CN100358799C - Method for synthesizing ferro-silicon nitride by microwave - Google Patents
Method for synthesizing ferro-silicon nitride by microwave Download PDFInfo
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- CN100358799C CN100358799C CNB2005100324389A CN200510032438A CN100358799C CN 100358799 C CN100358799 C CN 100358799C CN B2005100324389 A CNB2005100324389 A CN B2005100324389A CN 200510032438 A CN200510032438 A CN 200510032438A CN 100358799 C CN100358799 C CN 100358799C
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Abstract
The present invention provides a silicon iron nitride microwave-synthesizing method, which uses silicon iron as a raw material for microwave synthesis. Silicon iron ore is ground into manganese powder with the particle size smaller than 0.5mm, the silicon iron powder is placed into a microwave synthesis reaction cavity, an additive agent containing ammonium with a raw material weight ratio of 5% is added in, and the mixture is homogeneously mixed. Nitrogen gas is led in to carry out microwave synthesis for 0.5-3 h under the conditions that the microwave frequency is from 300 MHz to 300GHz, the pressure is from 0.1 to 0.12MPa and the synthesis temperature is from 800 to 1800 DEG C, and the obtained synthetics are cooled to obtain finished products of silicon iron nitride. The present invention is different from the traditional convection, conduction or radiation heating mode. Special wave bands of the microwave and the basic structure of a material are coupled to produce heat to heat in the mode that the material is heated integrally by the medium loss of the material, and the present invention has the advantages of low synthesis temperature, short synthesis time, low energy consumption, etc.
Description
Technical field
The present invention relates to a kind of preparation method of ceramic ferro-silicon nitride.
Background technology
Ferro-silicon nitride (Fe-Si
3N
4) in essential substance be silicon nitride, as structured material and oxidation-resistant material, can improve the hot strength and the oxidation-resistance of silicon carbide refractory material.Mix with other materials, can make the refractory materials of anti-molten metal excellent property.As make coating casting thing any surface finish is blazed, the life-span prolongs.Because the nitrogenous rate height of ferro-silicon nitride can be again that various nitrogenous corrosion resistant alloy material additives are preferred.In addition, ferro-silicon nitride also is applied in materials such as high-temperature structural material, high temperature appliance material, humidifying appliance material.
And so far, the preparation of ferro-silicon nitride is still very traditional, i.e. the long-time nitrogenize in high temperature nitrogen with ferrosilicon powder and silica flour.The weak point of traditional method is that mainly nitridation time is long, and the nitrogen content of product is on the low side.Unit such as Shanghai Silicate Inst., Chinese Academy of Sciences has designed a kind of preparation method of self propagating high temperature synthesizing silicon nitride iron powder for this reason.Requirement is synthesized under 1400 ℃ of high temperature in high pressure vessel.Experts such as the grandson Jia Lin of University of Science ﹠ Technology, Beijing have designed the preparation method of a kind of low-pressure combustion synthesizing silicon nitride or ferro-silicon nitride, require size range 0.01～0.075mm, nitrogen pressure 0.01～3MPa, and temperature is between 900～1850 ℃.
Summary of the invention
The technical problem to be solved in the present invention is, at the defective that prior art exists, proposes a kind of synthetic method of new ferro-silicon nitride, adopts this method, can be in lower temperature, short time, and synthesizing silicon nitride iron under lower nitrogen pressure.Simultaneously, the present invention is by improving technology, and having overcome ordinary method needs the more interpolation thinner and the problem of crystal seed, has improved efficient.
Technical solution of the present invention is, the microwave synthesis method of described ferro-silicon nitride, be that to be that raw material carries out microwave synthetic with the ferrosilicon, its technical characterstic is, described raw material ferrosilicon is the ferrosilicon powder that sieves and form after grinding with conventional Ginding process, granularity is less than 0.5mm, the gained ferrosilicon powder is inserted in the microwave building-up reactions cavity, and interpolation contains ammonium additive, uniform mixing, the microwave frequency span is 300MHz～300GHz, pressure 0.1～0.12MPa, 800～1800 ℃ of synthesis temperatures, it is synthetic that feeding nitrogen carries out microwave, generated time 0.5～3 hour, the cooling of gained synthetics is the finished product ferro-silicon nitride.
Principle of work of the present invention is: utilize micro-wave energy to be converted into the heat energy of material, pass to nitrogen with a kind of " mode of body heating " whole even heating to certain temperature, be incubated 0.5～3 hour, realize synthetic.
The invention has the beneficial effects as follows that microwave is synthetic to be to utilize microwave heating that material is synthesized, it is with traditional type of heating difference.Traditional heating is to rely on heating element that heat energy is passed to heated material by convection current, conduction or radiation mode to reach a certain temperature, and heat transmits from outside to inside, and generated time is long, the energy consumption height; And microwave synthetic be utilize special wave band that microwave has and material basic structure coupling and generation heat, the dielectric loss of material makes a kind of type of heating of its material monolithic heating, thereby a series of advantages such as it is low to have a synthesis temperature, and generated time is short, and energy consumption is low.So the efficiency of microwave heating height than traditional method power saving 30～70%, greatly reduce production cost, and industrial microwave oven is simple in structure, automatic operating is easy to safeguard.
