CN102249685A - Method for rapidly preparing LiAlON transparent ceramic powder - Google Patents

Method for rapidly preparing LiAlON transparent ceramic powder Download PDF

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CN102249685A
CN102249685A CN2011101255269A CN201110125526A CN102249685A CN 102249685 A CN102249685 A CN 102249685A CN 2011101255269 A CN2011101255269 A CN 2011101255269A CN 201110125526 A CN201110125526 A CN 201110125526A CN 102249685 A CN102249685 A CN 102249685A
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powder
lialon
transparent ceramic
lithium
ceramic powder
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CN102249685B (en
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王皓
刘啸
王为民
傅正义
王玉成
张清杰
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Wuhan University of Technology WUT
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Abstract

The invention relates to a method for rapidly preparing LiAlON transparent ceramic powder. The method comprises the following steps: 1) mixing alpha-aluminum oxide powder, aluminum nitride powder and lithium-containing compound powder according to a certain ratio to obtain a mixed powder material; dispersing the mixed powder material in dehydrated alcohol, carrying out ball milling for at least 24 hours to obtain slurry; 2) drying the slurry from the step 1) to obtain a mixture; 3) placing the dried mixture in a copple, placing the copple in a graphite reactor, directly exerting high current on the copple, and heating the copple to 1400-1800 DEG C at a heat rate of 100-400 DEG C per minute, then holding for 0-30 minutes, followed by carrying out natural cooling to obtain the LiAlON transparent ceramic powder. With the present invention, the method has characteristics of simple process, rapid synthesis speed, high preparation efficiency and the like; the prepared LiAlON transparent ceramic powder has high purity (more than or equal to 98wt%), uniform and small particle size (mean particle size less than or equal to 700 nm). In addition, the method provided by the present invention is substantially applicable for preparing the transparent ceramic.

Description

A kind of quick method for preparing the LiAlON transparent ceramic powder
Technical field
The present invention relates to a kind of method of the LiAlON of preparation transparent ceramic powder, belong to the synthetic and preparation field of stupalith.
Background technology
γ-AlON has excellent high-temperature performance, resistance to fouling and thermal shock resistance, is a kind of ideal high-temperature structural ceramics and refractory materials.In addition, because of it has excellent optical property, γ-AlON also can be used as optically transparent material and is widely used in optical window and nose cone etc.But γ-AlON is relatively poor in the thermostability below 1640 ℃, there are some researches show by solid solution metallic lithium ion in γ-AlON to form new single LiAlON thing phase, helps improving mechanical propertys such as the thermostability of crystalline ceramics and hardness.The LiAlON material is a kind of novel optical stupalith with spinel structure, has physics and chemical property such as excellent optics, mechanics, can be widely used in window, nose cone and transparent armor material.
People such as D.Clay (" Effect of LiAl 5O 8Additions on the sintering and optical transparency of LiAlON "; Journal of the European Ceramic Society; 26,2006, PP.1351-1362) adopt Alpha-alumina, aluminium nitride and lithium aluminate (LiAl 5O 8) mixed powder, first 35Mpa pre-molding after the 170-200Mpa isostatic cool pressing, adopts low pressure (0.5bar, N more then 2) or hot isostatic pressing (207Mpa, N 2) the solid state reaction sintering, and the structure of obtaining compact material and the relation of performance such as microstructure, optical property and mechanical property and composition, temperature of reaction and sintering process carried out research.Under 1900 ℃, 0.5bar low pressure sintering, be incubated 2h, under 2000 ℃, 207Mpa HIP sintering, be incubated 2h then, prepare thick 6.2mm, in visible region straight line transmitance near 65% LiAlON crystalline ceramics.At present, the research of LiAlON crystalline ceramics still is in the starting stage, does not see other relevant report.
