CN106735250A - A kind of preparation method of compound titanium alloy material - Google Patents
A kind of preparation method of compound titanium alloy material Download PDFInfo
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- CN106735250A CN106735250A CN201710022186.4A CN201710022186A CN106735250A CN 106735250 A CN106735250 A CN 106735250A CN 201710022186 A CN201710022186 A CN 201710022186A CN 106735250 A CN106735250 A CN 106735250A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
-
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
- B22F2003/185—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers by hot rolling, below sintering temperature
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Abstract
The invention discloses a kind of preparation method of compound titanium alloy material, using metal iron powder and the compound reduction system of hydrochloric acid come the graphene oxide water solution of reduction treatment dilute concentration, low raw-material cost, it is nontoxic, it is simple to operate, beneficial to batch production, preparation method also achieves the good combination of grapheme material and titanium, due to repeatedly big deformation, composite can be made to reach consistency very high, the mechanical property of matrix is improve, high performance new titanium matrix composite 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 compound titanium alloy material.
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 particle of reinforcement of gold also has fiber.The fatigue ratio matrix of silicon carbide fibre enhancing alloy 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.Added in titanium alloy substrate suitable
When fiber, the reinforcement such as particle can improve the wearability of material, reduce thermal coefficient of expansion etc..
Graphene(Graphene)Be one kind by carbon atom with sp2Hybridized orbit composition hexangle type is in honeycomb lattice
(honeycomb crystal lattice)The individual layer 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 a kind of good titanium matrix composite enhancing phase.
The content of the invention
The present invention provides a kind of preparation method of compound titanium alloy material, the Reduction Body being combined using metal iron powder and hydrochloric acid
System carrys out the graphene oxide water solution of reduction treatment dilute concentration, and low raw-material cost is nontoxic, simple to operate, beneficial to batch production,
Preparation method also achieves the good combination of grapheme material and titanium, due to repeatedly big deformation, can reach composite
To consistency very high, the mechanical property of matrix is improve, high performance new titanium matrix composite can be prepared.
To achieve these goals, the invention provides a kind of preparation method of compound titanium alloy material, the method includes
Following steps:
(1)Prepare graphene powder
It is mixed in reactor and electricity consumption by 250g native graphites and by the 5L nitration mixture that the 4.5L concentrated sulfuric acids and 0.5L SPAs are constituted
Control magnetic stirrer is uniform, and 500g potassium permanganate is slowly added in the case of less than 20 DEG C;Afterwards, sealed reactor is simultaneously
It is warming up to 85-90 DEG C to react 2-3 hours, product is taken out from reactor lower end, be diluted to 40L solution, adds 0.6L hydrogen peroxide
Obtain glassy yellow graphite oxide solution;Then, washed with acid and water alternating centrifugal, to pH value of solution=5-6, remove foreign ion;Most
Afterwards, ultrasonic disperse graphite oxide, configures certain density graphene oxide solution;
The 0.5mg/mL graphene oxide solutions of 2L are transferred in reactor, under magnetic stirring add 12-36g iron powders and
The concentrated hydrochloric acid of 0.8-1.8L, 75-90 DEG C is reacted 4-5 hours;Then stand, the iron powder of residual is removed with hydrochloric acid filtering and washing, then
Washing suction filtration deacidification;Last freeze-drying, grinds the graphene powder that sieves to obtain;
(2)Pure titanium or titanium alloy material are made annealing treatment, and caustic dip and clear water cleaning 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 with above-mentioned graphene powder, are stirred;
Mixed-powder is coated with above-mentioned treated pure titanium or titanium alloy material, is compacted and is sealed, then be pressed into forcing press pre-
Clamp dog;
Gained prefabricated section is rolled 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
It is 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 has vertical putting to put two ways with level, and when putting vertically, two sections of titanium tube is poured into a mould with titanium liquid and sealed;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 gas before hot rolling
Under carry out 3-7h sintering.
