CN108179326A - It is a kind of using hair engaging aperture made with aluminum foil for the method for graphene aluminum matrix composite - Google Patents
It is a kind of using hair engaging aperture made with aluminum foil for the method for graphene aluminum matrix composite Download PDFInfo
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- CN108179326A CN108179326A CN201810091196.8A CN201810091196A CN108179326A CN 108179326 A CN108179326 A CN 108179326A CN 201810091196 A CN201810091196 A CN 201810091196A CN 108179326 A CN108179326 A CN 108179326A
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- graphene
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/20—Acidic compositions for etching aluminium or alloys thereof
Abstract
The invention discloses it is a kind of using hair engaging aperture made with aluminum foil for the method for graphene aluminum matrix composite, belong to technical field of inorganic material synthesis.This method includes：Aluminium foil hair engaging aperture, graphene attachment and three processes of hot isostatic pressing, corrode hair engaging aperture, freezing microtome section makes its surface positively charged by aluminium alloy in sulfuric acid hydrochloric acid system first；By the progress graphene attachment of hair engaging aperture aluminium foil, graphene nanometer sheet using ethyl alcohol is disperseed and is divided to two parts, hair engaging aperture aluminium foil is added in into portion, another is added dropwise, stirring, heating, dry completion graphene are attached under vacuum；Then the compound hair engaging aperture aluminium foil is subjected to HIP sintering, obtains graphene aluminum matrix composite.Preparation method provided by the invention is simple, mild condition, graphene nanometer sheet is evenly distributed and retains prototype structure, graphene/aluminum interface cohesion is good, the performance of graphene aluminum matrix composite significantly improves, and the graphene Properties of Aluminum Matrix Composites synthesized when wherein HIP sintering temperature is 600 DEG C is best.
Description
Technical field
The present invention relates to technical field of inorganic material synthesis, specially a kind of to be answered using hair engaging aperture made with aluminum foil for graphene aluminium base
The method of condensation material.
Background technology
Composite material refers to that there are two types of either two or more materials of different nature by logistics or the method for chemistry,
Material of the composition with new capability.The basis material of composite material is divided into metal and nonmetallic two class, metallic matrix the most commonly used is
Aluminium, magnesium, titanium and its alloy, nonmetal basal body mainly have synthetic resin, rubber, ceramics, graphite, carbon etc..Reinforcing material mainly has
Graphene, glass fibre, carbon fiber, silicon carbide fibre, whisker, wire and hard particulates etc..Wherein graphene Yin Qigao is led
Electrically, the excellent properties such as high-termal conductivity, high intensity and high-specific surface area become the preferable reinforcing material of composite material, special
Two-dimensional structure and excellent physical and chemical performance cause the great interest of researcher, be added to polymer, ceramics,
One of current research hotspot is become in the materials such as metal to improve the performance of material.
Aluminum matrix composite is because of its high specific strength, specific stiffness, many advantages, such as high wear-resisting property and as most future
Metal-base composites, be used widely in fields such as Aeronautics and Astronautics.It can it is reported that adding in graphene in aluminum substrate
To significantly improve its intensity and hardness, and the high ductibility of aluminum substrate is kept, obtained graphene reinforced aluminum matrix composites
Thermal conductivity also significantly improve.Swallow nine et al. the methods for mixing powder+hot isostatic pressing+hot extrusion using wet ball mills that continue are prepared for graphene
Aluminum matrix composite, not only intensity is obviously improved prepared graphene aluminum matrix composite, and elongation percentage also has slightly
Degree improves.Muhammad Rashad etc. carry out clad surface modification using nanometer aluminium powder to graphene, using graphene and
The adhesive of electrostatic attraction and auxiliary between nano aluminum, makes nanometer aluminium powder be coated on graphene surface, then again by nanometer
The graphene of aluminium cladding carries out mechanical mixture to prepare aluminium graphene composite powder, prepared graphite with aluminum matrix alloy powder
Alkene aluminum matrix composite intensity, plasticity are all improved.
But there are still much still unsolved difficulties for the preparation of graphene aluminum matrix composite at present：1. graphene in aluminium
Reunion, graphene dispersion is poor, in aluminum substrate, when graphene content is higher, is easy to agglomeration occur, drops instead
The low performance of composite material；2. interface compound Al4C3Formation, the interfacial reactions of graphene reinforced aluminum matrix composites is difficult
With control, Al is easily formed4C3Frangible compounds destroy the performances such as the mechanics of composite material；3. the profit of graphene and aluminum substrate
Wet, the wetability of graphene and aluminum substrate is generally poor, is not easy to form stronger interface cohesion.
