CN108203794A - A kind of short carbon fiber aluminum matrix composite and preparation method thereof - Google Patents
A kind of short carbon fiber aluminum matrix composite and preparation method thereof Download PDFInfo
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- CN108203794A CN108203794A CN201810008701.8A CN201810008701A CN108203794A CN 108203794 A CN108203794 A CN 108203794A CN 201810008701 A CN201810008701 A CN 201810008701A CN 108203794 A CN108203794 A CN 108203794A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/02—Pretreatment of the fibres or filaments
- C22C47/04—Pretreatment of the fibres or filaments by coating, e.g. with a protective or activated covering
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
- C22C49/04—Light metals
- C22C49/06—Aluminium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
- C23C18/40—Coating with copper using reducing agents
- C23C18/405—Formaldehyde
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Abstract
The invention discloses a kind of short carbon fiber aluminum matrix composites and preparation method thereof, preparation method include surface treatment, electroless copper, mixing, be sintered and etc., prepared short carbon fiber aluminum matrix composite, including mass percent be 8wt%~10wt% copper facing short carbon fiber and mass percent be 90wt%~92wt% aluminium powder；Wherein, copper facing short carbon fiber length is 2~3mm, and diameter is less than 20 μm, and copper coating thickness is 1um, and the grain size of aluminium powder is 20~100um.It is 98.5% to measure short fibre consistency, hardness 92.38Mpa, tensile strength 202.05Mpa, bending strength 376.05Mpa.Using the method for the present invention can solve short carbon fiber in the composite bad dispersibility the technical issues of, prepared short carbon fiber aluminum matrix composite, superior performance can meet the use demand of special occasions.
Description
Technical field
The invention belongs to carbon fibre composite preparing technical fields, and in particular to a kind of short carbon fiber aluminum matrix composite
And preparation method thereof.
Background technology
Nowadays traditional material is difficult to deal with the performance needed for technological progress.During advanced material is found, research
Personnel innovate a variety of materials system, and metal-base composites is one of material system most protruded in recent decades.
Due to the unusual combination of rigidity, intensity and weight ratio, high-temperature behavior and hardness, they aircraft technology, electronics industry and
The application in other fields significantly increases.Wherein, aluminum matrix composite material is considered as a kind of excellent metal-based compound
Material since density is low, is readily produced, therefore advantage of lower cost.The research of aluminum matrix composite start from the 1950s,
The common reinforcing material of aluminum substrate is silicon carbide, aluminium oxide and aluminosilicate.In addition in recent years, the performance of carbon fiber obtains
The raising advanced by leaps and bounds, carbon fiber can also be considered as excellent since it possesses low cost, high-modulus, high specific strength and specific stiffness
Reinforcing material, but due to interface problem and manufacturing issue, carbon fiber aluminum-based compound material is still in conceptual phase.Prevent carbon fiber
Reacting between matrix, while it is to solve aluminum matrix composite to improve the caking property between wetability and carbon fiber and aluminum substrate
The key of interface problem, carbon fiber surface metallization are the key that improve one of fibre reinforced composites performance, it can be hindered
Only fiber and matrix react, and can improve wetability, and interface is also made to have certain binding force, reach and effectively transmit load and carry
The mechanical property of high composite material.Therefore, carbon fibre reinforced composite just becomes the more excellent engineering structure of comprehensive performance
Material and the functional material with property.
The metallization of carbon fiber is to form single metal or alloy coat on the surface thereof using plating, chemical plating and CVD.
Chemical plating is relatively outstanding in terms of cost and stability is reduced.And traditional carbon fiber surface chemical plating treated coating
Thickness and stability are not enough to the barrier carbon fiber in follow-up prepare and generation brittlement phase Al are reacted with aluminium base4C3And reduce composite wood
The properties of material.And existing method is during subsequently composite material is prepared, it will usually since carbon fiber disperses unevenness
And seriously affect the performance of composite material.
Invention content
For the above-mentioned prior art, the present invention provides a kind of short carbon fiber method for preparing aluminum-based composite material, to solve to adopt
The technical issues of metal-based carbon fiber poor performance prepared with traditional preparation methods.
