CN104860691B - The preparation method of high strength silicon nitride ferrum kiln furnitures - Google Patents

The preparation method of high strength silicon nitride ferrum kiln furnitures Download PDF

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CN104860691B
CN104860691B CN201510238615.2A CN201510238615A CN104860691B CN 104860691 B CN104860691 B CN 104860691B CN 201510238615 A CN201510238615 A CN 201510238615A CN 104860691 B CN104860691 B CN 104860691B
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kiln furnitures
silicon nitride
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preparation
ferrum
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CN104860691A (en
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李勇
秦海霞
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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Abstract

The invention belongs to high grade refractory field, relate to ceramic material and the preparation method of magnetic material sintering process auxiliary material, it is specifically related to the preparation method of high strength silicon nitride ferrum kiln furnitures, with ferrum silicon 75 alloy powder as raw material, nitridation burning in flash nitriding furnace, obtain a kind of cellular loose block ferro-silicon nitride original preform, through cutting, resin impregnating, dry, polish, ferro-silicon nitride kiln furnitures finished product can be obtained, and kiln furnitures finished product cold crushing strength is more than 90MPa.The invention has the beneficial effects as follows: this preparation method breaks through traditional kiln furnitures preparation method, kiln furnitures are without molding, without high temperature sintering, production technology is simple, use the ferro-silicon nitride kiln furnitures prepared of the method can Reusability, access times are more than 200 times, save the energy and production cost dramatically, it is simple to industrialization promotion and application.

