CN103030398A - Preparation method of silicon nitride ceramic - Google Patents

Preparation method of silicon nitride ceramic Download PDF

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Publication number
CN103030398A
CN103030398A CN 201210499198 CN201210499198A CN103030398A CN 103030398 A CN103030398 A CN 103030398A CN 201210499198 CN201210499198 CN 201210499198 CN 201210499198 A CN201210499198 A CN 201210499198A CN 103030398 A CN103030398 A CN 103030398A
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Prior art keywords
silicon nitride
preparation
sintering
raw material
batch mixing
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CN 201210499198
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李东炬
甄恒洲
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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 201210499198 priority Critical patent/CN103030398A/en
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Abstract

The invention relates to a preparation method of silicon nitride ceramic and belongs to the field of ceramic preparation. The invention provides the preparation method of the silicon nitride ceramic, comprising the following steps of mixing materials, carrying out ball milling, and sintering, wherein a ceramic raw material is formed by the following components according to mass percent: 80-95% of beta-Si3N4, 2-15% of Al2O3, 1-12% of MgO, 1-12% of Y2O3 and 1-12% of ZrO2. The preparation method disclosed by the invention can realize that the silicon nitride ceramic can be sintered under normal pressure; and meanwhile, the preparation method has simple steps and is convenient and feasible. The silicon nitride ceramic prepared by the method has the advantages of high strength, good compactness, high-temperature resistance and excellent wear resistance; and the silicon nitride ceramic can be widely applied to the fields with high requirements on material strength, and is particularly suitable for manufacturing a bearing rolling body.

Description

A kind of preparation method of silicon nitride ceramics
Technical field
The present invention relates to a kind of preparation method of silicon nitride ceramics, belong to ceramic preparation field.
Background technology
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.
Heat and other static pressuring processes is that goods are placed in the airtight container, applies each to equal pressure to goods, imposes simultaneously high temperature, and under the effect of High Temperature High Pressure, goods are able to sintering and densification.Hot isostatic pressing is powder compacting directly, and then the powder mould of packing into uses nitrogen, argon gas to make pressure medium, makes the powder metallurgical technique of powder direct heating pressure sintering moulding, and the pressure of its sintering is 150MPa ~ 200MPa.
Hot pressed sintering is that dry powder is filled in the model, adds the flanging heating from single shaft direction limit again, and pressure is about 70Mpa, a kind of sintering method that moulding and sintering are finished simultaneously.The method has the reduction sintering temperature, shortens sintering time, resists grain growth, obtains that crystal grain is tiny, density is high and the advantage of mechanical, that electric property is good product.Yet its sintering pressure is high, and process and equipment complexity, and production control requires tight, and moulding stock requires high, and energy consumption is large, and production efficiency is lower, the production cost height.
Atmosphere sintering is the method for ceramic body being carried out sintering in passing into the burner hearth of certain gas, and its sintering pressure is 5 ~ 10MPa.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of silicon nitride ceramics, this preparation method can be implemented in sintered silicon nitride ceramic under the normal pressure, utilize silicon nitride ceramics intensity height, good, the high temperature resistant and wear-resisting excellence of compactness of the method preparation, can be widely used in variously to the demanding field of the strength of materials, be particularly useful for making bearing roller.
A kind of preparation method of silicon nitride ceramics comprises the step of batch mixing, ball milling and sintering, and it is characterized in that: described ceramic raw material by mass percentage, is comprised of following component:
Figure BDA00002485298800021
The preferred described ceramic raw material of the preparation method of silicon nitride ceramics of the present invention by mass percentage, is comprised of following component:
Figure BDA00002485298800022
The preparation method of silicon nitride ceramics of the present invention is preferred described ceramic raw material further, by mass percentage, is comprised of following component:
Figure BDA00002485298800023
The preferred described step that is sintered to pressureless sintering of the preparation method of silicon nitride ceramics of the present invention, undertaken by following technique: under the normal pressure, powder is placed mould, speed with 60 ~ 80 ℃/min in sintering oven is warming up to 1600 ℃ ~ 1650 ℃, insulation 0.5h ~ 2h cools to room temperature with the furnace behind the stopped heating.
The preferred described ball milling step of the preparation method of silicon nitride ceramics 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 6h ~ 10h of 300 ~ 360r/min.
The preferred described batch mixing step of the preparation method of silicon nitride ceramics 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 silicon nitride ceramics of the present invention:
A kind of preparation method of silicon nitride 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 6h ~ 10h of 300 ~ 360r/min;
3. sintering: under the normal pressure, powder is placed mould, the speed with 60 ~ 80 ℃/min in sintering oven is warming up to 1600 ℃ ~ 1650 ℃, and insulation 0.5h ~ 2h cools to room temperature with the furnace behind the stopped heating.
The invention has the beneficial effects as follows: the invention provides a kind of preparation method of silicon nitride ceramics, comprise the step of batch mixing, ball milling and sintering, described ceramic raw material by mass percentage, is comprised of following component: β-Si 3N 4: 80% ~ 95%, Al 2O 3: 2% ~ 15%, MgO:1% ~ 12%, Y 2O 3: 1% ~ 12%, ZrO 2: 1% ~ 12%.This preparation method can be implemented in sintered silicon nitride ceramic under the normal pressure, and step is simple, convenient and easy simultaneously.Utilize the silicon nitride ceramics intensity of the method preparation high, good, the high temperature resistant and wear-resisting excellence of compactness, can be widely used in variously to the demanding field of the strength of materials, be 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 200 mesh sieves, described ceramic raw material by mass percentage, is comprised of following component:
Figure BDA00002485298800031
2. ball milling: under the normal temperature, will place ball mill through the powder of batch mixing, in the speed ball milling 8h of 300r/min;
3. sintering: under the normal pressure, powder is placed mould, the speed with 60 ℃/min in sintering oven is warming up to 1600 ℃, and insulation 1h cools to room temperature with the furnace behind the stopped heating.

Claims (7)

1. the preparation method of a silicon nitride 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 FDA00002485298700011
2. method according to claim 1, it is characterized in that: described ceramic raw material by mass percentage, is comprised of following component:
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: under the normal pressure, powder is placed mould, speed with 60 ~ 80 ℃/min in sintering oven is warming up to 1600 ℃ ~ 1650 ℃, insulation 0.5h ~ 2h cools to room temperature with the furnace behind the stopped heating.
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 6h ~ 10h 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 6h ~ 10h of 300 ~ 360r/min;
3. sintering: under the normal pressure, powder is placed mould, the speed with 60 ~ 80 ℃/min in sintering oven is warming up to 1600 ℃ ~ 1650 ℃, and insulation 0.5h ~ 2h cools to room temperature with the furnace behind the stopped heating.
CN 201210499198 2012-11-28 2012-11-28 Preparation method of silicon nitride ceramic Pending CN103030398A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104193343A (en) * 2014-08-25 2014-12-10 南通高欣耐磨科技股份有限公司 Method for preparing silicon nitride ceramic
CN104402484A (en) * 2014-10-29 2015-03-11 安徽省皖捷液压科技有限公司 Special ceramic nozzle with good corrosion resistance and good toughness, and manufacturing method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104193343A (en) * 2014-08-25 2014-12-10 南通高欣耐磨科技股份有限公司 Method for preparing silicon nitride ceramic
CN104402484A (en) * 2014-10-29 2015-03-11 安徽省皖捷液压科技有限公司 Special ceramic nozzle with good corrosion resistance and good toughness, and manufacturing method thereof

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Application publication date: 20130410