In order to achieve the above object, the technical solution adopted in the present invention is：A kind of short carbon fiber aluminum-base composite material is provided
Preparation method for material includes the following steps：
(1) by short carbon fiber successively after removing photoresist, being roughened, be sensitized, activate, restore and be dried, plated fiber must be treated；
(2) to treating that plated fiber carries out electroless copper processing obtained by step (1), copper facing short carbon fiber is obtained；During copper facing
40%NaOH solution is added into plating solution with the amount of 1ml/1.5min；Copper facing temperature is 55 DEG C~65 DEG C, the copper facing time for 40~
45min；
(3) copper facing short carbon fiber is evenly spread in absolute ethyl alcohol, a copper facing short carbon fiber is taken every 1~1.5min
It is added in the aluminium powder slurry under lasting stirring, until copper carbon fiber all adds in, continues 2~2.5h of stirring, so
It is dried in vacuo under the conditions of 60~65 DEG C afterwards, drying time is 2~2.5h, obtains mixed-powder；Wherein, aluminium powder slurry is aluminium
Powder is 1 by solid-to-liquid ratio with absolute ethyl alcohol:2~3 mixed products；
(4) discharge plasma sintering is carried out to mixed-powder obtained by step (3), sintering temperature is 550~620 DEG C, heat preservation
Time is 7~15min, and plus load is 30~40Mpa；Then 16~20h of ageing treatment under the conditions of 200~220 DEG C, obtains
Short fibre.
Based on the above technical solution, the present invention can also be improved as follows.
Further, the specific method of short carbon fiber processing is in step (1)：Short carbon fiber is heated to 425~475 DEG C,
Keep the temperature 55~65min；Short carbon fiber is placed in 55~65 DEG C of dense HNO after removing photoresist again380~100min of middle stirring；It then will be thick
Short carbon fiber after change is placed in sensitizing solution, and first 5~7min of sonic oscillation is stirred for 5~7min；Then by the short carbon after sensitization
Fiber is placed in 5~7min of stirring in silver ammino solution；The sodium hypophosphite that short carbon fiber after activation is placed in 15~20g/L again is molten
1~2min is stirred in liquid；Finally dry to treat plated fiber under the conditions of 50~60 DEG C；Deionization is all first used after each of the above step
Water rinses short carbon fiber to neutrality, then carries out next step.
Further, sensitizing solution SnCl2·2H2O solution is 1~2 by volume with HCl solution:The mixed solution of 1 mixing,
Wherein SnCl2·2H2A concentration of 25~30g/L of O solution, a concentration of 40~50mL/L of HCl solution；Silver ammino solution is AgNO3
Solution is 1 by volume with ammonium hydroxide:The mixed solution of 1~2 mixing, wherein, AgNO3A concentration of 5~10g/L of solution, ammonium hydroxide
A concentration of 8~12mL/L.
Further, plating solution includes in step (2)：
Further, the short carbon fiber after copper facing is disperseed using ultrasound in step (3), supersonic frequency for 15~
20kHz, 10~15min of ultrasonic time；Copper facing short carbon fiber presses 1 with aluminium powder slurry:15~20 volume ratio mixing.
Further, when spark plasma sintering is carried out in step (4), sintering temperature is 600 DEG C, soaking time 10min,
Plus load is 40Mpa.
Using above-mentioned preparation method, a kind of short carbon fiber aluminum matrix composite can be prepared, which includes quality
The aluminium powder that the copper facing short carbon fiber and mass percent that percentage is 3wt%~10wt% are 90wt%~97wt%；Wherein, it plates
Copper short carbon fiber length is 2~3mm, and diameter is less than 20 μm, and copper coating thickness is 1um, and the grain size of aluminium powder is 20~100um.
The beneficial effects of the invention are as follows：
1. being up to 25% with the carbon fiber surface oxygen content after roughening treatment by removing photoresist, and do not have under strongly acidic conditions yet
There is destruction carbon fiber.The activation point being evenly distributed by sensitization-activation-reducing condition carbon fiber surface so that chemical plating
Middle coating is more divided equally and possesses certain binding force.
2. coating compares relatively thin in traditional chemical copper-plating technique, copper grain graininess difference is big, and does not have in the presence of part
The fiber of layers of copper is plated, especially end is particularly evident.And in the present invention by improving ingredient in chemical plating fluid and in plating solution
The second bipyridine of middle addition 300mg/L, it is suppressed that copper particle is grown up so that copper grain graininess approaches in coating, thickness of coating
It is thicker and more uniform, so as to effectively obstruct being in direct contact for aluminium base and short carbon fiber.
