generalA sintering method of hoisting the green body and inhibiting deformation by using gravity is adopted, but the method has special requirements on sintering equipment, and also puts forward more rigorous requirements in the processes of powder mixing and green body forming. How to not change Al2O3Under the condition of main compositions of the-SiC complex phase ceramics, a sintering method with the lowest cost is not used for inhibiting the shape deformation of the ceramic product at present. The invention proposes to use Al2O3Adding a small amount of Y into SiC powder2O3Partially stabilized tetragonal phase ZrO2By using Y2O3Partially stabilized tetragonal phase ZrO2The volume expansion effect in the temperature reduction process is used for inhibiting the deformation of the ceramic material, so that the dependence on equipment is completely avoided, and the cost is reduced.
Avoidance of Al2O3Base complex phase ceramic Al2O3The deformation and bending of the-SiC system during sintering can greatly improve the utilization rate of materials, reduce the defective rate and simultaneously enlarge the application range of ceramics.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides Al2O3A complex phase ceramic sintered sample and a shape control method.
The invention is realized by using Al2O3The shape control method of the base complex phase ceramic sintering sample comprises the following steps:
the method comprises the following steps: taking certain mass of Al2O3The powder and SiC powder were placed in a ball mill (Al)2O3The mass ratio of the Al to SiC is 1: 1-9: 1, and the Al is2O3The powder is nano powder with the purity of more than 99 percent; the granularity of SiC powder is more than 300 meshes, the purity is more than 98 percent), and then micro ZrO is added into the ball mill2Powder (ZrO)2The powder is micron-sized powder and consists of 2-8% of Y2O3Partially stabilized tetragonal phase ZrO2The addition amount is Al2O30.5-2% of the total mass of SiC), and then dropwise adding a small amount of absolute ethyl alcohol into the powder to be mixed; ball milling for 10-15h with ZrO as milling medium2Grinding ball(ii) a Finally obtaining complex phase powder;
step two: placing the mixed complex phase powder into a steel mould to be subjected to cold isostatic pressing under a certain pressure, wherein the molding pressure is 200-300 Mpa;
step three: preheating the blank formed by cold isostatic pressing in vacuum (the heat treatment temperature is 400-600 ℃), and removing water and volatile substances in the blank;
step four: setting a corresponding temperature rising system for the ceramic sintering equipment, and specifically comprising the following steps: room temperature-600 ℃: 3 ℃/min, 600-1000 ℃: 5 ℃/min, and preserving heat at 1000 ℃ for 1-2 h, wherein the sintering temperature is 1000 ℃ -1650 ℃ (1400-1650 ℃): 10-15 ℃/min; sintering the blank in a sintering furnace according to a temperature rising system, and naturally cooling to room temperature to obtain Al2O3And (3) base complex phase ceramic sintering samples.
Further, the Al2O3The shape control method of the complex phase ceramic sintered sample is characterized in that the Al2O3A small amount of absolute ethyl alcohol is required to be dripped when the powder and the SiC powder are subjected to ball milling, so that the powder is prevented from hardening.
Further, the pressure during cold isostatic pressing is 200-300 MPa.
Further, the sintering system of the ceramic sintering equipment is set to be between room temperature and 600 ℃: 3 ℃/min, 600-1000 ℃: 5 ℃/min, and preserving heat at 1000 ℃ for 1-2 h, wherein the sintering temperature is 1000 ℃ -1650 ℃ (1400-1650 ℃): 10 to 15 ℃/min. And keeping the sintering temperature for 2-6 h.
Another object of the present invention is to provide a method for producing a crystalline silicon using the Al2O3Al prepared by shape control method of complex phase ceramic sintered sample2O3And (3) base complex phase ceramic sintering samples.
In summary, the advantages and positive effects of the invention are: by adding small amounts of Y2O3Partially stabilized tetragonal phase ZrO2The crystal structure changes in the cooling process, and the volume expansion effect is generated. The ceramic body is restrained from shrinking in volume and deforming in the sintering process. The method has no special requirement on sintering equipment, reduces cost, and improves yield and materialAnd (4) utilization rate.
