CN106431418A - Method for preparing nanometer AlN powder through hydrothermal method and intermediate and product produced through method - Google Patents
Method for preparing nanometer AlN powder through hydrothermal method and intermediate and product produced through method Download PDFInfo
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- CN106431418A CN106431418A CN201610850066.9A CN201610850066A CN106431418A CN 106431418 A CN106431418 A CN 106431418A CN 201610850066 A CN201610850066 A CN 201610850066A CN 106431418 A CN106431418 A CN 106431418A
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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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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- 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- 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
- C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
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- C—CHEMISTRY; METALLURGY
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- 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
- C04B2235/5463—Particle size distributions
Abstract
The invention discloses a method for preparing nanometer AlN powder through a hydrothermal method. The method includes the steps of selecting a proper aluminum source, a proper carbon source and a proper precipitator to prepare a precursor through the hydrothermal method, calcining the precursor in the nitrogen atmosphere at 1300 to 1600 DEG C, and conducting post-treatment to prepare the high-purity nanometer AlN powder. The raw materials are wide and easy to obtain, the process is simple, and the nanometer AlN powder high in purity, narrow in grain size distribution range and high in calcining activity is prepared. The invention further discloses a material of a wrapping structure, namely the precursor prepared through the method. The invention further discloses the pure-phase nanometer AlN powder prepared through the method.
Description
Technical field
The present invention relates to a kind of nano aluminum nitride AlN raw powder's production technology, belong to materials science field.
Background technology
Aluminium nitride is a kind of ceramic material with excellent comprehensive performance, its high heat conductance, low-k, excellent electricity
The features such as insulating properties, linear expansion coefficient that is corrosion-resistant and matching with silicon, making it substitute aluminum oxide becomes now
Preferably baseplate material and electron device package material.Aluminium nitride is a kind of typical covalent compound, and its diffusion coefficient is little, plus
The protective effect of upper epidermis pellumina, leads to be difficult to prepare the AlN ceramic of densification under the conditions of temperature is less than 1900 DEG C.Though
So AlN ceramic sintering temperature can be reduced using liquid-phase sintering by adding suitable sintering aid, but the second phase introducing
The thermal conductivity of AlN ceramic can be had a negative impact.Except adding appropriate sintering aid, the original particle size of powder and particle size
Distribution also can significantly reduce outside the sintering temperature of AlN ceramic.It is raw material using the tiny powder of particle diameter, it will help shorten atom
Diffusion length, increase ceramic post sintering motive force, thus accelerate the densification process of AlN ceramic sintering.Therefore, particle diameter tiny, point
Dissipate the sintering that uniform nanoscale AlN material powder can effectively facilitate AlN ceramic, avoid introducing the second phase simultaneously, will not be to pottery
The thermal conductivity of porcelain has a negative impact, and has broad application prospects.
The main method producing AlN powder at present is carbothermic method and direct nitridation method.Compared with direct nitridation method, carbon
, because its abundant raw material, technical process are simple, the powder purity of synthesis is high, particle diameter is little and the advantages of being evenly distributed for thermal reduction,
There is wider application in industrial production.At present, with micron order alumina powder jointed as raw material, real by carbothermic method
Show the large-scale production of high-quality micron order AlN powder.During carbon-thermal reduction, the particle size of AlN depends primarily on oxygen
Change the particle size of aluminium, how to obtain nano level AlN powder is problem demanding prompt solution.
Content of the invention
One side according to the application, there is provided a kind of method that hydro-thermal method prepares nano-aluminum nitride (aluminium nitride) powder, should
Method mild condition, can obtain average grain diameter be less than 100nm and the excellent pure phase nanometer AlN powder of granule-morphology.
Described hydro-thermal method prepare nano-aluminum nitride powder method it is characterised in that using hydro-thermal process by silicon source, carbon source and
Precipitating reagent prepares presoma, and presoma prepares described nano-aluminum nitride powder through calcining and post-processing.
Preferably, described presoma has clad structure, and described clad structure refers to core containing aluminium element by carbon coating.