3. copper facing short carbon fiber is all to prepare short fibre all the time in the uniformity of aluminium base
Difficulty.Traditional blending processes of powders such as ball milling can lead to the destruction of short carbon fiber copper plate, and the present invention mixes the work of powder using slurry
Skill, and effectively disperseed copper facing short carbon fiber using ultrasonic cell disrupte machine, so as to efficiently solve short carbon fiber
The problem of dispersed.
4. compared to the preparation method of other short fibres, the characteristic of discharge plasma sintering makes
There is sintering temperature is low, sintering time is short, heating rate is fast etc. during short fibre must be prepared
Advantage.These advantages are effectively reduced chance of the aluminium base with the contact of short carbon fiber, and a copper plate part in SPS sintering
It is spread to aluminum substrate, so as to form good interface.
5. in the performance comparison of the pure aluminum material prepared with same sample preparation method, short fibre
Consistency is 98.5% (pure aluminum material consistency is 98.5%), and hardness is up to 92.38Mpa (pure aluminum material hardness
49.37Mpa), tensile strength can reach 202.05Mpa (pure aluminum material tensile strength is 61.28Mpa), and bending strength is most
Height can reach 376.05Mpa (pure aluminum material bending strength is 115.63Mpa), and it is (pure that elasticity modulus can reach 80.68Mpa
Aluminum material elasticity modulus is 71.7Mpa).To sum up, using the short carbon fiber aluminum matrix composite prepared by the method for the present invention, property
Can be superior, the use demand of special occasions can be met.
Description of the drawings
Fig. 1 is that the displaing micro tissue topography of copper facing short carbon fiber schemes；
Fig. 2 is that the displaing micro tissue topography of short carbon fiber aluminum matrix composite schemes；
Fig. 3 is short carbon fiber and the interface fibr tissue shape appearance figure of aluminium base in short carbon fiber aluminum matrix composite；
Specific embodiment
The specific embodiment of the present invention is described in detail below in conjunction with the accompanying drawings.
Embodiment one
A kind of pre-prepared short carbon fiber aluminum matrix composite, the material include 9wt% copper facing short carbon fiber and 91wt%
Aluminium powder, wherein, the length of copper facing short carbon fiber is 2~3mm, and diameter is less than 20 μm, and the thickness of copper coating is 1um；Aluminium is grain
Diameter is the aluminium powder of 20~100um.Preparation method includes the following steps：
(1) the original short carbon fibers of T-700 are put into chamber type electric resistance furnace, high temperature is carried out to carbon fiber under the conditions of 400 DEG C
Processing, and 1h is kept the temperature, then it is furnace-cooled to room temperature.With the dense HNO that 250ml volume fractions are 65%~68%3It is short to be acidified 3g degummings
Carbon fiber.Maintaining temperature, magnetic agitation 1.5h is then washed with deionized water to neutrality at 60 DEG C.Finely dispersed short carbon is fine
Dimension adds in sensitizing solution and carries out sensitized treatment, and sensitizing solution is by 30g/L SnCl2·2H2O solution and the solution of 40mL/L HCl press 1:
1 volume ratio mixes, sensitized treatment by the way of " 5min sonic oscillation -7min magnetic agitations -5min is stored at room temperature ",
Then neutrality is washed till with deionization.Short carbon fiber after sensitized treatment is placed in silver ammino solution and carries out activation process, silver-colored ammonia is molten
Liquid is by AgNO3Solution is pressed with ammonium hydroxide by 1:1 volume ratio mixes, wherein, AgNO3A concentration of 10g/L of solution, ammonium hydroxide
A concentration of 8mL/L, activation process is by the way of " 5min magnetic agitations -5min is stored at room temperature ", in being then washed till with deionization
Property.Finally the short carbon fiber after activation is added in the ortho phosphorous acid sodium solution of 20g/L and carry out reduction treatment, activation process uses
" 1min manually stirs -3min and is stored at room temperature " mode, is then washed till neutrality with deionization.The short carbon fiber pre-processed is placed in
It is dried in 60 DEG C of drying box, must treat plated fiber.
