CN102976324A - Synthesis method of beta-SiC nano wire - Google Patents
Synthesis method of beta-SiC nano wire Download PDFInfo
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- CN102976324A CN102976324A CN2012105164206A CN201210516420A CN102976324A CN 102976324 A CN102976324 A CN 102976324A CN 2012105164206 A CN2012105164206 A CN 2012105164206A CN 201210516420 A CN201210516420 A CN 201210516420A CN 102976324 A CN102976324 A CN 102976324A
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Abstract
The invention provides a synthesis method of a beta-SiC nano wire, relates to a synthesis method of a SiC nano material and aims to solve the problems of high temperature, low product purity and high equipment requirement in the existing SiC nano wire synthesis method. The synthesis method comprises the following steps: 1, evenly mixing silicon powder, SiO2 powder and carbon nano tube powder according to a certain mass percentage, placing in a tube furnace, and sintering in argon gas at 1200-1500 DEG C to obtain a primary product; and 2, placing the primary product in heating equipment, decarbonizing while keeping the temperature at 300-700 DEG C, treating in hydrofluoric acid, filtering while depressurizing, then washing with water and ethanol, and drying to obtain the beta-SiC nano wire. According to the invention, the synthesis method has high product purity, favorable controllability, low sintering temperature and low equipment requirement and does not need to be subjected to depressurizing treatment. The invention is mainly used for the synthesis of a SiC nano material.
Description
Technical field
The present invention relates to a kind of synthetic method of SiC nano material.
Background technology
Carbofrax material is the third generation wide bandgap semiconductor materials that grows up afterwards from first-generation elemental semiconductors (Si) and s-generation compound semiconductor materials (GaAS, GaP, InP etc.).This kind material has the characteristics such as broad-band gap, high heat conductance, high disruptive critical voltage, high carrier saturation drift velocity, is mainly used in high temperature, high frequency, high-power, photoelectron and radioprotective device.Huge potential using value is especially arranged in high speed circuit device, high-temperature device and high-power component.Simultaneously, because silicon carbide has the characteristics such as high strength, high rigidity, high antioxidant, high corrosion resistance, high thermal conductivity and low thermal coefficient of expansion, so the SiC material also is one of main wild phase of preparation high temperature composite large-size components.The special structure of SiC monodimension nanometer material, excellent physicals, the integrated circuit technology with current maturation is compatible mutually with comparalive ease, can bring into play its unique performance again aspect nanometer, has possessed the block materials excellent properties that is beyond one's reach.Therefore, the quick preparation of SiC nano wire is for the microminiaturization, the high performance that promote product, and energy-conservation, efficient, low consumption, high integration etc. have great importance.
The main method of preparation SiC nano wire has arc discharge, reduced atmosphere sintering process, vapour deposition process, Polymer-pyrolysis method, microwave sintering method etc. at present.But all there is certain shortcoming in these methods, need the higher metal catalyst of cost as arc discharge and vapour deposition process, and the final product that obtains is impure.Polymer-pyrolysis method complex process, product pattern and composition poor controllability, preparation cost is higher, and contaminate environment.At present, document " Catalytic synthesis andphotoluminescence of needle-shaped 3C – SiC nanowires[Solid State Communications 128 (2003) 295-297] " introduced a kind of with iron as catalyzer, decompression 5.0 * 10
-2Torr is heated to 1700 ℃, insulation 2h, and the product that the method makes contains catalyzer, and complicated through decompression, 1700 ℃ of high temperature, equipment requirements, and cost is higher.Document " Synthesis, characterization, and photoluminescence properties of bulk-quantity β-SiC/SiO
xCoaxial nanowires[Materials Chemistry and Physics 135 (2012) 1005-1011] " reported with Si, SiO
2, graphite is that raw material prepares the SiC nano wire, utilization be the microwave sintering method, higher to equipment requirements at decompression and 1400 ℃ of sintering, cost height, complicated operation.Can find out that microwave sintering method and reduced atmosphere sintering are very high for equipment requirements, the equipment resistance to air loss of requirement will be got well, and needs vacuum or low pressure sintering in the experimentation, and danger is larger.In addition, the preparation method of many reports often adopts carbon dust as carbon source, and this just causes the reproducibility of material relatively poor, and there is the totally different shortcoming of pattern difference in the SiC nano wire of different batches preparation.