From existing research, still have nothing to do at present in the single-phase powder synthetic report of LiAlON.The traditional preparation process method of LiAlON crystalline ceramics is a reaction sintering method, and reaction process is wayward, the time is long and temperature is high.In order to prepare high-performance and to possess the LiAlON crystalline ceramics of complicated shape, need the high performance LiAlON ceramic powder of preparation earlier, then it is carried out moulding and sintering.Therefore, the active LiAlON ceramic powder of high-purity, fine, the high sintering of preparation is the key of preparation high-performance LiAlON ceramic sintered bodies.In addition, the LiAlON reaction sintering process of having reported at present is a pressure sintering process, is different with the building-up process of its powder.
As everyone knows, the sintering activity of powder is directly related with the particle diameter of powder, and the sintering motivating force is proportional to 1/r 2, r represent powder particle radius (Reveue de Chimie Minerale, V22,1985, therefore P.437-483), obtaining the active powder of thinner higher sintering is vital to the preparation of crystalline ceramics.
Summary of the invention
The method that the purpose of this invention is to provide a kind of quick LiAlON of preparation transparent ceramic powder, it is fast that this method prepares speed, and gained LiAlON transparent ceramic powder purity height, particle diameter are tiny evenly.
To achieve these goals, technical scheme of the present invention is: a kind of method of the quick LiAlON of preparation transparent ceramic powder is characterized in that it comprises the steps:
1) by alpha-alumina powder, aluminium nitride powder and the shared mass percent of lithium-containing compound powder is: alpha-alumina powder 67.93wt%-93.51wt%, aluminium nitride powder 3.04wt%-24.84wt%, lithium-containing compound powder 0.5wt%-28.82wt%, with alpha-alumina powder, aluminium nitride powder and lithium-containing compound powder mixes, obtain mixed powder; Proportioning by mixed powder and dehydrated alcohol is 100g:200mL-100g:500mL, and mixed powder is scattered in the dehydrated alcohol, and ball milling is no less than 24 hours, gets slurry;
2) with the slurry drying of step 1), get mixture;
3) dried mixture is placed crucible, crucible places graphiote reactor, graphiote reactor places big current response synthesizer, is filled with nitrogen in the big current response synthesizer or contains the mixed gas of nitrogen, and the body pressure of inflating is not more than 0.07MPa; Graphiote reactor is directly applied big electric current, be heated to 1400 ℃-1800 ℃ with the heat-up rate of 100 ℃ of-400 ℃/min, soaking time is 0-30min, behind the naturally cooling, the LiAlON transparent ceramic powder.
The purity of described alpha-alumina powder is greater than 99.5wt%, and median size is less than or equal to 1 μ m, and the concentration of contained metallic impurity is lower than 500ppm.
The purity of described aluminium nitride powder is greater than 98wt%, and median size is less than or equal to 200nm, and the concentration of contained metallic impurity is lower than 5000ppm.
The purity of described lithium-containing compound powder is 98wt%, and median size is less than or equal to 5 μ m.
Described lithium-containing compound powder is that in Lithium Oxide 98min, lithium nitrate or the Quilonum Retard powder one or more mix arbitrarily.
The described mixing of step 1) can mix the sufficiently long time in the mixing equipment of any kind of, thereby obtains uniform mixture.For example: mixing time can be 24-48 hour in ball mill.Above-mentioned mixing can be adopted to do and mix or wet mixing technology.Wet mixing can be used water-free organic solvent, for example methyl alcohol, dehydrated alcohol, Virahol or toluene etc.
Step 2) drying of described mixture is generally carried out in dry gas atmosphere, anyly in the drying temperature scope can not be used as dry gas with the gas of described mixture generation chemical reaction, for example: nitrogen, argon gas, helium and air etc. are preferably selected air.Drying can be carried out under normal pressure or negative pressure.Drying temperature generally is no more than 600 ℃, and needs time enough to make described mixture complete drying.
