CN104402452A - Aluminum nitride ceramic powder preparation method - Google Patents
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Abstract
The invention relates to the technical field of ceramic powder preparation, and relates to a high-purity aluminum nitride ceramic powder preparation method. The method comprises the following steps: metal aluminum is hydrolysed; an Al source and C source mixed slurry is obtained; the slurry is gelled; the gel is dried and crushed; the gel powder is subjected to a carbothermal reduction nitriding treatment; and decarbonization treatment is carried out. According to the invention, with the hydrolysis reaction of high-purity aluminum, an aluminum oxide precursor is obtained; high-purity cane sugar is adopted as the C source; a gel solid-phase method is combined with the carbothermal reduction nitriding process; Through the controlling over Al source and C source purities and through the non-air oxidative atmosphere decarbonization process treatment, ultrahigh-purity and high-sintering-activity aluminum nitride powder with a purity up to 99.99% can be obtained. With the method provided by the invention, aluminum nitride powder with ultrahigh purity and high sintering activity can be obtained, such that requirements on ultrahigh-purity aluminum nitride powder in the fields of laser weapons and microelectronic technology can be satisfied.
Description
Technical field
The invention belongs to a kind of ceramic powder fabricating technology field, relate to a kind of preparation method of ultra-high purity aluminium nitride powder.
Background technology
Aluminium nitride (AlN) is the third generation semiconductor material grown up after first-generation Ge, Si semi-conductor, s-generation GaAs, InP, GaP compound semiconductor.It is a kind of group III-nitride of hexagonal wurtzite structure, owing to having energy gap large (6.2eV), breakdown electric field high (14MV/cm), electron transfer rate large good characteristic and good chemistry, thermostability and the capability of resistance to radiation such as (300cm2/Vs), thermal conductivity high (260W/mK), it is the ideal basic material making high frequency, high temperature, high pressure, high-power electronic device.Particularly compared to existing GaAs or InP-base device, AlN base THz emissive source can provide more high-power and higher frequency.Therefore, for improving the performance of the core devices such as Terahertz quantum cascaded laser, High Electron Mobility Transistor, schottky diode, particularly high temperature, high frequency (Terahertz frequency range), high-power output etc., more ripe Si, GaAs material system can not meet the demands; And just become development trend with the material system that nitride (as AlN, GaN) is representative.The realization of these core devices needs the base mateirals such as highly purified AlN, GaN, and they become the basis of the core devices performance boosts such as Terahertz quantum cascaded laser, High Electron Mobility Transistor, schottky diode.For ensureing the effect of AlN base THz emissive source in terahertz imaging radar, to core material wherein---high-purity AlN film and high fine and close AlN ceramic (target) thereof propose higher technical requirements: on the one hand, require that AlN film has high purity (>=99.995%) and specific stoichiometric ratio (atom N is than >=50%); On the other hand, target material composition and structure are directly connected to the quality of deposit film, require that AlN target has high purity (>=99.999%) and high-compactness (>=98%).
In order to obtain high-purity, high fine and close AlN target, the acquisition of high-purity, high sintering active A lN powder is crucial.At present, the method for synthesizing AlN powder the most frequently used mainly contains aluminium powder direct nitridation method and carbothermic method.Aluminium powder direct nitridation method is in aluminium powder Direct-Nitridation process, and the aluminium nitride film of the surfaces nitrided formation of aluminium powder can make its further nitrogenize become difficulty, thus causes the incomplete problem of nitrogenize.And O impurity easily brought into by the pellumina that aluminium powder raw material surface is formed, and affects the purity of AlN powder.Again because aluminium nitride is very easily oxidized, so, the AlN powder of ultra-high purity be obtained, first must by the carbothermic reduction of Al source, removing O element wherein.Secondly, carbon removal treatment must be carried out under non-air oxidizing atmosphere, prevent the oxidation of aluminium nitride.Aluminium nitride powder prepared by current existing carbothermic reduction technology cannot reach the requirement of ultra-high purity.As 201010527703.1 " method of aluminium nitride powder is prepared in a kind of co-precipitation-carbothermic reduction ", Tai-Ace S 150 is adopted to press as aluminium source in this method, carbon black is carbon source, obtains precursor, carbonization treatment under certain condition after precursor carbothermal reduction-nitridation by adding precipitation agent bicarbonate of ammonia." 200810229583.X a kind of macromolecule network preparation method of high-purity ultra-fine aluminum nitride powder ".In this method, by adopting aluminum nitrate to be carbon source as aluminium source, sucrose, after carbothermal reduction-nitridation, carry out carbon removal treatment in atmosphere.All cannot obtain the ultra-high purity aluminium nitride powder of high purity 99.99% in above method, the ultra-high purity requirement of the field such as laser weapon and microelectronics to aluminium nitride powder cannot be met.
