CN103553043A - Preparation method for SiC nanometer microsphere with high specific surface area - Google Patents
Preparation method for SiC nanometer microsphere with high specific surface area Download PDFInfo
- Publication number
- CN103553043A CN103553043A CN201310468042.3A CN201310468042A CN103553043A CN 103553043 A CN103553043 A CN 103553043A CN 201310468042 A CN201310468042 A CN 201310468042A CN 103553043 A CN103553043 A CN 103553043A
- Authority
- CN
- China
- Prior art keywords
- surface area
- specific surface
- mixed powder
- microsphere
- vacuum sintering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a preparation method for a SiC nanometer microsphere with a high specific surface area. The method comprises the following steps: uniformly mixing a carbon microsphere with a silica microsphere to obtain mixed powder, wherein the particle size of the carbon microsphere is 200 to 400 nm, and the particle size of the silica microsphere is 100 to 200 nm; putting the mixed powder in a vacuum sintering furnace, vacuumizing the vacuum sintering furnace, introducing argon, allowing a temperature to rise to 1200 DEG C from room temperature under the protection of argon, then vacuumizing the vacuum sintering furnace again, continuing heating to a temperature of 1300 to 1500 DGE C and carrying out sintering at the temperature of 1300 to 1500 DGE C so as to obtain a product; and calcining the product at a temperature of 400 to 600 DEG C so as to obtain the SiC nanometer microsphere with a high specific surface area. The method provided by the invention has the advantages of simple operation, low cost, good repeatability and capacity of realizing industrial production. The prepared SiC nanometer microsphere has uniform granularity, high purity, a controllable diameter in a range of 200 to 500 nm and a specific surface area of 25 to 60 m<2>/g.
Description
Technical field
The invention belongs to inorganic materials preparing technical field, be specifically related to a kind of method of preparing high-specific surface area SiC Nano microsphere.
Background technology
SiC is the covalent linkage compound consisting of carbon and silicon, has similar adamantine tetrahedral structural unit, thereby has extraordinary chemical stability, high physical strength and hardness, and good heat-conductivity conducting performance.Compare with traditional aluminum oxide, silicon oxide, activated carbon catalyst solid support material, SiC obviously has advantages of following aspect as catalyst support material: the heat-conductivity conducting performance that (1) is good, is conducive to the heat transmission of catalyzer in reaction process and the electronics transmission between catalyst activity component and carrier; (2) chemical stability is good, is difficult for producing and interacting with active ingredient, is conducive to keep the stable of catalyst structure; (3) high physical strength and hardness, be conducive to improve intensity and the abrasion resistance properties of catalyzer, extending catalyst life-span.Based on above-mentioned advantage, SiC, as support of the catalyst, has been successfully applied in the middle of some important chemical reactions.Yet, in more than 100 year history of heterogeneous catalysis technology development, but seldom see that SiC is at the figure of industrial applications.Tracing it to its cause, is because its specific surface area of SiC that commercial methods is produced is difficult to meet the requirement of catalyst support material.Therefore, the exploitation of high-specific surface area silicon carbide has caused investigator's attention, and relevant research is increasing.
In recent years, the development of nanotechnology, a frontier of having opened up specific area SiC.Nano SiC not only can increase substantially its specific surface area, and rise, has more the even irreplaceable performance of some brilliance, demonstrates unusual effect in some chemical reactions, becomes a kind of support of the catalyst that has much potentiality.Especially the SiC of Nano microsphere structure is with its unique character, as single dispersion, stability, Modulatory character, be self-assembled into as the research field becoming more and more important in Materials science forward position in recent years.Kun Wang etc. are at Synthesis of nanostructured silicon carbide spheres from mesoporous C-SiO
2nanocomposites[Chem.Commun., 2010,46,303 – 305] in using tetraethoxy and furfuryl alcohol respectively as silicon source and carbon source, first synthetic C-SiO
2meso-porous nano matrix material, then obtain SiC microballoon through 1350 ℃ of carbothermic reduction reactions.Yet the method is at synthetic C-SiO
2in compound system, need to add triblock copolymer P123, simultaneously synthetic C-SiO
2presoma also needs through the calcination process of 550 ℃ under condition of nitrogen gas.The method preparation process more complicated, C-SiO
2c/Si mol ratio in compound system is difficult to control.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing high-specific surface area SiC Nano microsphere, it is simple to operate, and favorable repeatability is conducive to suitability for industrialized production.
