CN101602609A - A kind of Fe-Si for preparing 3N 4The method of refractory raw material - Google Patents
A kind of Fe-Si for preparing 3N 4The method of refractory raw material Download PDFInfo
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Abstract
The present invention relates to a kind of Fe-Si of preparation
3N
4The method of refractory raw material belongs to the refractory material preparing technical field.Fe-Si
3N
4Have high temperature resistant, good non-oxidizability and good thermo-chemical stability, belong to a kind of raw material for refractory with gradient sintering function, be mainly used in blast furnace stemming fire-proof material, can also be for the preparation of other heat resistant and wear resistant material.The present invention is take fine iron breeze, silica flour and coke blacking etc. as primary raw material, design by component, under suitable temperature schedule, carry out the carbothermal reduction-nitridation sintering, after the cooling that product is broken and levigate, but Application and preparation is in the high performance Fe-Si of various stemming fire-proof materials
3N
4The refractory raw material powder.The composition phase of the prepared ferro-silicon nitride of the present invention is mainly β-Si
3N
4, α-Si
3N
4, Fe
3Si, Fe and a small amount of Si
2ON
2, Sialon, FeSi and C etc.This preparation Fe-Si that the present invention relates to
3N
4The new method of high-performance refractory material feedstock has the outstanding advantage that cost is low, the preparation process consumed energy is few.
Description
Technical field:
The present invention relates to a kind of Fe-Si of preparation
3N
4The new method of refractory raw material, this Fe-Si
3N
4The powder of refractory raw material is mainly used in the stemming fire-proof material of blast furnace, belongs to the refractory material preparing technical field.
Background technology:
Along with Chinese economic development, increasing to the demand of iron and steel.The iron and steel output of China is zooming trend year by year.The iron and steel output of China in 2007 reaches 48,966 ten thousand tons, accounts for 36.4% of Gross World Product then.Can reach so high output is because the new blast furnace that the investment of domestic iron and steel enterprises newly increased fixed assets is built is produced on the one hand, on the other hand, be that China ironmaking enterprise transforms on original blast furnace foundation, expansion volume and strengthening smelting raising output are produced.No matter be the transformation to old blast furnace, still invest newly-built blast furnace, because the significantly lifting of production capacity, also just require more and more higher to the life-span of blast furnace and the time of tapping a blast furnace.
In recent decades, more and more around the research that how to prolong the life of the blast furnace, blast-furnace technique obtains develop rapidly, is embodied in: high heat size enlarges, by original small furnace (300～1000m
3) generally begin to large blast furnace (2500m
3More than) change; Smelting technique also improves rapidly, and the ironmaking quality increases greatly, and blast furnace can reach high yield and low power consuming; Also than greatly increasing in the past, can extend to more than 15 years the life of the blast furnace.The maintenance and operation of iron notch is depended in the safety operation of the behaviour in service of iron-smelting blast furnace, productivity and stokehold to a great extent.
Iron notch is position important in the iron-smelting blast furnace structure, also is weak position.The elementary operation of iron notch is slagged tap exactly and is tapped a blast furnace.After blast furnace maximizes, the slag notch setting of having removed former blast furnace, so that productivity ratio improves, the routine use that more needs to strengthen blast furnace iron notch is safeguarded by high-temperature hot-air winding-up, oxygen-enriched injection, high-voltage safety operation etc.Safeguard that blast furnace iron notch will accomplish: safeguard normal enough tapping hole degree of depth, iron bicker degree and iron mouth diameter keep normal range (NR), keep iron mouth mud cover intact, control safe slag iron amount etc. in the blast furnace burner hearth well.
Stemming is used to stop up blast furnace iron notch, is important iron-smelting blast furnace one of refractory materials.The stemming that present blast furnace stifled iron notch is used can be divided into hydrous taphole loam and no water stemming two classes.The difference of hydrous taphole loam and anhydrous stemming mainly is the selection of bond.Hydrous taphole loam is as wedding agent with water, and the anhydrous stemming preparation time is to be binding agent with anthracene oil, tar, pitch, resin etc., and same respectively then refractory aggregate, clay, coke powder and pitch reach in proportion that sequencing joins the system of grinding on the pug mill and extrude by mud extruder and forms.
