CN107869047A - A kind of graphene boron-nitride fibre composite and preparation method thereof - Google Patents
A kind of graphene boron-nitride fibre composite and preparation method thereof Download PDFInfo
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- CN107869047A CN107869047A CN201711150776.1A CN201711150776A CN107869047A CN 107869047 A CN107869047 A CN 107869047A CN 201711150776 A CN201711150776 A CN 201711150776A CN 107869047 A CN107869047 A CN 107869047A
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- boron nitride
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- 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
- D06M11/73—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 carbon or compounds thereof
- D06M11/74—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 carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
Abstract
The invention discloses a kind of graphene boron-nitride fibre composite and preparation method thereof, and the crosslinking to boron nitride fiber can be realized using the swelling and fusion of the graphite oxide ene coatings on boron nitride fiber surface.Graphene oxide, can be to the uniform coating of boron nitride fiber as sizing agent and crosslinking agent, and cross-linking process is quick and easy, and cross-link intensity is high.After further reduction, graphene oxide cross-linked layer is changed into graphene cross-linked layer, enhances the interaction between boron nitride fiber, reduces interfibrous contact resistance, so that boron nitride fiber shows excellent mechanical property and electrical and thermal conductivity, the enhancing phase available for composite.It is this to be crosslinked the method for boron nitride fiber with very big researching value using graphene and be widely applied prospect.
Description
Technical field
The invention belongs to composite fibre field, more particularly to a kind of graphene-boron-nitride fibre composite and its preparation
Method.
Background technology
For boron nitride fiber as a kind of new type high temperature ceramic fibre, it has unusual combination property, as high temperature resistant,
Resistant to chemical etching, excellent dielectric properties, and the chemical compatibility good with material interface, turn into ceramic base composite day
One of optimal reinforcing material of irdome, in occupation of indispensable important in the field such as Aeronautics and Astronautics and missile armament technology
Status.At home, the preparation method of boron nitride fiber is mainly inorganic chemistry conversion method.Due to preparation technology particularity and
The characteristics of material itself so that the humidity resistance of boron nitride fiber is poor.Water can react to form one layer of oxidation with boron nitride
Boron layer, and then be converted into the further moisture absorption of boric acid, the raising of fiber combination property of this phenomena impair, and then to constrain its fine
The development of composite is tieed up, therefore the introducing of boron nitride fiber surface moisture protection coating technology is imperative.It is fine in boron nitride
Dimension table face carries out coating treatment, can not only improve the humidity resistance of fiber, improves the vapour resistant erosiveness of fiber, increase
The stability of fibre property, and the defects of fiber surface stomata, micro-crack can be repaired, improve the superficiality of fiber
Energy, improve the tensile strength of fiber.
Graphene is a kind of two-dimentional carbon material with monoatomic layer thickness, has low-density, high mechanical strength, heat
Conductance and electrical conductivity and excellent corrosion resistance.Six-membered carbon ring in graphene has minimum space, and nearly all molecule is all
It can not be passed through from graphene layer, therefore many people attempt to make water proof oxygen barrier Cai's material using graphite ene coatings or compound method
Material.There is the boron oxide of nitridation boron surface the oxygen-containing functional group on high-hydrophilic, and graphene oxide can form high forces, shape
Into effective coating.Therefore using pure graphene crosslinking boron nitride fiber, boron nitride fiber can be realized by non-melt means
Boundling and non-woven fabrics, mechanical strength, the water resistance of boron nitride fiber can not only be maintained well, and material can be improved
Electrical and thermal conductivity, overall proportion is reduced, can be used as the obturator of high-performance composite materials.
The nitrogen of pure graphene crosslinking is prepared using graphene oxide swelling in a solvent and fusion by the present invention
Change boron fibre, the method compared to melting crosslinking can more preferably keep the intensity of boron nitride fiber in itself, compared to using other changes
Method crosslinking is more simple and easy, green.Due to property such as graphene high conductivity in itself, high-termal conductivity, barriers
Can, after being coated to boron nitride fiber surface, boron nitride fiber electrical and thermal conductivity in itself and water resistance can be lifted, and by
In the presence of graphene crosslinking, boron nitride fiber surface can form conductive and heat-conductive network, make in the reinforcement for composite
Enhancing can more efficiently be realized.
