阅读说明：本技术 一种氮化硼复合材料的制备方法 (Preparation method of boron nitride composite material ) 是由 姜明 罗佳伟 岳锋 于 2020-06-01 设计创作，主要内容包括：一种氮化硼复合材料的制备方法,包括：将原料置于搅拌桶内,加入40％质量分数的酒精,开启搅拌机混合3小时；将烘干的物料捣碎,过50目筛网；粉体填装,分2-5道工序填装,每道分10次装料,并缓慢施加压强1-10MPa,预压填装致密度小于40-55％；升温速率8-12℃/min,加压温度1000-1200℃,缓慢加压0.5-5MPa递增,并保压26MPa,烧结温度1700℃,保温时间大于2小时至行程不变,保证烧结产品均有高的致密度。本发明采用酒精湿法混合保证粉体充分均匀混合,且氮化硼不产生水解氧化硼影响产品高温使用性能；造粒过50目筛,保证造粒后原料颗粒均匀,保证烧结后各项产品性能的均匀。(A preparation method of a boron nitride composite material comprises the following steps: putting the raw materials into a stirring barrel, adding 40% of alcohol by mass fraction, starting a stirrer and mixing for 3 hours; mashing the dried materials, and sieving the smashed materials with a 50-mesh sieve; filling powder, namely filling the powder by 2-5 working procedures, wherein each procedure is divided into 10 times of filling, and slowly applying pressure intensity of 1-10MPa, wherein the density of prepressing filling is less than 40-55%; the heating rate is 8-12 ℃/min, the pressurizing temperature is 1000-1200 ℃, the slow pressurizing is carried out by 0.5-5MPa, the pressure is maintained by 26MPa, the sintering temperature is 1700 ℃, the heat preservation time is more than 2 hours until the stroke is unchanged, and the sintered products are ensured to have high density. According to the invention, the alcohol wet mixing is adopted to ensure that the powder is fully and uniformly mixed, and the boron nitride does not generate boron oxide hydrolysis to influence the high-temperature service performance of the product; and (3) granulating and sieving by a 50-mesh sieve, so that the uniform raw material particles after granulation are ensured, and the uniform performance of each product after sintering is ensured.)

1. A preparation method of a boron nitride composite material is characterized by comprising the following steps: the method comprises the following steps:

the method comprises the following steps: mixing raw materials:

the raw materials comprise: high-purity BN: 64.4 percent of high-purity SiO₂10.3 percent of high-purity Al₂O₃15.5% high purity ZrO₂:9.8％；

Putting the raw materials into a stirring barrel, adding 40% of alcohol by mass, starting a stirrer to mix for 3 hours, and ensuring that the materials are uniformly mixed;

the mixed liquid is filled into a tray, the liquid height is ensured to be less than 5mm, layering caused by different material precipitation rates in the drying process is reduced, and the mixed liquid is dried in an oven to constant weight;

step two: charging:

mashing the dried materials, and sieving the smashed materials with a 50-mesh sieve;

filling powder, namely filling the powder by 2-5 working procedures, wherein each procedure is divided into 10 times of filling, and slowly applying pressure intensity of 1-10MPa, wherein the density of prepressing filling is less than 40-55%;

step three: and (3) sintering:

the heating rate is 8-12 ℃/min, the pressurizing temperature is 1000-1200 ℃, the slow pressurizing is carried out by 0.5-5MPa, the pressure is maintained by 26MPa, the sintering temperature is 1700 ℃, the heat preservation time is more than 2 hours until the stroke is unchanged, and the sintered products are ensured to have high density.

[ technical field ] A method for producing a semiconductor device

The invention relates to a preparation method of a boron nitride composite material.

[ background of the invention ]

With the rapid development of 3D printing technology and powder metallurgy, the metal powder preparation technology is continuously updated, and the powder prepared by vacuum atomization is rapidly developed due to good flowing property. The refractory nozzle is a consumable material, and boron nitride composite materials are widely used as nozzle materials at present, so that the refractory nozzle has good processing performance and erosion resistance.