Correspondingly the quality of the used stemming of blast furnace is had higher requirement, stemming turns to functional refractory materials from simple expendable refractory materials of past.In order to satisfy the iron-smelting blast furnace requirement of safe production.Scientific worker both domestic and external and engineers and technicians have carried out many-sided tackling key problem to stemming, as improve raw-material purity to reduce the content of impurity in the stemming; Replace water to mix and stir the stemming material to improve the associativity of stemming with different organic bonds; In stemming, add new functional material with the aggressivity of the anti-slag iron liquation that improves stemming and erosion etc.All these is that the operating environment that improves the stokehold, the labour intensity that alleviates the workman have played positive effect, and the particularly utilization of new functional material is more obvious to the performance that improves stemming.
In order to satisfy the blast furnace tapping hole to the needs of high-quality stemming, in recent years, along with researcher's going deep into stemming research, increasing non-oxidized substance additive is added in the stemming, to strengthening the erosion-resisting characteristics of stemming, to improving the resistance to elevated temperatures of stemming, the prolongation time of tapping a blast furnace has all been played very useful effect.
Domestic and international big-and-middle-sized blast furnace generally adds Fe-Si at present with stemming
3N
4Raw material, because the introducing of metallic iron and silicon nitride, so that add Fe-Si
3N
4Blast furnace mud not only have good corrosion resistance and scour resistance, but also have the gradient sintering function so that the process ratio of tapping outlet is easier to.Facts have proved Fe-Si
3N
4The introducing stemming in after, the stemming performance has increased greatly, Fe-Si
3N
4To become one of very promising big gun refractory material important source material.
At present, domestic and international big-and-middle-sized blast furnace mud Fe-Si
3N
4The raw material its preparation method generally adopts the FeSi75 alloyed powder as the raw material of nitridation reaction, the FeSi75 alloyed powder is placed the nitriding furnace nitrogenize and the product after the nitrogenize is carried out obtaining Fe-Si after the fine powder processing
3N
4Material powder.What also have to adopt is that the FeSi75 alloyed powder is joined in the high temperature nitrogen in the stove continuously by the Flash Smelting Furnace furnace roof, and the flashing combustion nitrogenize generates Fe-Si in high temperature nitrogen
3N
4, the Fe-Si that this reaction forms
3N
4Be loose block, the product after the nitrogenize carries out obtaining Fe-Si after the fine powder processing
3N
4Material powder.But adopt the cost of FeSi75 alloyed powder very high, energy consumption big (smelt the FeSi75 alloy and just consumed a large amount of electric energy), the price height has had a strong impact on Fe-Si
3N
4Material powder applying in most of blast furnace mud.A kind of new cost is lower, the preparation Fe-Si of less energy intensive so develop
3N
4Method have very important energy-saving significance.
Summary of the invention:
Fe-Si
3N
4Have high temperature resistant, good non-oxidizability and good thermo-chemical stability, belong to a kind of raw material for refractory with gradient sintering function, be mainly used in blast furnace stemming fire-proof material, can also be for the preparation of other heat resistant and wear resistant material.The present invention by the component design, carry out the carbothermal reduction-nitridation sintering under suitable temperature schedule, but Application and preparation is in the high performance Fe-Si of various stemming fire-proof materials take fine iron breeze, silica flour and coke blacking etc. as primary raw material
3N
4Refractory raw material.
The present invention relates to a kind of Fe-Si of preparation
3N
4The new method of refractory raw material, it is characterized by: the present invention is take fine iron breeze, silica flour and coke blacking etc. as primary raw material, add the normal temperature bond, ball milling mixes by a certain percentage, the material that ball milling is mixed adds and mixes after adding suitable quantity of water in the batch mixer, then material is shaped to base substrate (or be configured as spheric granules with nodulizer) at make-up machine, also can directly is contained in batch in the saggar or is placed on the fire-resistant supporting plate.Burn till, cool off, pulverize then the technical process such as processing by drying, loading of kiln, carbothermal reduction-nitridation, can prepare Fe-Si
3N
4The powder of refractory raw material.The composition phase of the prepared iron silicon nitride of the present invention is mainly β-Si
3N
4, α-Si
3N
4, Fe
3Si, Fe and a small amount of Si
2ON
2, Sialon, FeSi and C etc.The mass percent of the add-on of described fine iron breeze is 0.1～90.0%%, described silica powder add-on is 0.1～90.0%%, the mass percent of described coke powder add-on is 0.1～90.0%%, and the described add-on that adds wedding agent commonly used is 0.2～15% of total batching quality.
