CN109666821A - A kind of titanium composite material and preparation method thereof - Google Patents
A kind of titanium composite material and preparation method thereof Download PDFInfo
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- CN109666821A CN109666821A CN201910114634.2A CN201910114634A CN109666821A CN 109666821 A CN109666821 A CN 109666821A CN 201910114634 A CN201910114634 A CN 201910114634A CN 109666821 A CN109666821 A CN 109666821A
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 239000010936 titanium Substances 0.000 title claims abstract description 73
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 73
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 184
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 98
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 98
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 76
- 238000005245 sintering Methods 0.000 claims abstract description 39
- 239000011259 mixed solution Substances 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008187 granular material Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000009413 insulation Methods 0.000 claims abstract description 8
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000010790 dilution Methods 0.000 claims abstract description 4
- 239000012895 dilution Substances 0.000 claims abstract description 4
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 4
- 239000010439 graphite Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000007731 hot pressing Methods 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 238000000643 oven drying Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims 1
- 238000007710 freezing Methods 0.000 claims 1
- 230000002787 reinforcement Effects 0.000 abstract description 10
- 238000005054 agglomeration Methods 0.000 abstract description 5
- 230000002776 aggregation Effects 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 19
- 230000006835 compression Effects 0.000 description 16
- 238000007906 compression Methods 0.000 description 16
- 230000002708 enhancing effect Effects 0.000 description 14
- 239000011812 mixed powder Substances 0.000 description 7
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- 229910007948 ZrB2 Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- 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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
- C22C2026/002—Carbon nanotubes
Abstract
The invention discloses a kind of titanium composite material and preparation method thereof, titanium composite material the preparation method comprises the following steps: 1, graphene oxide solution diluted with dehydrated alcohol, 2, carbon nanotube powder is added ultrasonic disperse in dilution graphene oxide solution；3, after ultrasonic disperse being added in titanium valve again, the mixed solution of graphene oxide/carbon nanotube and titanium valve is obtained；4, it is completely dried in an oven, obtains the composite granule of graphene oxide/carbon nanotube and titanium valve；5, by the graphite jig of composite granule merging hot-pressed sintering furnace, heat-insulation pressure keeping is sintered in argon gas protection environment.Additionally provide a kind of titanium composite material prepared by above-mentioned preparation method.The present invention can effectively improve the agglomeration traits of reinforcement in the base using graphene oxide/carbon nanotube mixing as reinforcement, improve the dispersibility of reinforcement in the base, to improve the mechanical property of matrix to the maximum extent.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of graphene oxide/carbon nanotube enhancing titanium-based is multiple
Condensation material and preparation method thereof.
Background technique
Titanium composite material due to having that specific strength is high, specific modulus is high, high-temperature behavior is good and the series of advantages such as corrosion-resistant,
It is widely used in the fields such as space flight and aviation, auto industry, medical instrument, is most promising structural material and function
One of energy material.
Select the reinforcement that light weight, fusing point are high, intensity is high most important to the performance for improving titanium composite material.At present
Reinforcement type in titanium composite material is mainly with TiB, TiC, Al2O3、B4C、TiN、ZrB2Equal ceramic particles reinforcement with
And based on the fibre reinforcements such as SiC.The volume fraction of reinforced phase is generally in 10-20%.However, ceramic particle hardness itself is high, modeling
Property is poor, is often substantially reduced the toughness of composite material；Simultaneously because the elongation of material is lower, to titanium composite material into
One step plastic processing also becomes very difficult, and processing cost significantly improves.In addition, although fiber can be mentioned significantly as reinforced phase
The performances such as the elasticity modulus of titanium composite material are risen, but the problems such as coefficient of thermal expansion mismatch, anisotropy and process costs limits
Its industrial application is made.