For achieving the above object, the present invention adopts following technical scheme:
The present invention includes following steps: comprise the following steps:
1) by carbosphere and silicon dioxide microsphere (1:1)～(2:1) mix in mass ratio, obtain mixed powder; Wherein carbosphere particle diameter is 200～400nm, with the particle diameter of silicon dioxide microsphere be 100～200nm;
2) mixed powder is put into vacuum sintering furnace, to after vacuum sintering stove evacuation, pass into argon gas, and under argon shield when room temperature is warming up to 1200 ℃ by vacuum sintering stove evacuation, then continue to be warming up to 1300 ℃～1500 ℃, sintering at 1300 ℃～1500 ℃, then be naturally cooled to room temperature, obtain product;
3) product is calcined at 400-600 ℃, naturally cooled to room temperature, obtain high-specific surface area SiC Nano microsphere.
Described step 2) in, mixed powder is put into vacuum sintering stokehold, first mixed powder is put into corundum crucible, and keep mixed powder natural packing, mixed powder piling height is controlled in 10mm.
Described step 2) in, the time of reaction is 30～90min.
In described step 3), calcining is carried out in retort furnace.
The time of calcining in described step 3) is 1-2 hour.
The present invention has following beneficial effect: the present invention is with carbosphere, SiO
2microballoon is raw material, using the carbosphere as carbon source with as the SiO in silicon source
2microballoon, after mixing, inserts reaction sintering in vacuum sintering furnace, the product after sintering is being calcined in air to the residual carbon of removal, obtains the SiC Nano microsphere of high-specific surface area.The present invention is simple to operate, with low cost, and favorable repeatability is conducive to suitability for industrialized production.The epigranular of the prepared SiC Nano microsphere of the present invention, purity is high, and diameter is 200～500nm, and specific surface area can reach 25～60m
2/ g.
Accompanying drawing explanation
Fig. 1 is scanning electron microscope (SEM) photo of the SiC Nano microsphere prepared of the present invention.
Embodiment
Below in conjunction with accompanying drawing, by embodiment, the present invention is elaborated.
In the present invention, carbosphere is according to method preparation described in patent 201210235639.9, and silicon dioxide microsphere is according to method preparation described in patent 201210235695.2.
Embodiment 1
1) by carbosphere, be that 2:1 mixes under mechanical stirring with silicon dioxide microsphere according to mass ratio, obtain mixed powder, wherein carbosphere particle diameter is 200～400nm, SiO
2the particle diameter of microballoon is 100～200nm.
2) mixed powder is placed in corundum crucible, and keeps mixed powder natural packing, avoids pressing, and mixed powder piling height is controlled as 1mm;
3) corundum crucible that installs mixed powder is put into vacuum sintering furnace, will after vacuum sintering stove evacuation, pass into argon gas, and when room temperature is warming up to 1200 ℃, vacuumize under argon shield, then continue to be warming up to 1300 ℃, and react 90min at 1300 ℃;
4) product is put into retort furnace, at 400 ℃, calcine and remove residual carbon in 2 hours, naturally cool to room temperature, obtain high-specific surface area SiC Nano microsphere.
The SiC Nano microsphere diameter of the present embodiment gained is in 200nm left and right, and specific surface area is about 60m
2/ g.
Embodiment 2
Step 1: carbosphere is mixed according to mass ratio 1:1 with silicon dioxide microsphere under mechanical stirring, obtain mixed powder; Wherein, carbosphere particle diameter is 200～400nm, and the particle diameter of SiO2 microballoon is 100～200nm.
Step 2: mixed powder is placed in corundum crucible, and keeps mixed powder natural packing, avoid pressing, mixed powder piling height is controlled as 10mm;
Step 3: the corundum crucible that installs mixed powder is put into vacuum sintering furnace, to after vacuum sintering stove evacuation, pass into argon gas, and when being warming up to 1200 ℃, room temperature vacuumizes under argon shield, then continue to be warming up to 1500 ℃, and react 30min at 1500 ℃, then be naturally cooled to room temperature, obtain product;
4) product is put into retort furnace, at 600 ℃, calcine and remove residual carbon in 1 hour, naturally cool to room temperature, obtain high-specific surface area SiC Nano microsphere.
