CN105967187A - Preparation method of carbon nano tube @SiC composite powder - Google Patents
Preparation method of carbon nano tube @SiC composite powder Download PDFInfo
- Publication number
- CN105967187A CN105967187A CN201610304749.4A CN201610304749A CN105967187A CN 105967187 A CN105967187 A CN 105967187A CN 201610304749 A CN201610304749 A CN 201610304749A CN 105967187 A CN105967187 A CN 105967187A
- Authority
- CN
- China
- Prior art keywords
- carbon nano
- nano tube
- cnt
- sic composite
- preparation
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of carbon nano tube @SiC composite powder. The preparation method of the carbon nano tube @SiC composite powder is characterized by comprising the following steps of adopting ammonium persulfate to oxidate a carbon nano tube so as to introduce carboxyl: adding the carbon nano tube into an ammonium persulfate solution, adding a silver nitrate solution at the same time, and filtering and drying to obtain a carboxylation carbon nano tube; adding the carboxylation carbon nano tube into dimethylsulfoxide, heating and refluxing, then removing unreacted dimethylsulfoxide through distilling, and obtaining an acylating chlorination carbon nano tube; dispersing the acylating chlorination carbon nano tube into dichloromethane, adding a silane coupling agent, reacting under an ice-bath condition, and spraying a mixed liquor onto silicon carbide powder, so as to obtain the carbon nano tube @SiC composite powder. The invention provides the preparation method of the carbon nano tube @SiC composite powder, which adopts a chemical bonding method to attach the multiwalled carbon nano tube onto the surface of SiC powder in a bonding way to form the composite material, is simple in process and low in cost, and can realize mass production.
Description
Technical field
The present invention relates to the preparation method of a kind of CNT@SiC composite granule, be specifically related to a kind of by changing
Learn the method that the method for bonding prepares CNT@SiC composite granule.
Background technology
As in industrial circle important parts-mechanical seal ring, having half of materials is carborundum, these
High performance sealing member has been successfully applied at auto pump, chemical industry, petroleum refining, mining, paper pulp, paper
The wide spectrums such as reason, Mixing Machine, refrigerant condenser.Along with the progress of science and technology and opening up of carborundum application
Exhibition, the performance of carbofrax material is had higher requirement by people.The carborundum using CNT to strengthen is multiple
Condensation material, not only can improve the toughness of material, moreover it is possible to significantly improve the intensity of material.CNT strengthens carbonization
The lifting of silicon composite performance, can improve the reliability of carborundum sealing member, expands the range of device,
The physical life of elongate member.
Existing CNT strengthens SiC raw material powder two kinds of methods, and a kind of is the method for simple and mechanical mixing.
Another kind is to utilize CVD method at surface of SiC in-situ growing carbon nano tube.The method low cost of mechanical mixture,
Technique is simple, but the lack of homogeneity of material powder, the adhesion between CNT and SiC powder body is weak, carbon nanometer
Toughness reinforcing DeGrain, prepared material property cannot obtain raising, even result in decline.CVD is former
Mixed powder uniformity prepared by the method for position growth is good, and between CNT and SiC powder body, adhesion is strong, but work
Skill complexity cost is high, is unfavorable for that Large scale processes produces.
Summary of the invention
To be solved by this invention is the high performance CNT of strong bonding/SiC composite granule large-scale production
Problem.
In order to solve the problems referred to above, the invention provides the preparation method of a kind of CNT@SiC composite granule,
It is characterized in that, use ammonium persulfate oxide/carbon nanometer tube to introduce carboxyl, specifically comprise the following steps that
Step 1): in the ammonium persulfate solution that 1 liter of concentration is 1mol/L, add 2g CNT, simultaneously
Adding 1mL concentration is the silver nitrate solution of 0.1mol/L, and stirring 3-8 is after individual hour, and filtration drying obtains carboxylic
Base carbon nano tube；
Step 2): in step 1) obtained by carboxylic carbon nano-tube, join in 200mL dimethyl sulfoxide,
It is heated to reflux 1-3 hour, then removes unreacted dimethyl sulfoxide by distillation, it is thus achieved that chloride carbon nanometer
Pipe；
Step 3): by step 2) obtained by chloride CNT be dispersed in 100mL dichloromethane,
Add 1mL silane coupler, react 5-8 hour under condition of ice bath；
Step 4): under mechanical agitation, by step 3) prepare mixed liquor be sprayed onto 100g-2000g
On silicon carbide powder, and stir 30 minutes, be then dried, it is thus achieved that CNT@SiC composite granule.
