CN101863668A - Method for synthesizing SiC/FexSiy composite material by using iron ore tailings - Google Patents
Method for synthesizing SiC/FexSiy composite material by using iron ore tailings Download PDFInfo
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Abstract
The invention belongs to the technical field of comprehensive utilization of ceramics, fire-proof materials and mineral solid wastes, and provides a method for synthesizing a SiC/FexSiy composite material by using iron ore tailings. In the method, a process technique is mature and is easy to control, the low raw material cost is low, and a product has high application values. The method uses the iron ore tailings as the main raw material added with carbon powder as a reducing agent, and performs mechanical pressing to obtain a blank with uniform components. In the preparation process, the technological parameters such as the mixture ratio, the sintering temperature, a temperature raising system, the soaking time and the like are controlled to obtain high-purity SiC/FexSiy composite powder, and then the SiC/FexSiy composite material is prepared by performing secondary material blending and forming on the composite powder, burying silicon powder and performing reaction sintering. The main raw material of the method is the iron ore tailings which harm the environment, so the method has a low cost and is favorable for protecting the ecological environment, the process technique is mature and is easy to control, and the obtained product has high added values. The SiC/FexSiy composite material synthesized by the method has outstanding heat conductivity, high thermal expansion resistance and oxidation resistance and the like, and can be widely used in the industrial fields of metallurgy, chemical industry, electric power, energy source and the like.
Description
Technical field
The invention belongs to pottery, refractory materials and mineral products solid waste comprehensive utilization technique field, provide a kind of with the synthetic SiC/Fe of iron ore mine
xSi
yThe method of matrix material, raw materials cost is cheap, and product has higher using value.
Background technology
Characteristics such as the SiC material possesses intensity height, thermal conductivity height, erosion resistance is strong, shock-resistance is good can be used as material in the kiln of various abominable operational conditions, are the extremely wide high grade refractories of a kind of range of application.Various SiC fire resistant materials all have excellent high temperature use properties, and are big as high-temperature machinery intensity, high volume is stable and good thermal shock stability etc., are out of shape hardly, do not ftracture etc. medium-term and long-term use of circulation environment.The SiC based composites also is one of commanding elevation of high-temperature structural material technology, and its developmental level can reflect the design and the manufacturing capacity of an advanced aerospacecraft of country and advanced weaponry equipment.And the harm of metallic ore mine tailing is obvious to all, and the national economy that causes every year and people's property damage are startling.Thereby making full use of the chemical constitution characteristics of metallic ore mine tailing, exploitation SiC based composites has vast potential for future development.
Zhang Shuhui, Xue Xiangxin, Jiang Tao etc. have carried out the research of iron ore tailings laboratory synthesizing silicon carbide powder.On the basis of thermomechanical analysis, be main raw material with the iron tailings, adopt carbothermic method to synthesize the SiC powder.Tentatively inquired into technological process with the synthetic SiC composite granule of iron tailings, but the SiC based composites that does not obtain having good use properties.
Provide a kind of method of utilizing the blue spar ore in-situ synthesis of SiC material in the Chinese invention patent application of publication number for CN101177270.Gather the kyanite ore, ore is made fine powder, and cross 0.074 μ m sieve, add binding agent, moulding, drying is burnt till, and de-carbon extracts the SiC composition.It is 60%-90% that this kind method is burnt till gained SiC component proportions, and the composition fluctuation is big, and more impurity can influence the goods use properties.
A kind of α type SiC-β type SiC mating type reaction sintering SiC material and its preparation method are provided in the Chinese invention patent application of publication number for CN101503295, obtain α type SiC powder by normal pressure or pressure sintering, carbon dust and described α type SiC powder mixes are obtained carbon-α type SiC mixture, after heating described carbon-α type SiC mixture it being shaped, under the vacuum high-temperature environment, with the molten silicon reaction of adjusted good resistance, thereby obtain the β type SiC material that resistance accords with electrology characteristic.The described vacuum high-temperature environment of this method makes synthetic technological condition have relatively high expectations, and has strengthened production cost.
Nowadays, the domestic and international report of SiC based composites is a lot, but does not find as yet to utilize iron ore mine to synthesize SiC/Fe
xSi
yThe relevant report of matrix material.
Summary of the invention
The invention provides a kind of iron ore mine that utilizes and be feedstock production SiC/Fe
xSi
yThe method of matrix material, purpose are to find a strip metal ore deposit mine tailing efficiently to utilize approach, reduce environmental pollution.