(2) chemical plating fluid of 1000ml is prepared, by ultrasonic cleaner so that 15g CuSO45H2O is substantially soluble in
In suitable deionized water, this is considered as first group of solution.Then a new beaker is separately taken to weigh 25g EDTA-2Na, equally
It is made to be completely dissolved in deionized water by ultrasonic cleaner, then the sodium potassium tartrate tetrahydrate of addition 20g fully dissolves wherein,
This is considered as second group of solution.Slowly first group of solution of preparation is added in second group of solution, then adds in 300mg/L bis-
Bipyridyl.Then 3g carbon fibers are added in, are settled to 1000ml.The chemical plating fluid prepared is put and is protected in 60 DEG C of thermostat water bath
Temperature, and low-speed machinery stirs.When bath temperature is close to 60 DEG C, it is 12.5 to adjust pH value of solution with 10%NaOH solution, and first is added dropwise
After aldehyde solution 5ml, 3min, then 10ml formalins are slowly dropped into plating solution.Copper facing total duration is 45min.In experiment
In the process, since reaction can consume NaOH, 40%NaOH solution is prepared, plating solution is added drop-wise to the rate of 1ml/1.5min
In, it can maintain to react required pH.Carbon fiber is cleaned with deionized water after copper facing, the plating solution of remained on surface is washed
Totally, it is washed till neutrality.Then ultrasound impregnates 3min in absolute ethyl alcohol, and moisture removal is removed using the low boiling point of ethyl alcohol, avoids carbon fine
The layers of copper in dimension table face is aoxidized in the environment for having water and oxygen, influences the performance of material, is finally placed in 60 DEG C of drying box
It is dried.
(3) the copper facing short carbon fiber and the aluminium powder of 91wt% that mass fraction is 9wt% are mixed using slurry powder mixing method
Powder.Absolute ethyl alcohol is added in copper carbon fiber, 10min is disperseed using the ultrasonic echography of 20kHz, wherein taking one every 1min
The secondary uniform carbon fiber of magnetic agitation is added to just in churned mechanically aluminium powder slurry, until whole copper carbon fibers add in,
Wherein, it is 1 that aluminium powder slurry, which is the solid-to-liquid ratio of aluminium powder and absolute ethyl alcohol,:2~3 mixed products, the copper carbon fiber of addition without
Hydrous ethanol solution and the volume ratio of aluminium powder slurry are 1:15.The mechanical agitation of 2.5h is carried out therewith.Mixed-powder is put into later
It is dried in vacuo in 60 DEG C of thermostatic drying chambers, removes absolute ethyl alcohol.
(4) mixed-powder is filled into progress discharge plasma sintering processing, sintering condition in graphite sintering mold is：It burns
600 DEG C, plus load 30MPa of junction temperature, keeps the temperature 10min, and vacuum degree used is 0.05mbar.In 200 DEG C of items after the completion of sintering
Ageing treatment 20h under part, obtains short fibre.
Embodiment two
(1) the original short carbon fibers of T-700 are put into chamber type electric resistance furnace, high temperature is carried out to carbon fiber under the conditions of 480 DEG C
Processing, and 50min is kept the temperature, then it is furnace-cooled to room temperature.With the dense HNO that 250ml volume fractions are 65%~68%3It is acidified 3g degummings
Short carbon fiber.Maintaining temperature, magnetic agitation 100min is then washed with deionized water to neutrality at 55 DEG C.It will be finely dispersed short
Carbon fiber adds in sensitizing solution and carries out sensitized treatment, and sensitizing solution is by 25g/L SnCl2·2H2The solution of O solution and 40mL/L HCl
By 2:1 volume ratio mixes, and sensitized treatment is using " 7min sonic oscillation -5min magnetic agitations -5min is stored at room temperature "
Mode is then washed till neutrality with deionization.Short carbon fiber after sensitized treatment is placed in silver ammino solution and carries out activation process, silver
Ammonia solution is by AgNO3Solution is pressed with ammonium hydroxide by 1:2 volume ratio mixes, wherein, AgNO3A concentration of 2g/L of solution, ammonium hydroxide
A concentration of 12mL/L, activation process is then washed till by the way of " 7min magnetic agitations -5min is stored at room temperature " with deionization
It is neutral.Finally the short carbon fiber after activation is added in the ortho phosphorous acid sodium solution of 20g/L and carry out reduction treatment, activation process is adopted
With " 2min manually stirs -3min and is stored at room temperature " mode, then neutrality is washed till with deionization.The short carbon fiber pre-processed is put
It is dried in 60 DEG C of drying box, must treat plated fiber.