The described crucible of step 3) does not at high temperature react with nitrogen or the mixed gas, aluminium nitride, aluminum oxide, the lithium-containing compound powder that contain nitrogen and the material that can bear high temperature and thermal shocking is made.For example, boron nitride or aluminium nitride crucible or be coated with the crucible such as graphite, aluminum oxide, silicon nitride of boron nitride or aluminium nitride coating at inwall.
The described lithium-containing compound powder of step 1) comprises any lithium-containing compound that the lithium source is provided by physics or chemical reaction process, it can be a kind of lithium-containing compound, also can be any mixing of two or more lithium-containing compounds, be not limited to the embodiment of the invention.
Principle of the present invention is: based on alpha-alumina powder, aluminium nitride powder, lithium-containing compound three-phase solid state reaction, use pulse high current synthesizer synthetic powder.The adding of lithium-containing compound and in building-up process the fast intensification of pulse high current and cooling rate and short soaking time, effectively suppressed growing up of product crystal grain.Based on pulse high current in the building-up process special roles such as evolution of powder surface have been promoted greatly to reduce reaction between powder synthesis temperature and improved transformation efficiency.
The invention has the beneficial effects as follows:
1, with after Alpha-alumina, aluminium nitride and lithium-containing compound powder mixes and the drying, (100 ℃-400 ℃/min) carry out solid state reaction and form the LiAlON transparent ceramic powder with very short soaking time (0-30min), the preparation speed of this method is fast, efficient is high, energy consumption is low with quickish temperature rise rate.
2, synthetic LiAlON transparent ceramic powder particle diameter is even, tiny and need not special ball mill crushing, through the X-ray diffraction analysis products obtained therefrom is single LiAlON phase, 100% grain graininess is less than 1 μ m, median size need not to grind the starting material requirement that can obtain the preparation of crystalline ceramics sintering less than 700nm.
3, the LiAlON transparent ceramic powder have high purity (〉=98wt%).
Description of drawings
Fig. 1 has 3 spectral lines for the XRD figure spectrum of LiAlON transparent ceramic powder of the present invention, is respectively the LiAlON transparent ceramic powder that makes among embodiment 3, embodiment 4, the embodiment 7.
Fig. 2 is the SEM photo of the LiAlON transparent ceramic powder that makes in the embodiment of the invention 3.
Fig. 3 is the SEM photo of the LiAlON transparent ceramic powder that makes in the embodiment of the invention 4.
Fig. 4 is the SEM photo of the LiAlON transparent ceramic powder that makes in the embodiment of the invention 7.
Fig. 5 has 3 distribution curves, the LiAlON transparent ceramic powder laser particle size distribution curve that makes among embodiment 3, embodiment 4, the embodiment 7 respectively for the laser particle size distribution plan of LiAlON transparent ceramic powder of the present invention.Label a among Fig. 5 represents embodiment 3, and label b represents embodiment 4, and label c represents embodiment 7.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with accompanying drawing, embodiment and not only be confined to the following examples.
Following embodiment 1-8 is adopted: the purity of alpha-alumina powder is greater than 99.5wt%, and median size is less than or equal to 1 μ m, and the concentration of contained metallic impurity is lower than 500ppm.The purity of aluminium nitride powder is greater than 98wt%, and median size is less than or equal to 200nm, and the concentration of contained metallic impurity is lower than 5000ppm.The purity of lithium-containing compound powder is 98wt%, and median size is less than or equal to 5 μ m.
Embodiment 1:
A kind of quick method for preparing the LiAlON transparent ceramic powder, it comprises the steps:
1) take by weighing the 87.25g alpha-alumina powder, 3.04g aluminium nitride powder and 9.71g Lithium Oxide 98min powder are put into the batch mixing bottle and are mixed, and obtain mixed powder; Press ball material (material is mixed powder) and add alumina balls than 4:1, add the 200mL dehydrated alcohol, roller ball mill 24 hours gets slurry;
2) with the slurry drying (50 ℃ of following vacuum-dryings) of step 1), get mixture;
3) drying is good mixture is crossed 100 mesh sieve, getting the 3g inwall of packing into scribbles in the plumbago crucible of boron nitride, crucible places graphiote reactor, and graphiote reactor places big current response synthesizer, feeds 0.05Mpa nitrogen as shielding gas in the big current response synthesizer; Graphiote reactor is directly applied big stream, be heated to 1700 ℃ with the heat-up rate of 100 ℃/min, and be incubated 10min under this temperature, reduce to room temperature then naturally, gained is the LiAlON transparent ceramic powder.
