CN102491332B - Method for preparing SiC nanobelts on SiC ceramic surface - Google Patents
Method for preparing SiC nanobelts on SiC ceramic surface Download PDFInfo
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Abstract
The invention relates to a method for preparing SiC nanobelts on an SiC ceramic surface. The method provided by the invention is characterized in that Si powder, C powder and SiO2 powder are utilized as raw materials; ferrocene as a catalyst is introduced; and a large amount of pure SiC nanobelts can be prepared on an SiC ceramic surface by a chemical vapor deposition method in the preparation period. The method provided by the invention can realize simple, low-cost and high-efficiency preparation of a large amount of pure SiC nanobelts, and can control nanobelt morphology and a nanobelt size through adjustment of preparation processes.
Description
Technical field
The present invention relates to a kind of method for preparing silicon carbide (SiC) nano belt, prepare the method for SiC nano belt at the SiC ceramic surface.
Background technology
In recent years, because nano material is in the potential using value in modern science and technology field, be subject to paying close attention to widely about the technology of preparing of monodimension nanometer material (comprising: nanotube, nano wire, nanometer rod, nano belt etc.).The one dimension SiC nano material has excellent electrology characteristic, optical characteristics and mechanical property, emission on the scene, nano electron device and advanced composite material field have potential huge applications and are worth, and wherein the SiC nano belt is the desirable monodimension nanometer material of using as emission on the scene, nano electron device and advanced composite material field.But at present domestic and international investigator reports less about the preparation method of SiC nano belt.
Document 1: " Quantum confinement effect and field emission characteristics of ultrathin3C-SiC nanobelts.Chemical Physics Letters, 461 (2008): 242～245 " have introduced a kind of Si of utilization powder, C powder and SiO
2Powder is raw material, adopts microwave method to prepare the SiC nano belt.But contain a large amount of C powder, Si powder and SiO in the product of the method preparation
2Powder need to carry out oxidative purification and sour purification process to it, and then make the preparation process of SiC nano belt more complicated.What is more important, in the oxidative purification process, the SiC nano belt of preparation also can be oxidized to a certain extent, is difficult to prepare pure SiC nano belt.Above-mentioned shortcoming has seriously limited the widespread use of this material.
Summary of the invention
The technical problem that solves
For fear of the deficiencies in the prior art part, the present invention proposes a kind of method for preparing the SiC nano belt at the SiC ceramic surface, can be simply, low-cost, prepare a large amount of pure SiC nano belt efficiently, and can control pattern and the size of nano belt by adjusting preparation technology.
Technical scheme
A kind of preparation method of SiC nano belt is characterized in that step is as follows:
Step 1: be 10～15% Si powder with mass percent, 15～30% C powder, 40～70% SiO
2Powder and 5～15% ferrocene powder mix, and then place the rosin ball grinder, ball milling combination treatment 2～4 hours;
Step 2: powder evenly is paved with the plumbago crucible bottom, above the powder of a branch of 3k carbon fiber binding SiC ceramic plate rear-mounted in plumbago crucible;
Step 3: plumbago crucible is put into the hot pressing vacuum reaction stove that graphite is heating element, after vacuum oven carried out vacuum-treat, logical Ar rose to 1600～1800 ℃ with furnace temperature from room temperature with 5～10 ℃/min heat-up rate to normal pressure, be incubated 1～3 hour, powered-down naturally cools to room temperature; Logical Ar protection in the whole process;
Step 4: take out plumbago crucible, the carbon fiber on the cleaning SiC ceramic plate obtains the SiC nano belt at the SiC ceramic plate.
Putting into baking oven after described SiC ceramic plate cleans dries.
Describedly vacuum oven is carried out vacuum-treat be: after vacuumizing 30 minutes vacuum tightness is reached-0.09MPa, empty 30 minutes of fidelity.
The purity of described Si powder is 99.5%, granularity is 300 orders.
The purity of described C powder is 99%, and granularity is 320 orders.
Described SiO
2The purity of powder is that analytical pure, granularity are 300 orders.
Described Al
2O
3The purity of powder is analytical pure, and granularity is 100～200 orders.
The purity of described ferrocene powder is analytical pure, and granularity is 300 orders.
Beneficial effect
A kind of method for preparing the SiC nano belt at the SiC ceramic surface that the present invention proposes.The method is with Si powder, C powder and SiO
2Powder is raw material, introduces simultaneously ferrocene as catalyzer, adopts chemical Vapor deposition process to go out a large amount of pure SiC nano belt at SiC ceramic surface one time to produce.The method can be simply, low-cost, prepare a large amount of pure SiC nano belt efficiently, and can control pattern and the size of nano belt by adjusting preparation technology.