A kind of iron ore mine that utilizes synthesizes SiC/Fe
xSi
yThe method of matrix material, the present invention is a main raw material with the iron ore mine, allocates carbon dust into and obtains the uniform ingredients base substrate for the reductive agent mechanical pressing; Mine tailing, carbon dust (graphite or carbon black) mass ratio are 1.35-2.25: 1.In preparation process,, obtain SiC/Fe by processing parameters such as control ratio of components, sintering temperature, temperature increasing schedule, soaking times
xSi
yComposite granule.Composite granule makes SiC/Fe by the secondary reaction sintering then
xSi
yMatrix material, technical process is as follows:
(1) feedstock analysis: related iron ore mine main component is SiO among the present invention
2And Fe
3O
4, also contain a small amount of Al
2O
3, MgO, K
2O, Na
2Composition such as O, CaO.
Iron ore mine moiety table:
| Composition | ??SiO 2 | ??Fe 3O 4 | ??MgO | ??Al 2O 3 | ??K 2O、Na 2O, CaO etc. |
| Mass percent/% | ??80-85 | ??12-15 | ??1-1.5 | ??0.5-1 | ??1-6.5 |
(2) iron ore mine raw material pulverizing is crossed the 0.074mm standard sieve, then with mine tailing, carbon dust (graphite or carbon black) according to 1.35-2.25: 1 mass percent is mixed;
(3) add dehydrated alcohol in the compound as dispersion agent and grinding aid, ground at normal temperatures 5-7 hour, make it full and uniform mixing; The add-on of dehydrated alcohol is the 4-10% of compound total mass;
(4) mixed powder mixes binding agent, places the grinding tool mechanical pressing, after the demoulding under 50-100 ℃ of temperature dry 18-24 hour; Per 10 gram hybrid reaction material adding additives amounts are 1～6ml; Binding agent is 3-5%PVA (polyvinyl alcohol), and all the other are water;
(5) base substrate after the drying is put into crucible, bury carbon dust (carbon dust coats sample), place tube furnace then, following temperature increasing schedule heats up: 5-35 ℃ 60min to 200 ℃, 200 ℃ through 200min to 800 ℃, insulation 30min, temperature rise rate with 2-8 ℃/min is warming up to 1450-1650 ℃ then, be incubated 4-8 hour, naturally cool to 5-35 ℃, take out goods; And then put into retort furnace, carbon residue was removed in 800 ℃ of insulations in 5-7 hour.Obtaining principal crystalline phase is SiC/Fe
xSi
yComposite granule.
(6) with SiC/Fe
xSi
yComposite powder and carbon black are 5% mixed by mass percentage, stir.In ball grinder, be medium with ethanol then, composite powder and carbon black: ball: ethanol=1: 1.5: 1.5, mix grinding 12 hours dries naturally, is wedding agent with PVA, and is dry-pressing formed, compression moulding under the forming pressure of 140MPa, drying.At last the green compact sample is put into plumbago crucible, and add metallic silicon power (burying the Si powder), in the tube furnace stove, carry out reaction sintering under the nitrogen protection atmosphere to sample is coated.At last, obtain product S iC/Fe
xSi
yMatrix material.
This research and utilization iron ore mine is a main raw material, and the method by double sintering makes SiC/Fe
xSi
yMatrix material.The Technology maturation is easy to control, obtains product and has significant high heat conductance characteristic and good folding strength, fracture toughness property, thermal expansion and antioxidant property etc.
The present invention has following outstanding feature: main raw material is environmentally hazardous iron ore mine, and is with low cost and help ecological environmental protection; Technical maturity is easy to control; Products obtained therefrom added value height.
The invention has the advantages that:
1, preparation technology is simple, need not complicated processing unit and technological process, and the while, turns waste into wealth as raw material with a large amount of discarded tailings, alleviates the pressure of depleted mine tailing to environment.
2, the SiC/Fe that obtains
xSi
yMatrix material.Have outstanding heat conductivity and less heat resistanceheat resistant swelling property and good oxidation-resistance etc.
Description of drawings
Fig. 1 is different soaking times, the XRD figure spectrum of the final composite products of gained.
Embodiment
With iron ore mine, carbon (graphite or carbon black) mass percent batch mixing, in anhydrous ethanol medium, ground 6 hours according to 1.50: 1.