(2) chemical plating fluid of 1000ml is prepared, by ultrasonic cleaner so that 15g CuSO45H2O is substantially soluble in
In suitable deionized water, this is considered as first group of solution.Then a new beaker is separately taken to weigh 25g EDTA-2Na, equally
It is made to be completely dissolved in deionized water by ultrasonic cleaner, then the sodium potassium tartrate tetrahydrate of addition 20g fully dissolves wherein,
This is considered as second group of solution.Slowly first group of solution of preparation is added in second group of solution, then adds in 300mg/L bis-
Bipyridyl.Then 3g carbon fibers are added in, are settled to 1000ml.The chemical plating fluid prepared is put and is protected in 60 DEG C of thermostat water bath
Temperature, and low-speed machinery stirs.When bath temperature is close to 65 DEG C, it is 12.5 to adjust pH value of solution with 10%NaOH solution, and first is added dropwise
After aldehyde solution 5ml, 3min, then 10ml formalins are slowly dropped into plating solution.Copper facing total duration is 40min.In experiment
In the process, since reaction can consume NaOH, 40%NaOH solution is prepared, plating solution is added drop-wise to the rate of 1ml/1.5min
In, it can maintain to react required pH.Carbon fiber is cleaned with deionized water after copper facing, the plating solution of remained on surface is washed
Totally, it is washed till neutrality.Then ultrasound impregnates 3min in absolute ethyl alcohol, and moisture removal is removed using the low boiling point of ethyl alcohol, avoids carbon fine
The layers of copper in dimension table face is aoxidized in the environment for having water and oxygen, influences the performance of material, is finally placed in 60 DEG C of drying box
It is dried.
(3) the copper facing short carbon fiber and the aluminium powder of 91wt% that mass fraction is 9wt% are mixed using slurry powder mixing method
Powder.Absolute ethyl alcohol is added in copper carbon fiber, 15min is disperseed using the ultrasonic echography of 15kHz, wherein being taken every 1.5min
Uniform carbon fiber of magnetic agitation is added to just in churned mechanically aluminium powder slurry, until whole copper carbon fibers add
Enter, wherein, aluminium powder slurry is that the solid-to-liquid ratio of aluminium powder and absolute ethyl alcohol is 1:2~3 mixed products, the copper carbon fiber of addition
The volume ratio of ethanol solution and aluminium powder slurry is 1:15.The mechanical agitation of 2.5h is carried out therewith.Mixed-powder is put later
Enter and be dried in vacuo in 60 DEG C of thermostatic drying chambers, remove absolute ethyl alcohol.
(4) mixed-powder is filled into progress discharge plasma sintering processing, sintering condition in graphite sintering mold is：It burns
550 DEG C, plus load 40MPa of junction temperature, keeps the temperature 15min, and vacuum degree used is 0.05mbar.In 220 DEG C of items after the completion of sintering
Ageing treatment 16h under part, obtains short fibre.
Comparative example one
(1) the original short carbon fibers of T-700 are put into chamber type electric resistance furnace, high temperature is carried out to carbon fiber under the conditions of 400 DEG C
Processing, and 1h is kept the temperature, then it is furnace-cooled to room temperature.With the dense HNO that 250ml volume fractions are 65%~68%3It is short to be acidified 3g degummings
Carbon fiber.Maintaining temperature, magnetic agitation 1.5h is then washed with deionized water to neutrality at 60 DEG C.Finely dispersed short carbon is fine
Dimension adds in sensitizing solution and carries out sensitized treatment, and sensitizing solution is by 30g/L SnCl2·2H2O solution and the solution of 40mL/L HCl press 1:
1 volume ratio mixes, sensitized treatment by the way of " 5min sonic oscillation -7min magnetic agitations -5min is stored at room temperature ",
Then neutrality is washed till with deionization.Short carbon fiber after sensitized treatment is placed in silver ammino solution and carries out activation process, silver-colored ammonia is molten
Liquid is by AgNO3Solution is pressed with ammonium hydroxide by 1:1 volume ratio mixes, wherein, AgNO3A concentration of 10g/L of solution, ammonium hydroxide
A concentration of 8mL/L, activation process is by the way of " 5min magnetic agitations -5min is stored at room temperature ", in being then washed till with deionization
Property.Finally the short carbon fiber after activation is added in the ortho phosphorous acid sodium solution of 20g/L and carry out reduction treatment, activation process uses
" 1min manually stirs -3min and is stored at room temperature " mode, is then washed till neutrality with deionization.The short carbon fiber pre-processed is placed in
It is dried in 60 DEG C of drying box, must treat plated fiber.