The described core containing aluminium element is able to high degree of dispersion (nanoscale) by way of the coating cladding by carbon elements, and has
Effect avoids the Sintering Problem in calcining and last handling process.The nano-aluminum nitride diameter of particle that technical scheme obtains is less than
100nm and centralized particle diameter.
It is further preferred that the diameter range of the core of described aluminium element is 30nm～60nm.
Preferably, described hydro-thermal process temperature is 180～220 DEG C, and hydrothermal conditions are 6～24 hours.Excellent further
Selection of land, described hydrothermal conditions are 8～20 hours.It is further preferred that described hydrothermal conditions are 10～14 hours.
As a specific embodiment, described hydrothermal conditions are 12 hours.
Preferably, source of aluminium is at least one of aluminum nitrate, aluminium chloride, aluminium isopropoxide, aluminum sulfate, aluminum acetate.
Further preferably source of aluminium is at least one of aluminum nitrate, aluminium chloride, aluminium isopropoxide.
Preferably, described carbon source is soluble monose or disaccharide
It is further preferred that described carbon source is glucose, sucrose, fructose, at least one of lactose.
Preferably, described precipitating reagent is urea or ammoniacal liquor.
Preferably, in described raw material silicon source, carbon source and precipitating reagent mol ratio Al：C：Precipitating reagent=1：3～6：2～4.
Preferably, described post processing is to be incubated 2～4 hours in 600～800 DEG C of air atmosphere.
It is further preferred that described post processing is to be incubated 2～4 hours in 650～750 DEG C of air atmosphere.
Preferably, methods described at least comprises the following steps：
A) silicon source, carbon source and precipitating reagent are dissolved in solvent, form the initial mixing that silicon source concentration is 0.5～3.0mol/L
Thing I；
B) the original mixture I that step a) obtains is proceeded in water heating kettle, at a temperature of 180～220 DEG C hydro-thermal process 6～
24 hours, obtain presoma；
C) under the presoma that step b) is obtained and nitrogen atmosphere, calcine 2～5 hours for 1300～1600 DEG C, obtain powder
I；
D) the powder I that step c) obtains is incubated 2～4 hours in 600～800 DEG C of air atmosphere, obtain described in receive
Rice AlN powder.
It is further preferred that in described step a), mol ratio Al of silicon source, carbon source and precipitating reagent：C：Precipitating reagent=1：3～
6：2～4.In the application, the mol ratio of source of aluminium, carbon source and precipitating reagent, refer in the molal quantity of aluminium atom in silicon source, carbon source
The ratio of the molal quantity of the molal quantity of carbon atom and precipitation agent molecule.
Preferably, described step a) is first silicon source to be dissolved in solvent, and forming silicon source concentration is the molten of 0.5～3.0mol/L
Liquid I, then carbon source is added in solution I, obtain solution II, then precipitating reagent is added in solution II, obtain original mixture I.
Preferably, described step b) is that the original mixture I obtaining step a) proceeds in water heating kettle, at 180～220 DEG C
At a temperature of hydro-thermal process 10～14 hours, after suction filtration and drying, obtain presoma.
It is further preferred that described step c) be the presoma that step b) is obtained in a nitrogen atmosphere, 1300～1600
DEG C calcining 2～4 hours, obtain powder I.
As one preferred embodiment, methods described at least comprises the following steps：
A1) silicon source is dissolved in solvent, forms the solution I that silicon source concentration is 0.5～3.0mol/L；
A2) carbon source is added step a1) in the solution I that obtains, obtain solution II；
A3) precipitating reagent is added step a1) in the solution II that obtains, obtain original mixture I；
B) by step a3) the original mixture I that obtains proceeds in water heating kettle, hydro-thermal process 6 at a temperature of 180～220 DEG C
～24 hours, obtain presoma；
C) under the presoma that step b) is obtained and nitrogen atmosphere, calcine 2～5 hours for 1300～1600 DEG C, obtain powder
I；
D) the powder I that step c) obtains is incubated 2～4 hours in 600～800 DEG C of air atmosphere, obtain described in receive
Rice AlN powder.