The SiC Nano microsphere diameter of the present embodiment gained is in 500nm left and right, and specific surface area is about 25m
2/ g.
Embodiment 3
Step 1: carbosphere is mixed according to mass ratio 1.5:1 with silicon dioxide microsphere under mechanical stirring, obtain mixed powder, wherein carbosphere particle diameter is 200～400nm, SiO
2the particle diameter of microballoon is 100～200nm.
Step 2: mixed powder is placed in corundum crucible, and keeps mixed powder natural packing, avoid pressing, mixed powder piling height is controlled as 5mm;
Step 3: the corundum crucible that installs mixed powder is put into vacuum sintering furnace, to after vacuum sintering stove evacuation, pass into argon gas, and when being warming up to 1200 ℃, room temperature vacuumizes under argon shield, then continue to be warming up to 1400 ℃, and react 90min at 1400 ℃, then be naturally cooled to room temperature, obtain product;
Step 4: product is put into retort furnace, calcine at 500 ℃ and remove residual carbon in 1 hour, naturally cool to room temperature, obtain high-specific surface area SiC Nano microsphere.
The SiC Nano microsphere diameter of the present embodiment gained is in 300nm left and right, and specific surface area is about 40m
2/ g.
Embodiment 4
Step 1: carbosphere is mixed according to mass ratio 1.2:1 with silicon dioxide microsphere under mechanical stirring, obtain mixed powder, wherein carbosphere particle diameter is 200～400nm, SiO
2the particle diameter particle diameter of microballoon is 100～200nm.
Step 2: mixed powder is placed in corundum crucible, and keeps mixed powder natural packing, avoid pressing, mixed powder piling height is controlled as 3mm;
Step 3: the corundum crucible that installs mixed powder is put into vacuum sintering furnace, to after vacuum sintering stove evacuation, pass into argon gas, and when being warming up to 1200 ℃, room temperature vacuumizes under argon shield, then continue to be warming up to 1350 ℃, and react 50min at 1350 ℃, then be naturally cooled to room temperature, obtain product;
Step 4: product is put into retort furnace, calcine at 450 ℃ and remove residual carbon in 1 hour, naturally cool to room temperature, obtain high-specific surface area SiC Nano microsphere.
Embodiment 5
Step 1: carbosphere is mixed in mechanical stirring according to mass ratio 1.7:1 with silicon dioxide microsphere, obtain mixed powder, wherein carbosphere particle diameter is 200～400nm, SiO
2the particle diameter of microballoon is 100～200n.
Step 2: mixed powder is placed in corundum crucible, and keeps mixed powder natural packing, avoid pressing, mixed powder piling height is controlled as 8mm;
Step 3: the corundum crucible that installs mixed powder is put into vacuum sintering furnace, to after vacuum sintering stove evacuation, pass into argon gas, and when being warming up to 1200 ℃, room temperature vacuumizes under argon shield, then continue to be warming up to 1450 ℃, and react 70min at 1500 ℃, then be naturally cooled to room temperature, obtain product;
Step 4: product is put into retort furnace, calcine at 550 ℃ and remove residual carbon in 1.7 hours, naturally cool to room temperature, obtain high-specific surface area SiC Nano microsphere.
Refer to shown in Fig. 1, Fig. 1 is the SEM pattern of the SiC Nano microsphere prepared of the present invention.As seen from Figure 1: the surface irregularity of SiC Nano microsphere prepared by the present invention, the small-particle by many diameters at 10～20nm forms, for the high-specific surface area of SiC Nano microsphere provides favourable condition.
The present invention is simple to operate, and favorable repeatability is conducive to suitability for industrialized production.The SiC Nano microsphere epigranular that the present invention obtains, purity is high, and diameter is controlled between 200～500nm, and specific surface area can reach 25～60m
2/ g.
Claims (5)
1. a method of preparing high-specific surface area SiC Nano microsphere, is characterized in that, comprises the following steps:
1) by carbosphere and silicon dioxide microsphere (1:1)～(2:1) mix in mass ratio, obtain mixed powder; Wherein carbosphere particle diameter is 200～400nm, with the particle diameter of silicon dioxide microsphere be 100～200nm;
2) mixed powder is put into vacuum sintering furnace, to after vacuum sintering stove evacuation, pass into argon gas, and under argon shield when room temperature is warming up to 1200 ℃ by vacuum sintering stove evacuation, then continue to be warming up to 1300 ℃～1500 ℃, sintering at 1300 ℃～1500 ℃, then be naturally cooled to room temperature, obtain product;
3) product is calcined at 400-600 ℃, naturally cooled to room temperature, obtain high-specific surface area SiC Nano microsphere.