Summary of the invention
The object of the invention is the preparation method proposing the aluminum nitride ceramic powder that a kind of purity is high, sintering activity is high.
Technical scheme of the present invention is: the operation steps of the method is as follows:
(1) metallic aluminium hydrolysis
The metallic aluminium of high purity 99.99% is placed in beaker, add pure water, the mass ratio of aluminium and pure water is 1:2-1:5, heating water temperature to 80 DEG C-150 DEG C, carry out rapid stirring process, make metallic aluminium and water generation hydrolysis reaction, churning time is 1-5 hour simultaneously, until react completely, obtain the hydrolysis slip of aluminium;
(2) mixed slurry preparation
In said hydrolyzed slip, add the sucrose of high purity 99.99% by proportioning, the mol ratio of metallic aluminium and sucrose is 1:0.1-1:5, stirs and obtain the Homogeneous phase mixing slip in Al source and C source after sucrose dissolved;
(3) slurry gel
Organic monomer is added successively in above-mentioned mixed slurry, linking agent and initiator, organic monomer is acrylamide or Methacrylamide, linking agent is methylene-bisacrylamide or many ethyleneglycol dimethacrylates, the mass ratio of organic monomer and linking agent is chosen between 10:1-30:1, total add-on of organic monomer and linking agent is the 5-30% of pure water amount, initiator is ammonium persulphate, add-on is the 0.2-0.6% of organic monomer, stir to be placed in baking oven and heat, Heating temperature is between 50-100 DEG C, heat-up time is 10-20 minute, obtain wet gel body,
(4) gelinite drying, pulverizing
Put into baking oven after being cut into small pieces by wet gel body dry, drying temperature is between 80-120 DEG C, and time of drying is 10-15 hour, and dried gel piece is carried out ball mill pulverizing in planetary mills, obtains gel powder;
(5) carbothermal reduction-nitridation
Above-mentioned gel powder is placed in N
2in atmosphere furnace, at N
2calcine under atmosphere, allow gel powder carry out carbothermal reduction-nitridation reaction, calcining temperature is 1000 DEG C-1600 DEG C, and soaking time is 5-10 hour;
(6) carbon removal treatment
Reacted for above-mentioned carbothermal reduction-nitridation powder is placed in CO
2in atmosphere furnace, at CO
2carry out secondary clacining under atmosphere, remove unnecessary C, calcination time is 600 DEG C-1000 DEG C, and soaking time is 5-15 hour, obtains aluminum nitride ceramic powder after abundant carbon removal treatment.
Adopt metallic aluminium as aluminium source, utilize metallic aluminium hydrolysis properties obtain Al
2o
3presoma, sucrose is as C source.
Advantage of the present invention is:
The first, the present invention, by the control of Al source and C source purity in synthesis aluminium nitride powder process, ensures the ultra-high purity (99.99%) of synthetic powder.
The second, the present invention adopts high purity metal aluminium to be raw material, compared with other rafifinal sources, and 99.99% high pure metal aluminium wide material sources, with low cost.
3rd, the present invention adopts sucrose to be C source, and sucrose is very easily water-soluble, and therefore, C source is present in mixed slurry with the form of molecule, can be hydrolyzed the Al obtained by stirring with Al
2o
3presoma fully and Homogeneous phase mixing, is conducive to the abundant reaction of Al source and carbon source.
4th, the present invention adopts gel solid-phase synthesis, by adding monomer, linking agent and initiator, the mixed slurry of aluminium source and carbon source is made to form gel in a heated condition, the formation of gel makes aluminium source be fixed with carbon source and fully contact, and is conducive to carrying out fast and reacting completely of carbothermic reduction reaction.
5th, the present invention adopts CO
2carry out carbon removal treatment, due to CO
2oxidation capacity compare O
2weak, at high temperature can only react with once calcining C remaining in rear powder, and AlN powder can not be oxidized, thus ensure that the ultra-high purity of AlN.If direct carbon removal treatment in atmosphere, the O in air
2not only with C reaction, also can react with the AlN powder once calcining rear generation, bring O impurity into.
6th, equipment used herein is all general-purpose equipment, and operating process is simple.
