CN105948726A - Preparation method for nanocrystalline alumina ceramic - Google Patents
Preparation method for nanocrystalline alumina ceramic Download PDFInfo
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- CN105948726A CN105948726A CN201610255614.3A CN201610255614A CN105948726A CN 105948726 A CN105948726 A CN 105948726A CN 201610255614 A CN201610255614 A CN 201610255614A CN 105948726 A CN105948726 A CN 105948726A
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- temperature
- sintering
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- aluminium oxide
- nanocrystalline
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
- C04B35/111—Fine ceramics
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
Abstract
The invention discloses a preparation method for a nanocrystalline alumina ceramic. According to the preparation method, the nanocrystalline alumina ceramic is prepared from micrometer alumina powder in a discharge plasma sintering furnace through low-temperature presintering and high-temperature sintering under a discharge plasma sintering condition. The method realizes refinement of micrometer crystals through low-temperature presintering and clotting of refined crystal grain through high-temperature sintering in virtue of the special condition that the discharge plasma sintering furnace has a pulse direct-current electric field. Since the micrometer powder is used as a raw material, production cost can be greatly reduced. The method is also capable of optimizing the microscopic structure of the alumina ceramic, so the alumina ceramic has more excellent mechanical performance and thermophysical characteristics.
Description
Technical field
The present invention relates to the preparation method of a kind of nanocrystalline aluminium oxide ceramics, be that one utilizes discharge plasma sintering stove, with micron
Alumina powder jointed for raw material, the technique preparing nanocrystalline aluminium oxide ceramics by low temperature presintering and high temperature sintering.
Background technology
Aluminium oxide ceramics has the features such as mechanical strength is high, hardness is high, electrical insulation capability is excellent, and wear-resisting, high temperature resistant, resistance to
Oxidation, corrosion-resistant, therefore, it has heavily in fields such as metallurgy, chemical industry, the energy, machinery, electronics, optics and Aero-Space
The application wanted.Along with the development of science and technology, the requirement to material property is more and more harsh, uses ceramic material to substitute conventional metals material
Material has become as a kind of trend, thus, the development prospect of alumina ceramic material is considerable.With traditional aluminium oxide ceramics phase
Ratio, uses high-performance aluminium oxide ceramics prepared by novel sintered technique, because uniform microstructure, crystallite dimension is more tiny, from
And show more excellent performance in many aspects, and such as high intensity, high tenacity, high light transmission rate, superplasticity, and higher
Radiation damage tolerance limit etc..
In sintering process, the fast growth of crystal grain is Ultra-fine Grained and the disaster that faces of nanostructured aluminium oxide ceramics preparing densification
Topic.Prepare what Ultra-fine Grained and nano-structural ceramic realized generally by the method suppressing grain growth at present, conventional preparation
Method includes high-pressure sintering process, two-step sintering method, microwave sintering method, discharge plasma sintering method and flash burning etc..Such as: Dibyendu
Chakravarty et al. use 100nm alumina powder, at 900-1150 DEG C, under conditions of 25-100MPa, by electric discharge wait from
Son sintering is prepared for nano aluminium oxide pottery.Yann Aman et al. uses the α-Al of 170nm2O3Existed by discharge plasma sintering
1150 and 1300 DEG C are prepared for nano aluminium oxide pottery.The preparation method of the nano ceramics that foregoing is directed to, is desirable that use nano powder
Body is raw material, and nano-powder is prepared relatively difficult, and is prone to owing to activity is higher pollute, and improves factorial praluction cost.
By by discharge plasma sintering technique, use low temperature presintering and the method for high temperature sintering, it is possible to achieve utilize the micro-powder to be
Raw material prepares Ultra-fine Grained and nanostructured aluminium oxide ceramics.
The present invention relates to the preparation method of a kind of nano aluminium oxide pottery, it is possible to be applicable to alumina ceramic material, can be effective
Ground has homogenous superfine crystalline substance or the alumina ceramic material of nanostructured for preparation.
Summary of the invention
In view of the above deficiency of prior art, the purpose of the present invention is to propose to the preparation method of a kind of aluminium oxide nano crystalline substance pottery, make
The disadvantage mentioned above overcoming prior art, it is possible to be effectively realized and have that homogenous superfine is brilliant or the preparation of nanocrystalline aluminium oxide ceramics.