The content of the invention
Due to being difficult to boundling, electrical and thermal conductivity is poor, and water resistance is bad, and the application of existing boron nitride fiber receives
Limitation.The purpose of the present invention is to be directed to existing technical deficiency, there is provided a kind of graphene-boron-nitride fibre composite and its system
Preparation Method.
The purpose of the present invention is achieved through the following technical solutions：A kind of graphene-boron-nitride fibre composite, stone
Black alkene is coated on boron nitride fiber surface, and boron nitride fiber surface is connected with graphene film by Van der Waals force and hydrogen bond.Nitridation
Crosslinking is realized by being coated on the graphene on surface between boron fibre, forms zero twisted yarn, non-woven fabrics or chopped mat.
A kind of preparation method of graphene-boron-nitride fibre composite, comprises the following steps：
(1) surface coating is carried out to boron nitride fiber using graphene oxide dispersion, obtaining surface after drying is coated with
The boron nitride fiber of graphene oxide.
(2) boron nitride fiber for coating graphene oxide is placed in progress surface swelling in solvent, then merged fiber
The zero twisted yarn is formed after drying, or fiber is mutually overlapped and forms the non-woven fabrics or chopped mat after drying, dries temperature
Degree is less than 100 DEG C.
(3) graphene-boron-nitride fibre composite is obtained after reducing.
Further, the concentration of graphene oxide dispersion is 7mg/g in the step (1), and dispersant is water, N, N- bis-
It is NMF, DMAC N,N' dimethyl acetamide, ethanol, ethylene glycol, 1-METHYLPYRROLIDONE, tetrahydrofuran, dimethyl sulfoxide, two sweet
Alcohol, pyridine, dioxane, butanone, isopropanol etc..
Further, boron nitride fiber is repeatedly coated using graphene oxide dispersion in the step (1), often
Dried after secondary coating, final dried graphene oxide thickness degree is 3 μm.
Further, solvent is water, methanol, ethanol, isopropanol, ethylene glycol, glycerine, diethylene glycol (DEG) in the step (2)
Deng the organic acids such as alcohols, formic acid, acetic acid, propionic acid, butyric acid, valeric acid, ethanedioic acid, malonic acid, succinic acid, acrylic acid, acetone, fourth
Ketone, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, tetrahydrofuran, dimethyl sulfoxide, 1-METHYLPYRROLIDONE, pyridine, two
The ring of oxygen six, the aqueous solution of sodium chloride, the aqueous solution of calcium chloride, the aqueous solution of sodium nitrate, the aqueous solution of calcium nitrate, the water of sodium phosphate
Solution, the aqueous solution of potassium chloride, the aqueous solution of ammonium chloride, the aqueous solution of potassium hydroxide, sodium hydroxide the aqueous solution or these are molten
The mixed liquor of liquid.
Further, restoring method is to use hydroiodic acid, hydrazine hydrate, Vitamin C, sodium borohydride etc. in the step (3)
Chemical reducing agent is reduced or 100~600 DEG C of thermal reductions.
The beneficial effects of the present invention are：
(1) pure graphene is uniform as boron nitride fiber surface distributed, and interface adhesive strength is high, and immersion does not take off in a solvent
Fall.
(2) pure graphene is high as the cross-linking agents intensity of boron nitride fiber.Using graphene oxide in a solvent
Swelling fusion realizes the crosslinking of boron nitride fiber, and method is simple, time saving, and the solvent environmental protection of use, cross-linking effect is good, compares
Other cross-linking methods have very big application value.
