CN106513663B - A kind of graphene and titanium alloy mixed-powder preparation method - Google Patents
A kind of graphene and titanium alloy mixed-powder preparation method Download PDFInfo
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- CN106513663B CN106513663B CN201610928885.0A CN201610928885A CN106513663B CN 106513663 B CN106513663 B CN 106513663B CN 201610928885 A CN201610928885 A CN 201610928885A CN 106513663 B CN106513663 B CN 106513663B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 80
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 80
- 239000011812 mixed powder Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 52
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000012545 processing Methods 0.000 claims abstract description 15
- 239000000956 alloy Substances 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 229910052786 argon Inorganic materials 0.000 claims abstract description 11
- 238000000889 atomisation Methods 0.000 claims abstract description 11
- 238000010907 mechanical stirring Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000006185 dispersion Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000009689 gas atomisation Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 229910045601 alloy Inorganic materials 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 239000002775 capsule Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000004806 packaging method and process Methods 0.000 claims description 6
- 238000005266 casting Methods 0.000 claims description 5
- 230000033116 oxidation-reduction process Effects 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000009461 vacuum packaging Methods 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- 238000007872 degassing Methods 0.000 claims 1
- 238000005538 encapsulation Methods 0.000 claims 1
- 238000004663 powder metallurgy Methods 0.000 abstract description 4
- 239000004615 ingredient Substances 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000011017 operating method Methods 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract description 2
- 238000009849 vacuum degassing Methods 0.000 abstract 1
- 238000007789 sealing Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 description 2
- 210000004907 gland Anatomy 0.000 description 2
- 230000003760 hair shine Effects 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
Classifications
-
- B22F1/0003—
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
Abstract
The invention belongs to powder metallurgy titanium alloy Material Fields, are related to a kind of nano material and titanium alloy mixed-powder preparation method, more particularly, to a kind of graphene and titanium alloy mixed-powder preparation method.Spherical titanium alloy powder is prepared using argon gas atomization or plasma rotating electrode atomization method first, then the graphene nanometer sheet of accurate weighing is added in absolute ethyl alcohol, decentralized processing is carried out using high speed dispersion blender and ultrasonic cell disrupte machine, prepare graphene solution, then spherical titanium alloy powder with graphene solution in the quantitative ingredient tank of temperature control mechanical stirring device is stirred and mixed, graphene and titanium alloy mixed-powder slurry are prepared, graphene and titanium alloy mixed-powder are obtained after drying and processing and vacuum degassing.Dispersiveness of the graphene nanometer sheet in titanium alloy powder is the method improve, operating method is simple, and process parameter control is accurate, the batch of graphene and titanium alloy mixed-powder is suitble to prepare, application prospect is extensive.
Description
Technical field
The invention belongs to powder metallurgy titanium alloy Material Fields, are related to a kind of nano material and titanium alloy mixed-powder preparation side
Method, more particularly, to a kind of graphene and titanium alloy mixed-powder preparation method.
Background technology
With the spanning development of advanced weaponry equipment and the progress of large-scale component Lightweight Technology, to the comprehensive of titanium alloy material
It closes performance and proposes higher requirement.Using conventional process techniques prepare the performance of titanium alloy already close to or reached theoretical pole
Limit, thus the great attention that new change technology modified titanium alloy causes countries in the world is sought in recent years.
Graphene rapidly becomes structure-function integration material when with excellent mechanical performance and physical and chemical performance
Preferable reinforcement, for titanium materials technology development, comprehensive performance further improves and provide new approaches.However, due to stone
Nature difference between black alkene and titanium alloy is big, the features such as easily chemically reacting, and is difficult to using processes such as vacuum meltings
By being added in titanium alloy for graphene uniform.
Powder metallurgy becomes a kind of most possible process realized graphene and uniformly dispersed in titanium alloy.Graphene
The key foundation of modified powder titanium alloy is in the dispersiveness in graphene in titanium alloy powder, i.e. graphene and titanium alloy mixing
The quality of powder.Mixed-powder poor quality will be unable to realize effective enhancing of the graphene to powder metallurgy titanium alloy, can not meet new
The design requirement of material.Therefore, it is the skill for perplexing numerous scientific and technical personnel how graphene uniform to be distributed in titanium alloy powder
Art problem.
The content of the invention
Easily reunite the purpose of the present invention is being directed to graphene nanometer sheet, graphene and titanium alloy are difficult to uniformly to mix etc. asks
Topic, proposes that a kind of ultrasonic disperse prepares graphene and titanium alloy mixed-powder with the process that mechanical agitation is combined.
