CN109518307A - One kind having test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method - Google Patents
One kind having test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method Download PDFInfo
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- CN109518307A CN109518307A CN201811573337.6A CN201811573337A CN109518307A CN 109518307 A CN109518307 A CN 109518307A CN 201811573337 A CN201811573337 A CN 201811573337A CN 109518307 A CN109518307 A CN 109518307A
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- multilevel structure
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- nano line
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/80—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides
- D06M11/81—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides with boron; with boron halides; with fluoroborates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Carbon And Carbon Compounds (AREA)
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Abstract
The invention discloses one kind to have test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method, the method is using carbon fiber felt as carbon source, and unformed boron powder is boron source, and metal salt solution is catalyst, carries out high temperature sintering in an inert atmosphere, ultimately forms test tube brush type B4C nano line/fiber C multilevel structure fiber.B prepared by the present invention4C nano line/fiber C multilevel structure fiber has unique test tube brush type pattern and multilevel structure, and pattern is adjustable, can adjust B in multilevel structure fiber by change sintering reaction temperature, sintered heat insulating time, catalyst concn4The quantity and length of C branch nano wire.That method of the invention has the advantages that is convenient, is easy to amplify and industrial production, the B of preparation4C nano line/fiber C multilevel structure fiber can be used for Protective armor, inhale wave, catalysis, environmental protection, semiconductor material and nuclear defence material.
Description
Technical field
The invention belongs to field of material technology, are related to a kind of with test tube brush type B4C nano line/fiber C multilevel structure is fine
The preparation method of dimension.
Background technique
Boron carbide is a kind of with hardness is high, wearability is good, resistance to acid and alkali is strong and the lesser material of density.In nature
In, the hardness of boron carbide is only second to diamond and cubic boron nitride material.In addition, there is boron carbide good neutron and oxygen to inhale
Receipts ability has been applied to wear-resistant material, refractory material, nuclear industry, shellproof, aerospace and high temperature high-energy particle radiation environment etc. at present
Field.There are a large amount of covalent bond in boron carbide material, directionality keeps traditional boron carbide ceramics material there are brittleness big
Disadvantage.The boron carbide nano material of one-dimentional structure has excellent mechanical property, has in resin, ceramics and metal enhancing field
Important application prospect.Preparation method currently about one-dimensional boron carbide nano wires material is extremely limited, mainly uses and is received with carbon
Mitron is the preparation process of template or chemical vapor deposition.These preparation methods process is cumbersome, and time and money cost is high,
It cannot achieve the large-scale production of industrialization.Also, current boron carbide one-dimentional structure material structure and ingredient are single, test tube brush type
Multilevel structure design makes test tube brush type villiform material and limb material there are higher geometric effect and a large amount of branch node,
The transfer and polarization for being conducive to electronics between reinforcing material are led in high-energy radiation protection, energy storage, catalysis and electro-magnetic wave absorption etc.
Domain has broad application prospects.
Summary of the invention
In order to solve the problems, such as that existing one-dimensional boron carbide nano material expanding production difficulty and structure are single, the present invention provides
A kind of easy, low cost has test tube brush type B suitable for industrial volume production4C nano line/fiber C multilevel structure fiber system
Preparation Method.
The purpose of the present invention is what is be achieved through the following technical solutions:
One kind having test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method, includes the following steps:
One, pre-treatment: carbon fiber felt material being sequentially placed into cleaning solution and ethanol solution and is ultrasonically treated, after dry
Carbon fiber felt after obtaining pre-treatment；
Two, boron source-metallic catalyst mixed solution configuration: boron source and metallic catalyst are dissolved in solvent respectively, so
After mix ultrasonic disperse, obtain uniformly mixed boron source-metallic catalyst mixed solution；
Three, immersion treatment: by the soak carbon fibre felt after pre-treatment in boron source-metallic catalyst mixed solution, then
Drying is taken out, the carbon fiber felt raw material that load has boron source and metallic catalyst is obtained；
Four, sintering processes: the carbon fiber felt raw material of boron source and metallic catalyst is placed in crucible load, with inertia
Gas is sintered in tube furnace, is cooled to room temperature after reaction, can be obtained the B with test tube brush type as protection gas4C
Nano wire/fiber C multilevel structure fiber.