Beneficial effect of the present invention: the method production cost is low, technique is simple, preparation cycle is short, and productive rate and the purity of synthetic SiC nano belt are high; In addition, can effectively control pattern and the size of synthesizing the SiC nano belt by content and the preparation temperature of adjusting ferrocene.These advantages make the method have the potentiality that the large-scale industry of developing into becomes to produce.
Description of drawings
Fig. 1: the low power SEM photo that is the prepared SiC nano belt of inventive embodiments 2
Fig. 2: the high power SEM that is the prepared SiC nano belt of inventive embodiments 2 shines
Embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
Embodiment 1:
Take by weighing respectively the Si powder of 10g, the C powder of 15g, the SiO of 70g
2The ferrocene powder of powder and 5g.Place the rosin ball grinder, get the agate ball of different quantities different diameter and put into the rosin ball grinder, carry out ball milling combination treatment 2h at planetary ball mill, obtain powder.
Above-mentioned powder is put into plumbago crucible, make it evenly be paved with crucible bottom, the SiC ceramic plate with oven dry bundlees rear-mounted above the powder surface with a branch of 3K carbon fiber again, then plumbago crucible is put into the vacuum reaction stove.After vacuumizing 30 minutes vacuum tightness is reached-0.09MPa, empty 30 minutes of fidelity is observed vacuum meter and is indicated whether to change, and as unchanged, the illustrative system sealing is intact.Logical argon gas is to normal pressure.This process triplicate.Furnace temperature is risen to 1600 ℃ afterwards, temperature rise rate is 5 ℃/min, then is incubated 3 hours.Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process.Take out subsequently plumbago crucible, the carbon fiber on the cleaning SiC ceramic plate.At last, obtain a small amount of SiC nano belt at the SiC ceramic plate.
Embodiment 2:
The SiC ceramic plate is clean with absolute ethanol washing, dry for standby in baking oven.
Take by weighing respectively the Si powder of 13g, the C powder of 22g, the SiO of 55g
2The ferrocene powder of powder and 10g.Place the rosin ball grinder, get the agate ball of different quantities different diameter and put into the rosin ball grinder, carry out ball milling combination treatment 3h at planetary ball mill, obtain powder.
Above-mentioned powder is put into plumbago crucible, make it evenly be paved with crucible bottom, the SiC ceramic plate with oven dry bundlees rear-mounted above the powder surface with a branch of 3K carbon fiber again, then plumbago crucible is put into the vacuum reaction stove.After vacuumizing 30 minutes vacuum tightness is reached-0.09MPa, empty 30 minutes of fidelity is observed vacuum meter and is indicated whether to change, and as unchanged, the illustrative system sealing is intact.Logical argon gas is to normal pressure.This process triplicate.Furnace temperature is risen to 1700 ℃ afterwards, temperature rise rate is 7 ℃/min, then is incubated 2 hours.Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process.Take out subsequently plumbago crucible, the carbon fiber on the cleaning SiC ceramic plate.At last, obtain a large amount of SiC nano belt at the SiC ceramic plate.By Fig. 1 and 2 as seen, have a large amount of SiC nano belt at the SiC ceramic surface, wherein the length of nano belt is 0.1～1mm, and width is 0.5～3 μ m, and thickness is 40～200nm.
Embodiment 3:
The SiC ceramic plate is clean with absolute ethanol washing, dry for standby in baking oven.
Take by weighing respectively the Si powder of 15g, the C powder of 30g, the SiO of 40g
2The ferrocene powder of powder and 15g.Place the rosin ball grinder, get the agate ball of different quantities different diameter and put into the rosin ball grinder, carry out ball milling combination treatment 4h at planetary ball mill, obtain powder.
Above-mentioned powder is put into plumbago crucible, make it evenly be paved with crucible bottom, the SiC ceramic plate with oven dry bundlees rear-mounted above the powder surface with a branch of 3K carbon fiber again, then plumbago crucible is put into the vacuum reaction stove.After vacuumizing 30 minutes vacuum tightness is reached-0.09MPa, empty 30 minutes of fidelity is observed vacuum meter and is indicated whether to change, and as unchanged, the illustrative system sealing is intact.Logical argon gas is to normal pressure.This process triplicate.Furnace temperature is risen to 1800 ℃ afterwards, temperature rise rate is 10 ℃/min, then is incubated 1 hour.Powered-down naturally cools to room temperature subsequently, logical argon shield in the whole process.Take out subsequently plumbago crucible, the carbon fiber on the cleaning SiC ceramic plate.At last, obtain a small amount of SiC nano belt at the SiC ceramic plate.
Among all embodiment, the purity of Si powder is 99.5%, granularity is 300 orders, and the purity of C powder is 99%, and granularity is 320 orders, SiO
2The purity of powder is that analytical pure, granularity are 300 orders, Al
2O
3The purity of powder is analytical pure, and granularity is 100～200 orders, and the purity of ferrocene powder is analytical pure, and granularity is 300 orders.