In recent years, novel nano carbonaceous material includes carbon nanotube and the graphene mechanics and object low, excellent due to density
Rationality can cause extensive concern, it is considered to be the ideal reinforcement material of titanium composite material.However due to carbon nanotube
With graphene large specific surface area, and all there is stronger Van der Waals force, Yi Fu between graphene sheet layer between carbon nanotube
Reunite in condensation material, to cause the effect for the improvement of material property being much not achieved theoretical prediction.According to document " Rapid
and low temperature spark plasma sintering synthesis of novel carbon nanotube
Reinforced titanium matrix composites " FC Wang, Carbon, 2015,95,396-407(is fast
The titanium composite material of fast low temperature discharge plasma sintering synthesizing carbon nanotubes enhancing, FC Wang, Carbon, volume 95,
The 396-407 pages, 2015) it records: carbon nanotube limit content evenly dispersed in Titanium base is extremely limited, additive amount
It is usually no more than 0.5 wt.%.If desired increase substantially substrate performance, then to continue improve additive amount, this again and agglomeration traits
Form contradiction.This contradiction seriously constrains the promotion of composite property, and it is multiple to become nanometer carbon material enhancing Metal Substrate
The critical bottleneck problem of condensation material technology development.
Summary of the invention
In view of the problems of the existing technology, the technical problem to be solved by the invention is to provide a kind of titanium-based composite woods
Material and preparation method thereof, it can overcome existing single graphene or carbon nanotube to enhance easy to reunite in production procedure to cause material
The problem of performance improvement deficiency, to substitute single graphene or carbon nanotube as the novel enhanced body of titanium composite material.
Insight of the invention is that be that chemical method prepares the one kind generated during graphene important for graphene oxide (GO)
Graphene derivative, a large amount of oxygen-containing functional group is contained in structure, causes graphene oxide in water and various organic solutions
In all have good dispersibility.The present invention increases carbon nanotube by surface of graphene oxide oxygen-containing functional group effect abundant
Dispersibility, it is multiple as titanium-based to substitute single graphene or carbon nanotube to use graphene oxide and carbon nanotube hybrid dispersions
The novel enhanced body of condensation material, solution carbon nanotube agglomeration traits, while utilization graphene oxide cooperate with work with carbon nanotube
With greatly improving the mechanical property of composite material.
In order to solve technical problem of the invention:
Present invention firstly provides a kind of methods for preparing titanium composite material, comprising the following steps:
Step 1 prepares graphene oxide solution with improved Hummers method, and is diluted to obtain graphene oxide with dehydrated alcohol
Solution；
Step 2 mixes the graphene oxide after dilution with carbon nanotube powder, using ultrasonic stirrer ultrasonic disperse, obtains
Graphene oxide/carbon nanotube mixed solution；
Step 3 mixes graphene oxide/carbon nanotube mixed solution with titanium valve, using ultrasonic stirrer ultrasonic disperse, obtains
The mixed solution of graphene oxide/carbon nanotube and titanium valve；
The mixed solution of graphene oxide/carbon nanotube and titanium valve is placed in water-bath magnetic stirring apparatus and stirs to basic by step 4
It after drying, is dried with baking oven, obtains the composite granule that graphene oxide/carbon nanotube is mixed with titanium valve；
The resulting composite granule of step 4 is put into hot-pressed sintering furnace mold by step 5, is kept the temperature under argon gas protection environment
Pressure maintaining sintering, naturally cools to room temperature after sintering.
Specifically,
In above-mentioned steps 2, in graphene oxide/carbon nanotube mixed solution, the mass ratio of carbon nanotube and graphene oxide
It is 1: 0.1 ~ 5.
In above-mentioned steps 3, in the mixed solution of graphene oxide/carbon nanotube and titanium valve, carbon nanotube and titanium valve quality
Ratio is 1: 167, and the purity of titanium valve is 99.5%, and the grain diameter of titanium valve is less than 50 μm.
In above-mentioned steps 4, water-bath magnetic stirring apparatus water temperature is lower than 78 DEG C, mixing time at least 4h, and oven drying temperature is low
In 78 DEG C, drying time at least 12 h.
