CN103011834A - Preparation method for high-compactness composite ceramic - Google Patents

Preparation method for high-compactness composite ceramic Download PDF

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Publication number
CN103011834A
CN103011834A CN 201210496669 CN201210496669A CN103011834A CN 103011834 A CN103011834 A CN 103011834A CN 201210496669 CN201210496669 CN 201210496669 CN 201210496669 A CN201210496669 A CN 201210496669A CN 103011834 A CN103011834 A CN 103011834A
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sintering
preparation
batch mixing
raw material
ball milling
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李东炬
韩吉光
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DALIAN DAYOU HI-TECH CERAMIC Co Ltd
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DALIAN DAYOU HI-TECH CERAMIC Co Ltd
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Priority to CN 201210496669 priority Critical patent/CN103011834A/en
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Abstract

The invention relates to a preparation method for high-compactness composite ceramic, belonging to the preparation field of ceramic. The preparation method for the high-compactness composite ceramic comprises the following steps of: mixing materials, ball-milling and sintering; the ceramic materials comprise the following components in percentage by weight: 70%-90% of beta-Si3N4, 5%-25% of AlN, 1%-3% of BN, 0.1%-1% of Y2O3 and 0.1%-1% of CaF2. The preparation method can realize the sintering of a silicon nitride-aluminum nitride-cubic boron nitride composite ceramic material under the normal pressure, has simple steps, and is easy and convenient to carry out. The silicon nitride ceramic prepared by the method provided by the invention has high strength, good compactness, heat resistance and excellent abrading agent resistance, can be extensively used for the field with high material strength requirements, and is particular applicable to manufacturing a bearing rolling element.

Description

A kind of preparation method of high-compactness composite ceramics
Technical field
The present invention relates to a kind of preparation method of high-compactness composite ceramics, belong to ceramic preparation field.
Background technology
Cubic boron nitride ceramic all has good thermotolerance, thermostability, thermal conductivity, is desirable heat sink material and high temperature insulating material.The chemical stability of boron nitride is good, can resist the etch of most of molten metal.It also has good self lubricity.Yet its hardness is low than other high-strength ceramics, is applicable to make high-temperature bearing.Yet the sintering condition of cubic boron nitride ceramic is extremely harsh, in order to reduce its sintering temperature and condition, need to add other sintering aids in sintering process.
It is very high and extremely high temperature resistant that silicon nitride ceramics has high intensity, and its intensity does not descend at 1200 ℃ high temperature, can not be melt into after being heated and melt body, simultaneously, its resistance to chemical corrosion is excellent, the mineral acid that ability is nearly all and 30% following caustic soda soln, the also a lot of organic acid corrosion of ability.The sintering process of silicon nitride ceramics is generally three kinds: hot isostatic pressing (HIP), hot pressing (HP) and gas pressure sintering.The pressure of atmosphere sintering is 5 ~ 10MPa, and the pressure of hot pressed sintering is about 70Mpa, and the pressure of the sintering of hot isostatic pressing is 150MPa ~ 200MPa.
For thermal conductivity and the self lubricity that strengthens silicon nitride ceramics, a kind of multiphase composite material need to be provided, and reduce sintering pressure, realize pressureless sintering.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of high-compactness composite ceramics, this preparation method can realize sintered silicon nitride-aluminium nitride under normal pressure-cubic boron nitride composite ceramic material, utilize the advantage that composite ceramics intensity is high, compactness good, wear-resisting row excellent, self-lubricating property is good of the method preparation, be particularly useful for making the rolling body of ceramic ball bearing.
A kind of preparation method of high-compactness composite ceramics comprises the step of batch mixing, ball milling and sintering, and in the described batch mixing step, ceramic raw material by mass percentage, is comprised of following component:
Figure BDA00002484761100011
The preferred described ceramic raw material of the preparation method of the fine and close composite ceramics of height of the present invention by mass percentage, is comprised of following component:
Figure BDA00002484761100021
The preferred described ceramic raw material of the preparation method of the fine and close composite ceramics of height of the present invention by mass percentage, is comprised of following component:
Figure BDA00002484761100022
The preferred described step that is sintered to pressureless sintering of the preparation method of the fine and close composite ceramics of height of the present invention, undertaken by following technique: in the nitrogen atmosphere, powder is placed mould, speed with 10 ~ 20 ℃/min in sintering oven is warming up to 1500 ℃ ~ 1750 ℃, insulation 2h ~ 6h, cool to room temperature behind the stopped heating with the furnace, wherein nitrogen flow rate is 1 ~ 5L/min.
The preferred described ball milling step of the preparation method of the fine and close composite ceramics of height of the present invention is undertaken by following technique: under the normal temperature, will place ball mill through the powder of batch mixing, in speed ball milling 2h ~ 6h of 300 ~ 360r/min.
The preferred described batch mixing step of the preparation method of the fine and close composite ceramics of height of the present invention is undertaken by following technique: ceramic raw material is after drying mixed in proportion, cross 80 ~ 200 mesh sieves.
The further preferred following technical proposals of the preparation method of the fine and close composite ceramics of height of the present invention:
A kind of preparation method of high fine and close composite ceramics comprises following processing step:
1. batch mixing: ceramic raw material is after drying mixed in proportion, cross 80 ~ 200 mesh sieves;
2. ball milling: under the normal temperature, will place ball mill through the powder of batch mixing, in speed ball milling 2h ~ 6h of 300 ~ 360r/min;
3. sintering: in the nitrogen atmosphere, powder is placed mould, the speed with 10 ~ 20 ℃/min in sintering oven is warming up to 1500 ℃ ~ 1750 ℃, and insulation 2h ~ 6h cools to room temperature with the furnace behind the stopped heating, and wherein nitrogen flow rate is 1 ~ 5L/min.
The invention has the beneficial effects as follows: a kind of preparation method of high-compactness composite ceramics comprises by mass percentage, being made of the described ceramic raw material of step of batch mixing, ball milling and sintering: β-Si following component 3N 4: 70% ~ 90%, AlN:5% ~ 25%, BN:1% ~ 3%, Y 2O 3: 0.1% ~ 1%, CaF 2: 0.1% ~ 1%, this preparation method can realize sintered silicon nitride-aluminium nitride under normal pressure-cubic boron nitride composite ceramic material, step is simple, convenient and easy simultaneously.Utilize the silicon nitride ceramics intensity of the method preparation high, compactness good, high temperature resistant and wear-resisting excellence, can be widely used in variously to the demanding field of the strength of materials, is particularly useful for making bearing roller.
Embodiment
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
Embodiment 1
1. batch mixing: ceramic raw material is after drying mixed in proportion, cross 120 mesh sieves, described ceramic raw material by mass percentage, is comprised of following component:
2. ball milling: under the normal temperature, will place ball mill through the powder of batch mixing, in the speed ball milling 5h of 300r/min;
3. sintering: sintering: in the nitrogen atmosphere, powder is placed mould, the speed with 15 ℃/min in sintering oven is warming up to 11750 ℃, and insulation 3h cools to room temperature with the furnace behind the stopped heating, and wherein nitrogen flow rate is 2L/min.