(2) chemical plating fluid of 1000ml is prepared, by ultrasonic cleaner so that 15g CuSO45H2O is substantially soluble in
In suitable deionized water, this is considered as first group of solution.Then a new beaker is separately taken to weigh 25g EDTA-2Na, equally
It is made to be completely dissolved in deionized water by ultrasonic cleaner, then the sodium potassium tartrate tetrahydrate of addition 20g fully dissolves wherein,
This is considered as second group of solution.Slowly first group of solution of preparation is added in second group of solution, then adds in 300mg/L bis-
Bipyridyl.Then 3g carbon fibers are added in, are settled to 1000ml.The chemical plating fluid prepared is put and is protected in 60 DEG C of thermostat water bath
Temperature, and low-speed machinery stirs.When bath temperature is close to 60 DEG C, it is 12.5 to adjust pH value of solution with 10%NaOH solution, and first is added dropwise
After aldehyde solution 5ml, 3min, then 10ml formalins are slowly dropped into plating solution.Copper facing total duration is 45min.In experiment
In the process, since reaction can consume NaOH, 40%NaOH solution is prepared, plating solution is added drop-wise to the rate of 1ml/1.5min
In, it can maintain to react required pH.Carbon fiber is cleaned with deionized water after copper facing, the plating solution of remained on surface is washed
Totally, it is washed till neutrality.Then ultrasound impregnates 3min in absolute ethyl alcohol, and moisture removal is removed using the low boiling point of ethyl alcohol, avoids carbon fine
The layers of copper in dimension table face is aoxidized in the environment for having water and oxygen, influences the performance of material, is finally placed in 60 DEG C of drying box
It is dried.
(3) dried copper facing short carbon fiber is added directly into aluminium powder slurry, wherein, aluminium powder slurry is aluminium powder and nothing
The solid-to-liquid ratio of water-ethanol is 1:2~3 mixed products.The mechanical agitation of 2.5h is carried out therewith.Mixed-powder is put into later
It is dried in vacuo in 60 DEG C of thermostatic drying chambers, removes absolute ethyl alcohol.
(4) mixed-powder is filled into progress discharge plasma sintering processing, sintering condition in graphite sintering mold is：It burns
600 DEG C, plus load 30MPa of junction temperature, keeps the temperature 10min, and vacuum degree used is 0.05mbar.In 200 DEG C of items after the completion of sintering
Ageing treatment 16h under part, obtains short fibre.
Comparative example two
(1) the original short carbon fibers of T-700 are put into chamber type electric resistance furnace, high temperature is carried out to carbon fiber under the conditions of 400 DEG C
Processing, and 1h is kept the temperature, then it is furnace-cooled to room temperature.With the dense HNO that 250ml volume fractions are 65%~68%3It is short to be acidified 3g degummings
Carbon fiber.Maintaining temperature, magnetic agitation 1.5h is then washed with deionized water to neutrality at 60 DEG C.Finely dispersed short carbon is fine
Dimension adds in sensitizing solution and carries out sensitized treatment, and sensitizing solution is by 30g/L SnCl2·2H2O solution and the solution of 40mL/L HCl press 1:
1 volume ratio mixes, sensitized treatment by the way of " 5min sonic oscillation -7min magnetic agitations -5min is stored at room temperature ",
Then neutrality is washed till with deionization.Short carbon fiber after sensitized treatment is placed in silver ammino solution and carries out activation process, silver-colored ammonia is molten
Liquid is by AgNO3Solution is pressed with ammonium hydroxide by 1:1 volume ratio mixes, wherein, AgNO3A concentration of 10g/L of solution, ammonium hydroxide
A concentration of 8mL/L, activation process is by the way of " 5min magnetic agitations -5min is stored at room temperature ", in being then washed till with deionization
Property.Finally the short carbon fiber after activation is added in the ortho phosphorous acid sodium solution of 20g/L and carry out reduction treatment, activation process uses
" 1min manually stirs -3min and is stored at room temperature " mode, is then washed till neutrality with deionization.The short carbon fiber pre-processed is placed in
It is dried in 60 DEG C of drying box, must treat plated fiber.