Described fine iron breeze raw material is usually commercially available iron ore raw material, also can replace by other materials that contain ferric oxide and iron with iron phosphorus powder and troilite powder etc.; Require in fine iron breeze or the surrogate that wherein the Fe percentage composition is greater than 50%, median size is less than 0.30mm.
Described silica powder is common commercially available raw mineral materials, can contain SiO with other
2The replacements such as (being commonly called as the silicon ash) of high material such as ultrafine silica powder; Require SiO in silica powder or the surrogate
2Percentage composition is greater than 88%, and median size is less than 0.30mm.
Described coke powder is usually commercially available raw material, also can be with other carbon material as replacements such as the charcoal piece that uses front and back and graphite electrode powder, electric calcined anthracite powder, asphalt powder, petroleum coke powder, gac, coal dusts.Require the C percentage composition greater than 90% in coke blacking or the substitute, average grain diameter is less than 0.30mm.Add the normal temperature bond in the described preparation process and adopt industrial dextrin solution or the refractory materials such as calcium lignosulfonate solution or poly-vinyl alcohol solution or Ludox or pitch or tar or resin bond commonly used.
Dry good base substrate (or the spheroidal particle after being shaped) places thermal kiln furnace loading of kiln, heating and carbothermal reduction-nitridation to burn till, and thermal kiln furnace can be the nitriding furnace, microwave nitriding furnace, induction nitriding furnace, tubular type nitriding furnace, vertical nitriding furnace of nitriding electric furnace, Ma Fushi combustion gas kiln or coal-fired kiln or oil-firing kiln etc.Base substrate places the nitrogen kiln to adopt and buries the carbon granule protection.Burn till through the carbothermal reduction-nitridation in the temperature range of normal temperature to 1700 ℃, programming rate does not have particular requirement, can be incubated respectively certain hour under corresponding temperature, and insulation is 10 minutes～50 hours under the highest roasting; Take out base substrate or spheric granules after naturally cooling to room temperature, through pulverizing the technical process of processing, can prepare Fe-Si as required
3N
4The powder of the different fineness of refractory raw material.
The composition phase of the prepared ferro-silicon nitride of the present invention is mainly β-Si
3N
4, α-Si
3N
4, Fe
3Si, Fe and a small amount of Si
2ON
2, Sialon, FeSi and C etc.The Fe-Si that the present invention is prepared
3N
4, wherein the nitrogen content of product, iron content and silicone content can be adjusted by the proportioning of control raw material.The chemical constitution of typical ferro-silicon nitride is: w (Si) 〉=48%, w (N) 〉=30%, w (Fe)=11%～19%, w (O)≤0.5%, w (C)≤6.5%.
This preparation Fe-Si that the present invention relates to
3N
4The new method of refractory raw material has the outstanding advantage that cost is low, the preparation process consumed energy is few.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further:
In the preparation process of the present invention when batching each raw material add-on and specification of quality as follows: fine iron breeze (or iron filings powder, steel rolling iron scale, troilite powder etc. other contain the material of ferric oxide and iron) requires wherein the Fe percentage composition greater than 50%, median size is less than 0.30mm, and add-on is 0.1～90.0%; Silica powder (or surrogate) requires wherein SiO
2Percentage composition is greater than 88%, and median size is less than 0.30mm, and add-on is 0.1～90.0%; Coke powder (or the charcoal piece before and after using and graphite electrode powder, electric calcined anthracite powder, asphalt powder, petroleum coke powder, gac, coal dust etc.) requires wherein that the C percentage composition is greater than 90%, and median size is less than 0.30mm, and add-on is 0.1～90.0%; Wedding agent requires to adopt industrial dextrin solution or refractory materialss such as calcium lignosulfonate solution or polyvinyl alcohol solution or silicon sol or pitch or tar or resin wedding agent commonly used, and the add-on that adds wedding agent commonly used is 0.2～15% of total batching quality.
