CN106676304A - Preparation method of graphene titanium-based composite material - Google Patents
Preparation method of graphene titanium-based composite material Download PDFInfo
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- CN106676304A CN106676304A CN201710022174.1A CN201710022174A CN106676304A CN 106676304 A CN106676304 A CN 106676304A CN 201710022174 A CN201710022174 A CN 201710022174A CN 106676304 A CN106676304 A CN 106676304A
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- titanium
- graphene
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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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
Abstract
The invention discloses a preparation method of a graphene titanium-based composite material. Graphene is stripped off through stripping liquid, grinding or stirring cooperates, the requirement for the grinding or stirring speed can be lowered, and stripping of the graphene can be achieved without ultra-high speed shearing of a graphene sheet. By means of the preparation method, a graphene material is well combined with titanium; and due to repeated large deformation, the compactness of the composite material is very high, the mechanical properties of a base body are improved, and the novel titanium-based composite material with high properties can be prepared.
Description
Technical field
The present invention relates to alloy material manufacture field, and in particular to a kind of preparation method of Graphene titanium matrix composite.
Background technology
Research of the people to titanium matrix composite is long-standing, the development course of the three generations that passed by till now, and titanium is closed
The existing granule of reinforcement of gold also has fiber.Silicon carbide fibre strengthens the fatigue ratio matrix of alloy and increases by more than 50%.It is brilliant
Palpus (chopped fiber) and continuous fiber are also several primary strengthening phases of current titanium matrix composite.Add in titanium alloy substrate suitable
When fiber, the reinforcement such as granule can improve the wearability of material, reduce thermal coefficient of expansion etc..
Graphene（Graphene）Be one kind by carbon atom with sp2Hybrid orbital composition hexangle type is in honeycomb lattice
（honeycomb crystal lattice）The monolayer flat film being arranged to make up, the two-dimentional material of only one of which carbon atom thickness
Material.It is but also most hard nano material that Graphene is currently world most thin, with excellent mechanical property and minimum size,
It is that a kind of good titanium matrix composite strengthens phase.
The content of the invention
The present invention provides a kind of preparation method of Graphene titanium matrix composite, and using stripper Graphene is peeled off, and coordinates
Grinding is stirred, it is possible to decrease to grinding or the requirement of mixing speed, without the need for being capable of achieving to stone to graphite flake layer ultra high shear
The stripping of black alkene, preparation method also achieves the good combination of grapheme material and titanium, due to repeatedly big deformation, can make
Composite reaches very high consistency, improves the mechanical property of matrix, can prepare high performance new titanio and be combined
Material.
To achieve these goals, the invention provides a kind of preparation method of Graphene titanium matrix composite, the method
Comprise the steps：
（1）Prepare graphene powder
By purity more than 99%, particle diameter is in 100 ~ 300 μm of graphite flakes and stripper kettle of the injection with agitator, to open
The motor of dynamic kettle is stirred, make material mix homogeneously, and wherein stripper is consisted of：The parts by weight of ethylene glycol 90, poly- third
The parts by weight of olefin(e) acid ester 40, the parts by weight of silicon dioxide/poly- (methyl methacrylate~styrene) bivalve layer complex microsphere 1,
The parts by weight of lithium chloride 1.Wherein, the particle diameter of silicon dioxide/poly- (methyl methacrylate~styrene) bivalve layer complex microsphere
Below 50 microns, more than 20 nanometers, the thickness of shell is more than 10 nanometers for the particle diameter of silica core；Polyacrylate
More than 100000, the weight ratio of graphite flakes and stripper is 1 to number-average molecular weight：3；
Heating kettle, keeps kettle body temperature to be 90 DEG C, and pressure is 3atm, and agitator shaft speed is 1500 rpm/min, during reaction
Between 3h；After stopped reaction upper strata suspension is expelled in storage tank by discharging opening, stands 24h head products derived above；Will
The graphene suspension in storage tank for obtaining is delivered in centrifuge, and centrifuge speed is 1500rpm/min, centrifugation time
1h, takes the supernatant, and vacuum filter obtains filter cake in vacuum apparatus, and the filter cake for obtaining is washed with appropriate distillation
Wash, filter cake more than lyophilization 4h in freeze drying plant obtains graphene powder；
（2）Pure titanium or titanium alloy material are made annealing treatment, and caustic dip and clean water are carried out to its surface, it is cool after cleaning
Dry or drying；
Pure titanium or titanium alloy powder are sufficiently mixed according to a certain percentage, are stirred with above-mentioned graphene powder；
With the above-mentioned pure titanium for processing or titanium alloy material cladding mixed-powder, it is compacted and seals, then is pressed into forcing press pre-
Clamp dog；
Gained prefabricated section is rolled into into final finished；
Wherein, titanium valve used can be pure titanium valve or titanium alloy powder, and granular size is 150-200 mesh, cladding used
Titanium can be the section bar of tubing, sheet material or other titanium or titanium alloy etc, the content matter of above-mentioned graphene powder used
Amount fraction representation is represented with volume fraction, and mass fraction is 2.5%-6%（Account for the mass percent of titanium valve used）, volume fraction
For 2%-8%（Account for the percent by volume of titanium valve used）.