7th, aluminum nitride ceramic powder purity prepared by present method can up to 99.99%.
Embodiment
Below the present invention is described in further details.A preparation method for aluminum nitride ceramic powder, the operation steps of the method is as follows:
1, a kind of preparation method of aluminum nitride ceramic powder.
The operation steps of the method is as follows:
(1) metallic aluminium hydrolysis
The metallic aluminium of high purity 99.99% is placed in beaker, add pure water, the mass ratio of aluminium and pure water is 1:2-1:5, heating water temperature to 80 DEG C-150 DEG C, carry out rapid stirring process, make metallic aluminium and water generation hydrolysis reaction, churning time is 1-5 hour simultaneously, until react completely, obtain the hydrolysis slip of aluminium;
(2) mixed slurry preparation
In said hydrolyzed slip, add the sucrose of high purity 99.99% by proportioning, the mol ratio of metallic aluminium and sucrose is 1:0.1-1:5, stirs and obtain the Homogeneous phase mixing slip in Al source and C source after sucrose dissolved;
(3) slurry gel
Organic monomer is added successively in above-mentioned mixed slurry, linking agent and initiator, organic monomer is acrylamide or Methacrylamide, linking agent is methylene-bisacrylamide or many ethyleneglycol dimethacrylates, the mass ratio of organic monomer and linking agent is chosen between 10:1-30:1, total add-on of organic monomer and linking agent is the 5-30% of pure water amount, initiator is ammonium persulphate, add-on is the 0.2-0.6% of organic monomer, stir to be placed in baking oven and heat, Heating temperature is between 50-100 DEG C, heat-up time is 10-20 minute, obtain wet gel body,
(4) gelinite drying, pulverizing
Put into baking oven after being cut into small pieces by wet gel body dry, drying temperature is between 80-120 DEG C, and time of drying is 10-15 hour, and dried gel piece is carried out ball mill pulverizing in planetary mills, obtains gel powder;
(5) carbothermal reduction-nitridation
Above-mentioned gel powder is placed in N
2in atmosphere furnace, at N
2calcine under atmosphere, allow gel powder carry out carbothermal reduction-nitridation reaction, calcining temperature is 1000 DEG C-1600 DEG C, and soaking time is 5-10 hour;
(6) carbon removal treatment
Reacted for above-mentioned carbothermal reduction-nitridation powder is placed in CO
2in atmosphere furnace, at CO
2carry out secondary clacining under atmosphere, remove unnecessary C, calcination time is 600 DEG C-1000 DEG C, and soaking time is 5-15 hour, obtains aluminum nitride ceramic powder after abundant carbon removal treatment.
Embodiment 1
Take 200g high pure metal aluminium flake, purity is 99.99%, aluminium flake is of a size of 10mm × 10mm × 1mm, is placed in beaker, adds pure water 500g, heating water temperature to 90 DEG C, carry out rapid stirring process simultaneously, make metallic aluminium and water generation hydrolysis reaction, stir 3 hours, react completely, obtain the hydrolysis slip of aluminium.Then add the high-purity sucrose of 350g and continue stirring 20 minutes, sucrose dissolve completely and Homogeneous phase mixing after, add acrylamide 50g, methylene-bisacrylamide 2.5g, ammonium persulphate 0.25g, stirring to be placed in baking oven is heated to 70 DEG C, after slurry gel, wet gel is cut into small pieces and puts into baking oven and be warming up to 100 DEG C and carry out drying, dry 12 hours.Dried gel piece is carried out in planetary mills wet-milling pulverize and drying be placed in atmosphere furnace, at N
2lower 1500 DEG C of atmosphere is calcined, and is incubated 6 hours.By reacted for carbothermal reduction-nitridation powder at CO
2lower 800 DEG C of atmosphere carries out secondary clacining, is incubated and removes unnecessary C in 8 hours.Ultra-high purity, high sintering active nitride aluminium ceramic powder can be obtained after abundant carbon removal treatment.