The invention utilizes the conventional sintering equipment and does not utilize special methods and conditions under the condition of Al2O3Adding trace ZrO into-SiC complex phase powder2Powder of effectively inhibiting Al2O3The deformation of the-SiC ceramic body in the sintering process promotes the normal use of the material, and the defective rate of the ceramic material can be greatly reduced.
Drawings
FIG. 1 shows Al provided in examples of the present invention2O3A flow chart of a shape control method of a complex phase ceramic sintering sample.
FIG. 2 shows Al provided in examples of the present invention2O3-XRD pattern of SiC complex phase ceramic.
FIG. 3 is a diagram showing a comparison of the sintered shape of the complex phase ceramic according to the embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The following detailed description of the principles of the invention is provided in connection with the accompanying drawings.
As shown in FIG. 1, Al provided in the examples of the present invention2O3The shape control method of the base complex phase ceramic sintering sample comprises the following steps:
s101: taking certain mass of Al2O3The powder and SiC powder were placed in a ball mill (Al)2O3The mass ratio of the Al to SiC is 1: 1-9: 1, and the Al is2O3The powder is nano powder with the purity of more than 99 percent; the granularity of SiC powder is more than 300 meshes, the purity is more than 98 percent), and then micro ZrO is added into the ball mill2Powder (ZrO)2The powder is micron-sized powder and consists of 2-8% of Y2O3Partially stabilized tetragonal phase ZrO2The addition amount is Al2O30.5-2% of the total mass of SiC), and then dropwise adding a small amount of absolute ethyl alcohol into the powder to be mixed;ball milling for 10-15h with ZrO as milling medium2Grinding balls; finally obtaining complex phase powder;
s102: placing the mixed complex phase powder into a steel mould to be subjected to cold isostatic pressing under a certain pressure, wherein the molding pressure is 200-300 Mpa;
s103: preheating the blank formed by cold isostatic pressing in vacuum (the heat treatment temperature is 400-600 ℃), and removing water and volatile substances in the blank;
s104: after the green body is placed in a sintering furnace, a corresponding temperature rise system of equipment is set, and the method specifically comprises the following steps: room temperature-600 ℃: 3 ℃/min, 600-1000 ℃: 5 ℃/min, and preserving heat at 1000 ℃ for 1-2 h, wherein the sintering temperature is 1000 ℃ -1650 ℃ (1400-1650 ℃): 10-15 ℃/min; sintering the blank in a sintering furnace according to a temperature rising system, keeping the sintering temperature for 2-6 h, and naturally cooling to room temperature to obtain Al2O3And (3) base complex phase ceramic sintering samples.
Al2O3A small amount of absolute ethyl alcohol is required to be dripped when the powder and the SiC powder are subjected to ball milling, so that the powder is prevented from hardening.
And the pressure during cold isostatic pressing is 200-300 MPa.
The sintering system of the ceramic sintering equipment is set to be between room temperature and 600 ℃: 3 ℃/min, 600-1000 ℃: 5 ℃/min, and preserving heat at 1000 ℃ for 1-2 h, wherein the sintering temperature is 1000 ℃ -1650 ℃ (1400-1650 ℃): 10 to 15 ℃/min.
The present invention provides a method for producing a crystalline silicon using the Al2O3Al prepared by shape control method of complex phase ceramic sintered sample2O3And (3) base complex phase ceramic sintering samples.
The present invention is further described below with reference to specific examples and experiments.
With the above-mentioned Al2O3Powder, SiC powder and ZrO2Taking the powder as a raw material, and carrying out Al according to a specific embodiment2O3Sintering of the-SiC ceramic to give a ceramic material whose main phase remains Al2O3And SiC (fig. 2).
As is apparent from FIG. 3, the addition of the corresponding ZrO2The powder has very obvious effect of inhibiting the shape deformation of the sintered ceramic blank. In the absence of added ZrO2When the ceramic powder is used, the ceramic is obviously bent after sintering; after adding ZrO2When in powder form; the ceramic is still in a long square column shape after being sintered and basically has the same shape as the formed green body.