Description

The preparation method of high strength silicon nitride ferrum kiln furnitures
Technical field
The invention belongs to high grade refractory field, relate to ceramic material and the preparation method of magnetic material sintering process auxiliary material, be specifically related to the preparation method of high strength silicon nitride ferrum kiln furnitures.
Background technology
Kiln furnitures are a kind of at a kind of important auxiliary material of ceramic material and magnetic material, play support and protective effect in the sintering process of material.On the one hand, kiln furnitures burnt product to be protected so that it is pollute from combustion gas, dust etc. and corrode;On the other hand, kiln furnitures play Sheng and support effect.Therefore, kiln furnitures should bear the weight of burnt product, does not produces chemical reaction with goods and brings pollution, it is desirable to kiln furnitures have a following key property: (1) high fire resistance, good heat stability and chemical stability;(2) higher room temperature is pressure and crushing strength under high temperature;(3) good heat conductivity, relatively low heat accumulation;(4) outward appearance is regular, and size is accurate.
Along with the development of ceramic industry, higher requirement is proposed for kiln furnitures, burnt till converted to flaming open setting firing mode by the employing saggar that burns till of conventional articles;Kiln furniture material towards high intensity, the thin body of wall is light, be amenable to quick high-temp burns till, has the direction of higher regularity and degree of accuracy to develop.
At present both at home and abroad kiln furnitures can be largely classified into three major controls: magnalium silicon system kiln furnitures, carborundum system kiln furnitures and novel kiln furnitures.At present, in the kiln furnitures of domestic use, High-Alumina kiln furnitures intensity is low, poor heat stability, and service life is short;Mullite kiln furnitures cost is high, is unfavorable for large-scale industrialization promotion;Silicon carbide kiln furniture is owing to containing Fe in internal sources2O3, performance is affected, and molding needs elevated pressures, general device to be difficult to reach, and production cost is higher.Domestic kiln furnitures level of development is compared with abroad, and the most certain gap, kiln furnitures degraded performance seriously hinders renewal and the development of ceramic industry.Therefore, selecting the raw material of high-quality low-cost, use simple technique, prepare function admirable stable, regularity and the high kiln furniture material of precision, and large-scale industrialization promotion, to alleviate the situation that SiC kiln furnitures are difficult to use in a large number, be the direction of domestic kiln furnitures development.
High strength silicon nitride ferrum kiln furnitures of the present invention, have higher intensity, can meet the demand of the support of kiln furnitures, load-bearing;The porosity is higher, is a kind of porous ceramics, has preferable thermal shock resistance;Ferro-silicon nitride dominant is silicon nitride mutually, uses temperature higher;Ferro-silicon nitride will not produce melt and gas phase under the conditions of using, and has preferable chemical stability;Only needing to produce kiln furnitures by cutting ferro-silicon nitride original preform, processing technique is simple, and cost is extremely low, it is simple to industrialization promotion and large-scale application;Ferro-silicon nitride is a kind of cellular porous pottery, it is simple to cutting, meets kiln furnitures for regularity and the requirement of degree of accuracy.High strength silicon nitride ferrum kiln furnitures the most of the present invention, can meet ceramic industry under the new situation for kiln furniture material towards high intensity, the thin body of wall is light, be amenable to the demand that quick high-temp burns till, has the direction of higher regularity and degree of accuracy to develop.
Summary of the invention
Not enough for prior art, the invention provides the preparation method of a kind of high strength silicon nitride ferrum kiln furnitures that can be used for ceramic material and magnetic material firing process.
The technical scheme is that the preparation method of high strength silicon nitride ferrum kiln furnitures, the method specifically includes following steps:
Step 1. prepares block: with ferrum silicon 75 alloy powder as raw material, nitridation burning in flash nitriding furnace, obtains a kind of cellular loose block ferro-silicon nitride original preform, and the thing of described ferro-silicon nitride original preform is Fe mutually3Si and Si3N4, Fe3Si mass fraction is 20%-30%, and silicon nitride mass fraction is 70%-80%, and apparent porosity is 20%-40%;Bulk density is 2.4-2.7g/cm3
Step 2. is cut: ferro-silicon nitride base substrate step 1 obtained cuts according to kiln furnitures production requirement, it is thus achieved that required form kiln furnitures;
Step 2 is prepared kiln furnitures and puts in vacuum tank by step 3., is evacuated to 10-1~10-3MPa, the phenolic resin of carbon yield >=50% is heated to 150-250 DEG C, phenolic resin after heating is put in the device connected with vacuum tank, open the valve between vacuum tank and device, after making phenolic resin be full of equipped with the vacuum tank of kiln furnitures, it is forced into 5 ~ 10MPa, makes ferro-silicon nitride kiln furnitures impregnate 5-10 h in phenolic resin;
Step 4. is dried: will put into drying baker by kiln furnitures after step 3 processes, and is 200 DEG C in temperature, dries 20-24 h;
Ferro-silicon nitride kiln furnitures after step 5. will be dried are polishing to smooth, can obtain ferro-silicon nitride kiln furnitures finished product, and kiln furnitures finished product cold crushing strength is more than 90MPa.
Further, described vacuum tank can bear the pressure of more than 15MPa.
Adding phenolic resin in the present invention, phenolic resin at high temperature decomposes, and leaves a certain amount of carbon residue in ferro-silicon nitride kiln furnitures.Under high temperature, carbon reacts with the silicon nitride in ferro-silicon nitride, forms carborundum, form silicon nitride bonded silicon silicon nitride structure, have more preferable high-temperature behavior, can improve structural stability during the use under high temperature harsh conditions.Adding phenolic resin and can close the part holes in ferro-silicon nitride kiln furnitures, reduction rate is up to the 30% of original porosity.The carbon residue stayed after the resin decomposition on ferro-silicon nitride kiln furnitures surface, can reduce the angle of wetting between sample, makes product will not react with kiln furnitures.