Embodiment
Embodiment 1, adopts 100kg 75# ferrosilicon ore (FeSi75) to make raw material, and ordinary method is made powder, through sieving, granularity 0.05mm adds ammonium bicarbonate additive 5kg, uniform mixing places that to carry out microwave in the microwave building-up reactions cavity synthetic, and microwave frequency is 2450MHz.Feed nitrogen, pressure is 0.12MPa, and 1250 ℃ of synthesis temperatures, generated time were controlled at 2 hours, and the cooling of gained synthetics is the ferro-silicon nitride finished product.After measured, it is nitrogenous 26.41% to make ferro-silicon nitride, and XRD analysis result is α-Si
3N
4, β-Si
3N
4, FeSi.
Embodiment 2, adopt 20t75# ferrosilicon ore (FeSi75) to make raw material, and ordinary method is made powder, through sieving, granularity 0.074mm adds ammonium bicarbonate additive 1t, uniform mixing places that to carry out microwave in the microwave building-up reactions cavity synthetic, and microwave frequency is 2450MHz.Feed nitrogen, pressure is 0.12MPa, and 1250 ℃ of synthesis temperatures, generated time were controlled at 2 hours, and the cooling of gained synthetics is the ferro-silicon nitride finished product.After measured, it is nitrogenous 31.05% to make ferro-silicon nitride, and XRD analysis result is α-Si
3N
4, β-Si
3N
4, Fe
2Si.
Claims (1)
1, a kind of microwave synthesis method of ferro-silicon nitride, it is synthetic with the ferrosilicon to be that raw material carries out microwave, it is characterized in that, described raw material ferrosilicon is the ferrosilicon powder that sieves and form after grinding with conventional Ginding process, granularity is less than 0.5mm, the gained ferrosilicon powder is inserted in the microwave building-up reactions cavity, add bicarbonate of ammonia, uniform mixing, microwave frequency are 2450MHz, pressure 0.1～0.12MPa, 800～1800 ℃ of synthesis temperatures, it is synthetic that feeding nitrogen carries out microwave, generated time 0.5～3 hour, and the cooling of gained synthetics is the finished product ferro-silicon nitride.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100324389A CN100358799C (en) | 2005-11-25 | 2005-11-25 | Method for synthesizing ferro-silicon nitride by microwave |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100324389A CN100358799C (en) | 2005-11-25 | 2005-11-25 | Method for synthesizing ferro-silicon nitride by microwave |
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| Publication Number | Publication Date |
|---|---|
| CN1775662A CN1775662A (en) | 2006-05-24 |
| CN100358799C true CN100358799C (en) | 2008-01-02 |
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| CNB2005100324389A Expired - Fee Related CN100358799C (en) | 2005-11-25 | 2005-11-25 | Method for synthesizing ferro-silicon nitride by microwave |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102795855B (en) * | 2011-05-27 | 2015-08-26 | 中国科学院金属研究所 | One utilizes microwave method to prepare Y 4si 2o 7n 2the method of powder body material |
| 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 |
| CN108411066A (en) * | 2018-03-16 | 2018-08-17 | 重庆大学 | A kind of preparation method of steel-making ferro-silicon nitride |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5874377A (en) * | 1994-03-31 | 1999-02-23 | Microwear Corporation | Sintered silicon nitride product |
| US6148764A (en) * | 1997-12-29 | 2000-11-21 | Jet Process Corporation | Multiple micro inlet silane injection system for the jet vapor deposition of silicon nitride with a microwave discharge jet source |
| CN1281833A (en) * | 1999-07-22 | 2001-01-31 | 青岛大学 | Microwave sintering method of composite ceramics |
| CN1458913A (en) * | 2001-02-08 | 2003-11-26 | 住友电气工业株式会社 | Porous ceramic and method for prepartion thereof and microstrip substrate |
| CN1473140A (en) * | 2001-09-04 | 2004-02-04 | 住友电气工业株式会社 | Porous silicon nitride ceramic and its manufacturing method |
| CN1609057A (en) * | 2004-11-12 | 2005-04-27 | 清华大学 | Fast microwave sintering process of combined silicon nitride-silicon carbide refractorg material |
-
2005
- 2005-11-25 CN CNB2005100324389A patent/CN100358799C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5874377A (en) * | 1994-03-31 | 1999-02-23 | Microwear Corporation | Sintered silicon nitride product |
| US6148764A (en) * | 1997-12-29 | 2000-11-21 | Jet Process Corporation | Multiple micro inlet silane injection system for the jet vapor deposition of silicon nitride with a microwave discharge jet source |
| CN1281833A (en) * | 1999-07-22 | 2001-01-31 | 青岛大学 | Microwave sintering method of composite ceramics |
| CN1458913A (en) * | 2001-02-08 | 2003-11-26 | 住友电气工业株式会社 | Porous ceramic and method for prepartion thereof and microstrip substrate |
| CN1473140A (en) * | 2001-09-04 | 2004-02-04 | 住友电气工业株式会社 | Porous silicon nitride ceramic and its manufacturing method |
| CN1609057A (en) * | 2004-11-12 | 2005-04-27 | 清华大学 | Fast microwave sintering process of combined silicon nitride-silicon carbide refractorg material |
Non-Patent Citations (1)
| Title |
|---|
| 较低温度霞制备自结合氮化硅铁制品. 陈俊红等.北京科技大学学报，第27卷第5期. 2005 * |
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Address after: Hunan city Changsha Zhanggongling Longping high tech Park Changxing Road No. 178 Patentee after: Changsha Longtai Science & Technology Co., Ltd. Address before: M6 group 1, hi tech Industrial Development Zone, Hunan, Changsha Patentee before: Changsha Longtai Science & Technology Co., Ltd. |
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