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 (2)
1. Al (aluminum)2O3The shape control method of the complex phase ceramic sintered sample is characterized in that the Al2O3The shape control method of the base complex phase ceramic sintering sample comprises the following steps:
the method comprises the following steps: taking certain mass of Al2O3Placing the powder and SiC powder in a ball mill, and adding trace ZrO into the ball mill2Powder, then a small amount of absolute ethyl alcohol is dripped into the powder to be mixed; ball milling for 10-15h with ZrO as milling medium2Grinding balls; finally obtaining complex phase powder;
step two: carrying out cold isostatic pressing on the mixed complex-phase powder through a steel die under a certain pressure, wherein the molding pressure is 200-300 Mpa;
step three: preheating the blank formed by cold isostatic pressing in vacuum at 400-600 ℃, and removing water and volatile substances in the blank;
step four: setting a corresponding heating system for the ceramic sintering equipment; sintering the blank in a sintering furnace according to a temperature rising system, and naturally cooling to room temperature to obtain Al2O3Sintering a sample based on the complex phase ceramic;
in the first step, Al2O3The mass ratio of the Al to SiC is 1: 1-9: 1, and the Al is2O3The powder is nano powder with the purity of more than 99 percent; the granularity of the SiC powder is more than 300 meshes, and the purity is more than 98 percent;
ZrO2the powder is micron-sized powder,the composition is 2 to 8 percent of Y2O3Partially stabilized tetragonal phase ZrO2，ZrO2The powder is added with Al2O30.5-2% of the total mass of SiC;
the cold isostatic pressing pressure is 200-300 MPa;
the sintering system of the ceramic sintering equipment is as follows: room temperature-600 ℃: 3 ℃/min; 600-1000 ℃: 5 ℃/min; and preserving heat for 1-2 h at 1000 ℃, wherein the sintering temperature is 1400-1650 ℃ between 1000 ℃ and the temperature: 10-15 ℃/min; and keeping the sintering temperature for 2-6 h.
2. Use of Al as defined in claim 12O3Al prepared by shape control method of complex phase ceramic sintered sample2O3And (3) base complex phase ceramic sintering samples.
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| US4796127A (en) * | 1986-04-23 | 1989-01-03 | Sumitomo Special Metals Co., Ltd. | Recording head slider |
| CN1986483A (en) * | 2006-12-25 | 2007-06-27 | 西南科技大学 | Nano-nano type Al2O3-base heterogeneous ceramic and its preparing method |
| JP4104944B2 (en) * | 2002-09-18 | 2008-06-18 | 淳 小泉 | Prediction method of displacement behavior of structures in underpinning |
| JP4243960B2 (en) * | 2003-02-25 | 2009-03-25 | ヤマハファインテック株式会社 | Work sorting apparatus and sorting method |
| CN108358614A (en) * | 2018-03-05 | 2018-08-03 | 段高峰 | Creep resistant abrasion-proof stick and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH04104944A (en) * | 1990-08-21 | 1992-04-07 | Nitsukatoo:Kk | Al2o3-sic-zro2 composite sinter |
| JPH0813702B2 (en) * | 1991-01-30 | 1996-02-14 | 東レ株式会社 | Composite ceramics |
| CN102515720A (en) * | 2011-12-08 | 2012-06-27 | 西安交通大学 | Preparation method of transparent alumina ceramic |
| CN107417286B (en) * | 2017-08-22 | 2021-01-08 | 东北大学 | Reinforced ultra-low carbon Al2O3-ZrO2Preparation method of-SiC-C refractory material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4796127A (en) * | 1986-04-23 | 1989-01-03 | Sumitomo Special Metals Co., Ltd. | Recording head slider |
| JP4104944B2 (en) * | 2002-09-18 | 2008-06-18 | 淳 小泉 | Prediction method of displacement behavior of structures in underpinning |
| JP4243960B2 (en) * | 2003-02-25 | 2009-03-25 | ヤマハファインテック株式会社 | Work sorting apparatus and sorting method |
| CN1986483A (en) * | 2006-12-25 | 2007-06-27 | 西南科技大学 | Nano-nano type Al2O3-base heterogeneous ceramic and its preparing method |
| CN108358614A (en) * | 2018-03-05 | 2018-08-03 | 段高峰 | Creep resistant abrasion-proof stick and preparation method thereof |
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