A kind of another aspect according to the application, there is provided clad structure material, is that any of the above-described method prepares
Described presoma, this clad structure material is prepared by hydro-thermal method, is used for preparing nano-aluminum nitride powder, can obtain particle diameter
Less than 100nm and the excellent pure phase nanometer AlN powder of granule-morphology.Described clad structure material include core containing aluminium element and
Carbon coating, the diameter range of described core is 30nm～60nm.
A kind of another aspect according to the application, there is provided nano-aluminum nitride powder, is prepared by any of the above-described method
And/or above-mentioned clad structure material prepares as presoma it is characterised in that described nano-aluminum nitride powder is pure phase AlN powder
Body, described nano-aluminum nitride powder average grain diameter is less than 100nm.
The beneficial effect that the application can produce includes：
1) method provided herein, synthesis condition is gentle, raw material is extensively easy to get, process is simple, be prepared for purity high,
The nano-aluminum nitride powder that particle size distribution range is narrow, sintering activity is good.
2) nano-aluminum nitride powder provided herein, has average grain diameter and is less than 100nm, the good advantage of sintering activity.
3) clad structure material provided herein, can effectively reduce the reaction temperature preparing AlN powder and stop oxygen
Change aluminium grain to grow up, the nano-aluminum nitride powder that prepared particle size distribution range is narrow, sintering activity is good.
Brief description
The transmission electron microscope photo of the presoma that Fig. 1 prepares for a kind of embodiment of the application.
The nano-aluminum nitride powder powder x-ray diffraction spectrogram that Fig. 2 prepares for the application.
The nano-aluminum nitride powder stereoscan photograph that Fig. 3 prepares for a kind of embodiment of the application.
The nano-aluminum nitride powder stereoscan photograph that Fig. 4 prepares for a kind of embodiment of the application.
Specific embodiment
With reference to embodiment in detail the application is described in detail, but the application is not limited to these embodiments.
If no special instructions, the raw material in embodiments herein is all bought by commercial sources.
In embodiments herein, analysis method is as follows：
Tecnai G2F20 type TEM using FEI Co. carries out presoma phenetic analysis.
Derive instrument using the Miniflex600 type X-ray of Rigaku company and carry out XRD phenetic analysis.
SU8010 type ESEM using Hitachi company obtains scanning electron microscope (SEM) photograph.
Embodiment 1
Weigh 0.1mol aluminum nitrate first to be dissolved in 100ml deionized water, then by the urea of 0.2mol and 0.05mol
Sucrose add above-mentioned solution, after being uniformly mixed, by solution move into water heating kettle in.Water heating kettle is warmed up to 200 DEG C of insulations
12h, takes out after being cooled to room temperature.The sediment of hydrothermal solution, through suction filtration, after being dried, obtains the presoma of brown, transmission electricity
Mirror chart its micro-structural bright is clad structure, sees Fig. 1, in figure arrow indication is the core containing aluminium element.By above-mentioned brown forerunner
Body loads graphite crucible after grinding, in flowing nitrogen atmosphere high temperature tube furnace, with the intensification speed of 5 DEG C/min～10 DEG C/min
Degree rises to the powder that 1500 DEG C of insulation 3h obtain black, and above-mentioned black powder is placed in Muffle furnace, with the intensification speed of 5 DEG C/min
Spend and carry out obtaining final product canescence powder except carbon to 700 DEG C of insulation 2h.X-ray diffraction testing result shows that powder product is pure AlN phase
(see Fig. 2), scanning electron microscope (SEM) photograph shows its average grain diameter about 80nm, and wherein particle diameter distribution accounts for more than 80% in 60nm-100nm
(see Fig. 3).
Embodiment 2～5
With embodiment 1, raw material and response parameter are shown in Table 1 for operation.The X-ray diffraction detection of the product that embodiment 2～5 obtains
, with embodiment 1 consistent (see Fig. 2), scanning electron microscope (SEM) photograph shows its particle diameter for nanoscale and particle size distribution range is narrow for result.Wherein real
Apply the scanning electron microscope (SEM) photograph that example 2 obtains and see Fig. 4.