Technical scheme includes techniques below means: the preparation method of a kind of nanocrystalline aluminium oxide ceramics, utilizes electric discharge etc.
Ion sintering furnace, is used micrometer alumina powder body as raw material, is had all by low temperature presintering and two step preparations of high temperature sintering
Even Ultra-fine Grained or nanocrystalline aluminium oxide ceramics, concrete steps comprise:
1) precompressed of ceramic powder:
It is that 1-10 μm powder body is poured in graphite jig by granularity, under 5MPa pressure, molds 60s;
2) sintering of ceramic powder:
The sample just molded is inserted in discharge plasma sintering stove, is heated to 700-1000 with the heating rate of 150 DEG C/min
DEG C, and it is incubated 5-60min at this temperature;After insulation terminates, continue to be heated to the heating rate of 150 DEG C/min
1200-1600 DEG C, and it is incubated 2-60min at this temperature;Naturally cool to room temperature subsequently;In sintering process, pressure is first
It is pre-loaded to 5kN, during low temperature presintering, is the most slowly pressurized to 30-100MPa;Mode of heating is Current Heating, circulation
Pulse process is set to individual pulse time 3-5ms, rests 6-10ms after continuous impulse 12 times, and final acquisition has all
Even Ultra-fine Grained or nanocrystalline aluminium oxide ceramics.
The preparation method of aluminium oxide nano crystalline substance of the present invention pottery, by discharge plasma sintering technique, with micrometer alumina powder body be
Raw material, uses low temperature presintering and the technique of high temperature sintering, it is achieved have that homogenous superfine is brilliant or the preparation of nanocrystalline aluminium oxide ceramics,
Effectively reduce energy consumption and reduce cost of material.This is special to there is duration impulse electric field action by discharge plasma sintering stove
Different condition, realizes, by low temperature presintering, the refinement that micron is brilliant under the conditions of plasma discharging, and high temperature sintering is to ensure that low temperature refining
Grained sintered together.Use micro-powder to be possible not only to be greatly reduced production cost as raw material, and there is optimization oxidation
The good result of aluminum microstructure of ceramics, thus realize more excellent mechanical performance and thermophysical property.
Accompanying drawing explanation
Fig. 1: the picture of 3 micrometer alumina powder body of the present invention.
Picture (800 DEG C/10min of pre-burning, the sintering temperature 1300 DEG C/2 of Fig. 2: the nanocrystalline aluminium oxide ceramics prepared by the present invention
min)。
Picture (950 DEG C/5min of pre-burning, the sintering temperature 1300 DEG C/2 of Fig. 3: the nanocrystalline aluminium oxide ceramics prepared by the present invention
min)。
Detailed description of the invention
Embodiment 1: use low temperature presintering, that the technique of high temperature sintering prepares the concrete preparation process of nanocrystalline aluminium oxide ceramics is as follows:
1. the precompressed of ceramic powder:
It is that 3 μm powder body are poured in Φ 20mm graphite jig by 2.5g granularity, under 5MPa pressure, molds 60s;
2. the sintering of ceramic powder:
The sample molded is inserted in discharge plasma sintering stove, be heated to 800 DEG C with the heating rate of 150 DEG C/min, and at this
At a temperature of be incubated 10min;After insulation terminates, continue to be heated to 1300 DEG C with the heating rate of 150 DEG C/min, and temperature at this
It is incubated 2min under degree;Naturally cool to room temperature subsequently.In sintering process, pressure is first pre-loaded to 5kN, during low temperature presintering again
Slowly it is pressurized to 50MPa.Mode of heating is Current Heating, and cycle pulse process is set to individual pulse time 3.3ms,
6.6ms is rested after continuous impulse 12 times.Final acquisition has the aluminium oxide ceramics that even is brilliant.
Embodiment 2: use low temperature presintering, that the technique of high temperature sintering prepares the concrete preparation process of nanocrystalline aluminium oxide ceramics is as follows:
1. the precompressed of ceramic powder:
It is that 3 μm powder body are poured in Φ 20mm graphite jig by 2.5g granularity, under 5MPa pressure, molds 60s;
2. the sintering of ceramic powder:
The sample molded is inserted in discharge plasma sintering stove, be heated to 950 DEG C with the heating rate of 150 DEG C/min, and at this
At a temperature of be incubated 5min;After insulation terminates, continue to be heated to 1300 DEG C with the heating rate of 150 DEG C/min, and in this temperature
Lower insulation 2min;Naturally cool to room temperature subsequently.In sintering process, pressure is first pre-loaded to 5kN, the slowest during low temperature presintering
It is pressurized to 50MPa.Mode of heating is Current Heating, and cycle pulse process is set to individual pulse time 3.3ms, continuously
6.6ms is rested after pulse 12 times.Final acquisition has the aluminium oxide ceramics that even is brilliant.