This preparation Fe-Si that the present invention proposes
3N
4The new method of refractory raw material, its principal character is: described method is with after various raw materials pulverizing or being ground to desired particle size, is preparing burden in described ratio, joins ball mill and mixes; The material that ball milling is mixed adds and mixes after adding suitable quantity of water in the batch mixer, then material is shaped to base substrate (or be configured as spheric granules with nodulizer) at make-up machine.Moulding is also dry, dry good adobe (or the spheric granules after being shaped) places thermal kiln furnace loading of kiln, heating and carbothermal reduction-nitridation to burn till, and thermal kiln furnace can be the nitriding furnace, microwave nitriding furnace, induction nitriding furnace, tubular type nitriding furnace, vertical nitriding furnace of nitriding electric furnace, Ma Fushi gas-combustion kiln or coal-fired kiln or oil-firing kiln etc.Base substrate places the nitrogen kiln to adopt and buries the carbon granule protection.Burn till through the carbothermal reduction-nitridation in the temperature range of normal temperature to 1700 ℃, programming rate does not have particular requirement, can be incubated respectively certain hour under corresponding temperature, and insulation is 10 minutes～50 hours under the highest roasting; Take out base substrate or spheric granules after naturally cooling to room temperature, through pulverizing the technical process of processing, can prepare Fe-Si as required
3N
4The powder of the different fineness of refractory raw material.This preparation Fe-Si that the present invention relates to
3N
4The new method of refractory raw material has the outstanding advantage that cost is low, the preparation process consumed energy is few.
A kind of Fe-Si
3N
4Preparation technology's flow process of high-performance refractory material feedstock is:
Raw material → batching → batch mixing → moulding → drying → nitrogenize is burnt till → is checked
Embodiment 1
Raw material and proportioning:
The fine iron breeze add-on is 12wt.%, and wherein the Fe percentage composition is 65.0%, and median size is less than 0.088mm; The silica powder add-on is 60wt.%, wherein SiO
2Percentage composition is 98.0%, and median size is less than 0.088mm; The coke powder add-on is 28wt.%, and wherein the C percentage composition is 98.0%, and median size is less than 0.088mm.The add-on that adds wedding agent (silicon sol) is 2～3% of total batching quality.
Batching, batch mixing:
At first with various raw materials according to the above-mentioned ratio mixer of packing into, dry grinding 10h, the raw material thorough mixing is even, and granularity is less than 0.088mm, the aperture sieve screen over-size is less than 2.0wt.%.
Be shaped or granulation:
The material that ball milling is mixed adds and mixes after adding suitable quantity of water in the batch mixer, then material is shaped to base substrate (or be configured as spheric granules with nodulizer) at make-up machine.
Dry:
Sample after the moulding is seasoning 12h at room temperature, then in dry kiln in 100 ℃ of dry 4h, make water ratio≤3.0% of sample.
Carbothermal reduction-nitridation burns till:
The sample that drying is good is packed into, and carbothermal reduction-nitridation burns till 1550 ℃ of firing temperatures in the nitriding electric furnace.Calcining system is: 1500 ℃ of insulation 1h, 1550 ℃ are incubated 8 hours.
Check:
Sample after burning till is carried out the composition check on request.
The main chemical constitution of resulting product is as follows: w (Si) 〉=51.0%, w (N) 〉=34.0%, w (Fe) 〉=14.6%, w (O)≤0.5%, w (C)≤0.5%.
Embodiment 2
Raw material and proportioning:
Fine iron breeze (rhombohedral iron ore) add-on is 6wt.%, and wherein the Fe percentage composition is 59%, and median size is less than 0.088mm; Silicon ash add-on is 65wt.%, wherein SiO
2Percentage composition is 93.0%, and median size is less than 0.074mm; The petroleum coke powder add-on is 29wt.%, and wherein the C percentage composition is 90.0%, and median size is less than 0.088mm.The add-on that adds wedding agent (calcium lignin sulphonate) is 2～3% of total batching quality.
Batching, batch mixing:
At first with various raw materials according to the above-mentioned ratio mixer of packing into, dry grinding 5h, the raw material thorough mixing is even, and granularity is less than 0.088mm, the aperture sieve screen over-size is less than 2.0wt.%.