The technical scheme is that the preparation method comprises the following steps,
(1) Φ 45mm- Φ 150mm titan alloy casting ingots or bar are put into argon gas powder by atomization equipment, open argon gas mist
Change powder manufacturing apparatus and prepare spherical titanium alloy powder, powder diameter is 30 μm~150 μm, oxygen content is less than 1000ppm；
(2) 0.1~10% graphene nanometer sheet of titanium alloy powder quality is added in absolute ethyl alcohol, using at a high speed
Dispersing stirrer carries out mechanical agitation, and the blender working time is 20min~30min, and rotating speed is 6000r/min~15000r/
Then min carries out decentralized processing using ultrasonic cell disrupte machine, graphene solution is prepared, when ultrasonic cell disrupte machine works
Between for 30min~50min, working frequency is vibration 2s, gap 3s；
(3) graphene solution that spherical titanium alloy powder prepared by step (1) is obtained with step (2) is stirred in temperature control machinery
It mixes and is stirred in the material-compound tank of device, prepare graphene and titanium alloy mixed-powder slurry, mixing speed 500r/min
~3000r/min, mixing time are 30min~180min, and whipping temp is no more than 80 DEG C；
(4) graphene and titanium alloy mixed-powder slurry are transferred in baking oven and carry out drying and processing, obtain graphene and
Titanium alloy mixed-powder, baking oven heating temperature are 50 DEG C~80 DEG C, and heating time is 5h~20h；
(5) graphene and titanium alloy mixed-powder are transferred in soft packaging bag, are carried out using vacuum packing machine except sealing gland
Dress processing, vacuum degree are less than 0.1kPa.
The gross mass of alloy element is not less than 10% in the titan alloy casting ingot or bar chemical composition.
The argon gas powder by atomization equipment is substituted by plasma rotating electrode atomization powder manufacturing apparatus.
The graphene nanometer sheet is prepared using oxidation-reduction method.
The whipping temp of the temperature control mechanical stirring device is automatically stopped and is cooled down more than 80 DEG C, cooling time 1
~3h.
The soft packaging bag is substituted by metal capsule, and vacuumize process is then carried out to metal capsule, and vacuum degree is less than 5
×10-2Pa。
The present invention has the following advantages and high-lighting effect：
(1) present invention be easy to using mechanical agitation with graphene solution prepared by process that ultrasonic disperse is combined and
Titanium alloy powder uniformly mixes, and optimizes the interfacial characteristics of graphene and titanium alloy powder；(2) present invention is stirred using temperature control machinery
It mixes mode to handle graphene and titanium alloy mixed-powder slurry, improves graphene nanometer sheet in titanium alloy powder
Dispersiveness avoids the overtemperature oxidation of titanium alloy powder, the quality of graphene and titanium alloy mixed-powder greatly improved；(3)
The present invention obtains graphene and the apparent density of titanium alloy mixed-powder reaches more than the 70% of theoretical density, improves rear continued powder
Last metallurgical mouldability；(4) operating method of the present invention is simple, and process parameter control is accurate, is suitble to graphene and titanium alloy mixing
Prepared by the batch of powder, have a extensive future.
Description of the drawings
Fig. 1 is the field emission scanning electron microscope photo of graphene nanometer sheet.
Fig. 2 is that the field emission scanning electron microscope of graphene and 1# titanium alloy mixed-powders shines under typical process parameter
Piece.
Fig. 3 is the field emission scanning electron microscope photo of graphene nanometer sheet and 1# titanium alloy powder interface cohesions.
Fig. 4 is that the field emission scanning electron microscope of graphene and 2# titanium alloy mixed-powders shines under typical process parameter
Piece.
Fig. 5 is the field emission scanning electron microscope photo of graphene nanometer sheet and 2 # titanium alloy powder interface cohesions.
Specific embodiment
The preparation method comprises the following steps：
(1) Φ (45-150) mm titan alloy casting ingots or bar are put into argon gas powder by atomization equipment, open argon gas atomization
Powder manufacturing apparatus prepares spherical titanium alloy powder, is then transferred in ultrasonic vibration screening instrument, by 2~3 vibrosieves, obtains
Obtain the spherical titanium alloy powder that grain size is less than 1000ppm for 30 μm~150 μm, oxygen content.