Adopt XRD that this powder is carried out thing and detect mutually, the gained powder is single phase LiAlON, does not find residual alpha-alumina powder, aluminium nitride powder and Lithium Oxide 98min powder.Through quantitative analysis as can be known, the purity that obtains LiAlON thing phase in the powder is 99.6wt%.Laser particle size analysis shows LiAlON median size 650.5nm.
Embodiment 2:
A kind of quick method for preparing the LiAlON transparent ceramic powder, it comprises the steps:
1) take by weighing the 93.51g alpha-alumina powder, 5.99g aluminium nitride powder and 0.5g Lithium Oxide 98min powder are put into the batch mixing bottle and are mixed, and obtain mixed powder; Press ball material (material is mixed powder) and add alumina balls than 4:1, add the 200mL dehydrated alcohol, roller ball mill 24 hours gets slurry;
2) with the slurry drying (50 ℃ of following vacuum-dryings) of step 1), get mixture;
3) drying is good mixture is crossed 100 mesh sieve, getting the 3g inwall of packing into scribbles in the plumbago crucible of boron nitride, crucible places graphiote reactor, and graphiote reactor places big current response synthesizer, feeds 0.02Mpa nitrogen as shielding gas in the big current response synthesizer; Graphiote reactor is directly applied big stream, be heated to 1650 ℃ with the heat-up rate of 200 ℃/min, and be incubated 5min under this temperature, reduce to room temperature then naturally, gained is the LiAlON transparent ceramic powder.
Adopt XRD that this powder is carried out thing and detect mutually, the gained powder is single phase LiAlON, does not find residual alpha-alumina powder, aluminium nitride powder and Lithium Oxide 98min powder.Through quantitative analysis as can be known, the purity that obtains LiAlON thing phase in the powder is 99.4wt%.Laser particle size analysis shows LiAlON median size 630.02nm.
Embodiment 3:
A kind of quick method for preparing the LiAlON transparent ceramic powder, it comprises the steps:
1) take by weighing the 75.12g alpha-alumina powder, 14.92g aluminium nitride powder and 9.96g Quilonum Retard powder are put into the batch mixing bottle and are mixed, and obtain mixed powder; Press ball material (material is mixed powder) and add alumina balls than 4:1, add the 250mL dehydrated alcohol, roller ball mill 24 hours gets slurry;
2) with the slurry drying (50 ℃ of following vacuum-dryings) of step 1), get mixture;
3) drying is good mixture is crossed 100 mesh sieve, getting the 3g inwall of packing into scribbles in the plumbago crucible of boron nitride, crucible places graphiote reactor, and graphiote reactor places big current response synthesizer, feeds 0.05Mpa nitrogen as shielding gas in the big current response synthesizer; Graphiote reactor is directly applied big stream, be heated to 1600 ℃ with the heat-up rate of 300 ℃/min, and be incubated 2min under this temperature, reduce to room temperature then naturally, gained is the LiAlON transparent ceramic powder.
Adopt XRD that this powder is carried out thing and detect mutually, the gained powder is single phase LiAlON, does not find residual alpha-alumina powder, aluminium nitride powder and Quilonum Retard powder.Through quantitative analysis as can be known, the purity that obtains LiAlON thing phase in the powder is 99.1wt%.Laser particle size analysis shows LiAlON median size 616.8nm.