Be shaped or balling-up:
The material that ball milling is mixed adds and mixes after adding suitable quantity of water in the batch mixer, then material is molded into base substrate (or be configured as spheric granules with nodulizer) at make-up machine.
Dry:
Sample after the moulding is seasoning 10h at room temperature, then in dry kiln in 120 ℃ of dry 6h, make water ratio≤3.0% of sample.
Carbothermal reduction-nitridation burns till:
The sample that drying is the good nitrogen kiln roasting of packing into, 1580 ℃ of firing temperatures.Calcining system is: 1500 ℃ of insulation 1h, 1580 ℃ are incubated 7 hours.
Check:
Sample after burning till is carried out the composition check on request.
The main chemical constitution of resulting product is as follows: w (Si) 〉=55.0%, w (N) 〉=37.0%, w (Fe) 〉=7.0%, w (O)≤0.5%, w (C)≤0.5%.
Embodiment 3
Raw material and proportioning:
Steel rolling iron scale (steel scale of steel rolling) add-on is 24wt.%, and wherein the Fe percentage composition is 67%, and median size is less than 0.088mm; The silica powder add-on is 50wt.%, wherein SiO
2Percentage composition is 98.0%, and median size is less than 0.088mm; The graphite electrode powder add-on is 26wt.%, and wherein the C percentage composition is 98.0%, and median size is less than 0.074mm.The add-on that adds wedding agent (industrial dextrin) is 2～3% of total batching quality.
Batching, batch mixing:
At first with various raw materials according to the above-mentioned ratio mixer of packing into, dry grinding 10h, the raw material thorough mixing is even, and granularity is less than 0.074mm, the aperture sieve screen over-size is less than 2.0wt.%.
Moulding:
The material that ball milling is mixed adds and mixes after adding suitable quantity of water in the batch mixer, then material is molded into base substrate (or be configured as spheric granules with nodulizer) at make-up machine.
Dry:
Sample after the moulding is seasoning 12h at room temperature, then in dry kiln in 110 ℃ of dry 10h, make water ratio≤3.0% of sample.
Carbothermal reduction-nitridation burns till:
The sample that drying is the good nitrogen kiln roasting of packing into, 1530 ℃ of firing temperatures.Calcining system is: 1500 ℃ of insulation 1h, 1530 ℃ are incubated 15 hours.
Check:
Sample after burning till is carried out the composition check on request.
The main chemical constitution of resulting product is as follows: w (Si) 〉=42.0%, w (N) 〉=28.0%, w (Fe) 〉=29.7%, w (O)≤0.5%, w (C)≤0.5%.
Claims (6)
1, the present invention relates to a kind of Fe-Si of preparation
3N
4The new method of refractory raw material, this Fe-Si
3N
4The powder of refractory raw material is mainly used in the stemming fire-proof material of blast furnace.It is characterized by: the present invention is take fine iron breeze, silica flour and coke blacking etc. as primary raw material; add the normal temperature bond; mix by a certain percentage; be shaped to then spheric granules or be compressed to base substrate (also can directly be contained in batch in the saggar or be placed on the fire-resistant supporting plate) drying, loading of kiln, carbothermal reduction-nitridation and burn till, cool off, pulverize the technical process such as processing, can prepare Fe-Si
3N
4The powder of refractory raw material.The composition phase of the prepared iron silicon nitride of the present invention is mainly β-Si
3N
4, α-Si
3N
4, Fe
3Si, Fe and a small amount of Si
2ON
2, Sialon, FeSi and C etc.The mass percent of the add-on of described fine iron breeze is 0.1～90.0%, described silica powder add-on is 0.1～90.0%, the mass percent of described coke powder add-on is 0.1～90.0%, and the described add-on that adds wedding agent commonly used is 0.2～15% of total batching quality.
2, a kind of Fe-Si for preparing according to claim 1
3N
4The method of refractory raw material is characterized in that: described fine iron breeze raw material is common commercially available iron ore raw material, also can replace by other materials that contain iron oxide and iron with iron filings powder, steel rolling iron scale (steel scale of steel rolling) and troilite powder etc.; Require in fine iron breeze or the substitute that wherein the Fe percentage composition is greater than 50%, average grain diameter is less than 0.30mm.