Claims (7)

1. the preparation method of a high-compactness composite ceramics comprises the step of batch mixing, ball milling and sintering, and it is characterized in that: in the described batch mixing step, ceramic raw material by mass percentage, is comprised of following component:
Figure FDA00002484761000011
2. method according to claim 1, it is characterized in that: described ceramic raw material by mass percentage, is comprised of following component:
Figure FDA00002484761000012
3. method according to claim 1, it is characterized in that: described ceramic raw material by mass percentage, is comprised of following component:
4. method according to claim 1, it is characterized in that: the described step that is sintered to pressureless sintering, undertaken by following technique: in the nitrogen atmosphere, powder is placed mould, speed with 10 ~ 20 ℃/min in sintering oven is warming up to 1500 ℃ ~ 1750 ℃, insulation 2h ~ 6h cools to room temperature with the furnace behind the stopped heating, wherein nitrogen flow rate is 1 ~ 5L/min.
5. method according to claim 1 is characterized in that: described ball milling step, undertaken by following technique: under the normal temperature, will place ball mill through the powder of batch mixing, in speed ball milling 2h ~ 6h of 300 ~ 360r/min.
6. method according to claim 1 is characterized in that: described batch mixing step, undertaken by following technique: ceramic raw material is after drying mixed in proportion, cross 80 ~ 200 mesh sieves.
7. the described method of arbitrary claim according to claim 1 ~ 6 is characterized in that: comprise following processing step:
1. batch mixing: ceramic raw material is after drying mixed in proportion, cross 80 ~ 200 mesh sieves;
2. ball milling: under the normal temperature, will place ball mill through the powder of batch mixing, in speed ball milling 2h ~ 6h of 300 ~ 360r/min;
3. sintering: in the nitrogen atmosphere, powder is placed mould, the speed with 10 ~ 20 ℃/min in sintering oven is warming up to 1500 ℃ ~ 1750 ℃, and insulation 2h ~ 6h cools to room temperature with the furnace behind the stopped heating, and wherein nitrogen flow rate is 1 ~ 5L/min.
CN 201210496669 2012-11-28 2012-11-28 Preparation method for high-compactness composite ceramic Pending CN103011834A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103803950A (en) * 2014-03-13 2014-05-21 中国人民解放军国防科学技术大学 Boron nitride nanotube reinforced ceramic-based composite material and preparation method thereof
CN105272269A (en) * 2015-10-20 2016-01-27 西安邮电大学 Preparation method of Si3N4/h-BN nano-composite ceramics
CN106631041A (en) * 2017-01-06 2017-05-10 张海波 Production and manufacturing technology of silicon nitride ceramic tiny component
CN106866155A (en) * 2017-03-14 2017-06-20 浙江海洋大学 A kind of ultra-low penetration core and preparation method thereof
CN111196729A (en) * 2020-01-09 2020-05-26 中国科学院上海硅酸盐研究所 Method for preparing porous silicon nitride ceramic by using ultralow-content sintering aid

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103803950A (en) * 2014-03-13 2014-05-21 中国人民解放军国防科学技术大学 Boron nitride nanotube reinforced ceramic-based composite material and preparation method thereof
CN103803950B (en) * 2014-03-13 2015-07-01 中国人民解放军国防科学技术大学 Boron nitride nanotube reinforced ceramic-based composite material and preparation method thereof
CN105272269A (en) * 2015-10-20 2016-01-27 西安邮电大学 Preparation method of Si3N4/h-BN nano-composite ceramics
CN106631041A (en) * 2017-01-06 2017-05-10 张海波 Production and manufacturing technology of silicon nitride ceramic tiny component
CN106866155A (en) * 2017-03-14 2017-06-20 浙江海洋大学 A kind of ultra-low penetration core and preparation method thereof
CN106866155B (en) * 2017-03-14 2020-09-18 浙江海洋大学 Ultra-low permeability rock core and preparation method thereof
CN111196729A (en) * 2020-01-09 2020-05-26 中国科学院上海硅酸盐研究所 Method for preparing porous silicon nitride ceramic by using ultralow-content sintering aid
CN111196729B (en) * 2020-01-09 2021-08-06 中国科学院上海硅酸盐研究所 Method for preparing porous silicon nitride ceramic by using ultralow-content sintering aid

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Application publication date: 20130403