(2) chemical plating fluid of 1000ml is prepared, by ultrasonic cleaner so that 15g CuSO45H2O is substantially soluble in
In suitable deionized water, this is considered as first group of solution.Then a new beaker is separately taken to weigh 25g EDTA-2Na, equally
It is made to be completely dissolved in deionized water by ultrasonic cleaner, then the sodium potassium tartrate tetrahydrate of addition 20g fully dissolves wherein,
This is considered as second group of solution.Slowly first group of solution of preparation is added in second group of solution.Then 3g carbon fibers are added in,
It is settled to 1000ml.The chemical plating fluid prepared is put and is kept the temperature in 60 DEG C of thermostat water bath, and low-speed machinery stirs.Treat plating solution
When temperature is close to 60 DEG C, it is 12.5 to adjust pH value of solution with 10%NaOH solution, after formalin 5ml, 3min is added dropwise, then by 10ml
Formalin is slowly dropped into plating solution.Copper facing total duration is 45min.During experiment, since reaction can consume NaOH,
Therefore 40%NaOH solution is prepared, is added drop-wise in plating solution with the rate of 1ml/1.5min, can maintain to react required pH.Copper facing knot
Shu Houyong deionized waters clean carbon fiber, by the plating solution wash clean of remained on surface, are washed till neutrality.Then in absolute ethyl alcohol
Middle ultrasound impregnates 3min, removes moisture removal using the low boiling point of ethyl alcohol, avoids the layers of copper of carbon fiber surface in the ring for having water and oxygen
Border aoxidizes, and influences the performance of material, is finally placed in 60 DEG C of drying box and is dried.
(3) dried copper facing short carbon fiber is added directly into aluminium powder slurry, wherein, aluminium powder slurry is aluminium powder and nothing
The solid-to-liquid ratio of water-ethanol is 1:2~3 mixed products.The mechanical agitation of 2.5h is carried out therewith.Mixed-powder is put into later
It is dried in vacuo in 60 DEG C of thermostatic drying chambers, removes absolute ethyl alcohol.
(4) mixed-powder is filled into progress discharge plasma sintering processing, sintering condition in graphite sintering mold is：It burns
600 DEG C, plus load 30MPa of junction temperature, keeps the temperature 10min, and vacuum degree used is 0.05mbar.In 200 DEG C of items after the completion of sintering
Ageing treatment 16h under part, obtains short fibre.
Interpretation of result
What Fig. 1 was provided is displaing micro tissue topography's figure of the copper facing short carbon fiber in embodiment, there it can be seen that short carbon is fine
The copper grain graininess on the surface of dimension is not much different, and short carbon fiber surface is covered by logical particle, aluminium base and short carbon fiber
It will not be in direct contact.Fig. 3 gives short carbon fiber and the interface fibr tissue pattern of aluminium base in short carbon fiber aluminum matrix composite
Figure, it can be seen that short carbon fiber has good interface with aluminium base.Determine composite material in embodiment and comparative example
As a result consistency, hardness, tensile strength and bending strength are listed in table 1.
The performance evaluation of 1 composite material of table
| Embodiment one | Embodiment two | Comparative example one | Comparative example two | |
| Consistency/% | 98.5 | 98.5 | 82.1 | 87.4 |
| Hardness/MPa | 90.78 | 92.38 | 73.19 | 78.64 |
| Tensile strength/MPa | 198.58 | 202.05 | 172.36 | 181.47 |
| Bending strength/MPa | 359.73 | 376.05 | 278.89 | 298.34 |
As can be seen from the table, either embodiment or comparative example, the composite property prepared is compared with fine aluminium
It is improved, but embodiment is significantly more than what comparative example improved.Comparative example one is compared with embodiment one, short carbon fiber and aluminium powder
When slurry mixes, process is not fully dispersed for short carbon fiber, causes the interface between short carbon fiber and aluminium base poor, seriously affects
The performance of composite material.For comparative example two compared with embodiment one, short carbon fiber lacks bigeminy pyrrole when being electroplated, in plating solution
Pyridine, in electroplating process, it is impossible to inhibit growing up for copper particle, thickness of coating is uneven, and aluminium base and short carbon fiber can be in direct contact, shadow
Ring the performance of composite material.