(2) graphene nanometer sheet is prepared using oxidation-reduction method, graphene nano under field emission scanning electron microscope
Piece has typical folded structure feature, as shown in Figure 1 in featheriness, translucent；Then, accurate weighing titanium alloy powder
0.1~10% graphene nanometer sheet of quality is simultaneously added in the beaker for containing absolute ethyl alcohol, and electronic balance accuracy is
0.01g。
(3) open high speed dispersion blender and mixed processing, blender work are stirred to the graphene nanometer sheet in beaker
Make the time as 20min~30min, rotating speed is 6000r/min~15000r/min, and the graphene after being then stirred is muddy
Liquid liquid is transferred in ultrasonic cell disrupte machine, carries out homodisperse processing using ultrasonic cell disrupte machine, it is molten to prepare graphene
Liquid, ultrasonic cell disrupte machine working time are 30min~50min, and working frequency is vibration 2s, gap 3s.
(4) graphene solution that spherical titanium alloy powder prepared by step (1) is obtained with step (2) is transferred to control respectively
In the warm special quantitative ingredient tank of mechanical stirring device, temperature control mechanical stirring device is opened after sealing, graphene is prepared and titanium closes
Golden mixed-powder slurry, mixing speed are 500r/min~3000r/min, and mixing time is 30min~180min, and stirring is warm
Degree is no more than 80 DEG C, and special batching tank volume is 200ml~2000ml.
(5) graphene and titanium alloy mixed-powder slurry are transferred in baking oven and carry out drying and processing, obtain graphene and
Titanium alloy mixed-powder, baking oven heating temperature are 50 DEG C~80 DEG C, and heating time is 5h~20h.
(6) graphene and titanium alloy mixed-powder are transferred in soft packaging bag, are carried out using vacuum packing machine except sealing gland
Dress processing, vacuum degree are less than 0.1kPa.
The gross mass of alloy element is not less than 10% in the titan alloy casting ingot or bar chemical composition.
The argon gas powder by atomization equipment is substituted by plasma rotating electrode atomization powder manufacturing apparatus.
The whipping temp of the temperature control tool agitating device is automatically stopped and is cooled down more than 80 DEG C, cooling time for 1~
3h。
The soft packaging bag is substituted by metal capsule, and vacuumize process is then carried out to metal capsule, and vacuum degree is less than 5
×10-2Pa。
With reference to specific embodiment, the invention will be further described, but the present invention is not limited to following embodiments.
Embodiment 1
(1) 1# titanium alloy powders are prepared using plasma rotating electrode atomization powder manufacturing apparatus, then to the powder of preparation into
2 screenings of row, obtain the 1# titanium alloy powders 750g that grain size is 100~150 μm；
(2) graphene nanometer sheet for preparing 3g oxidation-reduction methodes is added in 100ml~500ml absolute ethyl alcohols, is utilized
High speed dispersion blender is stirred mixed processing, and the blender working time is 25min, rotating speed 9000r/min, Ran Houli
Graphene solution is prepared with ultrasonic cell disrupte machine, the ultrasonic cell disrupte machine working time is 40min, and working frequency is vibration
2s, gap 3s；
(3) graphene solution that the 1# titanium alloy powders for obtaining step (1) are prepared with step (2) is transferred to temperature control respectively
Temperature control mechanical stirring device is opened in the 500ml specification material-compound tanks of mechanical stirring device, after sealing uniformly to be mixed, and is prepared
Graphene and 1# titanium alloy mixed-powder slurries, mixing speed be 500r/min~3000r/min, mixing time for 60min~
80min, whipping temp are no more than 80 DEG C；
(4) after mechanical agitation, graphene and 1# titanium alloy mixed-powder slurries are transferred to heating temperature as 50 DEG C
Baking oven in drying and processing 5h~10h, obtain graphene and 1# titanium alloy mixed-powders, graphene uniform is dispersed in 1# titanium alloys
Powder surface, and it is good with 1# titanium alloy powder interface cohesions, as shown in Figures 2 and 3.