Invention content
In order to solve the deficiencies in the prior art, present invention offer is a kind of to utilize hair engaging aperture made with aluminum foil for graphene aluminium base
The method of composite material, method is mild, simple for process, and graphene dispersion is good, and the mechanical property of composite material is effectively promoted.
It is provided by the invention it is a kind of using hair engaging aperture made with aluminum foil for the method for graphene aluminum matrix composite, including following step
Suddenly：
S1, aluminium alloy is chosen as raw material, corrosion hair engaging aperture is carried out in sulfuric acid-hcl corrosion system, after hair engaging aperture
Aluminium foil freezes 20~25min in liquid nitrogen, and the thin slice of Ф 12 is cut into after freezing, and the thin slice for weighing certain mass is added to hexadecane
In base trimethylammonium bromide aqueous solution, stirring, washing, it is dry after obtain positively charged hair engaging aperture aluminium foil, mixing time for 30~
70min, drying temperature are 35~60 DEG C, and drying time is 50~100min；
S2, the multi-layer graphene nanometer sheet for weighing certain mass are simultaneously dissolved with ethyl alcohol, and 1~1.5h of ultrasonic disperse is obtained
The ethanol solution of graphene is equally divided into two parts by the ethanol solution of graphene, adds in S1 obtain in a solution thereto
Hair engaging aperture aluminium foil, the mechanical agitation that ultrasonic disperse and rotating speed are 100r/min is carried out at the same time, then by the second of another graphene
Alcoholic solution is added dropwise according to the speed of 2.5~3.5mL/min, and it is 500Pa~2000Pa's that vacuum degree is put into after being added dropwise to complete
Electromagnetic agitation is carried out in vacuum tank, mixing time is 24~40h, stops stirring after the color of slurries becomes limpid, in 75~80
It is heated at DEG C, then vacuum drying obtains the compound hair engaging aperture aluminium foil of graphene attachment；
The compound hair engaging aperture aluminium foil that S3, the graphene for obtaining S2 adhere to is packed into the aluminum pipe mold that size is 13 × 150mm of Ф
In, HIP sintering is carried out under inert atmosphere protection under 20MPa pressure, sintering temperature is 580~630 DEG C, sintering time
For 2~5h, graphene aluminum matrix composite is finally obtained.
Preferably, the raw material in S1 are 2A16 aluminium alloys.
Preferably, the substance withdrawl syndrome of cetyl trimethylammonium bromide aqueous solution is 1~1.2mol/L in S1, aluminium foil
The additional proportion of thin slice and cetyl trimethylammonium bromide aqueous solution is 1mg：10ml.
Preferably, the mass ratio of the graphene nanometer sheet in S2 and ethyl alcohol is 1：1000.
Preferably, the mass ratio of graphene nanometer sheet and hair engaging aperture aluminium foil is 0.2~0.5 in S2：99.8~99.5.
Preferably, the inert atmosphere in S3 is argon gas.
There is the prior art to compare, preparation method of the invention has the advantages that：The present invention passes through aluminium foil hair engaging aperture+stone
Graphene aluminum matrix composite is prepared in the method for black alkene attachment+hot isostatic pressing, and preparation method is simple, mild condition, graphite
Alkene nanometer sheet is uniformly adhered in the etch pit hole of aluminium foil and retains prototype structure, and graphene/aluminum interface cohesion is good, graphite
The performance of alkene aluminum matrix composite significantly improves, and the graphene aluminium base synthesized when wherein HIP sintering temperature is 600 DEG C is answered
Condensation material performance is best, and tensile strength, yield strength and elongation respectively reach 495MPa, 373MPa and 16.32%.
Description of the drawings
Fig. 1 is the surface of hair engaging aperture aluminium foil and the TEM pictures in vertical section；
Fig. 2 is the TEM pictures of graphene nanometer sheet；
Fig. 3 is the SEM pictures of hair engaging aperture aluminium foil surface and the SEM pictures of the graphene in etch pit of graphene attachment；
Fig. 4 is in the SEM pictures on graphene aluminum matrix composite surface in embodiment 1 and graphene aluminum matrix composite
The SEM pictures of graphene existing for portion；
Fig. 5 is the TEM pictures of graphene aluminum matrix composite in embodiment 1；
Fig. 6 is the load-deformation curve of graphene aluminum matrix composite and as-cast aluminum alloy 2A16 in embodiment 1；
Fig. 7 is that the stretching of the SEM pictures of 2A16 Aluminum alloy tensile fractures and the graphene aluminum matrix composite of embodiment 1 is broken
The SEM pictures of mouth；
Fig. 8 is the EDS collection of illustrative plates of the stretching fracture of graphene aluminum matrix composite in embodiment 1.