Embodiment 4:
A kind of quick method for preparing the LiAlON transparent ceramic powder, it comprises the steps:
1) take by weighing the 68.14g alpha-alumina powder, 3.04g aluminium nitride powder and 28.82g Quilonum Retard powder are put into the batch mixing bottle and are mixed, and obtain mixed powder; Press ball material (material is mixed powder) and add alumina balls than 4:1, add the 350mL dehydrated alcohol, roller ball mill 24 hours gets slurry;
2) with the slurry drying (50 ℃ of following vacuum-dryings) of step 1), get mixture;
3) drying is good mixture is crossed 100 mesh sieve, getting the 3g inwall of packing into scribbles in the plumbago crucible of boron nitride, crucible places graphiote reactor, and graphiote reactor places big current response synthesizer, feeds 0.07Mpa nitrogen as shielding gas in the big current response synthesizer; Graphiote reactor is directly applied big stream, be heated to 1800 ℃ with the heat-up rate of 400 ℃/min, and be incubated 30min under this temperature, reduce to room temperature then naturally, gained is the LiAlON transparent ceramic powder.
Adopt XRD that this powder is carried out thing and detect mutually, the gained powder is single phase LiAlON, does not find residual alpha-alumina powder, aluminium nitride powder and Quilonum Retard powder.Through quantitative analysis as can be known, the purity that obtains LiAlON thing phase in the powder is 98.8wt%.Laser particle size analysis shows LiAlON median size 434.0nm.
Embodiment 5:
A kind of quick method for preparing the LiAlON transparent ceramic powder, it comprises the steps:
1) take by weighing the 67.93g alpha-alumina powder, the 24.84g aluminium nitride powder, 3.13g Quilonum Retard and 4.10g lithium nitrate mixed powder are put into the batch mixing bottle and are mixed, and obtain mixed powder; Press ball material (material is mixed powder) and add alumina balls than 3:1, add the 500mL dehydrated alcohol, roller ball mill 36 hours gets slurry;
2) with the slurry drying (50 ℃ of following vacuum-dryings) of step 1), get mixture;
3) drying is good mixture is crossed 100 mesh sieve, getting the 3g inwall of packing into scribbles in the plumbago crucible of boron nitride, crucible places graphiote reactor, and graphiote reactor places big current response synthesizer, feeds 0.03Mpa nitrogen as shielding gas in the big current response synthesizer; Graphiote reactor is directly applied big stream, be heated to 1500 ℃ with the heat-up rate of 200 ℃/min, and be incubated 20min under this temperature, reduce to room temperature then naturally, gained is the LiAlON transparent ceramic powder.
Adopt XRD that this powder is carried out thing and detect mutually, the gained powder is single phase LiAlON, does not find residual alpha-alumina powder, aluminium nitride powder, Quilonum Retard powder and lithium nitrate powder.Through quantitative analysis as can be known, the purity that obtains LiAlON thing phase in the powder is 98.6wt%.Laser particle size analysis shows LiAlON median size 502.3nm.
Embodiment 6:
A kind of quick method for preparing the LiAlON transparent ceramic powder, it comprises the steps:
1) take by weighing the 67.93g alpha-alumina powder, 3.25g aluminium nitride powder and 28.82g lithium nitrate powder are put into the batch mixing bottle and are mixed, and obtain mixed powder; Press ball material (material is mixed powder) and add alumina balls than 4:1, add the 200mL dehydrated alcohol, roller ball mill 24 hours gets slurry;
2) with the slurry drying (50 ℃ of following vacuum-dryings) of step 1), get mixture;
3) drying is good mixture is crossed 200 mesh sieve, getting the 3g inwall of packing into scribbles in the plumbago crucible of boron nitride, crucible places graphiote reactor, and graphiote reactor places big current response synthesizer, feeds 0.04Mpa nitrogen as shielding gas in the big current response synthesizer; Graphiote reactor is directly applied big stream, be heated to 1500 ℃ with the heat-up rate of 300 ℃/min, and be incubated 8min under this temperature, reduce to room temperature then naturally, gained is the LiAlON transparent ceramic powder.