The invention has the beneficial effects as follows: owing to using technique scheme, the method can be cut into different size can be obtained high strength silicon nitride ferrum kiln furnitures by the demand of actual production variety classes kiln furnitures.And preparation method breaks through traditional kiln furnitures preparation method, kiln furnitures are without molding, without heat treatment, high temperature sintering, and production technology is simple, use the ferro-silicon nitride kiln furnitures prepared by the method can Reusability, access times are more than 200 times, save the energy and production cost dramatically.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme is described further.
The preparation method of high strength silicon nitride ferrum kiln furnitures of the present invention, the method specifically includes following steps:
Step 1. prepares block: with ferrum silicon 75 alloy powder as raw material, nitridation burning in flash nitriding furnace, obtains a kind of cellular loose block ferro-silicon nitride original preform, and the thing of described ferro-silicon nitride original preform is Fe mutually3Si and Si3N4, Fe3Si mass fraction is 20%-30%, and silicon nitride mass fraction is 70%-80%, and apparent porosity is 20%-40%;Bulk density is 2.4-2.7g/cm3
Step 2. is cut: ferro-silicon nitride base substrate step 1 obtained cuts according to kiln furnitures production requirement, it is thus achieved that required form kiln furnitures;
Step 2 is prepared kiln furnitures and puts in vacuum tank by step 3., is evacuated to 10-1~10-3MPa, the phenolic resin of carbon yield >=50% is heated to 150-250 DEG C, phenolic resin after heating is put in the device connected with vacuum tank, open the valve between vacuum tank and device, after making phenolic resin be full of equipped with the vacuum tank of kiln furnitures, it is forced into 5 ~ 10MPa, makes ferro-silicon nitride kiln furnitures impregnate 5-10 h in phenolic resin;
Step 4. is dried: will put into drying baker by kiln furnitures after step 3 processes, and is 200 DEG C in temperature, dries 20-24 h;
Ferro-silicon nitride kiln furnitures after step 5. will be dried are polishing to smooth, can obtain ferro-silicon nitride kiln furnitures finished product, and kiln furnitures finished product cold crushing strength is more than 90MPa.
Embodiment 1:
The preparation method of high strength silicon nitride ferrum kiln furnitures, the method specifically includes following steps:
Step 1. prepares block: with ferrum silicon 75 alloy powder as raw material, nitridation burning in flash nitriding furnace, obtains a kind of cellular loose block ferro-silicon nitride original preform, and the thing of described ferro-silicon nitride original preform is Fe mutually3Si and Si3N4, Fe3Si mass fraction is 25%, and silicon nitride mass fraction is 75%, and apparent porosity is 30%;Bulk density is 2.5g/cm3
Step 2. is cut: ferro-silicon nitride base substrate step 1 obtained cuts according to kiln furnitures production requirement, it is thus achieved that required form kiln furnitures;
Step 2 is prepared kiln furnitures and puts in vacuum tank by step 3., is evacuated to 10-2MPa, the phenolic resin of carbon yield >=50% is heated to 250 DEG C, phenolic resin after heating is put in the device connected with vacuum tank, open the valve between vacuum tank and device, after making phenolic resin be full of equipped with kiln furnitures vacuum tank, it is forced into 7.5MPa, makes ferro-silicon nitride kiln furnitures impregnate in phenolic resin 45 minutes;
Step 4. is dried: will put into drying baker by kiln furnitures after step 3 processes, and be 200 DEG C in temperature, and dry 24 h;
Ferro-silicon nitride kiln furnitures after step 5. will be dried are polishing to smooth, can obtain ferro-silicon nitride kiln furnitures finished product, and kiln furnitures finished product cold crushing strength is more than 90MPa.
Embodiment 2:
The preparation method of high strength silicon nitride ferrum kiln furnitures, the method specifically includes following steps:
Step 1. prepares block: with ferrum silicon 75 alloy powder as raw material, nitridation burning in flash nitriding furnace, obtains a kind of cellular loose block ferro-silicon nitride original preform, and the thing of described ferro-silicon nitride original preform is Fe mutually3Si and Si3N4, Fe3Si mass fraction is 30%, and silicon nitride mass fraction is 70%, and apparent porosity is 40%;Bulk density is 2.7g/cm3
Step 2. is cut: ferro-silicon nitride base substrate step 1 obtained cuts according to kiln furnitures production requirement, it is thus achieved that required form kiln furnitures;
Step 2 is prepared kiln furnitures and puts in vacuum tank by step 3., is evacuated to 10-3MPa, the phenolic resin of carbon yield >=50% is heated to 200 DEG C, phenolic resin after heating is put in the device connected with vacuum tank, open the valve between vacuum tank and device, after phenolic resin is full of equipped with kiln furnitures vacuum tank, it is forced into 10MPa, makes ferro-silicon nitride kiln furnitures impregnate 1 h in phenolic resin;
Step 4. is dried: will put into drying baker by kiln furnitures after step 3 processes, and be 200 DEG C in temperature, and dry 22 h;
Ferro-silicon nitride kiln furnitures after step 5. will be dried are polishing to smooth, can obtain ferro-silicon nitride kiln furnitures finished product, and kiln furnitures finished product cold crushing strength is more than 90MPa.
Embodiment 3:
The preparation method of high strength silicon nitride ferrum kiln furnitures, the method specifically includes following steps:
Step 1. prepares block: with ferrum silicon 75 alloy powder as raw material, nitridation burning in flash nitriding furnace, obtains a kind of cellular loose block ferro-silicon nitride original preform, and the thing of described ferro-silicon nitride original preform is Fe mutually3Si and Si3N4, Fe3Si mass fraction is 20%, and silicon nitride mass fraction is 80%, and apparent porosity is 25%;Bulk density is 2.4cm3
Step 2. is cut: ferro-silicon nitride base substrate step 1 obtained cuts according to kiln furnitures production requirement, it is thus achieved that required form kiln furnitures;
Step 2 is prepared kiln furnitures and puts in vacuum tank by step 3., is evacuated to 10-1MPa, the phenolic resin of carbon yield >=50% is heated to 150 DEG C, phenolic resin after heating is put in the device connected with vacuum tank, open the valve between vacuum tank and device, after phenolic resin is full of equipped with kiln furnitures vacuum tank, it is forced into 5MPa, makes ferro-silicon nitride kiln furnitures impregnate 0.5 h in phenolic resin;
Step 4. is dried: will put into drying baker by kiln furnitures after step 3 processes, and is 200 DEG C in temperature, dries 20h;
Ferro-silicon nitride kiln furnitures after step 5. will be dried are polishing to smooth, can obtain ferro-silicon nitride kiln furnitures finished product, and kiln furnitures finished product cold crushing strength is more than 90MPa.