Preferably, described silane coupler is KH550.
The invention provides a kind of method using chemical bonding and multi-walled carbon nano-tubes bonding is attached to SiC powder
Surface constitutes composite, and technique is simple, low cost, can realize large-scale production.
Detailed description of the invention
For making the present invention become apparent, hereby with preferred embodiment, it is described in detail below.
Embodiment 1
1. use ammonium persulfate oxide/carbon nanometer tube to introduce carboxyl: in the ammonium persulfate solution of 1 liter of 1mol/L
Add 2g CNT, be simultaneously introduced the silver nitrate solution of 1ml0.1mol/L, stir 5 hours.Then
Filtration drying obtains carboxylic carbon nano-tube.
2., by the carboxylic carbon nano-tube obtained by step 1, add 200ml dimethyl sulfoxide, be heated to reflux 1
Hour, then remove unreacted dimethyl sulfoxide by distillation, it is thus achieved that chloride CNT.
3. the chloride CNT obtained by step 2 is dispersed in 100ml dichloromethane, adds 1ml silicon
Alkane coupling agent KH550, reacts 8 hours under condition of ice bath.
4. under mechanical agitation, liquid mixed above is sprayed onto on 100g silicon carbide powder, and stirs
30 minutes, then it is dried, it is thus achieved that CNT@SiC composite granule.
Embodiment 2
1. use ammonium persulfate oxide/carbon nanometer tube to introduce carboxyl: in the ammonium persulfate solution of 1 liter of 1mol/L
Add 2g CNT, be simultaneously introduced the silver nitrate solution of 1ml0.1mol/L, stir 5 hours.Then
Filtration drying obtains carboxylic carbon nano-tube.
2., by the carboxylic carbon nano-tube obtained by step 1, add 200ml dimethyl sulfoxide, be heated to reflux 1
Hour, then remove unreacted dimethyl sulfoxide by distillation, it is thus achieved that chloride CNT.
3. the chloride CNT obtained by step 2 is dispersed in 100ml dichloromethane, adds 1ml silicon
Alkane coupling agent KH550, reacts 8 hours under condition of ice bath.
4. under mechanical agitation, liquid mixed above is sprayed onto on 500g silicon carbide powder, and stirs
30 minutes, then it is dried, it is thus achieved that CNT@SiC composite granule.
Embodiment 3
1. use ammonium persulfate oxide/carbon nanometer tube to introduce carboxyl: in the ammonium persulfate solution of 1 liter of 1mol/L
Add 2g CNT, be simultaneously introduced the silver nitrate solution of 1ml0.1mol/L, stir 5 hours.Then
Filtration drying obtains carboxylic carbon nano-tube.
2., by the carboxylic carbon nano-tube obtained by step 1, add 200ml dimethyl sulfoxide, be heated to reflux 1
Hour, then remove unreacted dimethyl sulfoxide by distillation, it is thus achieved that chloride CNT.
3. the chloride CNT obtained by step 2 is dispersed in 100ml dichloromethane, adds 1ml silicon
Alkane coupling agent KH550, reacts 8 hours under condition of ice bath.
4. under mechanical agitation, liquid mixed above is sprayed onto on 2000g silicon carbide powder, and stirs
30 minutes, then it is dried, it is thus achieved that CNT@SiC composite granule.
Claims (2)
1. the preparation method of a CNT SiC composite granule, it is characterised in that use ammonium persulfate carbonoxide
Nanotube introduces carboxyl, specifically comprises the following steps that
Step 1): in the ammonium persulfate solution that 1 liter of concentration is 1mol/L, add 2g CNT, simultaneously
Adding 1mL concentration is the silver nitrate solution of 0.1mol/L, and stirring 3-8 is after individual hour, and filtration drying obtains carboxylic
Base carbon nano tube；
Step 2): in step 1) obtained by carboxylic carbon nano-tube, join in 200mL dimethyl sulfoxide,
It is heated to reflux 1-3 hour, then removes unreacted dimethyl sulfoxide by distillation, it is thus achieved that chloride carbon nanometer
Pipe；
Step 3): by step 2) obtained by chloride CNT be dispersed in 100mL dichloromethane,
Add 1mL silane coupler, react 5-8 hour under condition of ice bath；
Step 4): under mechanical agitation, by step 3) prepare mixed liquor be sprayed onto 100g-2000g
On silicon carbide powder, and stir 30 minutes, be then dried, it is thus achieved that CNT@SiC composite granule.