The above method prepares test tube brush type B4C nano line/fiber C multilevel structure fiber principle is mainly B4C nano line
VLS growth mechanism.Firstly, metal salt substance is decomposed to form metal oxide (such as Ni (NO at high temperature3)2It is obtained after decomposition
NiO), then, C and B simple substance is reduced to metal simple-substance, while generating gas phase CO and B2O3, metallic catalyst is in hot conditions
Under exist with drops, adsorb the CO and B of gas phase2O3, finally on fiber C felt surface, forming core grows to obtain B4C nano line.With
Metal salt is Ni (NO3)2For, correlated response equation is as follows:
Ni(NO3)2→NiO (1)；
C+NiO→CO(g)+Ni (2)；
B+NiO→B2O3(g)+Ni (3)；
CO(g)+B2O3(g)→B4C+CO2(g) (4)。
Compared with the prior art, the present invention has the advantage that
1, carbon fiber felt used in the present invention is using activated carbon as raw material, itself is again fiber, is had the advantages that
(1) carbon fiber felt has the specific surface area and excellent adsorptivity ability of superelevation, boron source and gold in the sufficient adsorbent solution of energy
Metal catalyst is conducive to sufficiently reacting for boron source and carbon source；(2) carbon fiber felt is the felty texture of fiber interweaving, shape size
It is adjustable, have flexibility, compared with powdered carbon source, it is easier to be prepared can practical application composite fibre；(3) carbon fiber
The flexibility of felt geomery and cheap advantage are test tube brush type B4C nano line/fiber C multilevel structure fiber is big
Bulk industrial production is laid a good foundation.
2, B of the present invention4C nano line/fiber C multilevel structure fiber preparation method have it is convenient, be easy to amplify and industry
The advantages of production, the B of preparation4C nano line/fiber C multilevel structure fiber can be used for Protective armor, inhale wave, catalysis, environmental protection, half
Conductor material and nuclear defence material.
3, B prepared by the present invention4C nano line/fiber C multilevel structure fiber has unique test tube brush type pattern and multistage
Structure, and pattern is adjustable, it can be by changing sintering reaction temperature, sintered heat insulating time, catalyst concn adjusting multilevel structure
B in fiber4The quantity and length of C branch nano wire.
Detailed description of the invention
Fig. 1 is the SEM image of carbon fiber felt；
Fig. 2 is test tube brush type B prepared by embodiment 14C nano line/fiber C multilevel structure fiber SEM image, a-2 μm,
B-10 μm, c-10 μm,
Fig. 3 is test tube brush type B prepared by embodiment 24C nano line/fiber C multilevel structure fiber SEM image,
Fig. 4 is test tube brush type B prepared by embodiment 34C nano line/fiber C multilevel structure fiber SEM image.
Specific embodiment
Further description of the technical solution of the present invention with reference to the accompanying drawing, and however, it is not limited to this, all to this
Inventive technique scheme is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered
Within the protection scope of the present invention.
Specific embodiment 1: present embodiments provide for one kind to have test tube brush type B4C nano line/fiber C multistage knot
The preparation method of structure fiber, for the method using carbon fiber felt as carbon source, unformed boron powder is boron source, and metal salt solution is catalysis
Agent carries out high temperature sintering in an inert atmosphere, ultimately forms test tube brush type B4C nano line/fiber C multilevel structure fiber,
Specific implementation step is as follows:
One, by carbon fiber felt material cutting at the shape of appropriate size, cleaning solution and ethanol solution pre-treatment: are sequentially placed into
In be ultrasonically treated, obtain the carbon fiber felt after pre-treatment after dry, in which: the fibre diameter of the carbon fiber felt 5~
Between 10 μm；The cleaning solution is acid solution or aqueous slkali, and acid solution is HCl solution, H2SO4Solution and HNO3In solution
One kind, aqueous slkali are KOH solution, Ca (OH)2One of solution and NaOH solution；The concentration of the cleaning solution be 0.4~
20wt%；The sonication treatment time is 5~100min；The drying temperature is 30~200 DEG C；
Two, boron source-metallic catalyst mixed solution configuration: boron source and metallic catalyst are dissolved in solvent respectively, so
After mix ultrasonic disperse, obtain uniformly mixed boron source-metallic catalyst mixed solution, in which: the boron source is unformed to receive
Rice boron powder, partial size is between 0.2~5 μm；The solvent is water or ethyl alcohol；The metallic catalyst is nitrate, hydrochloride
Or sulfate；Concentration of the boron source in boron source-metallic catalyst mixed solution is 0.01~2.4g/mL；The boron source and
The molar ratio of metal salt is 6:0.2~2；The ultrasonic disperse time is 5~200min；
Three, immersion treatment: by the soak carbon fibre felt after pre-treatment in boron source-metallic catalyst mixed solution, then
Drying is taken out, the carbon fiber felt raw material that load has boron source and metallic catalyst is obtained, in which: the drying temperature is 25~200
℃；The soaking time is 0.1~5h；
Four, sintering processes: the carbon fiber felt raw material of boron source and metallic catalyst is placed in crucible load, with inertia
Gas is sintered in tube furnace, is cooled to room temperature after reaction, can be obtained the B with test tube brush type as protection gas4C
Nano wire/fiber C multilevel structure fiber, in which: the crucible is alumina crucible, silicon carbide crucible or graphite crucible；It is described
Inert gas is argon gas or nitrogen；The sintering temperature is 1100~1300 DEG C, and heating rate is 3~10 DEG C/min, heat preservation
Time is 2~6h.