Fig. 9 is the SEM pictures on graphene aluminum matrix composite surface in embodiment 2；
Figure 10 is the SEM pictures on graphene aluminum matrix composite surface in embodiment 3
Specific embodiment
Embodiment 1
It is a kind of using hair engaging aperture made with aluminum foil for the method for graphene aluminum matrix composite, include the following steps：
Aluminium alloy 2A16 is chosen as raw material, corrosion hair engaging aperture is carried out in sulfuric acid-hcl corrosion system, after hair engaging aperture
Aluminium foil freezes 20min in liquid nitrogen, and the thin slice of Ф 12 is cut into after freezing, and weighing the thin slice of 100g, to be added to 1000mL a concentration of
In the cetyl trimethylammonium bromide aqueous solution of 1mol/L, positively charged hair engaging aperture aluminium foil is obtained after stirring, washing, drying,
Mixing time is 70min, and drying temperature is 60 DEG C, drying time 100min；
S2, it weighs 0.2g multi-layer graphenes nanometer sheet and is dissolved with 200mL ethyl alcohol, ultrasonic disperse 1h obtains graphene
Ethanol solution, the ethanol solution of graphene is equally divided into two parts, thereto in portion 100mL solution add in 99.8gS1 in
Obtained hair engaging aperture aluminium foil carries out ultrasonic disperse and mechanical agitation, speed of agitator 100r/min, then by another 100mL stone
The ethanol solution of black alkene is added dropwise according to the speed of 3mL/min, and the vacuum tank that vacuum degree is 1000Pa is put into after being added dropwise to complete
Interior carry out electromagnetic agitation, mixing time is for 24 hours, stops stirring after the color of slurries becomes limpid, is heated at 75 DEG C, Ran Houzhen
Sky is dried to obtain the compound hair engaging aperture aluminium foil of graphene attachment；
The compound hair engaging aperture aluminium foil that S3, the graphene for obtaining S2 adhere to is packed into the aluminum pipe mold that size is 13 × 150mm of Ф
In, HIP sintering is carried out under argon gas protection under 20MPa pressure, sintering temperature is 600 DEG C, sintering time 2h, finally
Obtain graphene aluminum matrix composite.
Embodiment 2
Preparation method is same as Example 1, the difference is that the sintering temperature of the compound hair engaging aperture aluminium foil of graphene attachment is 580
℃。
Embodiment 3
Preparation method is same as Example 1, the difference is that the sintering time of the compound hair engaging aperture aluminium foil of graphene attachment is 1h.
The hair engaging aperture aluminium foil and graphene that we adhere to hair engaging aperture aluminium foil, graphene nanometer sheet, the graphene in embodiment 1
Aluminum matrix composite has carried out microscopic appearance characterization, has carried out scanning electron microscope test respectively and transmission electron microscope is surveyed
Examination., the graphene aluminum matrix composite of embodiment 2- embodiments 4 is carried out
Fig. 1 (a) and (b) are respectively the TEM pictures of hair engaging aperture aluminium foil surface and the TEM pictures in vertical section, can from Fig. 1
Go out, deep hole pass is neat in aluminium foil, and deep hole diameter is substantially uniform, and deep hole depth is basically identical, and aluminium foil surface is shallow there is also some
Hole, some shallow bore holes connection growth is together.
Fig. 2 (a) and the TEM pictures that (b) is graphene nanometer sheet, figure it is seen that the accordion of graphene nanometer sheet
Pattern is more apparent and very transparent, in featheriness, illustrates that the graphene thickness used in preparation process is very thin, radial dimension
In micron dimension.
Fig. 3 (a) and (b) are respectively the graphene in the SEM figures and etch pit of the hair engaging aperture aluminium foil surface of graphene attachment
SEM pictures, from figure 3, it can be seen that be attached to graphene nanometer sheet in the hole of aluminium foil, the pleated structure of graphene nanometer sheet
Preserved well, in order, graphene is evenly distributed in hole for the filling of graphene nanometer sheet, graphene platelet it
Between there are certain gaps.