In above-mentioned steps 5, after the hot-pressed sintering furnace mold equipped with composite granule is put into vacuum sintering funace, first
To being vacuumized in vacuum sintering funace, so that the vacuum degree in vacuum sintering funace is 20 Pa hereinafter, being re-filled with argon
Gas shielded carries out heat-insulation pressure keeping sintering, and heating rate is 15 DEG C/min or more, and hot pressing furnace applies graphite jig in sintering process
Pressure is 50 ± 3 MPa, and soaking time at least 30min, sintering temperature is 1200 DEG C.
The present invention provides a kind of titanium composite materials prepared by above-mentioned preparation method.
Preferably, in titanium composite material include graphene oxide, carbon nanotube and Titanium, carbon nanotube and oxidation stone
The mass ratio of black alkene is 1: 0.1 ~ 5；The mass ratio of carbon nanotube and titanium valve is 1: 167.
Compared with prior art, the solution have the advantages that:
1, the present invention improves the dispersibility of carbon nanotube by the surface functional group of graphene oxide, solves physical method point
It dissipates poor carbon nanotube dispersion effect, easy secondary agglomeration and chemical modification method and causes performance tight the damage of carbon nano tube structure
The problem of declining again significantly improves its dispersibility in the case where maintaining carbon nano tube structure.
2, the present invention has heating using hot pressing sintering method preparation graphene/carbon nano-tube collaboration enhancing titanium composite material
Fastly, the advantages that temperature control is precisely, pressure control range is big.Using heating precompressed, the technique of heat-insulation pressure keeping be can effectively improve
The bulk density of composite material.This technique can also effectively shorten sintering time, reduce sintering temperature, prevent crystal grain sintered
Excessively growing up in journey, reduces crystallite dimension.The high-compactness and fine grain of material can effectively promote the mechanical property of material
Energy.
3, titanium composite material of the invention has many advantages, such as that intensity is high, hardness is high.Preparation process is simple, operability
By force, reinforcement is evenly distributed in the base, and material property is good, has wide prospects for commercial application.
Detailed description of the invention
Detailed description of the invention of the invention is as follows:
Fig. 1 is the resulting composite granule scanning electron microscope microscopic appearance figure of step 4 in the step 3 and embodiment 2 ~ 4 of embodiment 1；
Carbon nanotube is marked with circle；
Fig. 2 is that compression stress-strain of the step 5 gained titanium composite material in the step 4 and embodiment 2 ~ 4 of embodiment 1 is bent
Line chart.
Specific embodiment
Content for a better understanding of the present invention combined with specific embodiments below retouches the preferred embodiment of the invention
It states, these descriptions are intended merely to further illustrate advantages of the present invention and technique, rather than the limitation to invention claim.
Embodiment 1
The mass ratio of selected carbon nanotube powder and graphene oxide is 1: 0, and preparation carbon nanotube enhances titanium composite material:
1,0.084 g carbon nanotube powder is added in dehydrated alcohol, is mixed with ultrasonic stirrer, the alcohol for obtaining carbon nanotube is molten
Liquid；
2,14 g titanium valves are added in the alcoholic solution of carbon nanotube, the mass ratio of carbon nanotube and titanium valve is 1: 167, by super
The mixing of sound blender, obtains the mixed solution of carbon nanotube and titanium valve；
3, by the mixed solution of carbon nanotube and titanium valve, stir about 4h is to substantially dry in 60 DEG C of stirring in water bath devices, then 60
Dry 12h is thoroughly dried in DEG C baking oven, obtains the mixed powder of carbon nanotube and titanium valve；
4, the mixed powder for obtaining step 3 is put into hot-pressed sintering furnace mold, is then placed in vacuum sintering funace in argon
Heat-insulation pressure keeping sintering is carried out under gas shielded environment, sintering heating rate is 15 DEG C/min, and sintering maximum temperature is 1200 DEG C, heat preservation
It is 50 ± 3 MPa that pressure head, which is applied to the pressure on hot-pressed sintering furnace mold, during pressure maintaining is burnt, and heat-insulation pressure keeping sintering time is 30
Min, then furnace cooling, obtains a kind of hot-forming carbon nanotube enhancing titanium composite material.