The excellent mechanical property of boron nitride fiber can be kept using this cross-linking method, and the conduction of fiber can be lifted
Property, thermal conductivity etc., so as to further expand the application of boron nitride fiber material.
Brief description of the drawings
Fig. 1 is the schematic diagram of the boron nitride fiber non-woven fabrics through graphene of the present invention crosslinking.
Fig. 2 is the non-twist fine schematic diagram of boron nitride fiber being crosslinked through graphene of the present invention.
Embodiment
The method for preparing graphene-boron-nitride fibre composite comprises the following steps：
(1) surface coating is carried out to boron nitride fiber using graphene oxide dispersion, obtaining surface after drying is coated with
The boron nitride fiber of graphene oxide.The concentration of the graphene oxide dispersion is 7mg/g, and dispersant is water, N, N- diformazans
It is base formamide, DMAC N,N' dimethyl acetamide, ethanol, ethylene glycol, 1-METHYLPYRROLIDONE, tetrahydrofuran, dimethyl sulfoxide, two sweet
Alcohol, pyridine, dioxane, butanone, isopropanol etc..Boron nitride fiber is repeatedly coated using graphene oxide dispersion,
Dried every time after coating, drying temperature is about 25~200 DEG C, and final dried graphene oxide thickness degree is 3 μm.(2) will
The boron nitride fiber of coating graphene oxide is placed in progress surface swelling in solvent, then merges fiber and forms institute after drying
Zero twisted yarn is stated, or fiber is mutually overlapped and forms the non-woven fabrics or chopped mat after drying, drying temperature is less than 100 DEG C.Institute
Solvent is stated as alcohols, formic acid, acetic acid, propionic acid, butyric acid, penta such as water, methanol, ethanol, isopropanol, ethylene glycol, glycerine, diethylene glycol (DEG)s
The organic acids such as acid, ethanedioic acid, malonic acid, succinic acid, acrylic acid, acetone, butanone, N,N-dimethylformamide, N, N- dimethyl
Acetamide, tetrahydrofuran, dimethyl sulfoxide, 1-METHYLPYRROLIDONE, pyridine, dioxane, the aqueous solution of sodium chloride, calcium chloride
The aqueous solution, the aqueous solution of sodium nitrate, the aqueous solution of calcium nitrate, the aqueous solution of sodium phosphate, the aqueous solution of potassium chloride, the water of ammonium chloride
Solution, the aqueous solution of potassium hydroxide, the mixed liquor of the aqueous solution of sodium hydroxide or these solution.(3) reduce after obtain graphene-
Boron-nitride fibre composite.The restoring method is to use the electronations such as hydroiodic acid, hydrazine hydrate, Vitamin C, sodium borohydride
Agent is reduced or 100~600 DEG C of thermal reductions.
To realize the crosslinking of boron nitride fiber, graphene oxide is coated to boron nitride fiber surface by the present invention, aoxidizes stone
Black alkene and the boron oxide on boron nitride fiber surface form hydrogen bond and van der Waals interaction, realize uniformly firmly coating.Then make nitrogen
Change boron fibre superficial oxidation graphene to be swelled in a solvent, lamella obtains the larger free degree, graphene oxide layer when drying
Due to the spontaneous Close stack by the π-π active forces between the capillary force and lamella caused by solvent volatilization, therefore nitrogenize
Boron fibre is cross-linked with each other, and such as Fig. 1, shown in 2, finally gives graphene-boron-nitride fibre composite, including zero twisted yarn, nonwoven
Cloth or chopped mat etc..The boron nitride fiber of graphene crosslinking maintains the mechanical strength of boron nitride fiber fiber itself, conduction, resistance to
The performances such as corrosion, improve the thermal conductivity of boron nitride fiber, have very big actual application value.
The present invention is specifically described below by embodiment, the present embodiment is served only for doing further the present invention
It is bright, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art makes one according to the content of foregoing invention
A little nonessential changes and adjustment belong to protection scope of the present invention.
Non-woven fabrics tensile strength refers to national standard GBT 15232-1994.