[ summary of the invention ]

The invention aims to provide a preparation method of a boron nitride composite material with corrosion resistance and excellent performance.

The invention is realized by the following steps:

a preparation method of a boron nitride composite material comprises the following steps:

the method comprises the following steps: mixing raw materials:

the raw materials comprise: high-purity BN: 64.4 percent of high-purity SiO₂:10.3% high purity Al₂O₃15.5% high purity ZrO₂:9.8％；

Putting the raw materials into a stirring barrel, adding 40% of alcohol by mass, starting a stirrer to mix for 3 hours, and ensuring that the materials are uniformly mixed;

the mixed liquid is filled into a tray, the liquid height is ensured to be less than 5mm, layering caused by different material precipitation rates in the drying process is reduced, and the mixed liquid is dried in an oven to constant weight;

step two: charging:

mashing the dried materials, and sieving the smashed materials with a 50-mesh sieve;

filling powder, namely filling the powder by 2-5 working procedures, wherein each procedure is divided into 10 times of filling, and slowly applying pressure intensity of 1-10MPa, wherein the density of prepressing filling is less than 40-55%;

step three: and (3) sintering:

the heating rate is 8-12 ℃/min, the pressurizing temperature is 1000-1200 ℃, the slow pressurizing is carried out by 0.5-5MPa, the pressure is maintained by 26MPa, the sintering temperature is 1700 ℃, the heat preservation time is more than 2 hours until the stroke is unchanged, and the sintered products are ensured to have high density.

The invention has the advantages that: 1. the ethanol wet mixing is adopted to ensure that the powder is fully and uniformly mixed, and the boron nitride does not generate hydrolyzed boron oxide to influence the high-temperature service performance of the product; 2. and (3) granulating and sieving by a 50-mesh sieve, so that the uniform raw material particles after granulation are ensured, and the uniform performance of each product after sintering is ensured.

[ detailed description ] embodiments

A preparation method of a boron nitride composite material comprises the following steps:

the method comprises the following steps: mixing raw materials:

the raw materials comprise: 64.4 percent of high-purity BN and high-purity SiO₂10.3 percent of high-purity Al₂O₃15.5% high purity ZrO₂9.8 percent; wherein the high-purity BN is hexagonal boron nitride (h-BN);

putting the raw materials into a stirring barrel, adding 40% of alcohol by mass, starting a stirrer to mix for 3 hours, and ensuring that the materials are uniformly mixed;

the mixed liquid is filled into a tray, the liquid height is ensured to be less than 5mm, layering caused by different material precipitation rates in the drying process is reduced, and the mixed liquid is dried in an oven to constant weight;

step two: charging:

mashing the dried materials, and sieving the smashed materials with a 50-mesh sieve;

powder is filled in 2-5 working procedures, each procedure is filled for 10 times, the pressure is slowly applied to 10MPa, and the density of the prepressing filling is less than 55%;

step three: and (3) sintering:

the heating rate is 8-12 ℃/min, the pressurizing temperature is 1000-1200 ℃, the slow pressurizing is carried out by 0.5-5MPa, the pressure is maintained by 26MPa, the sintering temperature is 1700 ℃, the heat preservation time is more than 2 hours until the stroke is unchanged, and the sintered products are ensured to have high density.

The invention adopts wet mixing to ensure that the powder is fully and uniformly mixed; alcohol is used as a dispersing agent to ensure that boron nitride does not generate boron oxide hydrolysis to influence the high-temperature service performance of the product; adding SiO₂、Al₂O₃Sintering to form mullite phase to enhance high-temperature strength; adding ZrO₂As a reinforcing phase, the high temperature resistance and high temperature strength of the material are improved; BN is used as a main matrix to improve the metal corrosion resistance and the processing performance of the material.

Table 1 is a comparison of properties of boron nitride composites produced by new and old processes:

table 1:

wherein the new process is referred to herein and the old process is the prior art process described in the "background" section.

As can be seen from Table 1, the boron nitride composite material prepared by the method of the invention has the advantages of greatly reduced deformation, high breaking strength and strong corrosion resistance compared with the prior art after being used.

The above description is only an example of the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.