Fig. 4 (a) and (b) are respectively the SEM figures on graphene aluminum matrix composite surface and graphene aluminum matrix composite
The SEM pictures of graphene existing for inside, from fig. 4, it can be seen that alloy structure is uniform, no hole, metallurgical quality is good, has no
Apparent metallurgical imperfection, graphene have sheet institutional framework in aluminium alloy, and spreadability is good on alloy matrix aluminum, piece
Layer diameter is about 0.5~1 μm, and the pleated structure of graphene remains to preserve during HIP sintering.
Fig. 5 is the TEM pictures of graphene aluminum matrix composite, observes that graphene enhancing metal-based nano is compound by Fig. 5
The form of graphene nanometer sheet in material, graphene nanometer sheet exist in crystal boundary and crystal.With reference to Fig. 3 (a) and Fig. 5
(a) it learns, graphene nanometer sheet is filled in the hair engaging aperture of aluminium foil, is filled between the graphene in hair engaging aperture that there are more skies
Gap during HIP sintering, generates fusion between aluminium foil hole wall, the graphene of the Nano grade between gap is mothballed
In crystal, for the larger graphene that occurs to reunite there are grain boundaries, the two has larger combination interface.It can see from Fig. 5 (b)
The two-dimensional film form of graphene nanometer sheet and pleated structure feature, the size for observing graphene nanometer sheet in crystal are about
20nm illustrates the graphene nanometer sheet not fragmentation in aluminium alloy alkene alloy substrate, after heat and other static pressuring processes, graphene nano
Piece maintains original structure architectural characteristic.
Then we close graphene aluminum matrix composite and 2A16 aluminium using 200 type electronic universal material testing machines of WDW
Gold has carried out room temperature tensile properties test, and microscopic appearance characterization and energy spectrum analysis have been carried out to stretching fracture.
Fig. 6 is the load-deformation curve of graphene aluminum matrix composite and 2A16 aluminium alloys, and table 1 is room temperature aluminium base alkene
Alloy and comparison Tensile Properties of Aluminum Alloy data.With reference to Fig. 6 and table 1 it is found that the yield strength of graphene aluminum matrix composite and
Tensile strength is substantially better than 2A16 aluminium alloys, and the addition of graphene nanometer sheet significantly improves the tensile strength of alloy, average anti-
Tensile strength is increased to 495MPa from 362MPa, increases 33%；Meanwhile the average yield strength of alloy is increased to from 237MPa
373MPa increases 54%, and increase rate is substantially better than the enhancing effect of other materials reinforced aluminum matrix composites.
The stretching experiment data of 1 aluminium alloy of table and graphene aluminum matrix composite
Fig. 7 (a) is the SEM pictures of 2A16 Aluminum alloy tensile fractures, and Fig. 7 (b) (c) (d) is graphene aluminum matrix composite
Stretching fracture SEM pictures, Fig. 8 be graphene aluminum matrix composite stretching fracture EDS collection of illustrative plates, obtained with reference to Fig. 7 and Fig. 8
Know, the stretching fracture of 2A16 aluminium alloys has a small amount of cleavage step, round dimple and tear rib, while also river pattern is deposited
Showing as partially brittle mixed fracture feature.After graphene nanometer sheet is added in its stretching fracture mainly by round dimple and
Rib composition is torn, and the quantity of dimple shows as ductile rupture than the showed increased of A216 aluminium alloy.It finds simultaneously in graphite
There are the filiform of lengthy motion picture shape in the stretching fracture section of alkene aluminum matrix composite, filiform shows good plasticity, Filamentous
The surface of object is relatively smooth or has stair-stepping tear rib, and in filiform part insertion alloy matrix aluminum, another part is then sudden and violent
It is exposed at fracture surface.It is analyzed by EDS it is found that the filiform is made of aluminium and carbon, it is seen that it has graphene in forming.By
There was only several nanometers in graphene thickness, the spacing between aluminium alloy crystal grain is very small, this is more advantageous to external force from aluminium alloy base
Body is transferred to graphene nanometer sheet, and graphene large specific surface area in matrix, fold is apparent, can there are a pleats in loading process
The process that wrinkle flattening is broken again, graphene has good plasticity in itself in addition and there are good interface knots between aluminum substrate
It closes, therefore there are the good filiforms of plasticity at aluminium base alkene Alloy Fracture.The existing tear rib in filiform surface is alternatively
There are good interface cohesions between bright graphene and aluminum substrate.