Embodiment 1：
(1) drying, cycle-index are coated repeatedly to boron nitride fiber surface using the aqueous dispersions of graphene oxide
For 15 times, the boron nitride fiber that surface is coated with graphene oxide is obtained.Graphene oxide thickness degree is 3 μm；
(2) boron nitride fiber for the coating graphene oxide that step (3) obtains is placed in water and carries out surface swelling, then
Fiber is mutually overlapped and forms non-woven fabrics after drying, drying temperature is less than 100 DEG C.
(3) the graphene oxide crosslinking boron nitride fiber that step (2) obtains is placed in the closed cauldron containing hydrazine hydrate, 80
Reduced 12 hours at DEG C.
Through above step, graphene coated passes through model on boron nitride fiber surface, boron nitride fiber surface with graphene film
De Huali connects with hydrogen bond.Between boron nitride fiber crosslinking, the unordered friendship of composite fibre are realized by being coated on the graphene on surface
It is folded to form nonwoven fabric construct, surface density 90.9g/m2, fracture strength 1.98GPa, it is broken by force after 24h is soaked in 25 DEG C of water
It is 86% to spend conservation rate, and conductance is 2.3 × 104S/m, thermal conductivity 29W/mK.
In addition, graphene oxide concentration and coating layer thickness are the optimal results obtained through repetition test.It can be seen by table 1
Go out, coat under same number, when the concentration of graphene oxide is 7mg/ml, graphite oxide ene coatings are on boron nitride fiber surface
Thickness is 3 μm, and fracture strength, conductance, the thermal conductivity highest of obtained boron nitride fiber non-woven fabrics, anti-hydrolysis ability is best,
Cross-linking effect is best.The concentration of graphene oxide is smaller, and thickness of the graphene oxide on boron nitride fiber surface is smaller, obtains
Fracture strength, conductance, the thermal conductivity of boron nitride fiber non-woven fabrics are smaller, and cross-linking effect and water resistance are poorer.Graphene oxide
Concentration it is higher, graphene oxide is bigger in boron nitride fiber surface thickness, and thickness distribution is uneven, cross-link intensity decline, obtain
Fracture strength, conductance, the thermal conductivity of the boron nitride fiber non-woven fabrics arrived reduce, and anti-hydrolysis ability reduces.
Embodiment 2：
(1) boron nitride fiber surface is coated repeatedly using the N,N-dimethylformamide dispersion liquid of graphene oxide
Dry, cycle-index is 13 times, obtains the boron nitride fiber that surface is coated with graphene oxide.Graphene oxide thickness degree is 3 μ
m；
(2) boron nitride fiber for the coating graphene oxide that step (1) obtains is placed in water and carries out surface swelling, then
Fiber is mutually overlapped and forms non-woven fabrics after drying, drying temperature is less than 100 DEG C.
(3) the graphene oxide crosslinking boron nitride fiber that step (2) obtains is placed in the closed cauldron containing hydrazine hydrate, 80
Reduced 12 hours at DEG C.
Through above step, graphene coated passes through model on boron nitride fiber surface, boron nitride fiber surface with graphene film
De Huali connects with hydrogen bond.Between boron nitride fiber crosslinking, the unordered friendship of composite fibre are realized by being coated on the graphene on surface
It is folded to form nonwoven fabric construct, surface density 91.1g/m2, fracture strength 1.94GPa, it is broken by force after 24h is soaked in 25 DEG C of water
It is 84% to spend conservation rate, and conductance is 1.7 × 104S/m, thermal conductivity 26W/mK.
Embodiment 3：
(1) drying, circulation time are coated repeatedly to boron nitride fiber surface using the alcohol dispersion liquid of graphene oxide
Number is 16 times, obtains the boron nitride fiber that surface is coated with graphene oxide.Graphene oxide thickness degree is 3 μm；
(2) boron nitride fiber for the coating graphene oxide that step (3) obtains is placed in water and carries out surface swelling, then
Fiber is mutually overlapped and forms non-woven fabrics after drying, drying temperature is less than 100 DEG C.
(3) the graphene oxide crosslinking boron nitride fiber that step (2) obtains is placed in the closed cauldron containing hydroiodic acid, 90
Reduced 18 hours at DEG C.
Through above step, graphene coated passes through model on boron nitride fiber surface, boron nitride fiber surface with graphene film
De Huali connects with hydrogen bond.Between boron nitride fiber crosslinking, the unordered friendship of composite fibre are realized by being coated on the graphene on surface
It is folded to form nonwoven fabric construct, surface density 91.7g/m2, fracture strength 1.99GPa, it is broken by force after 24h is soaked in 25 DEG C of water
It is 88% to spend conservation rate, and conductance is 2.7 × 104S/m, thermal conductivity 30W/mK.
Embodiment 4：
(1) boron nitride fiber surface arranged in parallel is coated repeatedly using the ethylene glycol dispersion liquid of graphene oxide
Dry, cycle-index is 12 times, and it is fine to obtain boron nitride fiber length of the surface coated with graphene oxide.Graphene oxide thickness degree
For 3 μm；
(2) the long fibre of boron nitride fiber for the coating graphene oxide that step (1) obtains is placed in ethylene glycol and carries out surface
Swelling, then fiber is merged and forms the zero twisted yarn after drying, drying temperature is less than 100 DEG C, ethylene glycol is volatilized.
(3) the graphene oxide crosslinking boron nitride fiber length fibre that step (2) obtains is placed in the closed cauldron containing hydroiodic acid
In, reduced 18 hours at 90 DEG C.
Through above step, graphene coated passes through model on boron nitride fiber surface, boron nitride fiber surface with graphene film
De Huali connects with hydrogen bond.Between boron nitride fiber crosslinking, composite fibre parallel are realized by being coated on the graphene on surface
Row form non-twist fine structure, and fracture strength 2.09GPa, rupture strength retention is 85% after 24h is soaked in 25 DEG C of water,
Conductance is 2.4 × 104S/m, thermal conductivity 26W/mK.
Embodiment 5：
(1) coating dry repeatedly is carried out to boron nitride fiber surface arranged in parallel using the aqueous dispersions of graphene oxide
Dry, cycle-index is 15 times, obtains the boron nitride fiber that surface is coated with graphene oxide.Graphene oxide thickness degree is 3 μm；
(2) boron nitride fiber for the coating graphene oxide that step (1) obtains is placed in progress surface swelling in ethylene glycol,
Then fiber is merged and forms the zero twisted yarn after drying, drying temperature is less than 100 DEG C, ethylene glycol is volatilized.
(3) the graphene oxide crosslinking boron nitride fiber length fibre that step (2) obtains is placed in the closed cauldron containing hydroiodic acid
In, reduced 18 hours at 90 DEG C.
Through above step, graphene coated passes through model on boron nitride fiber surface, boron nitride fiber surface with graphene film
De Huali connects with hydrogen bond.Between boron nitride fiber crosslinking, composite fibre parallel are realized by being coated on the graphene on surface
Row form non-twist fine structure, and fracture strength 2.14GPa, rupture strength retention is 85% after 24h is soaked in 25 DEG C of water,
Conductance is 3.1 × 104S/m, thermal conductivity 28W/mK.
Claims (6)
1. a kind of graphene-boron-nitride fibre composite, it is characterised in that graphene coated is in boron nitride fiber surface, nitrogen
Change boron fibre surface to be connected by Van der Waals force and hydrogen bond with graphene film.By being coated on the stone on surface between boron nitride fiber
Black alkene realizes crosslinking, forms zero twisted yarn, non-woven fabrics or chopped mat.
2. a kind of preparation method of graphene-boron-nitride fibre composite, it is characterised in that comprise the following steps：
(1) surface coating is carried out to boron nitride fiber using graphene oxide dispersion, surface is obtained after drying coated with oxidation
The boron nitride fiber of graphene.
(2) boron nitride fiber for coating graphene oxide is placed in progress surface swelling in solvent, then merged fiber through dry
The zero twisted yarn is formed after dry, or fiber is mutually overlapped and forms the non-woven fabrics or chopped mat after drying, drying temperature is low
In 100 DEG C.
(3) graphene-boron-nitride fibre composite is obtained after reducing.
3. according to the method for claim 2, it is characterised in that the concentration of graphene oxide dispersion in the step (1)
For 7mg/g, dispersant is water, DMF, DMA, ethanol, ethylene glycol, N- crassitudes
Ketone, tetrahydrofuran, dimethyl sulfoxide, diethylene glycol (DEG), pyridine, dioxane, butanone, isopropanol etc..
4. according to the method for claim 2, it is characterised in that graphene oxide dispersion pair is used in the step (1)
Boron nitride fiber is repeatedly coated, and is dried every time after coating, and final dried graphene oxide thickness degree is 3 μm.
5. according to the method for claim 2, it is characterised in that solvent is water, methanol, ethanol, isopropyl in the step (2)
The alcohols such as alcohol, ethylene glycol, glycerine, diethylene glycol (DEG), formic acid, acetic acid, propionic acid, butyric acid, valeric acid, ethanedioic acid, malonic acid, succinic acid,
The organic acids such as acrylic acid, acetone, butanone, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, tetrahydrofuran, dimethyl sulfoxide,
1-METHYLPYRROLIDONE, pyridine, dioxane, the aqueous solution of sodium chloride, the aqueous solution of calcium chloride, the aqueous solution of sodium nitrate, nitre
The aqueous solution of sour calcium, the aqueous solution of sodium phosphate, the aqueous solution of potassium chloride, the aqueous solution of ammonium chloride, the aqueous solution of potassium hydroxide, hydrogen
The mixed liquor of the aqueous solution of sodium oxide molybdena or these solution.
6. according to the method for claim 2, it is characterised in that restoring method is to use hydroiodic acid, water in the step (3)
The chemical reducing agents such as conjunction hydrazine, Vitamin C, sodium borohydride are reduced or 100~600 DEG C of thermal reductions.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711150776.1A CN107869047A (en) | 2017-11-18 | 2017-11-18 | A kind of graphene boron-nitride fibre composite and preparation method thereof |
| US16/617,531 US11542411B2 (en) | 2017-05-27 | 2018-03-13 | Method for preparing composites on basis of graphene bonding |
| PCT/CN2018/078765 WO2018219008A1 (en) | 2017-05-27 | 2018-03-13 | Method for preparing composites on basis of graphene bonding |
| JP2019565907A JP6952134B2 (en) | 2017-05-27 | 2018-03-13 | Method of manufacturing composite material based on graphene adhesive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711150776.1A CN107869047A (en) | 2017-11-18 | 2017-11-18 | A kind of graphene boron-nitride fibre composite and preparation method thereof |
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| CN107869047A true CN107869047A (en) | 2018-04-03 |
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| CN201711150776.1A Withdrawn CN107869047A (en) | 2017-05-27 | 2017-11-18 | A kind of graphene boron-nitride fibre composite and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104591551A (en) * | 2015-01-16 | 2015-05-06 | 东华大学 | Preparation method of graphene-coated glass fiber composite material |
| CN106948165A (en) * | 2017-04-28 | 2017-07-14 | 浙江大学 | A kind of graphene fiber of fusion certainly and preparation method thereof |
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2017
- 2017-11-18 CN CN201711150776.1A patent/CN107869047A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104591551A (en) * | 2015-01-16 | 2015-05-06 | 东华大学 | Preparation method of graphene-coated glass fiber composite material |
| CN106948165A (en) * | 2017-04-28 | 2017-07-14 | 浙江大学 | A kind of graphene fiber of fusion certainly and preparation method thereof |
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Application publication date: 20180403 |