Preferably, during carrying out being pressed into prefabricated section with titanium cladding powder, if titanium used is titanium tube,
Then titanium tube to have vertically put and puts two ways with level, and when vertically putting, two sections of titanium tube is sealed with the cast of titanium liquid；When level is put, titanium tube
Two sections compress sealing with forcing press, when prefabricated section is pressed with forcing press, have and cold pressing and hot pressing two ways, and hot pressing temperature is 600-
800℃；Rolling also has cold rolling and hot rolling two ways, and hot-rolled temperature is 500-700 DEG C, need to be in the environmental protection of argon before hot rolling
Under carry out 3-7h sintering.
It is an advantage of the current invention that peeling off Graphene using stripper, coordinate grinding or stir, it is possible to decrease to grinding or stirring
The requirement of speed is mixed, without the need for being capable of achieving the stripping to Graphene to graphite flake layer ultra high shear, preparation method is also achieved
Grapheme material and the good combination of titanium, due to repeatedly big deformation, can make composite reach very high consistency, carry
The high mechanical property of matrix, can prepare high performance new titanium matrix composite.
Specific embodiment
Embodiment one
By purity more than 99%, particle diameter is in 100 ~ 300 μm of graphite flakes and stripper kettle of the injection with agitator, to open
The motor of dynamic kettle is stirred, make material mix homogeneously, and wherein stripper is consisted of：The parts by weight of ethylene glycol 90, poly- third
The parts by weight of olefin(e) acid ester 40, the parts by weight of silicon dioxide/poly- (methyl methacrylate~styrene) bivalve layer complex microsphere 1,
The parts by weight of lithium chloride 1.Wherein, the particle diameter of silicon dioxide/poly- (methyl methacrylate~styrene) bivalve layer complex microsphere
Below 50 microns, more than 20 nanometers, the thickness of shell is more than 10 nanometers for the particle diameter of silica core；Polyacrylate
More than 100000, the weight ratio of graphite flakes and stripper is 1 to number-average molecular weight：3.
Heating kettle, keeps kettle body temperature to be 90 DEG C, and pressure is 3atm, and agitator shaft speed is 1500 rpm/min, instead
3h between seasonable；After stopped reaction upper strata suspension is expelled in storage tank by discharging opening, stands 24h primiparity derived above
Product；Graphene suspension in the storage tank for obtaining is delivered in centrifuge, centrifuge speed is 1500rpm/min, is centrifuged
Time 1h, takes the supernatant, and vacuum filter obtains filter cake in vacuum apparatus, by the filter cake for obtaining with appropriate distilled water
Washing, filter cake more than lyophilization 4h in freeze drying plant obtains graphene powder.
Pure titanium or titanium alloy material are made annealing treatment, and caustic dip and clean water are carried out to its surface, after cleaning
Airing or drying；Pure titanium or titanium alloy powder are sufficiently mixed according to a certain percentage, are stirred with above-mentioned graphene powder
It is even；With the above-mentioned pure titanium for processing or titanium alloy material cladding mixed-powder, it is compacted and seals, then is pressed into forcing press prefabricated
Block；Gained prefabricated section is rolled into into final finished.