It is an advantage of the current invention that using metal iron powder and the compound reduction system of hydrochloric acid come the oxygen of reduction treatment dilute concentration
Graphite aqueous solution, low raw-material cost is nontoxic, simple to operate, and beneficial to batch production, preparation method also achieves Graphene
Material and the good combination of titanium, due to repeatedly big deformation, can make composite reach consistency very high, improve base
The mechanical property of body, can prepare high performance new titanium matrix composite.
Specific embodiment
Embodiment one
It is mixed in reactor and electricity consumption by 250g native graphites and by the 5L nitration mixture that the 4.5L concentrated sulfuric acids and 0.5L SPAs are constituted
Control magnetic stirrer is uniform, and 500g potassium permanganate is slowly added in the case of less than 20 DEG C;Afterwards, sealed reactor is simultaneously
It is warming up to 85 DEG C to react 2-3 hours, product is taken out from reactor lower end, be diluted to 40L solution, adds 0.6L hydrogen peroxide to obtain bright
Oxide yellow graphite solution;Then, washed with acid and water alternating centrifugal, to pH value of solution=5-6, remove foreign ion;Finally, surpass
Sound disperses graphite oxide, configures certain density graphene oxide solution;
The 0.5mg/mL graphene oxide solutions of 2L are transferred in reactor, 12g iron powders and 0.8L are added under magnetic stirring
Concentrated hydrochloric acid, 75 DEG C react 4 hours;Then stand, the iron powder of residual is removed with hydrochloric acid filtering and washing, then wash suction filtration deacidification;
Last freeze-drying, grinds the graphene powder that sieves to obtain;Iron powder purity>99.0%, the mass fraction concentration of concentrated hydrochloric acid is 36%.
Pure titanium or titanium alloy material are made annealing treatment, and caustic dip and clear water cleaning 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 with above-mentioned graphene powder, are stirred
It is even;Mixed-powder is coated with above-mentioned treated pure titanium or titanium alloy material, is compacted and is sealed, then be pressed into forcing press prefabricated
Block;Gained prefabricated section is rolled into final finished.
Wherein, titanium valve used can be pure titanium valve or titanium alloy powder, and granular size is 150-200 mesh, used
Cladding titanium can be the section bar of 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
Put vertically and put two ways with level, when putting vertically, two sections of titanium tube is poured into a mould with titanium liquid and sealed;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 gas.
Embodiment two
It is mixed in reactor and electricity consumption by 250g native graphites and by the 5L nitration mixture that the 4.5L concentrated sulfuric acids and 0.5L SPAs are constituted
Control magnetic stirrer is uniform, and 500g potassium permanganate is slowly added in the case of less than 20 DEG C;Afterwards, sealed reactor is simultaneously
It is warming up to 90 DEG C to react 3 hours, product is taken out from reactor lower end, be diluted to 40L solution, adds 0.6L hydrogen peroxide to obtain bright orange
Color graphite oxide solution;Then, washed with acid and water alternating centrifugal, to pH value of solution=5-6, remove foreign ion;Finally, ultrasound
Dispersion graphite oxide, configures certain density graphene oxide solution;
The 0.5mg/mL graphene oxide solutions of 2L are transferred in reactor, 36g iron powders and 1.8L are added under magnetic stirring
Concentrated hydrochloric acid, 90 DEG C react 5 hours;Then stand, the iron powder of residual is removed with hydrochloric acid filtering and washing, then wash suction filtration deacidification;
Last freeze-drying, grinds the graphene powder that sieves to obtain;Iron powder purity>99.0%, the mass fraction concentration of concentrated hydrochloric acid is 36%.
Pure titanium or titanium alloy material are made annealing treatment, and caustic dip and clear water cleaning 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 with above-mentioned graphene powder, are stirred
It is even;Mixed-powder is coated with above-mentioned treated pure titanium or titanium alloy material, is compacted and is sealed, then be pressed into forcing press prefabricated
Block;Gained prefabricated section is rolled into final finished.