Claims (8)
1. method for preparing the nanometer silicon carbide band at the SiC ceramic surface is characterized in that step is as follows:
Step 1: be 10～15% Si powder, 15～30% C powder, 40～70% SiO with mass percent
2Powder and 5～15% ferrocene powder mix, and then place the rosin ball grinder, ball milling combination treatment 2～4 hours;
Step 2: the mixed powder of step 1 evenly is paved with the plumbago crucible bottom, above the powder of a branch of 3k carbon fiber binding SiC ceramic plate rear-mounted in plumbago crucible;
Step 3: plumbago crucible is put into the hot pressing vacuum reaction stove that graphite is heating element, after vacuum oven carried out vacuum-treat, logical Ar rose to 1600～1800 ℃ with furnace temperature from room temperature with 5～10 ℃/min heat-up rate to normal pressure, be incubated 1～3 hour, powered-down naturally cools to room temperature; Logical Ar protection in the whole process;
Step 4: take out plumbago crucible, the carbon fiber on the cleaning SiC ceramic plate obtains the SiC nano belt at the SiC ceramic plate.
2. the described method for preparing the nanometer silicon carbide band at the SiC ceramic surface according to claim 1 is characterized in that: put into baking oven after described SiC ceramic plate cleans and dry.
3. the described method for preparing the nanometer silicon carbide band at the SiC ceramic surface according to claim 1 is characterized in that: describedly vacuum oven is carried out vacuum-treat be: after vacuumizing 30 minutes vacuum tightness is reached-0.09MPa, empty 30 minutes of fidelity.
4. the described method for preparing the nanometer silicon carbide band at the SiC ceramic surface according to claim 1 is characterized in that: the purity of described Si powder is 99.5%, granularity is 300 orders.
5. the described method for preparing the nanometer silicon carbide band at the SiC ceramic surface according to claim 1, it is characterized in that: the purity of described C powder is 99%, granularity is 320 orders.
6. the described method for preparing the nanometer silicon carbide band at the SiC ceramic surface according to claim 1 is characterized in that: described SiO
2The purity of powder is that analytical pure, granularity are 300 orders.
7. the described method for preparing the nanometer silicon carbide band at the SiC ceramic surface according to claim 1 is characterized in that: described Al
2O
3The purity of powder is analytical pure, and granularity is 100～200 orders.
8. the described method for preparing the nanometer silicon carbide band at the SiC ceramic surface according to claim 1, it is characterized in that: the purity of described ferrocene powder is analytical pure, granularity is 300 orders.
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| CN102718527B (en) * | 2012-06-21 | 2013-11-06 | 西北工业大学 | Preparation method of nanobelt toughened silicon-based ceramic coating |
| CN102701207B (en) * | 2012-06-21 | 2013-10-09 | 西北工业大学 | Method for preparing Al-doped silicon carbide nanowires |
| CN106431412A (en) * | 2016-09-29 | 2017-02-22 | 芜湖市三山区绿色食品产业协会 | High-strength wear-resistant sintered silicon carbide pump shaft and production method thereof |
| CN107265460B (en) * | 2017-05-26 | 2020-02-18 | 宁波工程学院 | B-doped SiC nanobelt with large width-thickness ratio and preparation method thereof |
| CN107602154B (en) * | 2017-08-08 | 2020-10-27 | 华南理工大学 | Bead string-shaped SiC/SiO2Heterostructure and method of synthesis |
| CN115058885B (en) * | 2022-06-13 | 2024-01-30 | 西北工业大学 | Carbon fiber cloth surface orientation SiC nanowire array and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3445554A (en) * | 1966-03-11 | 1969-05-20 | Dow Corning | Manufacture of silicon carbide ribbons |
| CN1821072A (en) * | 2006-03-09 | 2006-08-23 | 中国人民解放军国防科学技术大学 | Process for preparing micrometer, sub micrometer and nonometer silicon carbide fiber |
| CN102126859A (en) * | 2011-03-03 | 2011-07-20 | 西北工业大学 | Method for preparing bamboo-shaped SiC nanowire-toughened HfC ceramic |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3445554A (en) * | 1966-03-11 | 1969-05-20 | Dow Corning | Manufacture of silicon carbide ribbons |
| CN1821072A (en) * | 2006-03-09 | 2006-08-23 | 中国人民解放军国防科学技术大学 | Process for preparing micrometer, sub micrometer and nonometer silicon carbide fiber |
| CN102126859A (en) * | 2011-03-03 | 2011-07-20 | 西北工业大学 | Method for preparing bamboo-shaped SiC nanowire-toughened HfC ceramic |
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