2. a kind of method of preparing high-specific surface area SiC Nano microsphere according to claim 1, it is characterized in that, described step 2) in, mixed powder is put into vacuum sintering stokehold, first mixed powder is put into corundum crucible, and keeping mixed powder natural packing, mixed powder piling height is controlled in 10mm.
3. a kind of method of preparing high-specific surface area SiC Nano microsphere according to claim 1, is characterized in that described step 2) in reaction time be 30～90min.
4. a kind of method of preparing high-specific surface area SiC Nano microsphere according to claim 1, is characterized in that, in described step 3), calcining is carried out in retort furnace.
5. according to a kind of method of preparing high-specific surface area SiC Nano microsphere described in claim 1 or 4, it is characterized in that, the time of calcining in described step 3) is 1-2 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310468042.3A CN103553043B (en) | 2013-09-30 | 2013-09-30 | Preparation method for SiC nanometer microsphere with high specific surface area |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310468042.3A CN103553043B (en) | 2013-09-30 | 2013-09-30 | Preparation method for SiC nanometer microsphere with high specific surface area |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103553043A true CN103553043A (en) | 2014-02-05 |
| CN103553043B CN103553043B (en) | 2015-04-22 |
Family
ID=50007468
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310468042.3A Active CN103553043B (en) | 2013-09-30 | 2013-09-30 | Preparation method for SiC nanometer microsphere with high specific surface area |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103553043B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108503230A (en) * | 2018-04-24 | 2018-09-07 | 佛山市奥耶克思机械设备有限公司 | A kind of package substrate composite material and preparation method |
| CN111484017A (en) * | 2020-06-22 | 2020-08-04 | 黑龙江冠瓷科技有限公司 | Method for preparing SiC nanoparticles based on silica microspheres @ C |
| CN111995406A (en) * | 2020-08-10 | 2020-11-27 | 裴小罗 | SiC wear-resistant refractory material based on nano carbon material modification |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5891028A (en) * | 1981-11-25 | 1983-05-30 | Toshiba Corp | Manufacture of silicon carbide powder |
| WO1990010595A1 (en) * | 1989-03-16 | 1990-09-20 | Davy Research And Development Limited | Process |
| JPH04149017A (en) * | 1990-10-09 | 1992-05-22 | Sumitomo Metal Ind Ltd | Silicon carbide powder and its production |
| JP3154773B2 (en) * | 1991-11-08 | 2001-04-09 | 東海カーボン株式会社 | Method for producing particulate silicon carbide |
| CN1472136A (en) * | 2003-07-15 | 2004-02-04 | 中国科学院理化技术研究所 | Method for preparing silicon carbide |
| CN101027251A (en) * | 2004-09-09 | 2007-08-29 | 哥伦比亚化学公司 | Metal carbides and process for producing same |
| CN102596802A (en) * | 2009-08-26 | 2012-07-18 | Lg伊诺特有限公司 | System and method for manufacturing silicon carbide pulverulent body |
-
2013
- 2013-09-30 CN CN201310468042.3A patent/CN103553043B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5891028A (en) * | 1981-11-25 | 1983-05-30 | Toshiba Corp | Manufacture of silicon carbide powder |
| WO1990010595A1 (en) * | 1989-03-16 | 1990-09-20 | Davy Research And Development Limited | Process |
| JPH04149017A (en) * | 1990-10-09 | 1992-05-22 | Sumitomo Metal Ind Ltd | Silicon carbide powder and its production |
| JP3154773B2 (en) * | 1991-11-08 | 2001-04-09 | 東海カーボン株式会社 | Method for producing particulate silicon carbide |
| CN1472136A (en) * | 2003-07-15 | 2004-02-04 | 中国科学院理化技术研究所 | Method for preparing silicon carbide |
| CN101027251A (en) * | 2004-09-09 | 2007-08-29 | 哥伦比亚化学公司 | Metal carbides and process for producing same |
| CN102596802A (en) * | 2009-08-26 | 2012-07-18 | Lg伊诺特有限公司 | System and method for manufacturing silicon carbide pulverulent body |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108503230A (en) * | 2018-04-24 | 2018-09-07 | 佛山市奥耶克思机械设备有限公司 | A kind of package substrate composite material and preparation method |