Embodiment 2:
Take 500g high purity granular shape aluminium ingot, purity is 99.99%, adds pure water 1500g, and heating water temperature to 80 DEG C, carries out rapid stirring process simultaneously, make metallic aluminium and water generation hydrolysis reaction, stir 5 hours, react completely, obtain the hydrolysis slip of aluminium.Then add the high-purity sucrose of 700g and continue stirring 20 minutes, sucrose dissolve completely and Homogeneous phase mixing after, add Methacrylamide 120g, many ethyleneglycol dimethacrylates 5g, ammonium persulphate 0.6g, stirring to be placed in baking oven is heated to 80 DEG C, after slurry gel, wet gel is cut into small pieces and puts into baking oven and be warming up to 100 DEG C and carry out drying, dry 12 hours.Dried gel piece is carried out in planetary mills wet-milling pulverize and drying be placed in atmosphere furnace, at N
2lower 1550 DEG C of atmosphere is calcined, and is incubated 5 hours.By reacted for carbothermal reduction-nitridation powder at CO
2lower 900 DEG C of atmosphere carries out secondary clacining, is incubated and removes unnecessary C in 6 hours.Ultra-high purity, high sintering active nitride aluminium ceramic powder can be obtained after abundant carbon removal treatment.
Claims (2)
1. a preparation method for aluminum nitride ceramic powder, is characterized in that,
The operation steps of the method is as follows:
(1) metallic aluminium hydrolysis
The metallic aluminium of high purity 99.99% is placed in beaker, add pure water, the mass ratio of aluminium and pure water is 1:2-1:5, heating water temperature to 80 DEG C-150 DEG C, carry out rapid stirring process, make metallic aluminium and water generation hydrolysis reaction, churning time is 1-5 hour simultaneously, until react completely, obtain the hydrolysis slip of aluminium;
(2) mixed slurry preparation
In said hydrolyzed slip, add the sucrose of high purity 99.99% by proportioning, the mol ratio of metallic aluminium and sucrose is 1:0.1-1:5, stirs and obtain the Homogeneous phase mixing slip in Al source and C source after sucrose dissolved;
(3) slurry gel
Organic monomer is added successively in above-mentioned mixed slurry, linking agent and initiator, organic monomer is acrylamide or Methacrylamide, linking agent is methylene-bisacrylamide or many ethyleneglycol dimethacrylates, the mass ratio of organic monomer and linking agent is chosen between 10:1-30:1, total add-on of organic monomer and linking agent is the 5-30% of pure water amount, initiator is ammonium persulphate, add-on is the 0.2-0.6% of organic monomer, stir to be placed in baking oven and heat, Heating temperature is between 50-100 DEG C, heat-up time is 10-20 minute, obtain wet gel body,
(4) gelinite drying, pulverizing
Put into baking oven after being cut into small pieces by wet gel body dry, drying temperature is between 80-120 DEG C, and time of drying is 10-15 hour, and dried gel piece is carried out ball mill pulverizing in planetary mills, obtains gel powder;
(5) carbothermal reduction-nitridation
Above-mentioned gel powder is placed in N
2in atmosphere furnace, at N
2calcine under atmosphere, allow gel powder carry out carbothermal reduction-nitridation reaction, calcining temperature is 1000 DEG C-1600 DEG C, and soaking time is 5-10 hour;
(6) carbon removal treatment
Reacted for above-mentioned carbothermal reduction-nitridation powder is placed in CO
2in atmosphere furnace, at CO
2carry out secondary clacining under atmosphere, remove unnecessary C, calcination time is 600 DEG C-1000 DEG C, and soaking time is 5-15 hour, obtains aluminum nitride ceramic powder after abundant carbon removal treatment.