Adopt XRD that this powder is carried out thing and detect mutually, the gained powder is single phase LiAlON, does not find residual alpha-alumina powder, aluminium nitride powder and lithium nitrate powder.Through quantitative analysis as can be known, the purity that obtains LiAlON thing phase in the powder is 98.7wt%.Laser particle size analysis shows LiAlON median size 450.3nm.
Embodiment 7:
A kind of quick method for preparing the LiAlON transparent ceramic powder, it comprises the steps:
1) take by weighing the 68.14g alpha-alumina powder, 3.04g aluminium nitride powder and 28.82g lithium nitrate powder are put into the batch mixing bottle and are mixed, and obtain mixed powder; Press ball material (material is mixed powder) and add alumina balls than 3:1, add the 250mL dehydrated alcohol, roller ball mill 24 hours gets slurry;
2) with the slurry drying (50 ℃ of following vacuum-dryings) of step 1), get mixture;
3) drying is good mixture is crossed 100 mesh sieve, getting the 3g inwall of packing into scribbles in the plumbago crucible of boron nitride, crucible places graphiote reactor, and graphiote reactor places big current response synthesizer, feeds 0.05Mpa nitrogen as shielding gas in the big current response synthesizer; Graphiote reactor is directly applied big stream, be heated to 1550 ℃ with the heat-up rate of 300 ℃/min, and be incubated 5min under this temperature, reduce to room temperature then naturally, gained is the LiAlON transparent ceramic powder.
Adopt XRD that this powder is carried out thing and detect mutually, the gained powder is single phase LiAlON, does not find residual alpha-alumina powder, aluminium nitride powder and lithium nitrate powder.Through quantitative analysis as can be known, the purity that obtains LiAlON thing phase in the powder is 98.7wt%.Laser particle size analysis shows LiAlON median size 415.5nm.
Embodiment 8:
A kind of quick method for preparing the LiAlON transparent ceramic powder, it comprises the steps:
1) take by weighing the 74.66g alpha-alumina powder, 24.84g aluminium nitride powder and 0.5g Lithium Oxide 98min powder are put into the batch mixing bottle and are mixed, and obtain mixed powder; Press ball material (material is mixed powder) and add alumina balls than 4:1, add the 300mL dehydrated alcohol, roller ball mill 24 hours gets slurry;
2) with the slurry drying (50 ℃ of following vacuum-dryings) of step 1), get mixture;
3) drying is good mixture is crossed 100 mesh sieve, getting the 3g inwall of packing into scribbles in the plumbago crucible of boron nitride, crucible places graphiote reactor, and graphiote reactor places big current response synthesizer, feeds 0.03Mpa nitrogen as shielding gas in the big current response synthesizer; Graphiote reactor is directly applied big stream, be heated to 1400 ℃ with the heat-up rate of 100 ℃/min, and be incubated 15min under this temperature, reduce to room temperature then naturally, gained is the LiAlON transparent ceramic powder.
Adopt XRD that this powder is carried out thing and detect mutually, the gained powder is single phase LiAlON, does not find residual alpha-alumina powder, aluminium nitride powder and Lithium Oxide 98min powder.Through quantitative analysis as can be known, the purity that obtains LiAlON thing phase in the powder is 98.8wt%.Laser particle size analysis shows LiAlON median size 470.7nm.
The bound value of each processing parameter of the present invention (as heat-up rate, temperature, time etc.), with and interval value, different lithium-containing compounds separately or mix and choose can both be realized the present invention, do not enumerate embodiment one by one at this.