Claims (2)

1. the preparation method of high strength silicon nitride ferrum kiln furnitures, it is characterised in that the method specifically includes following steps:
Step 1. prepares block: with ferrum silicon 75 alloy powder as raw material, nitridation burning in flash nitriding furnace, obtains a kind of cellular loose block ferro-silicon nitride original preform, and the thing of described ferro-silicon nitride original preform is Fe mutually3Si and Si3N4, Fe3Si mass fraction is 20%-30%, and silicon nitride mass fraction is 70%-80%, and apparent porosity is 20%-40%;Bulk density is 2.4-2.7g/cm3
Step 2. is cut: ferro-silicon nitride original preform step 1 obtained cuts according to kiln furnitures production requirement, it is thus achieved that required form kiln furnitures;
Step 2 is prepared kiln furnitures and puts in vacuum tank by step 3., is evacuated to 10-1-10-3MPa, the phenolic resin of carbon yield >=50% is heated to 150-250 DEG C, phenolic resin after heating is put in the device connected with vacuum tank, open the valve between vacuum tank and device, after making phenolic resin be full of equipped with the vacuum tank of kiln furnitures, it is forced into 5 ~ 10MPa, makes ferro-silicon nitride kiln furnitures impregnate 5-10 h in phenolic resin;
Step 4. is dried: will put into drying baker by kiln furnitures after step 3 processes, and is 200 DEG C in temperature, dries 20-24 h;
Ferro-silicon nitride kiln furnitures after step 5. will be dried are polishing to smooth, can obtain ferro-silicon nitride kiln furnitures finished product, and kiln furnitures finished product cold crushing strength is more than 90MPa.
Method the most according to claim 1, it is characterised in that described vacuum tank can bear the pressure of more than 15MPa.
CN201510238615.2A 2015-05-12 2015-05-12 The preparation method of high strength silicon nitride ferrum kiln furnitures Active CN104860691B (en)

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CN106862574B (en) * 2017-01-05 2019-04-12 南昌大学 A kind of method of high temeperature chemistry treatment process preparation sheet FeSiN alloy powder
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CN102603328A (en) * 2012-03-22 2012-07-25 大连工业大学 Fe-Si3N4-SiC complex phase refractory material as well as preparation and application thereof
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CN103304245B (en) * 2013-02-28 2014-11-19 北京科技大学 Unfired ferro silicon nitride-alumina composite carbon-free sliding plate and preparation method thereof
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