Specific embodiment 2: present embodiment and specific embodiment one is not both: in step 2, the nitrate
For ferric nitrate or cobalt nitrate；The hydrochloride is hydrochloric acid iron, hydrochloric acid cobalt or hydrochloric acid nickel；The sulfate is ferric sulfate, cobaltous sulfate
Or nickel sulfate.
Specific embodiment 3: present embodiment is not both with specific embodiment one: in step 4, the sintering reaction
Temperature is 1100 DEG C.
Specific embodiment 4: present embodiment is not both with specific embodiment one: in step 4, the sintering reaction
Temperature is 1300 DEG C.
Specific embodiment 5: present embodiment is not both with specific embodiment one: in step 4, the heating rate
For 10 DEG C/min.
Specific embodiment 6: present embodiment is not both with specific embodiment one: in step 4, the reaction heat preservation
Time is 2h.
Specific embodiment 7: present embodiment is not both with specific embodiment one: in step 4, the soaking time
For 6h.
Effect of the invention is verified using following embodiments:
Embodiment 1:
One kind having test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method, the method are specifically
It completes according to the following steps:
One, pre-treatment: by carbon fiber felt material cutting at 50mm × 30mm × 5mm shape, then successively in 10wt%
Dust technology and dehydrated alcohol in be ultrasonically treated 30min, obtain the carbon fiber felt after pre-treatment after dry；
Two, boron source-metallic catalyst mixed solution configuration: respectively by the unformed boron powder of 4g and 3.5gNi (NO3)2·
6H2O is dissolved in the ethanol solution of 40mL, then mixes ultrasonic disperse 40min, obtains uniformly mixed containing boron powder and Ni
(NO3)2·6H2The ethanol solution of O；
Three, the carbon fiber felt after pre-treatment immersion treatment: is being contained into boron powder and Ni (NO3)2·6H2In the ethanol solution of O
1.5h is impregnated, drying is then taken out, obtains the carbon fiber felt raw material that load has boron source and metallic catalyst；
Four, sintering processes: having the carbon fiber felt raw material of boron source and metallic catalyst to be placed in alumina crucible load,
It is then charged into tube furnace, using argon gas as protection gas, is warming up to 1200 DEG C with the rate of 5 DEG C/min, when sintered heat insulating
Between be 4h, be cooled to room temperature, can be obtained with test tube brush type B after reaction4C nano line/fiber C multilevel structure fiber.
The test tube brush type B that the present embodiment is prepared is observed using scanning electron microscope4C nano line/fiber C multistage knot
The pattern of structure fiber.As can be seen from Figure 1: for carbon fiber diameter between 5~10 μm, there is step-like striped on surface.From Fig. 2 b
Original state is preferably saved with can be seen that carbon fiber as inner core in the SEM image of Fig. 2 c, there are many suedes on its surface
Hairy B4C nano line, they are come out from carbon fiber surface growth in situ, and diameter is 200~500nm, and length is 10 μm of left sides
It is right.It can be seen that the carbon fiber surface in carbon fiber felt from the image of Fig. 2 a and all overgrow with uniform B4C nano line.This explanation
Method of the invention can obtain the test tube brush type B being evenly coated4C nano line/fiber C multilevel structure fiber.
Embodiment 2:
The present embodiment is unlike the first embodiment: the sintered heat insulating time in step 4 is 2h.It can from the SEM image of Fig. 3
To find out, as soaking time shorter (2h), it can be seen that the B on carbon fiber felt surface4C nano line number amount is with respect in embodiment 1
It is less, length is also shorter.
Embodiment 3:
The present embodiment is unlike the first embodiment: Ni (NO being added in step 23)2·6H2The quality of O is 8g.
It can be seen that from the SEM image of Fig. 4 when improving the content of metallic catalyst, can obviously observe carbon fiber
The B on felt surface4C nano line number quantitative change is more, and length also has greatly increased, part B4The length of C nano line 20 μm with
On.