Find out from Fig. 1 (picture for being labeled with 1: 0), apparent clustering phenomena is presented in the carbon nanotube in mixed powder.
The compression yield strength and compressive ultimate strength for measuring the carbon nanotube enhancing titanium composite material of the present embodiment, are surveyed
GB/T 7314-1987 testing standard is used, compression stress strain curve is (curve for being labeled with 1: 0) as shown in Figure 2: the carbon
The compression yield strength that nanotube enhances titanium composite material is 860.7 MPa, and compressive ultimate strength is 1473 MPa.It is micro- hard
Degree is 328 HV.
The temperature of stirring in water bath device and baking oven guarantees to be lower than 78 DEG C of ethyl alcohol boiling point in step 3, so that the second in mixed solution
Alcohol mildly volatilizees.For the preciseness of Experimental comparison, each embodiment all uses 60 DEG C to stir as magnetic force in present patent application
Mix process and drying course temperature, with guarantee obtained the performance test results only with carbon nanotube and graphene oxide ratio phase
It closes.
Embodiment 2
The mass ratio of selected carbon nanotube powder and graphene oxide is 1: 0.1, prepares graphene oxide/carbon nanotube enhancing titanium
Based composites:
1, using improved Hummers method, referring to document Improved Synthesis of Graphene Oxide.
Marcano D C, ACS NANO, 2010,4 (8): the improvement synthetic method Marcano D of 4806-4814(graphene oxide
C, ACS NANO, 2010, the 8th phase of volume 4, the 4806-4814 pages), prepare graphene oxide solution.By actual oxygen fossil
Black alkene content is that 0.0084g taking-up part is diluted with dehydrated alcohol, the graphene oxide solution after being diluted；
2, carbon nanotube powder 0.084g is added in graphene oxide solution after dilution, makes carbon nanotube and graphene oxide
Mass ratio be 1: 0.1, mixed with ultrasonic stirrer, obtain graphene oxide/carbon nanotube mixed solution；
3,14g titanium valve is added in graphene oxide/carbon nanotube mixed solution, makes the mass ratio of carbon nanotube and titanium valve
1: 167, it is mixed by ultrasonic stirrer, obtains the mixed solution of graphene oxide/carbon nanotube and titanium valve；
4, by the mixed solution of above-mentioned graphene oxide/carbon nanotube and titanium valve in 60 DEG C of stirring in water bath devices stir about 5h to base
This drying, then dry 12h is thoroughly dried in 60 DEG C of baking ovens, obtains the mixed powder of graphene oxide/carbon nanotube and titanium valve
Body；
5, the mixed powder for obtaining step 4 is put into hot-pressed sintering furnace mold, is then placed in vacuum sintering funace in argon
Heat-insulation pressure keeping sintering is carried out under gas shielded environment, sintering heating rate is 15 DEG C/min, and sintering maximum temperature is 1200 DEG C, heat preservation
It is 50 ± 3 MPa that pressure head, which is applied to the pressure on hot-pressed sintering furnace mold, during pressure maintaining is burnt, and heat-insulation pressure keeping sintering time is 30
Min, then furnace cooling.
Find out from Fig. 1 (picture for being labeled with 1: 0.1), after small amounts graphene is added, dispersibility has carbon nanotube
It is obviously improved, the size of the carbon nanotube of reunion is obviously less than 1 form of embodiment.