Claims (1)
1. a preparation method for nanocrystalline aluminium oxide ceramics, utilizes discharging plasma sintering equipment, first passes through pulse direct current electric field
Continuous action micrometer alumina powder body is carried out at low temperatures pretreatment, be then heated to the technique that high temperature is sintered;Adopt
With micrometer alumina powder body as raw material, in discharge plasma sintering stove through low temperature presintering and two steps of high temperature sintering just
Can realize that homogenous superfine is brilliant or the preparation of nanocrystalline aluminium oxide ceramics, thus obtain more excellent mechanical performance and thermal physical characteristic
Can, concrete steps comprise:
1) precompressed of ceramic powder:
It is that 1-10 μm is alumina powder jointed by granularity and pours in graphite jig, under 5-20MPa pressure, mold 60s;
2) sintering of ceramic powder:
The sample molded is inserted in discharge plasma sintering stove, be heated to 700-1000 DEG C with the heating rate of 150 DEG C/min, and
It is incubated 5-60min at this temperature;After insulation terminates, continue to be heated to 1200-1600 DEG C with the heating rate of 150 DEG C/min,
And it is incubated 2-60min at this temperature;Naturally cool to room temperature subsequently;In sintering process, pressure is first pre-loaded to 5kN, low
30-100MPa the most slowly it is pressurized to during temperature pre-burning;Mode of heating is Current Heating, and cycle pulse process is set to single arteries and veins
Rushing time 3-5ms, rest 6-10ms after continuous impulse 12 times, final acquisition has the aluminium oxide that homogenous superfine is brilliant or nanocrystalline
Pottery.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108264345A (en) * | 2018-02-01 | 2018-07-10 | 湖北工业大学 | A kind of BaTiO3/CoFe2O4/BaTiO3The preparation method of nanometer multilayer compound magnetoelectric ceramics |
CN109400123A (en) * | 2018-10-09 | 2019-03-01 | 广东工业大学 | A kind of fine-grained alumina ceramics and its preparation method and application |
CN111730732A (en) * | 2020-06-23 | 2020-10-02 | 姜家吉 | Process for improving advanced ceramic sintering yield |
CN112745112A (en) * | 2020-12-25 | 2021-05-04 | 东华大学 | Preparation method of high-strength and high-hardness fine-grain alpha-phase alumina ceramic |
CN112759408A (en) * | 2021-01-04 | 2021-05-07 | 苏州第一元素纳米技术有限公司 | Boron carbide ceramic and preparation method and application thereof |
-
2016
- 2016-04-22 CN CN201610255614.3A patent/CN105948726A/en active Pending
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108264345A (en) * | 2018-02-01 | 2018-07-10 | 湖北工业大学 | A kind of BaTiO3/CoFe2O4/BaTiO3The preparation method of nanometer multilayer compound magnetoelectric ceramics |
CN108264345B (en) * | 2018-02-01 | 2020-12-08 | 湖北工业大学 | BaTiO3/CoFe2O4/BaTiO3Preparation method of nano multilayer composite magnetoelectric ceramic |
CN109400123A (en) * | 2018-10-09 | 2019-03-01 | 广东工业大学 | A kind of fine-grained alumina ceramics and its preparation method and application |
CN111730732A (en) * | 2020-06-23 | 2020-10-02 | 姜家吉 | Process for improving advanced ceramic sintering yield |
CN112745112A (en) * | 2020-12-25 | 2021-05-04 | 东华大学 | Preparation method of high-strength and high-hardness fine-grain alpha-phase alumina ceramic |
CN112759408A (en) * | 2021-01-04 | 2021-05-07 | 苏州第一元素纳米技术有限公司 | Boron carbide ceramic and preparation method and application thereof |
CN112759408B (en) * | 2021-01-04 | 2022-12-23 | 苏州第一元素纳米技术有限公司 | Boron carbide ceramic and preparation method and application thereof |
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