Embodiment 2
(1) 2# titanium alloy powders are prepared using argon gas powder by atomization equipment, 2 screenings is carried out to the powder of preparation, are obtained
Grain size is 50 μm~100 μm of 2# titanium alloy powders 600g；
(2) graphene nanometer sheet for preparing 2g oxidation-reduction methodes is added in 100ml~500ml absolute ethyl alcohols, is utilized
High speed dispersion blender is stirred mixed processing, and the blender working time is 20min, rotating speed 6000r/min, Ran Houli
Graphene solution is prepared with ultrasonic cell disrupte machine, the ultrasonic cell disrupte machine working time is 40min, and working frequency is vibration
2s, gap 3s；
(3) graphene solution that the 2# titanium alloy powders for obtaining step (1) are prepared with step (2) is transferred to temperature control respectively
Temperature control mechanical stirring device is opened in the 500ml specification material-compound tanks of mechanical stirring device, after sealing uniformly to be mixed, and is prepared
Graphene and 2# titanium alloy mixed-powder slurries, mixing speed be 500r/min~3000r/min, mixing time for 60min~
80min, whipping temp are no more than 80 DEG C；
(4) after mechanical agitation, graphene and 2# titanium alloy mixed-powder slurries are transferred to heating temperature as 50 DEG C
Baking oven in drying and processing 5h~10h, obtain graphene and 2# titanium alloy mixed-powders, graphene uniform is dispersed in Titanium Powder
Last surface, and it is good with 2# titanium alloy powder interface cohesions, as shown in Figure 4 and Figure 5.
Claims (6)
1. a kind of graphene and titanium alloy mixed-powder preparation method, it is characterised in that：The preparation method comprises the following steps,
(1) Φ 45mm- Φ 150mm titan alloy casting ingots or bar are put into argon gas powder by atomization equipment, open argon gas atomization system
Powder equipment prepares spherical titanium alloy powder, and powder diameter is 30 μm~150 μm, oxygen content is less than 1000ppm；
(2) 0.1~10% graphene nanometer sheet of titanium alloy powder quality is added in absolute ethyl alcohol, utilizes high speed dispersion
Blender carries out mechanical agitation, and the blender working time is 20min~30min, and rotating speed is 6000r/min~15000r/min,
Then decentralized processing is carried out using ultrasonic cell disrupte machine, prepares graphene solution, the ultrasonic cell disrupte machine working time is
30min~50min, working frequency are vibration 2s, gap 3s；
(3) spherical titanium alloy powder prepared by step (1) is filled with the graphene solution that step (2) obtains in temperature control mechanical agitation
Be stirred in the material-compound tank put, prepare graphene and titanium alloy mixed-powder slurry, mixing speed for 500r/min~
3000r/min, mixing time are 30min~180min, and whipping temp is no more than 80 DEG C；
(4) graphene and titanium alloy mixed-powder slurry are transferred in baking oven and carry out drying and processing, obtained graphene and titanium closes
Golden mixed-powder, baking oven heating temperature are 50 DEG C~80 DEG C, and heating time is 5h~20h；
(5) graphene and titanium alloy mixed-powder are transferred in soft packaging bag, are carried out using vacuum packing machine at degasification encapsulation
Reason, vacuum degree are less than 0.1kPa.
2. a kind of graphene according to claim 1 and titanium alloy mixed-powder preparation method, it is characterised in that：The titanium
The gross mass of alloy element is not less than 10% in alloy cast ingot or bar chemical composition.
3. a kind of graphene according to claim 1 and titanium alloy mixed-powder preparation method, which is characterized in that the argon
Gas-atomized powder equipment is substituted by plasma rotating electrode atomization powder manufacturing apparatus.
4. a kind of graphene according to claim 1 and titanium alloy mixed-powder preparation method, which is characterized in that the stone
Black alkene nanometer sheet is prepared using oxidation-reduction method.
5. a kind of graphene according to claim 1 and titanium alloy mixed-powder preparation method, which is characterized in that the control
The whipping temp of warm mechanical stirring device is automatically stopped and is cooled down more than 80 DEG C, and cooling time is 1~3h.
6. a kind of graphene according to claim 1 and titanium alloy mixed-powder preparation method, which is characterized in that described soft
Packaging bag is substituted by metal capsule, and vacuumize process is then carried out to metal capsule, and vacuum degree is less than 5 × 10-2Pa。
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Cited By (1)
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| WO2020130830A1 (en) * | 2018-12-20 | 2020-06-25 | Smart Stronghold B.V. | A method for preparing a magnesium composite material; a magnesium composite material obtainable from the method according to the present invention |
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| CN107598175B (en) * | 2017-07-27 | 2019-06-28 | 中国航发北京航空材料研究院 | A kind of graphene and titanium alloy composite powder ball-milling preparation method |
| CN107557612B (en) * | 2017-07-27 | 2019-06-28 | 中国航发北京航空材料研究院 | A kind of graphene enhancing titanium-based nano composite material and preparation method |
| CN114558337B (en) * | 2022-03-15 | 2023-12-01 | 广东长信精密设备有限公司 | Metal atomizing powder process production facility |
| CN115301941A (en) * | 2022-08-12 | 2022-11-08 | 大连大学 | Brake copper-iron-based composite friction material and preparation method thereof |
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