Summary of the invention
To the objective of the invention is that existing synthetic SiC nano wire method needs high temperature, product purity is low and the problem high to equipment requirements in order solving, and a kind of synthetic method of beta-SiC nano-wire to be provided.
The synthetic method of beta-SiC nano-wire of the present invention follows these steps to realize:
One, presses the mass percent ratio with 15% ~ 40% silica flour, 25% ~ 65% SiO
2Powder and 15% ~ 55% carbon nanotube dust evenly are mixed to get mixed powder, then mixed powder are put into tube furnace and are placed argon atmospher with 1200～1500 ℃ temperature sintering, and insulation 1～8h obtains Primary product;
Two, the Primary product that step 1 is obtained is put into heating installation, under 300 ~ 700 ℃ sintering temperature, be incubated 2～10h carbon elimination, then put into mass concentration and be 30%～50% hydrofluoric acid and process 1～12h, difference water and washing with alcohol are 2～4 times behind filtration under diminished pressure, at 70～90 ℃ of lower dry 2～3h, obtain beta-SiC nano-wire again;
Wherein the described silica flour fineness of step 1 is 100～300 orders, SiO
2The particle diameter of powder is less than 80nm, and the diameter of carbon nanotube is 20 ~ 40nm, and length is 5 ~ 15um;
Purity of argon is greater than 99.99% in the argon atmospher described in the step 1.
The synthetic method of beta-SiC nano-wire of the present invention comprises following beneficial effect:
The diameter of the beta-SiC nano-wire that 1, obtains by synthetic method of the present invention is 20 ~ 30nm, and length is micron order, demonstrate prepared SiC nano wire by X ray diffracting spectrum and have higher purity, and the circulation ratio of product is high, controllability is good.
2, the SiC nano wire of the present invention's preparation is synthetic by tube furnace, and the argon gas atmosphere sintering process directly communicates with atmosphere, need not through reduced pressure treatment, requires low to instrument.Sintering temperature is 1200～1500 ℃, and sintering temperature is lower, and is easy and simple to handle.
3, of the present invention synthesizing from the former preparation process of expecting product, environmental pollution is little, and raw material availability is high, is mainly used in the synthetic of SiC nano material.
Description of drawings
Fig. 1 is the XRD figure of the beta-SiC nano-wire that obtains of embodiment eight;
Fig. 2 is the TEM figure of the beta-SiC nano-wire that obtains of embodiment eight.
Embodiment:
Embodiment one: the synthetic method of present embodiment beta-SiC nano-wire follows these steps to implement:
One, presses the mass percent ratio with 15% ~ 40% silica flour, 25% ~ 65% SiO
2Powder and 15% ~ 55% carbon nanotube dust evenly are mixed to get mixed powder, then mixed powder are put into tube furnace and are placed argon atmospher with 1200～1500 ℃ temperature sintering, and insulation 1～8h obtains Primary product;
Two, the Primary product that step 1 is obtained is put into heating installation, under 300 ~ 700 ℃ sintering temperature, be incubated 2～10h carbon elimination, then put into mass concentration and be 30%～50% hydrofluoric acid and process 1～12h, difference water and washing with alcohol are 2～4 times behind filtration under diminished pressure, at 70～90 ℃ of lower dry 2～3h, obtain beta-SiC nano-wire again;
Wherein the described silica flour fineness of step 1 is 100～300 orders, SiO
2The particle diameter of powder is less than 80nm, and the diameter of carbon nanotube is 20 ~ 40nm, and length is 5 ~ 15um;
Purity of argon is greater than 99.99% in the argon atmospher described in the step 1.
Present embodiment step 1 raw material silica flour, SiO
2The mass percent sum of powder and carbon nanotube dust is 100%, raw material silica flour, SiO
2Powder and carbon nanotube dust are the commercially available prod.
The diameter of the beta-SiC nano-wire that present embodiment obtains is 20 ~ 30nm, and length is micron order.The building-up process of beta-SiC nano-wire need not through reduced pressure treatment.
Embodiment two: present embodiment and embodiment one are different is step 1 by mass percent than with 18% ~ 23% silica flour, 35% ~ 48% SiO
2Powder and 34% ~ 42% carbon nanotube dust evenly are mixed to get mixed powder.Other step and parameter are identical with embodiment one.