Measure the compression yield strength and compressive ultimate strength of the carbon nanotube enhancing titanium composite material of the present embodiment, pressure
Stress under compression strain curve is (curve for being labeled with 1: 0.1) as shown in Figure 2: compression yield strength is 903.3 MPa, and compression limit is strong
Degree is 1898.2MPa, and yield strength and ultimate strength are all higher than embodiment 1.Microhardness is 330.2 HV, compares embodiment 1
Slightly promoted.
Embodiment 3
The mass ratio of selected carbon nanotube powder and graphene oxide is 1: 1, prepares graphene oxide/carbon nanotube enhancing titanium-based
Composite material.As different from Example 2:
It is being that 0.084g taking-up is partially diluted with dehydrated alcohol by practical graphene oxide content, after being diluted in step 1
Graphene oxide solution, so that the mass ratio of carbon nanotube and graphene oxide is after 0.084g carbon nanotube is added in step 2 kind
1∶1。
Find out from Fig. 1 (picture for being labeled with 1: 1), in the mixed-powder of the present embodiment, the distribution of carbon nanotube aggregate is bright
Show more uniform, carbon nanotube sizes are smaller than in embodiment 2, and carbon nanotube is more sparse in aggregate, and some regions have gone out
It is now completely independent existing single-root carbon nano-tube, the raising of graphene oxide ratio is conducive to the promotion of carbon nanotube dispersibility.
Measure the compression yield strength and compressive ultimate strength of the carbon nanotube enhancing titanium composite material of the present embodiment, pressure
Stress under compression strain curve is (curve for being labeled with 1: 1) as shown in Figure 2: compression yield strength is 1050.1 MPa, and compression limit is strong
Degree is that 1924.3 MPa, yield strength and ultimate strength are obviously improved again compared with embodiment 2.Microhardness is 476 HV, more in fact
Example 2 is applied to be obviously improved.
Embodiment 4
The mass ratio of selected carbon nanotube powder and graphene oxide is 1: 5, prepares graphene oxide/carbon nanotube enhancing titanium-based
Composite material.As different from Example 2:
It is being that 0.42g taking-up is partially diluted with dehydrated alcohol by practical graphene oxide content, after being diluted in step 1
Graphene oxide solution, so that the mass ratio of carbon nanotube and graphene oxide is after 0.084g carbon nanotube is added in step 2 kind
1∶5。
Find out that in the mixed-powder of the present embodiment, carbon nanotube is distributed in the base from Fig. 1 (picture for being labeled with 1: 5)
It is visibly homogeneous, exist substantially in the form of single-root carbon nano-tube in addition to the carbon nanotube being connect with graphene oxide.
Measure the compression yield strength and compressive ultimate strength of the carbon nanotube enhancing titanium composite material of the present embodiment, pressure
Stress under compression strain curve is (curve for being labeled with 1: 5) as shown in Figure 2: compression yield strength is 1387.1 MPa, and compression limit is strong
Degree is that 1950.2 MPa, yield strength and ultimate strength are still obviously improved compared with embodiment 3.Microhardness is 575 HV, more in fact
Example 3 is applied to be obviously improved.
Fig. 2 is the compressive stress strain curve figure of above-mentioned 4 kinds of materials, as can be seen from Figure 2 with graphene oxide and carbon
Nanotube ratio increases, and yield strength is continuously improved therewith with compressive strength, when carbon nanotube and graphene oxide ratio are 1:5
When, yield strength and ultimate strength all reach highest, compared to independent carbon nanotube enhancing titanium composite material yield strength and
Ultimate strength can promote 54 % and 32 % respectively.
In conclusion graphene oxide of the invention/carbon nanotube collaboration enhancing titanium composite material, utilizes graphite oxide
Alkene, carbon nanotube by alcoholic solution ultrasonic disperse mixing can be effectively improved single carbon nanotube reinforcement in the base
Agglomeration traits, to increase substantially the performances such as intensity and the hardness of material.Hot pressed sintering may be implemented compared with low frit temperature
Spend the high-compactness of lower material.Material preparation process is simple, and acquisition material mechanical performance is excellent, before industrial application with higher
Scape.