Fig. 9 and Figure 10 is the SEM figures on the graphene aluminum matrix composite surface of embodiment 2- embodiments 4, can be with from figure
Find out, the graphene aluminum matrix composite alloy structure of Fig. 9 is uniform, and no hole, metallurgical quality is good, has no apparent metallurgical scarce
It falls into, but since sintering time is inadequate, there are metallurgical imperfection, hole is more apparent for graphene aluminum matrix composite in Figure 10.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, several improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (6)
1. it is a kind of using hair engaging aperture made with aluminum foil for the method for graphene aluminum matrix composite, which is characterized in that include the following steps：
S1, aluminium alloy is chosen as raw material, corrosion hair engaging aperture is carried out in sulfuric acid-hcl corrosion system, by the aluminium foil after hair engaging aperture
20~25min is freezed in liquid nitrogen, the thin slice of preliminary dimension is cut into after freezing, the thin slice for weighing certain mass is added to hexadecane
In base trimethylammonium bromide aqueous solution, stirring, washing, it is dry after obtain positively charged hair engaging aperture aluminium foil, mixing time for 30~
70min, drying temperature are 35~60 DEG C, and drying time is 50~100min；
S2, the multi-layer graphene nanometer sheet for weighing certain mass are simultaneously dissolved with ethyl alcohol, and 1~1.5h of ultrasonic disperse obtains graphite
The ethanol solution of graphene is equally divided into two parts by the ethanol solution of alkene, adds in the hair obtained in S1 in a solution thereto
Hole aluminium foil is carried out at the same time the mechanical agitation of ultrasonic disperse and rotating speed for 100r/min, then that the ethyl alcohol of another graphene is molten
Liquid is added dropwise according to the speed of 2.5~3.5mL/min, and the vacuum that vacuum degree is 500Pa~2000Pa is put into after being added dropwise to complete
Electromagnetic agitation is carried out in case, mixing time is 24~40h, stops stirring after the color of slurries becomes limpid, at 75~80 DEG C
Heating, then vacuum drying obtain the compound hair engaging aperture aluminium foil of graphene attachment；
S3, the compound hair engaging aperture aluminium foil that the graphene that S2 is obtained adheres to is fitted into the aluminum pipe mold that size is 13 × 150mm of Ф, it is lazy
Property atmosphere protection under carry out HIP sintering under 20MPa pressure, sintering temperature is 580~630 DEG C, sintering time for 2~
5h finally obtains graphene aluminum matrix composite.
2. it is as described in claim 1 it is a kind of using hair engaging aperture made with aluminum foil for the method for graphene aluminum matrix composite, feature exists
In the raw material in the S1 are 2A16 aluminium alloys.
3. it is as described in claim 1 it is a kind of using hair engaging aperture made with aluminum foil for the method for graphene aluminum matrix composite, feature exists
In, in the S1 substance withdrawl syndrome of cetyl trimethylammonium bromide aqueous solution be 1~1.2mol/L, aluminium foil thin slice and ten
The additional proportion of six alkyl trimethyl ammonium bromide aqueous solutions is 1mg：10ml.
4. it is as described in claim 1 it is a kind of using hair engaging aperture made with aluminum foil for the method for graphene aluminum matrix composite, feature exists
In the mass ratio of graphene nanometer sheet and ethyl alcohol in the S2 is 1：1000.
5. it is as described in claim 1 it is a kind of using hair engaging aperture made with aluminum foil for the method for graphene aluminum matrix composite, feature exists
In the mass ratio of graphene nanometer sheet and hair engaging aperture aluminium foil is 0.2~0.5 in the S2：99.8~99.5.
6. it is described in claim 1 it is a kind of using hair engaging aperture made with aluminum foil for the method for graphene aluminum matrix composite, which is characterized in that
Inert atmosphere in the S3 is argon gas.
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| CN111321314A (en) * | 2020-02-28 | 2020-06-23 | 西安交通大学 | Preparation method of graphene reinforced aluminum matrix composite with strong interface bonding strength |
| CN112828291A (en) * | 2020-12-31 | 2021-05-25 | 宁波通导电子有限公司 | Manufacturing method of high-temperature operation robot |
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