Take out mixed powder, drying is added binding agent, and mechanical pressing is the circular sample piece of Φ 10 * 4mm under 40MPa pressure then, after the demoulding under 80 ℃ of temperature dry 20 hours.
Base substrate after the drying is put into crucible, bury carbon dust (carbon dust coats sample), put into tube furnace, room temperature is through 60min to 200 ℃, and 200 ℃ through 200min to 800 ℃, insulation 30min, be warming up to 1200 ℃ with 5 ℃/min temperature rise rate then, insulation 30min is warming up to 1500 ℃ with 3 ℃/min temperature rise rate again, is incubated 5 hours.
Sintering oven is reduced to 1200 ℃ with the speed of 4 ℃/min, then at 1200 ℃ of insulation 30min; Naturally cool to room temperature, take out goods; And then put into retort furnace, 800 ℃ are incubated 6 hours burning-off carbon residue.Obtain the composite granule that principal crystalline phase is SiC.
Allocate the carbon black of quality percentage composition 5% in the composite granule into.Ball milling, drying add binding agent compression moulding under the forming pressure of 140MPa, drying then.At last the green compact sample is put into plumbago crucible, and add metallic silicon power (burying the Si powder), in the tube furnace stove, carry out reaction sintering under the nitrogen protection atmosphere to sample is coated.At last, obtain SiC/Fe
xSi
yMatrix material.
Embodiment 2
With iron ore mine, carbon (graphite or carbon black) mass percent batch mixing, in anhydrous ethanol medium, ground 6 hours according to 2.00: 1.
Take out mixed powder, drying is added binding agent, and mechanical pressing is the circular sample piece of Φ 10 * 4mm under 40MPa pressure then, after the demoulding under 80 ℃ of temperature dry 20 hours.
Base substrate after the drying is put into crucible, bury carbon dust (carbon dust coats sample), put into tube furnace, room temperature is through 60min to 200 ℃, and 200 ℃ through 200min to 800 ℃, insulation 30min, be warming up to 1200 ℃ with 5 ℃/min temperature rise rate then, insulation 30min is warming up to 1500 ℃ with 3 ℃/min temperature rise rate again, is incubated 5 hours.
Sintering oven is reduced to 1200 ℃ with the speed of 4 ℃/min, then at 1200 ℃ of insulation 30min; Naturally cool to room temperature, take out goods; And then put into retort furnace, 800 ℃ are incubated 6 hours burning-off carbon residue.Obtain the composite granule that principal crystalline phase is SiC.
Allocate the carbon black of quality percentage composition 5% in the composite granule into.Ball milling, drying add binding agent compression moulding under the forming pressure of 140MPa, drying then.At last the green compact sample is put into plumbago crucible, and add metallic silicon power (burying the Si powder), in the tube furnace stove, carry out reaction sintering under the nitrogen protection atmosphere to sample is coated.At last, obtain SiC/Fe
xSi
yMatrix material.
Claims (1)
1. one kind prepares SiC/Fe with iron ore mine
xSi
yThe method of matrix material is characterized in that: with the iron ore mine is main raw material, and allocating carbon dust into is reductive agent, and mechanical pressing obtains the uniform ingredients base substrate; Mine tailing, carbon dust mass ratio are 1.35-2.25: 1; In preparation process,, obtain SiC/Fe by control ratio of components, sintering temperature, temperature increasing schedule, soaking time processing parameter
xSi
yComposite granule; Composite granule makes SiC/Fe by the secondary reaction sintering then
xSi
yMatrix material, technical process is as follows:
(1) feedstock analysis: related iron ore mine main component is SiO among the present invention
2And Fe
3O
4, also contain a small amount of Al
2O
3, MgO, K
2O, Na
2O, CaO composition;
Iron ore mine moiety table:
(2) iron ore mine raw material pulverizing is crossed the 0.074mm standard sieve, then mine tailing, carbon dust is mixed according to the mass ratio of 1.35-2.25:1;
(3) add dehydrated alcohol in the compound as dispersion agent and grinding aid, ground at normal temperatures 5-7 hour, make it full and uniform mixing; The add-on of dehydrated alcohol is the 4-10% of compound total mass;
(4) mixed powder mixes binding agent, places the grinding tool mechanical pressing, after the demoulding under 50-100 ℃ of temperature dry 18-24 hour; Per 10 gram hybrid reaction material adding additives amounts are 1～6ml; Binding agent is 3-5%PVA, and all the other are water;