Claims (10)
1. one kind has test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method, it is characterised in that the method
Include the following steps:
One, pre-treatment: carbon fiber felt material being sequentially placed into cleaning solution and ethanol solution and is ultrasonically treated, and is obtained after dry
Carbon fiber felt after pre-treatment；
Two, boron source-metallic catalyst mixed solution configuration: boron source and metallic catalyst are dissolved in solvent respectively, then mixed
Ultrasonic disperse is closed, uniformly mixed boron source-metallic catalyst mixed solution is obtained, control boron source is mixed in boron source-metallic catalyst
The concentration in solution is closed as 0.01~2.4g/mL, the molar ratio of boron source and metal salt is 6:0.2~2；
Three, it immersion treatment: by the soak carbon fibre felt after pre-treatment in boron source-metallic catalyst mixed solution, then takes out
It is dry, obtain the carbon fiber felt raw material that load has boron source and metallic catalyst；
Four, sintering processes: the carbon fiber felt raw material of boron source and metallic catalyst is placed in crucible load, with inert gas
It as protection gas, is sintered in tube furnace, is cooled to room temperature after reaction, that is, obtain the B with test tube brush type4C nano line/
Fiber C multilevel structure fiber, control sintering temperature are 1100~1300 DEG C, and heating rate is 3~10 DEG C/min, and soaking time is
2~6h.
2. according to claim 1 have test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method,
It is characterized in that in the step 1, the fibre diameter of carbon fiber felt is between 5~10 μm.
3. according to claim 1 have test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method,
It is characterized in that in the step 1, cleaning solution is acid solution or aqueous slkali, and acid solution is HCl solution, H2SO4Solution and HNO3
One of solution, aqueous slkali are KOH solution, Ca (OH)2One of solution and NaOH solution, the concentration of cleaning solution are 0.4
~20wt%
4. according to claim 1 have test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method,
It is characterized in that in the step 1, sonication treatment time is 5~100min, and drying temperature is 30~200 DEG C.
5. according to claim 1 have test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method,
It is characterized in that in the step 2, boron source is armorphous nano boron powder, and for partial size between 0.2~5 μm, solvent is water or second
Alcohol.
6. according to claim 1 have test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method,
It is characterized in that in the step 2, metallic catalyst is nitrate, hydrochloride or sulfate.
7. according to claim 6 have test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method,
It is characterized in that the nitrate is ferric nitrate or cobalt nitrate, hydrochloride is hydrochloric acid iron, hydrochloric acid cobalt or hydrochloric acid nickel, and sulfate is sulfuric acid
Iron, cobaltous sulfate or nickel sulfate.
8. according to claim 1 have test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method,
It is characterized in that in the step 2, the ultrasonic disperse time is 5~200min.
9. according to claim 1 have test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method,
It is characterized in that in the step 3, drying temperature is 25~200 DEG C；Soaking time is 0.1~5h.
10. according to claim 1 have test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method,
Be characterized in that in the step 4, crucible be alumina crucible, silicon carbide crucible or graphite crucible, inert gas be argon gas or
Nitrogen.
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| CN201811573337.6A CN109518307A (en) | 2018-12-21 | 2018-12-21 | One kind having test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method |
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| CN201811573337.6A CN109518307A (en) | 2018-12-21 | 2018-12-21 | One kind having test tube brush type B4C nano line/fiber C multilevel structure fiber preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112608156A (en) * | 2020-12-29 | 2021-04-06 | 黑龙江冠瓷科技有限公司 | Preparation method of micro-nano mixed SiC chopped fibers |
| CN114956842A (en) * | 2022-05-05 | 2022-08-30 | 武汉工程大学 | Boron carbide fiber/boron carbide ceramic composite material and preparation method thereof |
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| JPH0465519A (en) * | 1990-07-04 | 1992-03-02 | Toray Ind Inc | Polyester monofilament |
| CN101850969A (en) * | 2010-02-11 | 2010-10-06 | 浙江工业大学 | Method for synthesizing boron carbide nano wires by using plant fibers |
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2018
- 2018-12-21 CN CN201811573337.6A patent/CN109518307A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0465519A (en) * | 1990-07-04 | 1992-03-02 | Toray Ind Inc | Polyester monofilament |
| CN101850969A (en) * | 2010-02-11 | 2010-10-06 | 浙江工业大学 | Method for synthesizing boron carbide nano wires by using plant fibers |
Non-Patent Citations (2)
| Title |
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| XINYONG TAO等: ""B4C-Nanowires/Carbon-Microfiber Hybrid Structures and Composites from Cotton T-shirts"", 《ADVANCED MATERIALS》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112608156A (en) * | 2020-12-29 | 2021-04-06 | 黑龙江冠瓷科技有限公司 | Preparation method of micro-nano mixed SiC chopped fibers |
| CN114956842A (en) * | 2022-05-05 | 2022-08-30 | 武汉工程大学 | Boron carbide fiber/boron carbide ceramic composite material and preparation method thereof |
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