Table 1
Comparative example 1
Raw material, response parameter and operation, with embodiment 1, simply do not have hydro-thermal process to obtain the process of presoma, by solution
It is warmed up to 100 DEG C of insulation 12h, the direct suction filtration of the presoma obtaining after being cooled to room temperature is calcined after being dried and post-processed, and obtains
Powder average grain diameter is more than 300nm, and particle size distribution range width.
The above, be only several embodiments of the application, and not the application is done with any type of restriction although this Shen
Please with preferred embodiment disclose as above, but and be not used to limit the application, any those skilled in the art, do not taking off
In the range of technical scheme, make a little variation using the technology contents of the disclosure above or modification is all equal to
Effect case study on implementation, belongs in the range of technical scheme.
Claims (10)
1. a kind of method preparing nano-aluminum nitride powder is it is characterised in that carry out to the raw material containing silicon source, carbon source and precipitating reagent
Hydro-thermal process obtains presoma, and presoma prepares described nano-aluminum nitride powder through calcining and post-processing.
2. method according to claim 1 is it is characterised in that described presoma has clad structure, described clad structure
Refer to core containing aluminium element by carbon coating.
3. method according to claim 2 it is characterised in that the described core containing aluminium element diameter range be 30nm～
60nm.
4. method according to claim 1 is it is characterised in that described hydro-thermal process temperature is 180～220 DEG C, at hydro-thermal
The reason time is 6～24 hours.
5. method according to claim 1 is it is characterised in that silicon source in described raw material is selected from aluminum nitrate, aluminium chloride, different
At least one of aluminium propoxide, aluminum sulfate, aluminum acetate；Described carbon source be selected from glucose, sucrose, fructose, lactose, in maltose at least
A kind of；Described precipitating reagent is urea or ammoniacal liquor；
Mol ratio Al of silicon source, carbon source and precipitating reagent in described raw material：C：Precipitating reagent=1：3～7.5：2～4.
6. method according to claim 1 is it is characterised in that described post processing is in 600～800 DEG C of air atmosphere
Insulation 1～4 hour.
7. method according to claim 1 is it is characterised in that methods described at least comprises the following steps：
A) silicon source, carbon source and precipitating reagent are dissolved in solvent, form the original mixture I that silicon source concentration is 0.5～3.0mol/L；
B) the original mixture I that step a) obtains is proceeded in water heating kettle, at a temperature of 180～220 DEG C, hydro-thermal process 6～24 is little
When, obtain presoma；
C) presoma that step b) is obtained in a nitrogen atmosphere, 1300～1600 DEG C calcine 2～5 hours, obtain powder I；
D) the powder I that step c) obtains is incubated 2～4 hours in 600～800 DEG C of air atmosphere, obtains described nano-aluminum nitride
Powder.
8. method according to claim 7, it is characterised in that described step a) is first silicon source to be dissolved in solvent, is formed
Silicon source concentration is the solution I of 0.5～3.0mol/L, then carbon source is added in solution I, obtains solution II, then precipitating reagent is added
In solution II, the original mixture I that obtains；
Described step b) is that the original mixture I obtaining step a) proceeds in water heating kettle, hydro-thermal at a temperature of 180～220 DEG C
Process 10～14 hours, after suction filtration and drying, obtain presoma.
9. a kind of material of clad structure, is the described presoma that the method described in any one of claim 1 to 8 prepares,
It is characterized in that, described clad structure is core containing aluminium element by carbon coating, the diameter range of described core be 30nm～
60nm.