3, a kind of Fe-Si for preparing according to claim 1
3N
4The method of refractory raw material is characterized in that: described silica flour is common commercially available raw mineral materials, can contain SiO with other
2The replacements such as high material such as ultrafine silica powder (being commonly called as the silicon ash); Require SiO in silica flour or the substitute
2Percentage composition is greater than 88%, and average grain diameter is less than 0.30mm.
4, a kind of Fe-Si for preparing according to claim 1
3N
4The method of refractory raw material is characterized in that: described coke blacking is common commercially available raw material, also can be with other carbon material such as replacements such as the charcoal piece that uses front and back and graphite electrode powder, electric calcined anthracite powder, asphalt powder, petroleum coke powder, active carbon, coal dusts.Require the C percentage composition greater than 90% in coke blacking or the substitute, average grain diameter is less than 0.30mm.
5, a kind of Fe-Si for preparing according to claim 1
3N
4The method of refractory raw material is characterized in that: add the normal temperature bond in the described preparation process and adopt industrial dextrin solution or the refractory materials such as calcium lignosulfonate solution or poly-vinyl alcohol solution or Ludox or pitch or tar or resin bond commonly used.
6, a kind of Fe-Si for preparing according to claim 1
3N
4The method of refractory raw material, it is characterized in that: dry good base substrate (or the spheric granules after being shaped) places thermal kiln furnace loading of kiln, heating and carbothermal reduction-nitridation to burn till, and thermal kiln furnace can be the nitriding furnace, microwave nitriding furnace, induction nitriding furnace, tubular type nitriding furnace, vertical nitriding furnace of nitriding electric furnace, Ma Fushi gas-combustion kiln or coal-fired kiln or oil-firing kiln etc.Base substrate places the nitrogen kiln to adopt and buries the carbon granule protection.Burn till through the carbothermal reduction-nitridation in the temperature range of normal temperature to 1700 ℃, programming rate does not have particular requirement, can be incubated respectively certain hour under corresponding temperature, and insulation is 10 minutes～50 hours under the highest roasting; Take out base substrate or spheric granules after naturally cooling to room temperature, through pulverizing the technical process of processing, can prepare Fe-Si as required
3N
4The powder of the different fineness of refractory raw material.This preparation Fe-Si that the present invention relates to
3N
4The new method of refractory raw material has the outstanding advantage that cost is low, the preparation process consumed energy is few.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830714A (en) * | 2010-04-27 | 2010-09-15 | 北京通达耐火技术股份有限公司 | Alumina-silicon nitride iron compound abrasive brick for large-size cement kiln and manufacture method thereof |
| CN102583277A (en) * | 2012-02-16 | 2012-07-18 | 中国地质大学（北京） | Method for manufacturing silicon nitride in ribbon-like fiber shape |
| 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 |
| CN102633508A (en) * | 2012-02-22 | 2012-08-15 | 北京首钢耐材炉料有限公司 | Method for preparing ferrosilicon nitride powder |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1226425C (en) * | 2003-11-24 | 2005-11-09 | 北京科技大学 | Al*O*-SiC-C system waterless taphole mix containing ferrosilicon nitride |
| CN1562884A (en) * | 2004-04-16 | 2005-01-12 | 清华大学 | Fe-Sialon multiphase material of shock resistant and wearproof in high temperature and preparation method |
| CN1300341C (en) * | 2005-07-19 | 2007-02-14 | 中国地质大学（北京） | Tamping plug for blast furnace spout and its preparation method |
| CN100341821C (en) * | 2006-05-19 | 2007-10-10 | 王恩余 | Blast furnace taphole Al2O3-SiC-C system no-water cannon mire |
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2009
- 2009-07-24 CN CN2009100890498A patent/CN101602609B/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830714A (en) * | 2010-04-27 | 2010-09-15 | 北京通达耐火技术股份有限公司 | Alumina-silicon nitride iron compound abrasive brick for large-size cement kiln and manufacture method thereof |
| CN102583277A (en) * | 2012-02-16 | 2012-07-18 | 中国地质大学（北京） | Method for manufacturing silicon nitride in ribbon-like fiber shape |
| CN102633508A (en) * | 2012-02-22 | 2012-08-15 | 北京首钢耐材炉料有限公司 | Method for preparing ferrosilicon nitride powder |
| 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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|---|---|
| CN101602609B (en) | 2012-07-25 |
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