Embodiment three: present embodiment and embodiment one are different is step 1 by mass percent than with 22% silica flour, 43% SiO
2Powder and 35% carbon nanotube dust evenly are mixed to get mixed powder.Other step and parameter are identical with embodiment one.
Embodiment four: present embodiment is different from one of embodiment one to three is the described temperature sintering with 1200～1500 ℃ of step 1, the sintering heating mode is controlled as follows: 20 ~ 500 ℃ of heating-up times are 20～100min, 500 ~ 800 ℃ of heating-up times are 10～30min, 800 ~ 1000 ℃ of heating-up times are 20～90min, and 1000 ~ 1500 ℃ of heating-up times are 30～300min.Other step and parameter are identical with one of embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to three is the described temperature sintering with 1200～1500 ℃ of step 1, the sintering heating mode is controlled as follows: 20 ~ 500 ℃ of heating-up times are 50min, 500 ~ 800 ℃ of heating-up times are 30min, 800 ~ 1000 ℃ of heating-up times are 40min, and 1000 ~ 1500 ℃ of heating-up times are 80min.Other step and parameter are identical with one of embodiment one to three.
Embodiment six: present embodiment is different from one of embodiment one to five, and to be step 1 put into tube furnace with mixed powder places argon atmospher with 1400 ℃ temperature sintering, insulation 3h.Other step and parameter are identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six is that heating installation in the step 2 is retort furnace.Other step and parameter are identical with one of embodiment one to six.
Embodiment eight: the synthetic method of present embodiment beta-SiC nano-wire follows these steps to implement:
One, with the silica flour of 0.28g, the SiO of 0.6g
2The carbon nanotube dust of powder and 0.48g evenly is mixed to get mixed powder, then mixed powder is put into tube furnace and is placed argon atmospher with 1400 ℃ temperature sintering, and insulation 2h obtains Primary product;
Two, the Primary product that step 1 is obtained is put into retort furnace, then insulation 8h carbon elimination under 700 ℃ sintering temperature is put into mass concentration and is 40% hydrofluoric acid and process 10h, respectively water and washing with alcohol 3 times behind filtration under diminished pressure, at 80 ℃ of lower dry 2h, obtain beta-SiC nano-wire again;
Wherein the described silica flour fineness of step 1 is 200 orders, SiO
2The particle diameter of powder is 60nm, and the diameter of carbon nanotube is 30nm, and length is 10um;
Purity of argon is 99.999% in the argon atmospher described in the step 1;
The described temperature sintering with 1400 ℃ of step 1, the sintering heating mode is controlled as follows: 20 ~ 500 ℃ of heating-up times are 100min, 500 ~ 800 ℃ of heating-up times are 30min, and 800 ~ 1000 ℃ of heating-up times are 40min, and 1000 ~ 1400 ℃ of heating-up times are 140min.
The mass percent of silica flour is 20.6%, SiO in the present embodiment
2The mass percent of powder is 44.1%, and the mass percent of carbon nanotube dust is 35.3%.
The diameter of the beta-SiC nano-wire that present embodiment obtains is 20 ~ 30nm, length is micron order, building-up process need not through reduced pressure treatment, and sintering temperature is lower, therefore to instrument and equipment require low, its XRD figure as shown in Figure 1, the beta-SiC nano-wire that obtains of present embodiment has higher purity as can be known.
The TEM figure of the beta-SiC nano-wire that present embodiment obtains as shown in Figure 2.
Claims (7)
1. the synthetic method of a beta-SiC nano-wire is characterized in that the synthetic method of beta-SiC nano-wire follows these steps to realize:
One, presses the mass percent ratio with 15% ~ 40% silica flour, 25% ~ 65% SiO
2Powder and 15% ~ 55% carbon nanotube dust evenly are mixed to get mixed powder, then mixed powder are put into tube furnace and are placed argon atmospher with 1200～1500 ℃ temperature sintering, and insulation 1～8h obtains Primary product;
Two, the Primary product that step 1 is obtained is put into heating installation, under 300 ~ 700 ℃ sintering temperature, be incubated 2～10h carbon elimination, then put into mass concentration and be 30%～50% hydrofluoric acid and process 1～12h, difference water and washing with alcohol are 2～4 times behind filtration under diminished pressure, at 70～90 ℃ of lower dry 2～3h, obtain beta-SiC nano-wire again;
Wherein the described silica flour fineness of step 1 is 100～300 orders, SiO
2The particle diameter of powder is less than 80nm, and the diameter of carbon nanotube is 20 ~ 40nm, and length is 5 ~ 15um;
Purity of argon is greater than 99.99% in the argon atmospher described in the step 1.