Claims (8)
1. a kind of preparation method of titanium composite material, characterized in that the following steps are included:
Step 1 prepares graphene oxide solution with improved Hummers method, and is diluted to obtain graphene oxide with dehydrated alcohol
Solution；
Step 2 mixes the graphene oxide after dilution with carbon nanotube powder, using ultrasonic stirrer ultrasonic disperse, obtains
Graphene oxide/carbon nanotube mixed solution；
Step 3 mixes graphene oxide/carbon nanotube mixed solution with titanium valve, using ultrasonic stirrer ultrasonic disperse, obtains
The mixed solution of graphene oxide/carbon nanotube and titanium valve；
The mixed solution of graphene oxide/carbon nanotube and titanium valve is placed in water-bath magnetic stirring apparatus and stirs to basic by step 4
It after drying, is dried with baking oven, obtains the composite granule that graphene oxide/carbon nanotube is mixed with titanium valve；
The resulting composite granule of step 4 is put into hot-pressed sintering furnace mold by step 5, is kept the temperature under argon gas protection environment
Pressure maintaining sintering, naturally cools to room temperature after sintering.
2. preparation method according to claim 1, it is characterized in that: described state in step 2, graphene oxide/carbon nanotube
Mixed solution in, the mass ratio of carbon nanotube and graphene oxide is 1: 0.1 ~ 5.
3. preparation method according to claim 2, it is characterized in that: in the step 3, graphene oxide/carbon nanotube with
In the mixed solution of titanium valve, carbon nanotube and titanium valve mass ratio are 1: 167, and the purity of titanium valve is 99.5%, the particle of titanium valve
Diameter is less than 50 μm.
4. preparation method according to claim 3, it is characterized in that: water-bath magnetic stirring apparatus water temperature is lower than in the step 4
78 DEG C, mixing time at least 4h, oven drying temperature is lower than 78 DEG C, drying time at least 12 h.
5. the preparation method according to claim 4, it is characterized in that: burning the hot pressing equipped with composite granule in the step 5
After freezing of a furnace mold is put into vacuum sintering funace, first to being vacuumized in vacuum sintering funace, so that vacuum hotpressing
Vacuum degree in sintering furnace is 20 Pa hereinafter, being re-filled with argon gas protection carries out heat-insulation pressure keeping sintering, and heating rate is 15 DEG C/min
More than, it is 50 ± 3 MPa, soaking time at least 30min, sintering temperature that hot pressing furnace, which applies pressure to graphite jig, in sintering process
It is 1200 DEG C.
6. the titanium composite material of any one of -5 preparation method preparations according to claim 1.
7. titanium composite material according to claim 6, it is characterized in that: including graphene oxide, carbon nanotube and metal
The mass ratio of titanium, carbon nanotube and graphene oxide is 1: 0.1 ~ 5.
8. titanium composite material according to claim 7, it is characterized in that: the mass ratio of carbon nanotube and titanium valve is 1:
167。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110039042A (en) * | 2019-05-06 | 2019-07-23 | 安徽工业大学 | A kind of preparation method of carbon nanotube enhancing titanium magnesium alloy composite material |
| CN110952014A (en) * | 2019-12-19 | 2020-04-03 | 重庆大学 | Preparation method of low-melting-point metal-carbon nanotube-diamond composite material |
| CN112441777A (en) * | 2019-08-30 | 2021-03-05 | 西安美刚达科技发展有限公司 | Nano fireproof material and preparation method thereof |
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| CN110039042B (en) * | 2019-05-06 | 2021-04-13 | 安徽工业大学 | Preparation method of carbon nano tube reinforced titanium-magnesium alloy composite material |
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| CN113944246A (en) * | 2021-12-01 | 2022-01-18 | 安徽百维新材料有限公司 | Anti-bending insulation board for wall |
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