Wherein, titanium valve used can be pure titanium valve or titanium alloy powder, and granular size is 150-200 mesh, used
Cladding titanium can be the section bar of 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
It is 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
Put vertically and put two ways with level, when putting vertically, two sections of titanium tube is poured into a mould with titanium liquid and sealed;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 gas.
Claims (2)
1. a kind of preparation method of compound titanium alloy material, the method comprises the following steps:
(1)Prepare graphene powder
It is mixed in reactor and electricity consumption by 250g native graphites and by the 5L nitration mixture that the 4.5L concentrated sulfuric acids and 0.5L SPAs are constituted
Control magnetic stirrer is uniform, and 500g potassium permanganate is slowly added in the case of less than 20 DEG C;Afterwards, sealed reactor is simultaneously
It is warming up to 85-90 DEG C to react 2-3 hours, product is taken out from reactor lower end, be diluted to 40L solution, adds 0.6L hydrogen peroxide
Obtain glassy yellow graphite oxide solution;Then, washed with acid and water alternating centrifugal, to pH value of solution=5-6, remove foreign ion;Most
Afterwards, ultrasonic disperse graphite oxide, configures certain density graphene oxide solution;
The 0.5mg/mL graphene oxide solutions of 2L are transferred in reactor, under magnetic stirring add 12-36g iron powders and
The concentrated hydrochloric acid of 0.8-1.8L, 75-90 DEG C is reacted 4-5 hours;Then stand, the iron powder of residual is removed with hydrochloric acid filtering and washing, then
Washing suction filtration deacidification;Last freeze-drying, grinds the graphene powder that sieves to obtain;
(2)Pure titanium or titanium alloy material are made annealing treatment, and caustic dip and clear water cleaning 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 with above-mentioned graphene powder, are stirred;
Mixed-powder is coated with above-mentioned treated pure titanium or titanium alloy material, is compacted and is sealed, then be pressed into forcing press pre-
Clamp dog;
Gained prefabricated section is rolled 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 with titanium cladding powder be pressed into the process of prefabricated section
In, if titanium used is titanium tube, titanium tube has to put vertically puts two ways with level, and when putting vertically, 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 gas.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107267791A (en) * | 2017-06-11 | 2017-10-20 | 苏州南尔材料科技有限公司 | One kind enhancing aluminium alloy preparation method |
CN110512109A (en) * | 2019-09-20 | 2019-11-29 | 西安稀有金属材料研究院有限公司 | A kind of preparation method of graphene enhancing titanium composite material |
US10898769B1 (en) * | 2018-12-17 | 2021-01-26 | Callaway Golf Company | Golf club head cast from graphene reinforced titanium alloy |
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CN102864324A (en) * | 2012-09-06 | 2013-01-09 | 东北大学 | Preparation method for carbon nanomaterial enhanced aluminum base composite material |
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CN105132742A (en) * | 2015-10-20 | 2015-12-09 | 北京理工大学 | Graphene reinforced titanium-based composite and preparation method thereof |
CN106276879A (en) * | 2016-08-19 | 2017-01-04 | 苏州思创源博电子科技有限公司 | A kind of preparation method of Graphene fin |
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Patent Citations (5)
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US20110256014A1 (en) * | 2010-04-14 | 2011-10-20 | Soon Hyung Hong | Graphene/metal nanocomposite powder and method of manufacturing the same |
CN102864324A (en) * | 2012-09-06 | 2013-01-09 | 东北大学 | Preparation method for carbon nanomaterial enhanced aluminum base composite material |
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Cited By (4)
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CN107267791A (en) * | 2017-06-11 | 2017-10-20 | 苏州南尔材料科技有限公司 | One kind enhancing aluminium alloy preparation method |
US10898769B1 (en) * | 2018-12-17 | 2021-01-26 | Callaway Golf Company | Golf club head cast from graphene reinforced titanium alloy |
CN110512109A (en) * | 2019-09-20 | 2019-11-29 | 西安稀有金属材料研究院有限公司 | A kind of preparation method of graphene enhancing titanium composite material |
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