Claims (5)

1. a method for preparing the LiAlON transparent ceramic powder fast is characterized in that it comprises the steps:
By alpha-alumina powder, aluminium nitride powder and the shared mass percent of lithium-containing compound powder be: alpha-alumina powder 67.93wt%-93.51wt%, aluminium nitride powder 3.04wt%-24.84wt%, lithium-containing compound powder 0.5wt%-28.82wt%, with alpha-alumina powder, aluminium nitride powder and lithium-containing compound powder mixes, obtain mixed powder; Proportioning by mixed powder and dehydrated alcohol is 100g:200mL-100g:500mL, and mixed powder is scattered in the dehydrated alcohol, and ball milling is no less than 24 hours, gets slurry;
With the slurry drying of step 1), get mixture;
Dried mixture is placed crucible, and crucible places graphiote reactor, and graphiote reactor places big current response synthesizer, is filled with nitrogen in the big current response synthesizer or contains the mixed gas of nitrogen, and the body pressure of inflating is not more than 0.07MPa; Graphiote reactor is directly applied big electric current, be heated to 1400 ℃-1800 ℃ with the heat-up rate of 100 ℃ of-400 ℃/min, soaking time is 0-30min, behind the naturally cooling, the LiAlON transparent ceramic powder.
2. a kind of quick method for preparing the LiAlON transparent ceramic powder according to claim 1, it is characterized in that: the purity of described alpha-alumina powder is greater than 99.5wt%, median size is less than or equal to 1 μ m, and the concentration of contained metallic impurity is lower than 500ppm.
3. a kind of quick method for preparing the LiAlON transparent ceramic powder according to claim 1, it is characterized in that: the purity of described aluminium nitride powder is greater than 98wt%, and median size is less than or equal to 200nm, and the concentration of contained metallic impurity is lower than 5000ppm.
4. a kind of quick method for preparing the LiAlON transparent ceramic powder according to claim 1, it is characterized in that: the purity of described lithium-containing compound powder is 98wt%, median size is less than or equal to 5 μ m.
5. according to claim 1 or 4 described a kind of quick methods that prepare the LiAlON transparent ceramic powder, it is characterized in that: described lithium-containing compound powder is that in Lithium Oxide 98min, lithium nitrate or the Quilonum Retard powder one or more mix arbitrarily.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20170058429A1 (en) * 2015-09-01 2017-03-02 Yu-Feng Chuang Method for Growing Sapphire Crystal

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4481300A (en) * 1981-08-31 1984-11-06 Raytheon Company Aluminum oxynitride having improved optical characteristics and method of manufacture
FR2556711A1 (en) * 1983-12-14 1985-06-21 Centre Nat Rech Scient Transparent articles made of aluminium oxynitride and process for their manufacture
CN101045632A (en) * 2007-04-28 2007-10-03 武汉理工大学 Method for quickly preparing gamma aluminum nitride oxygen transparent ceramic powder
CN101700977A (en) * 2009-10-30 2010-05-05 武汉理工大学 Method for rapidly preparing MgAlON transparent ceramic powder

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4481300A (en) * 1981-08-31 1984-11-06 Raytheon Company Aluminum oxynitride having improved optical characteristics and method of manufacture
FR2556711A1 (en) * 1983-12-14 1985-06-21 Centre Nat Rech Scient Transparent articles made of aluminium oxynitride and process for their manufacture
CN101045632A (en) * 2007-04-28 2007-10-03 武汉理工大学 Method for quickly preparing gamma aluminum nitride oxygen transparent ceramic powder
CN101700977A (en) * 2009-10-30 2010-05-05 武汉理工大学 Method for rapidly preparing MgAlON transparent ceramic powder

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
D.CLAY ET AL.: "Effect of LiAl5O8 additions on the sintering and optical transparency of LiAlON", 《JOURNAL OF THE EUROPEAN CERAMIC SOCIETY》 *
SIDDHARTHA BANDYOPADHYAY ET AL.: "Effect of controlling parameters on the reaction sequences of formation of nitrogen-containing magnesium aluminate spinel from MgO, Al2O3, and AIN", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20170058429A1 (en) * 2015-09-01 2017-03-02 Yu-Feng Chuang Method for Growing Sapphire Crystal

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