2. the preparation method of CNT@SiC composite granule as claimed in claim 1, it is characterised in that described
Silane coupler is KH550.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610304749.4A CN105967187B (en) | 2016-05-10 | 2016-05-10 | A kind of preparation method of carbon nanotube@SiC composite granules |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610304749.4A CN105967187B (en) | 2016-05-10 | 2016-05-10 | A kind of preparation method of carbon nanotube@SiC composite granules |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105967187A true CN105967187A (en) | 2016-09-28 |
| CN105967187B CN105967187B (en) | 2018-10-26 |
Family
ID=56991513
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610304749.4A Active CN105967187B (en) | 2016-05-10 | 2016-05-10 | A kind of preparation method of carbon nanotube@SiC composite granules |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105967187B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110297021A (en) * | 2019-06-28 | 2019-10-01 | 济南大学 | Bismuth dopen Nano SiC/carbon nanotube paste electrode sensor preparation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW200934861A (en) * | 2008-02-01 | 2009-08-16 | Jun-Wei Su | Thermal interface material, manufacturing method thereof, and electronic device applying the material |
-
2016
- 2016-05-10 CN CN201610304749.4A patent/CN105967187B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW200934861A (en) * | 2008-02-01 | 2009-08-16 | Jun-Wei Su | Thermal interface material, manufacturing method thereof, and electronic device applying the material |
Non-Patent Citations (2)
| Title |
|---|
| TIANLE ZHOU等: "Improved thermal conductivity of epoxy composites using a hybrid multi-walled carbon nanotube/micro-SiC filler", 《CARBON》 * |
| YUBING WANG等: "Rapid, low temperature microwave synthesis of novel carbon nanotube–silicon carbide composite", 《CARBON》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110297021A (en) * | 2019-06-28 | 2019-10-01 | 济南大学 | Bismuth dopen Nano SiC/carbon nanotube paste electrode sensor preparation method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105967187B (en) | 2018-10-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105949760B (en) | A kind of spinning grade high heat conduction graphene/nylon composite materials in-situ polymerization method for preparing | |
| Sun et al. | Development of a dispersion process for carbon nanotubes in ceramic matrix by heterocoagulation | |
| CN106012082A (en) | Polyamide or blend/graphene composite material wire rod and preparation method thereof | |
| CN103922307B (en) | Magnetic carbon nanotube and preparation method thereof | |
| KR102596377B1 (en) | Carbonaceous magnesium-containing composite material and method for synthesizing the same | |
| CN102093715B (en) | Preparation method of carbon nanotube reinforced polyimide nano composite material | |
| JP2018524450A5 (en) | ||
| CN102992374B (en) | Preparation method of calcium carbonate micro-spheres | |
| Wang et al. | Direct liquid phase exfoliation of graphite to produce few-layer graphene by microfluidization | |
| CN105907042B (en) | A kind of functionalized carbon nano-tube epoxy resin nano composites and preparation method thereof | |
| CN105175781B (en) | The silicon dioxide modified carbon nanotube rod-like nano composite material of organic spherical shape and preparation method | |
| JPWO2018168346A1 (en) | Method for producing surface-treated carbon nanostructure | |
| CN101249959A (en) | Carbon/carbon composite nano-tube material having large specific surface area and preparation thereof | |
| CN104495779A (en) | Simple and efficient method for preparing three-dimensional carbon nanotubes/graphene hybrid material | |
| CN105967187A (en) | Preparation method of carbon nano tube @SiC composite powder | |
| CN106032587A (en) | Amido reinforced graphene fiber and preparation method thereof | |
| Chen et al. | Continuous productions of highly fluorescent carbon dots and enriched polymer nanofibers via microfluidic techniques | |
| CN103806088B (en) | Method for preparing calcium carbonate whisker by taking triethanolamine as aid | |
| CN106185866B (en) | A kind of preparation method of cold plasma N doping multi-walled carbon nanotube | |
| CN106629679A (en) | Mass production technique of graphene | |
| JP2015147187A (en) | Method for separation of nano material | |
| CN107384276A (en) | The preparation method of one specific admixture functionalized carbon nano-tube and nano particle modified synergic epoxyn | |
| CN108295899B (en) | Two-dimensional copper-based nanosheet catalyst, and preparation method and application thereof | |
| CN111620314A (en) | Preparation method and application of phenylboronic acid modified carbon nitride quantum dots | |
| CN104559340B (en) | Halobenzene functionalized and modified carbon nano tube and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |