CN108342897A - A kind of carbon fiber surface aluminium oxide nano film and preparation method thereof - Google Patents
A kind of carbon fiber surface aluminium oxide nano film and preparation method thereof Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 179
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 113
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 113
- 239000002120 nanofilm Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 40
- 238000001035 drying Methods 0.000 claims abstract description 38
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000001257 hydrogen Substances 0.000 claims abstract description 34
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 34
- 238000006056 electrooxidation reaction Methods 0.000 claims abstract description 21
- 239000004411 aluminium Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims description 15
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 8
- 238000005269 aluminizing Methods 0.000 claims description 7
- 230000001681 protective effect Effects 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 235000013339 cereals Nutrition 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 239000000835 fiber Substances 0.000 abstract description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 13
- 230000008569 process Effects 0.000 description 7
- 238000005229 chemical vapour deposition Methods 0.000 description 6
- 238000004506 ultrasonic cleaning Methods 0.000 description 6
- 238000000576 coating method Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 230000003078 antioxidant effect Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000009401 outcrossing Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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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
- D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/45—Oxides or hydroxides of elements of Groups 3 or 13 of the Periodic Table; Aluminates
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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
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
-
- 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
- D06M11/01—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 hydrogen, water or heavy water; with hydrides of metals or complexes thereof; with boranes, diboranes, silanes, disilanes, phosphines, diphosphines, stibines, distibines, arsines, or diarsines or complexes thereof
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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
- D06M11/83—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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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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
- 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 Or Physical Treatment Of Fibers (AREA)
- Inorganic Fibers (AREA)
Abstract
The present invention relates to carbon fibre material fields, in particular to a kind of carbon fiber surface aluminium oxide nano film and preparation method thereof.Including：Carbon fiber is handled in a hydrogen atmosphere, and to treated, carbon fiber is vacuum aluminum-coated；To carbon fiber surface aluminizer progress electrochemical oxidation, deionized water is then used to be cleaned by ultrasonic, is dry, vacuum suck alumina sol after drying, drying is simultaneously sintered.It is handled under hydrogen atmosphere, removes hydroxyl, carbonyl of carbon fiber surface etc., electrochemical oxidation makes aluminium film be converted into pellumina.Alumina sol is filled in micropore, is re-sintered, about 110 nanometers of the thickness for the carbon fiber surface aluminium oxide nano film being prepared, fine and close and not easily to fall off.The carbon fiber surface aluminium oxide nano film that preparation method provided in an embodiment of the present invention is prepared has many advantages, such as high intensity, high-modulus, high temperature resistant, low-density, corrosion-resistant.
Description
Technical field
The present invention relates to carbon fibre material field, in particular to a kind of carbon fiber surface aluminium oxide nano film and its
Preparation method.
Background technology
Carbon fiber has high intensity, high-modulus, high temperature resistant, low-density, the series of advantages such as corrosion-resistant, Aeronautics and Astronautics,
The various fields such as automobile are widely used.But carbon fiber starts to aoxidize for 400 DEG C or so in air, its intensity is made to drop significantly
It is low, intensity can be completely lost for a long time, seriously affected the application in high temperature air.
There are many antioxidant coating methods of carbon fiber, and wherein chemical vapour deposition technique (CVD) is to compare with sol-gal process
More common method.CVD method is to crack to form nano particle at high temperature using organic molecule, is subsequently deposited upon carbon fiber surface
Face forms dense protective layer, and this method temperature is generally greater than 1000 DEG C, long preparation period.Sol-gal process is usually to apply colloidal sol
Carbon fiber surface is overlayed on, forms protective layer after gelation, then sintering forms protective coating, but is often applied in gelation process
Layer cracking falls off, and effect is undesirable.Coating layer thickness prepared by above two method is big but defect is more, falls off when serious, rises not
To antioxidation.
Therefore, in order to solve the above-mentioned technical problem, inventor has invented a kind of new carbon fiber surface aluminium oxide nano film
Preparation method.
Invention content
The purpose of the present invention is to provide a kind of carbon fiber surface aluminium oxide nano film carbon fiber surface aluminium oxide nano films
The preparation method of aluminium oxide nano film, is intended to improve that existing carbon fiber antioxidant coating is easy to fall off, defect is big, anti-oxidant effect
The problems such as fruit is undesirable.
The present invention provides a kind of technical solution：
A kind of preparation method of carbon fiber surface aluminium oxide nano film, the preparation method of carbon fiber surface aluminium oxide nano film
Include mainly：
Carbon fiber is handled in a hydrogen atmosphere, and to treated, carbon fiber is vacuum aluminum-coated；To the aluminium film of carbon fiber surface into
Row electrochemical oxidation, then uses deionized water be cleaned by ultrasonic, be dry, and vacuum suck alumina sol after drying is dry simultaneously to burn
Knot.
The present invention also provides a kind of technical solutions：
A kind of carbon fiber surface aluminium oxide nano film；
The advantageous effect of carbon fiber surface aluminium oxide nano film provided in an embodiment of the present invention and preparation method thereof is：
Carbon fiber is handled in a hydrogen atmosphere, removes hydroxyl, carbonyl of carbon fiber surface etc., then carries out crossing aluminium and electrification
Oxidation is learned, aluminium film is made to be converted into pellumina.Alumina sol is sucked, alumina sol is attached in micropore, re-sinters,
About 110 nanometers of the thickness for the carbon fiber surface aluminium oxide nano film being prepared, it is fine and close and not easily to fall off.
The carbon fiber surface aluminium oxide nano film that preparation method provided in an embodiment of the present invention is prepared have high intensity,
High-modulus, high temperature resistant, low-density, it is corrosion-resistant the advantages that.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The preparation method of the carbon fiber surface aluminium oxide nano film of the embodiment of the present invention is specifically described below.
A kind of preparation method of carbon fiber surface aluminium oxide nano film includes mainly：
Carbon fiber is handled in a hydrogen atmosphere, and to treated, carbon fiber is vacuum aluminum-coated；To carbon fiber surface aluminizer into
Row electrochemical oxidation, then uses deionized water be cleaned by ultrasonic, be dry, and vacuum suck alumina sol after drying is dry simultaneously to burn
Knot.
Carbon fiber is handled in a hydrogen atmosphere, removes hydroxyl, carbonyl of carbon fiber surface etc., is carried out to carbon fiber surface pre-
Processing, is conducive to that the later stage is avoided to lead to falling off for pellumina since carbon fiber forms minimum gas at high temperature.
After being pre-processed to carbon fiber surface, electrochemical oxidation is carried out to carbon fiber surface aluminizer, electrochemical oxidation is
It is put into the solution or suspension of organic matter in a cell, by direct current, on anode capturing electronics makes carbon fiber surface
Aluminium coat is oxidized to oxidation aluminium coat.
The partial oxidation aluminium coat of carbon fiber surface can form certain micropore in forming process, in micropore and coating
Remained on surface impurity, is cleaned by ultrasonic using deionized water, in cleaning process, will be cleaned in pellumina micropore, meanwhile, it goes
Ionized water is cleaned by ultrasonic to be come from other of carbon fiber surface the ingredient in plating solution and cleans.It is dry to carbon fiber after cleaning
It is dry.
After deionized water is cleaned by ultrasonic, vacuum suck alumina sol, to be filled in coating micropore.
Alumina sol viscosity is relatively low, and the permeable place of water can be permeated, therefore dispersibility when being mixed with other materials
It is all very good with permeability.Alumina sol is attached in the micropore of above-mentioned oxidation aluminium coat, makes the oxidation of carbon fiber surface
Micropore between aluminium layer is filled by alumina sol.
Then it is dried and is sintered again.
When Aluminum sol moisture evaporation, colloidal particle is filled among micropore securely, is formed alumina between particle and is combined, effectively
Fill micropore.To ultimately form fine and close aluminium oxide nano protective film
The coating layer thickness that chemical vapour deposition technique (CVD) is prepared with sol-gal process is generally higher than 500 nanometers, this big thickness
Degree coating tends to fall off.It is prepared using the preparation method of carbon fiber surface aluminium oxide nano film provided in an embodiment of the present invention
About 110 nanometers of film thickness, it is fine and close and not easily to fall off.
In the present embodiment, in preparation process, carbon fiber ulking thickness is no more than 2mm, the carbon fiber surface prepared
Evenly, ulking thickness is less than 2mm to aluminium oxide nano film, and carbon fiber is in a more fluffy state, aluminize, aoxidize with
And with alumina sol drying process, be conducive to carbon fiber surface and equably aluminize, make final aluminium oxide nano film thickness
Uniformly.
In an embodiment of the present invention, carbon fiber is handled in a hydrogen atmosphere, and treatment temperature is 700-800 DEG C, when processing
Between be 25-35 minutes.Further, treatment temperature is 750 DEG C, and processing time is 30 minutes.
Further, in the present embodiment, hydrogen atmosphere pressure is normal pressure (atmospheric pressure), and the purity of hydrogen is more than
99.99vol% avoids introducing impurity.
Metallic aluminium is melted by high temperature under high vacuum state and is evaporated, is made on the vapor deposition to carbon fiber surface of aluminium,
In the present embodiment, during vacuum aluminum-coated, pressure is less than 9 millipascals, aluminizes time 8-9 second, and thickness of aluminizing is 40-60nm.In detail
Carefully, pressure is 8 millipascals, and the time of aluminizing is 8 seconds.
Then electrochemical oxidation is carried out to carbon fiber surface aluminium coated again, the DC voltage of electrochemical oxidation lies prostrate for 6-10
Spy, time are 2-5 minutes.
The carbon of aluminizing after electrochemical oxidation is cleaned by ultrasonic using fiber using deionized water, removes carbon fiber surface
Impurity, manifest the micropore on pellumina surface.
To the carbon fiber drying after ultrasonic cleaning, drying temperature is 100-120 DEG C, and drying time is 1-2 hours.
There is micropore, vacuum suck alumina sol so that alumina sol is attached to micro- on pellumina surface after drying
Alumina is formed in hole, between particle to combine, and improves the consistency of pellumina.
In the present embodiment, alumina sol grain size is 5-10nm, and the alumina sol solid content is 35-45wt%.
Further, alumina sol grain size is 5nm, and alumina sol solid content is 40wt%.
It is sintered, sintering temperature is 900-950 DEG C, and sintering time is 4-10 minutes.Carbon fiber surface is set to form one layer
Fine and close aluminium oxide nano film.
The present invention also provides a kind of technical solutions：
A kind of carbon fiber surface aluminium oxide nano film；
Carbon fiber surface aluminium oxide nano film by above-mentioned carbon fiber surface aluminium oxide nano film preparation method prepare and
At.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of carbon fiber surface aluminium oxide nano film, which mainly leads to
Following preparation process is crossed to be prepared：
The carbon fiber that ulking thickness is 2mm is handled in a hydrogen atmosphere, hydrogen atmosphere pressure is an atmospheric pressure, hydrogen
Purity be more than 99.99vol%；Treatment temperature is 800 DEG C to carbon fiber in a hydrogen atmosphere, and processing time is 25 minutes.
To treated, carbon fiber is vacuum aluminum-coated；During vacuum aluminum-coated, 7 millipascal of pressure aluminizes time 8-9 second, aluminizes
Thickness is 40nm.
The aluminium film of carbon fiber surface is subjected to electrochemical oxidation, the DC voltage of electrochemical oxidation is 6.2 volts, and the time is
2 minutes.Then deionized water is used to be cleaned by ultrasonic.
To the carbon fiber drying after ultrasonic cleaning, drying temperature is 120 DEG C, and drying time is 2 hours.
Vacuum suck alumina sol after drying, drying are simultaneously sintered.Wherein, alumina sol grain size is 5nm, the oxidation
Aluminum sol solid content is 35wt%.Sintering temperature is 950 DEG C, and sintering time is 10 minutes.
Embodiment 2
The present embodiment provides a kind of carbon fiber surface aluminium oxide nano film, which mainly leads to
Following preparation process is crossed to be prepared：
The carbon fiber that ulking thickness is 2mm is handled in a hydrogen atmosphere, hydrogen atmosphere pressure is an atmospheric pressure, hydrogen
Purity be more than 99.99vol%；Treatment temperature is 800 DEG C to carbon fiber in a hydrogen atmosphere, and processing time is 35 minutes.
To treated, carbon fiber is vacuum aluminum-coated；During vacuum aluminum-coated, 8 millipascal of pressure is aluminized 8 seconds time, thickness of aluminizing
Degree is 60nm.
The aluminium film of carbon fiber surface is subjected to electrochemical oxidation, the DC voltage of electrochemical oxidation is 6 volts, the time 2
Minute.Then deionized water is used to be cleaned by ultrasonic.
To the carbon fiber drying after ultrasonic cleaning, drying temperature is 100 DEG C, and drying time is 1 hour.
Vacuum suck alumina sol after drying, drying are simultaneously sintered.Wherein, alumina sol grain size is 10nm, the oxygen
Change Aluminum sol solid content is 35wt%.Sintering temperature is 900 DEG C, and sintering time is 10 minutes.
Embodiment 3
The present embodiment provides a kind of carbon fiber surface aluminium oxide nano film, which mainly leads to
Following preparation process is crossed to be prepared：
By thickness be 2mm carbon fiber handle in a hydrogen atmosphere, hydrogen atmosphere pressure be an atmospheric pressure, hydrogen it is pure
Degree is more than 99.99vol%；Treatment temperature is 800 DEG C to carbon fiber in a hydrogen atmosphere, and processing time is 35 minutes.
To treated, carbon fiber is vacuum aluminum-coated；During vacuum aluminum-coated, 8 millipascal of pressure is aluminized 8 seconds time, thickness of aluminizing
Degree is 60nm.
The aluminium film of carbon fiber surface is subjected to electrochemical oxidation, the DC voltage of electrochemical oxidation is 10 volts, the time 5
Minute.Then deionized water is used to be cleaned by ultrasonic.
To the carbon fiber drying after ultrasonic cleaning, drying temperature is 120 DEG C, and drying time is 2 hours.
Vacuum suck alumina sol after drying, drying are simultaneously sintered.Wherein, alumina sol grain size is 10nm, the oxygen
Change Aluminum sol solid content is 35wt%.Sintering temperature is 950 DEG C, and sintering time is 8 minutes.
Embodiment 4
The present embodiment provides a kind of carbon fiber surface aluminium oxide nano film, which mainly leads to
Following preparation process is crossed to be prepared：
By thickness be 2mm carbon fiber handle in a hydrogen atmosphere, hydrogen atmosphere pressure be an atmospheric pressure, hydrogen it is pure
Degree is more than 99.99vol%；Treatment temperature is 800 DEG C to carbon fiber in a hydrogen atmosphere, and processing time is 35 minutes.
To treated, carbon fiber is vacuum aluminum-coated；During vacuum aluminum-coated, 9 millipascal of pressure aluminizes time 8-9 second, aluminizes
Thickness is 50nm.
The aluminium film of carbon fiber surface is subjected to electrochemical oxidation, the DC voltage of electrochemical oxidation is 7 volts, the time 4
Minute.Then deionized water is used to be cleaned by ultrasonic.
To the carbon fiber drying after ultrasonic cleaning, drying temperature is 110 DEG C, and drying time is 1.5 hours.
Vacuum suck alumina sol after drying, drying are simultaneously sintered.Wherein, alumina sol grain size is 8nm, the oxidation
Aluminum sol solid content is 40wt%.Sintering temperature is 930 DEG C, and sintering time is 8 minutes.
Embodiment 5
The present embodiment provides a kind of carbon fiber surface aluminium oxide nano film, which mainly leads to
Following preparation process is crossed to be prepared：
By thickness be 2mm carbon fiber handle in a hydrogen atmosphere, hydrogen atmosphere pressure be an atmospheric pressure, hydrogen it is pure
Degree is more than 99.99vol%；Treatment temperature is 800 DEG C to carbon fiber in a hydrogen atmosphere, and processing time is 25 minutes.
To treated, carbon fiber is vacuum aluminum-coated；During vacuum aluminum-coated, 8 millipascal of pressure aluminizes time 8-9 second, aluminizes
Thickness is 40nm.
The aluminium film of carbon fiber surface is subjected to electrochemical oxidation, the DC voltage of electrochemical oxidation is 8 volts, the time 2
Minute.Then deionized water is used to be cleaned by ultrasonic.
To the carbon fiber drying after ultrasonic cleaning, drying temperature is 100 DEG C, and drying time is 1-2 hours.
Vacuum suck alumina sol after drying, drying are simultaneously sintered.Wherein, alumina sol grain size is 6nm, the oxidation
Aluminum sol solid content is 55wt%.Sintering temperature is 900-950 DEG C, and sintering time is 9 minutes.
Comparative example 1
Aluminium oxide nano film is prepared in carbon fiber surface using chemical vapour deposition technique.
Comparative example 2
Aluminium oxide nano film is prepared in carbon fiber surface using sol-gal process.
Test example
Carbon fiber surface aluminium oxide nano film and comparative example 1 to the offer of embodiment 1- embodiments 5, comparative example 2 provide
Aluminium oxide nano film be tested for the property.Test result such as table 1.
The performance of aluminium oxide nano protective film in 1 each embodiment of table and comparative example
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of carbon fiber surface aluminium oxide nano film, which is characterized in that the carbon fiber surface aluminium oxide is received
Rice film preparation method include mainly：
Carbon fiber is handled in a hydrogen atmosphere, and to treated, the carbon fiber is vacuum aluminum-coated；To the carbon fiber surface
Aluminium film carries out electrochemical oxidation, then uses deionized water to be cleaned by ultrasonic, is dry, and vacuum suck alumina sol after drying is done
It is dry and be sintered.
2. the preparation method of carbon fiber surface aluminium oxide nano film according to claim 1, which is characterized in that the carbon fiber
It ties up ulking thickness and is no more than 2mm.
3. the preparation method of carbon fiber surface aluminium oxide nano film according to claim 1, which is characterized in that the carbon fiber
Dimension is handled in a hydrogen atmosphere, and treatment temperature is 700-800 DEG C, and processing time is 25-35 minutes.
4. the preparation method of carbon fiber surface aluminium oxide nano film according to claim 1, which is characterized in that the carbon fiber
Dimension is handled in a hydrogen atmosphere, and the hydrogen atmosphere pressure is normal pressure, and the purity of the hydrogen is more than 99.99vol%.
5. the preparation method of carbon fiber surface aluminium oxide nano film according to claim 1, which is characterized in that the vacuum
During aluminizing, pressure is aluminized time 8-9 second less than 9 bold and unconstrained pas, and thickness of aluminizing is 40-60nm.
6. the preparation method of carbon fiber surface aluminium oxide nano film according to claim 1, which is characterized in that the carbon
Fiber carries out electrochemical oxidation, and DC voltage is 6-10 volts, and the time is 2-5 minutes.
7. the preparation method of carbon fiber surface aluminium oxide nano film according to claim 1, which is characterized in that clear to ultrasound
Carbon fiber drying after washing, drying temperature are 100-120 DEG C, and drying time is 1-2 hours.
8. the preparation method of carbon fiber surface aluminium oxide nano film according to claim 1, which is characterized in that the oxidation
Aluminum sol grain size is 5-10nm, and the alumina sol solid content is 35-45wt%.
9. the preparation method of carbon fiber surface aluminium oxide nano film according to claim 1, which is characterized in that described in sucking
It is dried and is sintered after alumina sol, sintering temperature is 900-950 DEG C, and sintering time is 4-10 minutes.
10. a kind of carbon fiber surface aluminium oxide nano protective film, which is characterized in that the carbon fiber surface aluminium oxide nano film by
The preparation method of claim 1-9 any one of them carbon fiber surface aluminium oxide nano films is prepared.
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| CN110219165A (en) * | 2019-05-20 | 2019-09-10 | 龙云峰 | A kind of preparation method of composite alumina coat carbon fiber |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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