| CN111484017A (en) * | 2020-06-22 | 2020-08-04 | 黑龙江冠瓷科技有限公司 | Method for preparing SiC nanoparticles based on silica microspheres @ C |
| CN111995406A (en) * | 2020-08-10 | 2020-11-27 | 裴小罗 | SiC wear-resistant refractory material based on nano carbon material modification |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103553043B (en) | 2015-04-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102992282B (en) | Mesoporous C3N4 photocatalytic material prepared by using molten salt method and application thereof in photocatalysis field | |
| Jin et al. | Highly ordered mesoporous carbon nitride nanoparticles with high nitrogen content: a metal‐free basic catalyst | |
| Luo et al. | Facile fabrication of ordered mesoporous graphitic carbon nitride for RhB photocatalytic degradation | |
| CN102320850B (en) | ZrB2-SiC composite powder and preparation method thereof | |
| Farzaneh et al. | New route for preparing nanosized boron carbide powder via magnesiothermic reduction using mesoporous carbon | |
| CN106622331B (en) | A kind of preparation method of high-specific surface area graphite phase carbon nitride photochemical catalyst | |
| EP2337631A1 (en) | Supported catalyst for synthesizing carbon nanotubes, method for preparing thereof and carbon nanotube using the same | |
| CN105174280A (en) | Nanpsheet-shaped SAPO-34 molecular sieve as well as ultrafast preparation method and application thereof | |
| US20150218004A1 (en) | Silicon carbide powder, and preparation method therefor | |
| CN103553043B (en) | Preparation method for SiC nanometer microsphere with high specific surface area | |
| CN110436934A (en) | A kind of preparation method of alpha-phase silicon nitride powder, overlength beta-silicon nitride nanowire | |
| Zhang et al. | One-pot solvothermal method to synthesize platinum/W 18 O 49 ultrafine nanowires and their catalytic performance | |
| CN105692642A (en) | Nano rodlike zirconium boride powder and preparation method thereof | |
| CN106946259A (en) | A kind of non-crystalline silicon raw powder's production technology | |
| CN105293479A (en) | Preparation method of three-dimensional orderly square-hole mesoporous graphene skeleton material | |
| CN107837816A (en) | Fe2O3/g‑C3N4Compound system and preparation method and application | |
| CN106478134B (en) | Preparation method of high-temperature-resistant low-temperature-synthesized massive spinel aerogel material | |
| CN105883805B (en) | A kind of preparation method of the high-specific surface area carbosphere based on tea seed shell base | |
| Liu et al. | Fabrication of CdS-decorated mesoporous SiC hollow nanofibers for efficient visible-light-driven photocatalytic hydrogen production | |
| CN114835122B (en) | Method for preparing silicon carbide aerogel powder from coal gangue | |
| Zheng et al. | Improving the sinterability of ZrC–SiC composite powders by Mg addition | |
| CN100432009C (en) | Carbon nanotube/nano clay nano composite materials and method for preparing same | |
| CN104445200B (en) | A kind of method preparing overlength silicon carbide nanometer line | |
| CN106423172B (en) | The inlaid hollow structure nickel-base catalyst and preparation method of carbon dioxide thermal reforming | |
| CN111569879A (en) | Method for preparing silicate/carbon composite material by using attapulgite and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20160602 Address after: 210000 Nanjing, Gulou District, Jiangsu Central Road, room 417, No. 806 Patentee after: Nanjing Xianfeng Nano Material Technology Co., Ltd. Address before: 710021 Shaanxi province Xi'an Weiyang University Park No. 1 Patentee before: Shaanxi University of Science and Technology |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20170502 Address after: 210000 Nanjing, Pukou District, Qiaolin Street step road, No. 29, No. Patentee after: Jiangsu Xianfeng nano Mstar Technology Ltd Address before: 210000 Nanjing, Gulou District, Jiangsu Central Road, room 417, No. 806 Patentee before: Nanjing Xianfeng Nano Material Technology Co., Ltd. |
|
| TR01 | Transfer of patent right |