阅读说明：本技术 一种亚微米级氮氧化铝陶瓷粉体及其制备方法 (A kind of submicron order aluminum oxynitride ceramic powder and preparation method thereof ) 是由 向明 周有福 初铭强 王瑶 张书彦 于 2019-07-25 设计创作，主要内容包括：本发明公开了一种亚微米级氮氧化铝陶瓷粉体的制备方法,包括以下步骤：S1：配制含有无机铝源、碳源和添加剂的原料溶液；S2：将原料溶液进行水热处理得到前驱体；所述无机铝源、碳源的铝当量、碳当量摩尔比为1：(0.6-1.2)；S3：将前驱体在氮气氛围中碳热煅烧、球磨得到亚微米级氮氧化铝陶瓷粉体。该制备方法得到的亚微米级氮氧化铝陶瓷粉体通过X射线衍射检测结果表明,其粉体产物为纯相氮氧化铝；经扫描电镜表明,其粉体粒径为亚微米级。该粉体的粒径分布范围窄、纯度高、形貌优良。(The invention discloses a kind of submicron order aluminum oxynitride ceramic raw powder's production technologies, comprising the following steps: S1: preparing the material solution containing inorganic silicon source, carbon source and additive；S2: material solution progress hydro-thermal process is obtained into presoma；The inorganic silicon source, the equivalent thickness of aluminium of carbon source, carbon equivalent molar ratio are 1:(0.6-1.2)；S3: by presoma, carbon forged is burnt, ball milling obtains submicron order aluminum oxynitride ceramic powder in nitrogen atmosphere.The submicron order aluminum oxynitride ceramic powder that the preparation method obtains shows that its powder product is pure phase aluminum oxynitride by X-ray diffraction testing result；Show that its diameter of particle is submicron order through scanning electron microscope.The particle size distribution range of the powder is narrow, with high purity, pattern is excellent.)

1. a kind of submicron order aluminum oxynitride ceramic raw powder's production technology, which comprises the following steps:

S1: the material solution containing inorganic silicon source, carbon source and additive is prepared；

The inorganic silicon source is soluble inorganic aluminium salt；The carbon source is soluble saccharide compound；The additive is ammonium salt And/or urea；The inorganic silicon source, the equivalent thickness of aluminium of carbon source, carbon equivalent molar ratio are 1:(0.6-1.2)；

S2: material solution progress hydro-thermal process is obtained into presoma；

S3: by presoma, carbon forged is burnt, ball milling obtains submicron order aluminum oxynitride ceramic powder in nitrogen atmosphere.

2. submicron order aluminum oxynitride ceramic raw powder's production technology as described in claim 1, which is characterized in that in S1, institute Stating inorganic silicon source is one or more of aluminum nitrate, aluminium chloride or aluminum sulfate.

3. submicron order aluminum oxynitride ceramic raw powder's production technology as described in claim 1, which is characterized in that in S1, institute Stating carbon source is one or more of sucrose, fructose or glucose.

4. submicron order aluminum oxynitride ceramic raw powder's production technology as described in claim 1, which is characterized in that in S1, institute Stating ammonium salt is ammonium nitrate or ammonium chloride.

5. submicron order aluminum oxynitride ceramic raw powder's production technology as described in claim 1, which is characterized in that, will in S1 Inorganic silicon source is dissolved in the water, and is configured to the silicon source solution that equivalent thickness of aluminium concentration is 0.5-2.0mol/L, is added into silicon source solution It is 0.6-1.2mol/L that carbon source, which forms carbon equivalent concentration,；Additive is added so that additive concentration is 1-5mol/L.

6. submicron order aluminum oxynitride ceramic raw powder's production technology as described in claim 1, which is characterized in that in S2, water The temperature of heat treatment is 160-240 DEG C, and the time of hydro-thermal process is 6-24h.

7. submicron order aluminum oxynitride ceramic raw powder's production technology as described in claim 1, which is characterized in that in S2, water Drying is filtered after heat, obtains presoma.

8. submicron order aluminum oxynitride ceramic raw powder's production technology as described in claim 1, which is characterized in that in S3, nitrogen Under gas atmosphere, 1700-1800 DEG C of carbon forged burn 2-4 hour, obtain powder, then obtain submicron order aluminum oxynitride after ball milling and make pottery Porcelain powder.

9. a kind of submicron order aluminum oxynitride ceramic powder obtained such as the described in any item preparation methods of claim 1-8.

Technical field

The present invention relates to aluminum oxynitride ceramic technical fields, and in particular to a kind of submicron order aluminum oxynitride ceramic powder and Preparation method.

Background technique

Aluminum oxynitride is the solid solution of aluminium oxide and aluminium nitride, as structure-function integration material, machinery Qiang Du Gao ﹑ The Hao ﹑ good corrosion resistance of thermal shock resistance and high light transmittance, have broad application prospects in optical field.However, due to nitrogen oxygen Changing aluminium is a kind of typical covalent compound, and diffusion coefficient is small, causes to be difficult to prepare under the conditions of temperature is lower than 1950 DEG C The aluminum oxynitride ceramic of high light transmittance.

Currently, most of aluminum oxynitride crystalline ceramics are all made of the inefficient and height by hot pressing or hot isostatic pressing technique Cost limits its large-scale commercial production.The ceramic powder for using partial size small is raw material, it will help shortens atom diffusion Distance, increase sintering motive force can reduce the sintering temperature of aluminum oxynitride ceramic to accelerate the densification process of sintering in this way Degree, and then reduce production cost.