2. the preparation method of a kind of aluminum nitride ceramic powder according to claim 1, is characterized in that, adopts metallic aluminium as aluminium source, utilizes the hydrolysis properties of metallic aluminium to obtain Al
2o
3presoma, sucrose is as C source.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105542071A (en) * | 2016-01-27 | 2016-05-04 | 王柳燕 | Method for preparing composite nanometer hydrogel precursor |
| CN105837223A (en) * | 2016-05-04 | 2016-08-10 | 中国科学院上海硅酸盐研究所 | Method for synthesizing aluminum nitride power |
| CN105884372A (en) * | 2016-04-12 | 2016-08-24 | 武汉理工大学 | Method for synthesizing AlN ceramic powder through organic network |
| CN107867863A (en) * | 2016-09-23 | 2018-04-03 | 中国人民解放军国防科学技术大学 | Aluminum oxynitride ceramic powder and preparation method thereof |
| CN107903069A (en) * | 2017-12-29 | 2018-04-13 | 苏州图纳新材料科技有限公司 | Aluminium nitride powder and preparation method thereof |
| CN109205579A (en) * | 2018-10-22 | 2019-01-15 | 厦门钜瓷科技有限公司 | The preparation method of aluminium nitride |
| CN109251040A (en) * | 2018-09-28 | 2019-01-22 | 航天特种材料及工艺技术研究所 | A kind of porous aluminum carbon matrix precursor and preparation method thereof |
| CN109293368A (en) * | 2018-12-06 | 2019-02-01 | 石家庄学院 | A kind of preparation method of aluminium nitride powder |
| CN110577403A (en) * | 2018-06-07 | 2019-12-17 | 有研稀土新材料股份有限公司 | high-purity aluminum nitride powder and preparation method thereof |
| CN110697665A (en) * | 2019-11-20 | 2020-01-17 | 航天特种材料及工艺技术研究所 | Purification method of aluminum nitride powder, aluminum nitride powder prepared by method and application of aluminum nitride powder |
| CN112897481A (en) * | 2020-12-30 | 2021-06-04 | 河北利福光电技术有限公司 | Aluminum nitride powder and preparation method thereof |
| CN112897482A (en) * | 2021-01-14 | 2021-06-04 | 中氢能源科技发展(内蒙古)有限公司 | Method for preparing aluminum nitride by using aluminum alloy as raw material |
| CN116396082A (en) * | 2023-05-24 | 2023-07-07 | 郑州大学 | Preparation method of aluminum nitride powder |
Citations (1)
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|---|---|---|---|---|
| CN101429031A (en) * | 2008-12-11 | 2009-05-13 | 沈阳大学 | Macromolecule network preparation method for high-purity ultra-fine aluminum nitride ceramic |
-
2014
- 2014-10-31 CN CN201410601847.5A patent/CN104402452B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101429031A (en) * | 2008-12-11 | 2009-05-13 | 沈阳大学 | Macromolecule network preparation method for high-purity ultra-fine aluminum nitride ceramic |
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| CN105542071A (en) * | 2016-01-27 | 2016-05-04 | 王柳燕 | Method for preparing composite nanometer hydrogel precursor |
| CN105884372A (en) * | 2016-04-12 | 2016-08-24 | 武汉理工大学 | Method for synthesizing AlN ceramic powder through organic network |
| CN105884372B (en) * | 2016-04-12 | 2018-11-13 | 武汉理工大学 | Organic network method synthesizes AlN ceramic powder method |
| CN105837223A (en) * | 2016-05-04 | 2016-08-10 | 中国科学院上海硅酸盐研究所 | Method for synthesizing aluminum nitride power |
| CN107867863B (en) * | 2016-09-23 | 2020-08-14 | 中国人民解放军国防科学技术大学 | Aluminum oxynitride ceramic powder and preparation method thereof |
| CN107867863A (en) * | 2016-09-23 | 2018-04-03 | 中国人民解放军国防科学技术大学 | Aluminum oxynitride ceramic powder and preparation method thereof |
| CN107903069A (en) * | 2017-12-29 | 2018-04-13 | 苏州图纳新材料科技有限公司 | Aluminium nitride powder and preparation method thereof |
| CN110577403A (en) * | 2018-06-07 | 2019-12-17 | 有研稀土新材料股份有限公司 | high-purity aluminum nitride powder and preparation method thereof |
| CN109251040A (en) * | 2018-09-28 | 2019-01-22 | 航天特种材料及工艺技术研究所 | A kind of porous aluminum carbon matrix precursor and preparation method thereof |
| CN109205579A (en) * | 2018-10-22 | 2019-01-15 | 厦门钜瓷科技有限公司 | The preparation method of aluminium nitride |
| CN109293368A (en) * | 2018-12-06 | 2019-02-01 | 石家庄学院 | A kind of preparation method of aluminium nitride powder |
| CN109293368B (en) * | 2018-12-06 | 2021-08-10 | 石家庄学院 | Preparation method of aluminum nitride powder |
| CN110697665A (en) * | 2019-11-20 | 2020-01-17 | 航天特种材料及工艺技术研究所 | Purification method of aluminum nitride powder, aluminum nitride powder prepared by method and application of aluminum nitride powder |
| CN112897481A (en) * | 2020-12-30 | 2021-06-04 | 河北利福光电技术有限公司 | Aluminum nitride powder and preparation method thereof |
| CN112897482A (en) * | 2021-01-14 | 2021-06-04 | 中氢能源科技发展(内蒙古)有限公司 | Method for preparing aluminum nitride by using aluminum alloy as raw material |
| CN116396082A (en) * | 2023-05-24 | 2023-07-07 | 郑州大学 | Preparation method of aluminum nitride powder |
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