Wherein, titanium valve used can be pure titanium valve or titanium alloy powder, and granular size is 150-200 mesh, used
Coat the section bar that titanium can be tubing, sheet material or other titanium or titanium alloy etc, the content of above-mentioned graphene powder used
Represented with mass fraction or represented with volume fraction, mass fraction is 2.5%（Account for the mass percent of titanium valve used）, volume integral
Number is 2%（Account for the percent by volume of titanium valve used）.
During carrying out being pressed into prefabricated section with titanium cladding powder, if titanium used is titanium tube, titanium tube has
Vertically put and put two ways with level, when vertically putting, two sections of titanium tube is sealed with the cast of titanium liquid；When level is put, two sections of titanium tube pressure
Power machine compresses sealing, when prefabricated section is pressed with forcing press, has and colds pressing and hot pressing two ways, and hot pressing temperature is 600 DEG C；Rolling
There is cold rolling and hot rolling two ways, hot-rolled temperature is 500 DEG C, need to carry out 3h sintering before hot rolling under the environmental protection of argon.
Embodiment two
By purity more than 99%, particle diameter is in 100 ~ 300 μm of graphite flakes and stripper kettle of the injection with agitator, to open
The motor of dynamic kettle is stirred, make material mix homogeneously, and wherein stripper is consisted of：The parts by weight of ethylene glycol 90, poly- third
The parts by weight of olefin(e) acid ester 40, the parts by weight of silicon dioxide/poly- (methyl methacrylate~styrene) bivalve layer complex microsphere 1,
The parts by weight of lithium chloride 1.Wherein, the particle diameter of silicon dioxide/poly- (methyl methacrylate~styrene) bivalve layer complex microsphere
Below 50 microns, more than 20 nanometers, the thickness of shell is more than 10 nanometers for the particle diameter of silica core；Polyacrylate
More than 100000, the weight ratio of graphite flakes and stripper is 1 to number-average molecular weight：3.
Heating kettle, keeps kettle body temperature to be 90 DEG C, and pressure is 3atm, and agitator shaft speed is 1500 rpm/min, instead
3h between seasonable；After stopped reaction upper strata suspension is expelled in storage tank by discharging opening, stands 24h primiparity derived above
Product；Graphene suspension in the storage tank for obtaining is delivered in centrifuge, centrifuge speed is 1500rpm/min, is centrifuged
Time 1h, takes the supernatant, and vacuum filter obtains filter cake in vacuum apparatus, by the filter cake for obtaining with appropriate distilled water
Washing, filter cake more than lyophilization 4h in freeze drying plant obtains graphene powder.
Pure titanium or titanium alloy material are made annealing treatment, and caustic dip and clean water are carried out to its surface, after cleaning
Airing or drying；Pure titanium or titanium alloy powder are sufficiently mixed according to a certain percentage, are stirred with above-mentioned graphene powder
It is even；With the above-mentioned pure titanium for processing or titanium alloy material cladding mixed-powder, it is compacted and seals, then is pressed into forcing press prefabricated
Block；Gained prefabricated section is rolled into into final finished.
Wherein, titanium valve used can be pure titanium valve or titanium alloy powder, and granular size is 150-200 mesh, used
Coat the section bar that titanium can be tubing, sheet material or other titanium or titanium alloy etc, the content of above-mentioned graphene powder used
Represented with mass fraction or represented with volume fraction, mass fraction is 6%（Account for the mass percent of titanium valve used）, volume fraction
For 8%（Account for the percent by volume of titanium valve used）.
During carrying out being pressed into prefabricated section with titanium cladding powder, if titanium used is titanium tube, titanium tube has
Vertically put and put two ways with level, when vertically putting, two sections of titanium tube is sealed with the cast of titanium liquid；When level is put, two sections of titanium tube pressure
Power machine compresses sealing, when prefabricated section is pressed with forcing press, has and colds pressing and hot pressing two ways, and hot pressing temperature is 800 DEG C；Rolling
There is cold rolling and hot rolling two ways, hot-rolled temperature is 700 DEG C, need to carry out 7h sintering before hot rolling under the environmental protection of argon.