2. the synthetic method of a kind of beta-SiC nano-wire according to claim 1 is characterized in that step 1 compares 18% ~ 23% silica flour, 35% ~ 48% SiO by mass percent
2Powder and 34% ~ 42% carbon nanotube dust evenly are mixed to get mixed powder.
3. the synthetic method of a kind of beta-SiC nano-wire according to claim 1 is characterized in that step 1 compares 22% silica flour, 43% SiO by mass percent
2Powder and 35% carbon nanotube dust evenly are mixed to get mixed powder.
4. the synthetic method of a kind of beta-SiC nano-wire according to claim 1 and 2, it is characterized in that the described temperature sintering with 1200～1500 ℃ of step 1, the sintering heating mode is controlled as follows: 20 ~ 500 ℃ of heating-up times are 20～100min, 500 ~ 800 ℃ of heating-up times are 10～30min, 800 ~ 1000 ℃ of heating-up times are 20～90min, and 1000 ~ 1500 ℃ of heating-up times are 30～300min.
5. the synthetic method of a kind of beta-SiC nano-wire according to claim 4, it is characterized in that the described temperature sintering with 1200～1500 ℃ of step 1, the sintering heating mode is controlled as follows: 20 ~ 500 ℃ of heating-up times are 50min, 500 ~ 800 ℃ of heating-up times are 30min, 800 ~ 1000 ℃ of heating-up times are 40min, and 1000 ~ 1500 ℃ of heating-up times are 80min.
6. the synthetic method of a kind of beta-SiC nano-wire according to claim 5 is characterized in that step 1 puts into tube furnace with mixed powder and place argon atmospher with 1400 ℃ temperature sintering, insulation 3h.
7. the synthetic method of a kind of beta-SiC nano-wire according to claim 6 is characterized in that the heating installation in the step 2 is retort furnace.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103878006A (en) * | 2014-03-26 | 2014-06-25 | 华南农业大学 | Preparation method of silicon carbide/carbon nano material composite visible-light photocatalyst |
| CN104167259A (en) * | 2014-07-16 | 2014-11-26 | 青岛科技大学 | Preparation technology for obtaining SiC@SiO2 nanometer cables with controllable cladding-layer thicknesses and cladding-free SiC nano wire |
| CN106564902A (en) * | 2016-09-08 | 2017-04-19 | 李志文 | Method for preparing silicon carbide quantum dot material from konilite |
| CN109110763A (en) * | 2018-08-31 | 2019-01-01 | 华南农业大学 | A kind of Sic nanotube and its preparation method and application |
| CN112266252A (en) * | 2020-11-04 | 2021-01-26 | 黑龙江冠瓷科技有限公司 | Preparation method of pressureless sintering micro-nano mixed silicon carbide granulation powder |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103878006A (en) * | 2014-03-26 | 2014-06-25 | 华南农业大学 | Preparation method of silicon carbide/carbon nano material composite visible-light photocatalyst |
| CN103878006B (en) * | 2014-03-26 | 2016-06-15 | 华南农业大学 | A kind of preparation method of silicon carbide/carbon nano-material composite visible light photocatalyst |
| CN104167259A (en) * | 2014-07-16 | 2014-11-26 | 青岛科技大学 | Preparation technology for obtaining SiC@SiO2 nanometer cables with controllable cladding-layer thicknesses and cladding-free SiC nano wire |
| CN106564902A (en) * | 2016-09-08 | 2017-04-19 | 李志文 | Method for preparing silicon carbide quantum dot material from konilite |
| CN109110763A (en) * | 2018-08-31 | 2019-01-01 | 华南农业大学 | A kind of Sic nanotube and its preparation method and application |
| CN112266252A (en) * | 2020-11-04 | 2021-01-26 | 黑龙江冠瓷科技有限公司 | Preparation method of pressureless sintering micro-nano mixed silicon carbide granulation powder |
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Application publication date: 20130320 |