Although being described in detail to the specific embodiment of the present invention, the protection to this patent should not be construed as
The restriction of range.In the described range of claims, those skilled in the art can make without creative work
Various modifications and deformation still belong to the protection domain of this patent.
Claims (8)
1. a kind of short carbon fiber aluminum matrix composite, it is characterised in that：Including the copper facing that mass percent is 3wt%~10wt%
Short carbon fiber, surplus are aluminium.
2. short carbon fiber aluminum matrix composite according to claim 1, it is characterised in that：The length of the copper facing short carbon fiber
It spends for 2~3mm, diameter is less than 20 μm, and the thickness of copper coating is 1um；Aluminium is the aluminium powder that grain size is 20~100um.
3. a kind of preparation method of short carbon fiber aluminum matrix composite as claimed in claim 1, which is characterized in that including with
Lower step：
(1) by short carbon fiber successively after removing photoresist, being roughened, be sensitized, activate, restore and be dried, plated fiber must be treated；
(2) to treating that plated fiber carries out electroless copper processing obtained by step (1), copper facing short carbon fiber is obtained；During copper facing with
The amount of 1ml/1.5min adds 40%NaOH solution into plating solution；Copper facing temperature is 55 DEG C~65 DEG C, the copper facing time for 40~
45min；
(3) copper facing short carbon fiber is evenly spread in absolute ethyl alcohol, a copper facing short carbon fiber is taken to add in every 1~1.5min
Into the aluminium powder slurry under lasting stirring, until copper carbon fiber all adds in, continue stirring 2~2.5h, Ran Hou
It is dried in vacuo under the conditions of 60~65 DEG C, drying time is 2~2.5h, obtains mixed-powder；Wherein, aluminium powder slurry for aluminium powder with
Absolute ethyl alcohol is 1 by solid-to-liquid ratio:2~3 mixed products；
(4) discharge plasma sintering is carried out to mixed-powder obtained by step (3), sintering temperature is 550~620 DEG C, soaking time
For 7~15min, plus load is 30~40Mpa；Then 16~20h of ageing treatment under the conditions of 200~220 DEG C, obtains short carbon
Fiber reinforced aluminum matrix composites.
4. short carbon fiber method for preparing aluminum-based composite material according to claim 2, which is characterized in that short in step (1)
Carbon fiber processing specific method be：Short carbon fiber is heated to 425~475 DEG C, keeps the temperature 55~65min；Again by short carbon fiber
It is placed in 55~65 DEG C of dense HNO380~100min of middle stirring；Then short carbon fiber is placed in sensitizing solution, first sonic oscillation 5~
7min is stirred for 5~7min；Short carbon fiber is then placed in 5~7min of stirring in silver ammino solution；Short carbon fiber is placed in 15 again
1~2min is stirred in the ortho phosphorous acid sodium solution of~20g/L；Finally dry to treat plated fiber under the conditions of 50~60 DEG C；More than
First short carbon fiber is rinsed after the completion of each step to neutrality with deionized water, then carry out next step.
5. short carbon fiber method for preparing aluminum-based composite material according to claim 4, it is characterised in that：The sensitizing solution is
SnCl2·2H2O solution is 1~2 by volume with HCl solution:The mixed solution of 1 mixing, wherein SnCl2·2H2O solution it is dense
It spends for 25~30g/L, a concentration of 40~50mL/L of HCl solution；The silver ammino solution is AgNO3Solution and ammonium hydroxide are by volume
It is 1:The mixed solution of 1~2 mixing, wherein, AgNO3A concentration of 5~10g/L of solution, a concentration of 8~12mL/L of ammonium hydroxide.
6. short carbon fiber method for preparing aluminum-based composite material according to claim 2, which is characterized in that plated in step (2)
Liquid includes：
7. according to short carbon fiber method for preparing aluminum-based composite material according to claim 2, it is characterised in that：Step (3)
When middle copper facing short carbon fiber is disperseed, supersonic frequency is 15~20kHz, 10~15min of ultrasonic time；Copper facing short carbon fiber with
Aluminium powder slurry presses 1:15~20 volume ratio mixing.
8. scheme is prepared according to short carbon fiber aluminum matrix composite according to claim 2, it is characterised in that：Step (4)
During middle progress spark plasma sintering, sintering temperature is 600 DEG C, soaking time 10min, plus load 40Mpa.
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