Claims (2)
1. a kind of preparation method of Graphene titanium matrix composite, the method comprises the steps：
（1）Prepare graphene powder
By purity more than 99%, particle diameter is in 100 ~ 300 μm of graphite flakes and stripper kettle of the injection with agitator, to open
The motor of dynamic kettle is stirred, make material mix homogeneously, and wherein stripper is consisted of：The parts by weight of ethylene glycol 90, poly- third
The parts by weight of olefin(e) acid ester 40, the parts by weight of silicon dioxide/poly- (methyl methacrylate~styrene) bivalve layer complex microsphere 1,
The parts by weight of lithium chloride 1,
Wherein, the particle diameter of silicon dioxide/poly- (methyl methacrylate~styrene) bivalve layer complex microsphere is below 50 microns,
More than 20 nanometers, the thickness of shell is more than 10 nanometers for the particle diameter of silica core；The number-average molecular weight of polyacrylate is big
In 100000, the weight ratio of graphite flakes and stripper is 1：3；
Heating kettle, keeps kettle body temperature to be 90 DEG C, and pressure is 3atm, and agitator shaft speed is 1500 rpm/min, during reaction
Between 3h；After stopped reaction upper strata suspension is expelled in storage tank by discharging opening, stands 24h head products derived above；Will
The graphene suspension in storage tank for obtaining is delivered in centrifuge, and centrifuge speed is 1500rpm/min, centrifugation time
1h, takes the supernatant, and vacuum filter obtains filter cake in vacuum apparatus, and the filter cake for obtaining is washed with appropriate distillation
Wash, filter cake more than lyophilization 4h in freeze drying plant obtains graphene powder；
（2）Pure titanium or titanium alloy material are made annealing treatment, and caustic dip and clean water are carried out to its surface, it is cool after cleaning
Dry or drying；
Pure titanium or titanium alloy powder are sufficiently mixed according to a certain percentage, are stirred with above-mentioned graphene powder；
With the above-mentioned pure titanium for processing or titanium alloy material cladding mixed-powder, it is compacted and seals, then is pressed into forcing press pre-
Clamp dog；
Gained prefabricated section is rolled into into final finished；
Wherein, titanium valve used can be pure titanium valve or titanium alloy powder, and granular size is 150-200 mesh, cladding used
Titanium can be the section bar of tubing, sheet material or other titanium or titanium alloy etc, the content matter of above-mentioned graphene powder used
Amount fraction representation is represented with volume fraction, and mass fraction is 2.5%-6%, and volume fraction is 2%-8%.
2. the method for claim 1, it is characterised in that carried out being pressed into the process of prefabricated section with titanium cladding powder
In, if titanium used is titanium tube, titanium tube to have vertically put puts two ways with level, and when vertically putting, two sections of titanium tube uses titanium liquid
Cast sealing；When level is put, two sections of titanium tube is compressed with forcing press and sealed, and when prefabricated section is pressed with forcing press, is had and is colded pressing and hot pressing
Two ways, hot pressing temperature is 600-800 DEG C；Rolling also has cold rolling and hot rolling two ways, and hot-rolled temperature is 500-700 DEG C,
3-7h sintering need to be carried out before hot rolling under the environmental protection of argon.
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| CN201710022174.1A CN106676304A (en) | 2017-01-12 | 2017-01-12 | Preparation method of graphene titanium-based composite material |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105063404A (en) * | 2015-06-25 | 2015-11-18 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of titanium matrix graphene alloy |
| CN105838921A (en) * | 2016-04-13 | 2016-08-10 | 北京理工大学 | Low-content few-layer graphene intensified titanium-based composite material and preparation method |
| CN106311581A (en) * | 2016-08-19 | 2017-01-11 | 苏州思创源博电子科技有限公司 | Manufacturing method for efficient composite heat sink for electronic product |
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2017
- 2017-01-12 CN CN201710022174.1A patent/CN106676304A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105063404A (en) * | 2015-06-25 | 2015-11-18 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of titanium matrix graphene alloy |
| CN105838921A (en) * | 2016-04-13 | 2016-08-10 | 北京理工大学 | Low-content few-layer graphene intensified titanium-based composite material and preparation method |
| CN106311581A (en) * | 2016-08-19 | 2017-01-11 | 苏州思创源博电子科技有限公司 | Manufacturing method for efficient composite heat sink for electronic product |
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Application publication date: 20170517 |