(5) base substrate after the drying is put into crucible, bury carbon dust, carbon dust coats sample, place tube furnace then, heat up by following temperature increasing schedule: 5-35 ℃ 60min to 200 ℃, 200 ℃ through 200min to 800 ℃, insulation 30min, temperature rise rate with 2-8 ℃/min is warming up to 1450-1650 ℃ then, be incubated 4-8 hour, naturally cool to 5-35 ℃, take out goods; And then put into retort furnace, and 800 ℃ of insulations were removed carbon residue in 5-7 hour, and obtaining principal crystalline phase is SiC/Fe
xSi
yComposite granule;
(6) with SiC/Fe
xSi
yComposite powder and carbon black are 5% mixed by mass percentage, stir, in ball grinder, be medium then with ethanol, composite powder and carbon black: ball: ethanol=1: 1.5: 1.5, mix grinding 12 hours, naturally drying, is wedding agent with PVA, dry-pressing formed, compression moulding under the forming pressure of 140MPa, drying; At last the green compact sample is put into plumbago crucible, and add metallic silicon power, bury the Si powder to sample is coated; In the tube furnace stove, carry out reaction sintering under the nitrogen protection atmosphere; At last, obtain product S iC/Fe
xSi
yMatrix material.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102719574A (en) * | 2011-03-29 | 2012-10-10 | 鞍钢股份有限公司 | Converter slag stability modifier and application method thereof |
| CN106631055A (en) * | 2016-11-22 | 2017-05-10 | 常州思宇知识产权运营有限公司 | Preparation method of refractory material |
| CN107686353A (en) * | 2017-08-22 | 2018-02-13 | 东北大学 | A kind of preparation method of high-strength conducting carbonization ferrosilicon composite porous ceramic |
| CN109160814A (en) * | 2018-09-20 | 2019-01-08 | 东北大学 | A kind of in-situ carbon SiClx-iron silicon composite and preparation method thereof |
| US10240046B2 (en) * | 2016-01-28 | 2019-03-26 | King Abdulaziz University | Method for fabrication of a hybrid dual phase filler for elastomers |
| RU2733966C1 (en) * | 2019-04-12 | 2020-10-08 | Федеральное государственное автономное образовательное учреждение высшего образования "Уральский федеральный университет имени первого Президента России Б.Н. Ельцина" | Method of producing composite oxide materials |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1850596A (en) * | 2006-05-22 | 2006-10-25 | 东北大学 | Method for preparing SiC complex-phase material utilizing iron ore tailings |
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2010
- 2010-05-24 CN CN 201010188613 patent/CN101863668A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1850596A (en) * | 2006-05-22 | 2006-10-25 | 东北大学 | Method for preparing SiC complex-phase material utilizing iron ore tailings |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102719574A (en) * | 2011-03-29 | 2012-10-10 | 鞍钢股份有限公司 | Converter slag stability modifier and application method thereof |
| CN102719574B (en) * | 2011-03-29 | 2015-05-06 | 鞍钢股份有限公司 | Converter slag stability modifier and application method thereof |
| US10240046B2 (en) * | 2016-01-28 | 2019-03-26 | King Abdulaziz University | Method for fabrication of a hybrid dual phase filler for elastomers |
| CN106631055A (en) * | 2016-11-22 | 2017-05-10 | 常州思宇知识产权运营有限公司 | Preparation method of refractory material |
| CN107686353A (en) * | 2017-08-22 | 2018-02-13 | 东北大学 | A kind of preparation method of high-strength conducting carbonization ferrosilicon composite porous ceramic |
| CN107686353B (en) * | 2017-08-22 | 2019-08-09 | 东北大学 | A kind of preparation method of conductive silicon carbide-iron composite porous ceramic |
| CN109160814A (en) * | 2018-09-20 | 2019-01-08 | 东北大学 | A kind of in-situ carbon SiClx-iron silicon composite and preparation method thereof |
| WO2020057096A1 (en) * | 2018-09-20 | 2020-03-26 | 东北大学 | In-situ silicon carbide-iron silicon composite material and preparation method therefor |
| RU2733966C1 (en) * | 2019-04-12 | 2020-10-08 | Федеральное государственное автономное образовательное учреждение высшего образования "Уральский федеральный университет имени первого Президента России Б.Н. Ельцина" | Method of producing composite oxide materials |
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Application publication date: 20101020 |