Preparing the main method of aluminum oxynitride powder at present is Direct-Nitridation Fa ﹑ carbothermic method and thermit reduction.With Other two methods are compared, and carbothermic method raw material is cheap and easy to get, and equipment requirement is low, are easier to obtain small, the with high purity nitrogen of granularity Alumina powder.But the synthesis temperature that traditional carbothermic method prepares aluminum oxynitride is high (>=1780 DEG C), and Product size The particle size of aluminium oxide is depended primarily on, how to obtain that partial size is small, the high aluminum oxynitride powder of activity is urgently to be resolved at present The problem of.

Summary of the invention

For overcome the deficiencies in the prior art, sub-micro is made using liquid phase method one of the objects of the present invention is to provide a kind of Meter level aluminum oxynitride ceramic raw powder's production technology.This method mild condition can obtain average grain diameter about 300nm and granulated The excellent pure phase aluminum oxynitride powder of looks.

The second object of the present invention is to provide the submicron order aluminum oxynitride ceramic powder that the preparation method obtains.

An object of the present invention adopts the following technical scheme that realization:

A kind of submicron order aluminum oxynitride ceramic raw powder's production technology, comprising the following steps:

S1: the material solution containing inorganic silicon source, carbon source and additive is prepared；

The inorganic silicon source is soluble inorganic aluminium salt；The carbon source is soluble saccharide compound；The additive is Ammonium salt and/or urea；The inorganic silicon source, the equivalent thickness of aluminium of carbon source, carbon equivalent molar ratio are 1:(0.6-1.2)；

S2: material solution progress hydro-thermal process is obtained into presoma；

S3: by presoma, carbon forged is burnt, ball milling obtains submicron order aluminum oxynitride ceramic powder in nitrogen atmosphere.

Further, in S1, the inorganic silicon source is one or more of aluminum nitrate, aluminium chloride or aluminum sulfate.

Further, in S1, the carbon source is one or more of sucrose, fructose or glucose.

Further, in S1, the ammonium salt is ammonium nitrate or ammonium chloride.

Further, in S1, inorganic silicon source is dissolved in the water, is configured to the aluminium that equivalent thickness of aluminium concentration is 0.5-2.0mol/L Source solution, it is 0.6-1.2mol/L that carbon source is added into silicon source solution and forms carbon equivalent concentration；Additive is added so that addition Agent concentration is 1-5mol/L.

Further, in S2, the temperature of hydro-thermal process is 160-240 DEG C, and the time of hydro-thermal process is 6-24h.

Further, in S2, drying is filtered after hydro-thermal, obtains presoma.

Further, in S3, under nitrogen atmosphere, 1700-1800 DEG C of carbon forged burn 2-4 hours, obtain powder, then through ball milling After obtain submicron order aluminum oxynitride ceramic powder.

The second object of the present invention adopts the following technical scheme that realization:

A kind of submicron order aluminum oxynitride ceramic powder obtained such as above-mentioned preparation method.

Compared with prior art, the beneficial effects of the present invention are:

It is of the invention provide it is a kind of with inorganic soluble carbon source, silicon source and additive, by liquid phase hydro-thermal method and carbothermy, High product uniform level, purity is high, the sub-micron aluminum oxynitride that particle size distribution range is narrow, pattern is uniform, sintering activity is strong is made Powder；It is high that the preparation method mild condition, raw material are not easy resistance to storage, simple process, repeatability, can large-scale application in industry Production, the requirement to factory site equipment are lower.

Detailed description of the invention

Fig. 1 is the sub-micron aluminum oxynitride powder powder x-ray diffraction spectrum that embodiment 1- embodiment 4 obtains.

Fig. 2 is the sub-micron aluminum oxynitride powder scanning electron microscope (SEM) photograph that embodiment 1 obtains.

Specific embodiment

In the following, being described further in conjunction with the drawings and specific embodiments to the present invention, it should be noted that in not phase Under the premise of conflict, new implementation can be formed between various embodiments described below or between each technical characteristic in any combination Example.

It is specific embodiment of the present invention below, used raw material, equipment etc. remove special limit in the following embodiments It can be obtained by buying pattern outside fixed.

Detecting instrument used in this application is as follows: utilizing the derivative instrument of the Miniflex600 type X-ray of Rigaku company Carry out XRD characterization analysis；Scanning electron microscope (SEM) photograph is obtained using the SU8010 type scanning electron microscope of Hitachi company.

In the application, the equivalent thickness of aluminium is the molar equivalent in silicon source in terms of aluminium element, carbon equivalent be in sugar in terms of carbon Molar equivalent.

The present invention provides a kind of submicron order aluminum oxynitride ceramic raw powder's production technology, comprising:

S1: the material solution containing inorganic silicon source, carbon source and additive is prepared；

The inorganic silicon source is soluble inorganic aluminium salt；The carbon source is soluble saccharide compound；The additive is Ammonium salt and/or urea；The inorganic silicon source, the equivalent thickness of aluminium of carbon source, carbon equivalent molar ratio are 1:(0.6-1.2)；

S2: material solution progress hydro-thermal process is obtained into presoma；

S3: by presoma, carbon forged is burnt, ball milling obtains submicron order aluminum oxynitride ceramic powder in nitrogen atmosphere.

The submicron order ceramics that form uniformity is high, particle size distribution range is narrow can be obtained in the preparation method.