10. a kind of nano-aluminum nitride powder, the method described in any one of claim 1 to 8 and/or the cladding described in claim 9
Structural material prepares as presoma it is characterised in that described nano-aluminum nitride powder is pure phase AlN powder, described nanometer
AlN powder average grain diameter is less than 100nm.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108689715A (en) * | 2018-04-18 | 2018-10-23 | 山东国瓷功能材料股份有限公司 | A kind of aluminium nitride powder and preparation method thereof |
| CN108818807A (en) * | 2018-04-26 | 2018-11-16 | 阜南县慧宏柳木工艺品有限公司 | A kind of preparation method of resistance to bubble health care wicker plaiting article pillow |
| CN110480004A (en) * | 2019-08-29 | 2019-11-22 | 南京理工大学 | The method that hydro-thermal method prepares carbon-coated aluminum nanoparticles |
| CN110511036A (en) * | 2019-07-25 | 2019-11-29 | 东莞材料基因高等理工研究院 | A kind of submicron order aluminum oxynitride ceramic powder and preparation method thereof |
| CN111732084A (en) * | 2020-06-23 | 2020-10-02 | 济南大学 | Method for preparing porous aluminum nitride metamaterial by utilizing two-dimensional carbon nitride template growth |
| CN112479724A (en) * | 2020-11-23 | 2021-03-12 | 中国科学院金属研究所 | Yb (Yb)2Si2O7Carbon coating-coprecipitation preparation method of superfine powder |
| CN113460981A (en) * | 2021-07-09 | 2021-10-01 | 南充三环电子有限公司 | Aluminum nitride powder and preparation method and application thereof |
| CN113860879A (en) * | 2021-11-24 | 2021-12-31 | 江西理工大学 | Method for preparing aluminum nitride powder by suspension reduction |
| CN114716250A (en) * | 2021-01-06 | 2022-07-08 | 中国科学院福建物质结构研究所 | Preparation method of AlON powder |
| CN116062714A (en) * | 2023-01-18 | 2023-05-05 | 大连海事大学 | Pure-phase nanometer AlN powder and preparation method and application thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108689715B (en) * | 2018-04-18 | 2021-01-15 | 山东国瓷功能材料股份有限公司 | Aluminum nitride powder and preparation method thereof |
| CN108689715A (en) * | 2018-04-18 | 2018-10-23 | 山东国瓷功能材料股份有限公司 | A kind of aluminium nitride powder and preparation method thereof |
| CN108818807A (en) * | 2018-04-26 | 2018-11-16 | 阜南县慧宏柳木工艺品有限公司 | A kind of preparation method of resistance to bubble health care wicker plaiting article pillow |
| CN110511036A (en) * | 2019-07-25 | 2019-11-29 | 东莞材料基因高等理工研究院 | A kind of submicron order aluminum oxynitride ceramic powder and preparation method thereof |
| CN110480004B (en) * | 2019-08-29 | 2021-11-09 | 南京理工大学 | Method for preparing carbon-coated nano aluminum powder by hydrothermal method |
| CN110480004A (en) * | 2019-08-29 | 2019-11-22 | 南京理工大学 | The method that hydro-thermal method prepares carbon-coated aluminum nanoparticles |
| CN111732084A (en) * | 2020-06-23 | 2020-10-02 | 济南大学 | Method for preparing porous aluminum nitride metamaterial by utilizing two-dimensional carbon nitride template growth |
| CN111732084B (en) * | 2020-06-23 | 2021-11-09 | 济南大学 | Method for preparing porous aluminum nitride supercapacitor material by utilizing two-dimensional carbon nitride template growth |
| CN112479724A (en) * | 2020-11-23 | 2021-03-12 | 中国科学院金属研究所 | Yb (Yb)2Si2O7Carbon coating-coprecipitation preparation method of superfine powder |
| CN112479724B (en) * | 2020-11-23 | 2022-01-14 | 中国科学院金属研究所 | Yb (Yb)2Si2O7Carbon coating-coprecipitation preparation method of superfine powder |
| CN114716250A (en) * | 2021-01-06 | 2022-07-08 | 中国科学院福建物质结构研究所 | Preparation method of AlON powder |
| CN113460981A (en) * | 2021-07-09 | 2021-10-01 | 南充三环电子有限公司 | Aluminum nitride powder and preparation method and application thereof |
| CN113460981B (en) * | 2021-07-09 | 2022-11-18 | 南充三环电子有限公司 | Aluminum nitride powder and preparation method and application thereof |
| CN113860879A (en) * | 2021-11-24 | 2021-12-31 | 江西理工大学 | Method for preparing aluminum nitride powder by suspension reduction |
| CN116062714A (en) * | 2023-01-18 | 2023-05-05 | 大连海事大学 | Pure-phase nanometer AlN powder and preparation method and application thereof |
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