CN109317678A - A kind of synthetic method of ultra-vacuum in-situ hot-pressing sintering graphene-reinforced stone-titanium-based composite material - Google Patents
A kind of synthetic method of ultra-vacuum in-situ hot-pressing sintering graphene-reinforced stone-titanium-based composite material Download PDFInfo
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- CN109317678A CN109317678A CN201811380037.6A CN201811380037A CN109317678A CN 109317678 A CN109317678 A CN 109317678A CN 201811380037 A CN201811380037 A CN 201811380037A CN 109317678 A CN109317678 A CN 109317678A
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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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
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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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- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F2003/145—Both compacting and sintering simultaneously by warm compacting, below debindering temperature
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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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
- B22F2003/208—Warm or hot extruding
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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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
A kind of synthetic method of ultravacuum hot pressed sintering graphene enhancing stone titanium composite material, belongs to titanium composite material technical field.Mainly use pure titanium valve and medical glucose solution as raw material, the method combined under conditions of appropriate dehydrated alcohol is added by mechanical stirring and ultrasonic disperse is evenly dispersed, the composite sludge that dispersion obtains first passes through vacuum hotpressing forming, it is sintered 1h under 1200 DEG C, the pressure of 30MPa in vacuum sintering funace again and obtains graphene enhancing stone titanium composite material.Single-layer graphene is obtained in Raman spectrum test surfaces sintered state composite material.This method is sintered the means combined by In-situ reaction and semisolid, structure optimization has been carried out to Titanium base from micro-nano structure, realize graphene in conjunction with half coherence of β-Ti, improve the intensity and toughness of composite material, the thermoelectricity capability for improving material simultaneously, realizes the design concept of the structure-function integration of material.
Description
Technical field
The present invention relates to field of material technology more particularly to a kind of ultravacuum in-situ hot pressing sintering graphite alkene to enhance stone titanium-based
The synthetic method of composite material.
Background technique
Titanium is due to use temperature range wide (- 30-600 DEG C), the low (4.5g/cm of density3), specific strength height etc. one
Serial excellent properties have a wide range of applications in aerospace, deep ocean work, modern each industry such as chemical, but gold
Belong to titanium the disadvantages of there is also heating conduction is poor, and the toughness and tenacity of the wear-resisting property of room temperature and high temperature is poor itself.Therefore, titanium and titanium
Application of the based composites in industry and defense structures material just receives serious limitation, especially in deep-sea detecting and too
The performance of titanium excellent properties potentiality in sky navigation.In view of the above-mentioned problems, researcher is it is necessary to propose further solution,
This method is sintered the means combined by In-situ reaction and semisolid, and it is excellent to have carried out structure to Titanium base from micro-nano structure
Change, realizes that graphene improves the intensity and toughness of composite material in conjunction with half coherence of β-Ti, while improving the thermoelectricity of material
Performance realizes the design concept of the structure-function integration of material.
Summary of the invention
In view of this, the present invention provides a kind of ultravacuum fabricated in situ to prepare graphene enhancing stone titanium composite material
Synthetic method, with overcome the deficiencies in the prior art.
In order to solve the above technical problem, the present invention provides a kind of ultravacuum fabricated in situ prepare graphene enhancing stone titanium
The synthetic method of based composites, it is characterised in that key step is as follows:
(1) pure titanium valve and medical glucose solution are weighed, mechanical stirring and ultrasonic disperse are used using dehydrated alcohol as dispersion machine
It combines；
(2) above-mentioned dispersing liquid is subjected to vacuum drying 2h at 80 DEG C, target is to remove most of dehydrated alcohol；
(3) the above-mentioned metal mud that obtains is put into the high purity graphite mold of Φ 30 in vacuumizing case, is then reloaded into true
In empty sintering furnace；30 prefabricated section is obtained with 30PMa pressure at 600 DEG C；The prefabricated section that forming obtains is entered into vacuum hotpressing again
Sinter molding in sintering furnace；
(4) by the prefabricated section sample of step (3), temperature is 1200 DEG C in vacuum sintering funace and pressure is that 30MPa hot pressing is burnt
60min is tied, sintering graphite alkene enhancing stone titanium composite material sample cools to room temperature with the furnace, takes out sample；
(5) by the sintering graphite alkene enhancing stone titanium composite material of step (4) in such as Fig. 1 extrusion die, according to extrusion speed
For 4mm/s, mould heating-up temperature is 500 DEG C, extrusion ratio 16:1, squeezes temperature and is squeezed for 1200 DEG C.
Present invention technical characteristic described further: pure titanium valve granularity is 50m, and medical glucose solution content is total constitution
The atomic ratio of 0wt%-20wt%, Ti and the C of amount are between 0-0.5；Dehydrated alcohol is as dispersion machine.
Present invention technical characteristic described further: hot forming and hot pressed sintering are two realized in same sintering furnace
A stage；The temperature of hot forming is 600 DEG C, hot pressing pressure 20MPa, hot pressing time 40min.To the composite material of sintering
It carries out obtaining single-layer graphene (as shown in Figure 2) in Raman spectrum test surfaces sintered state composite material.
Compared with prior art, the beneficial effects of the present invention are: the present invention is realized using the technological approaches settled at one go
The In-situ reaction of titanium and glucose, which generates graphene, enhances titanium composite material, is combined by In-situ reaction and semisolid sintering
Means, structure optimization carried out to Titanium base from micro-nano structure, has realized graphene with half coherence of β-Ti ining conjunction with, raising is answered
The intensity and toughness of condensation material, while the thermoelectricity capability of material is improved, realize the design reason of the structure-function integration of material
It reads.
Detailed description of the invention
Fig. 1 is that As-extruded sample of the invention prepares schematic diagram.Microstructure is carried out to the As-extruded composite material of acquisition
Analysis and Mechanics Performance Testing, specify hot extrusion deformation to the shadow of sintered state reticular structure titanium composite material tissue and performance
It rings.
Fig. 2 is the Raman spectrogram of sintered sample of the invention.
Fig. 3 is the scanning figure of sample after extruding of the invention.
Fig. 4 is the energy spectrum diagram of sample after extruding of the invention.
1, pressure head in the figure, 2, mould sleeve, 3, sample, 4, extrusion cup, 5, pedestal.
Specific embodiment
Embodiment 1
It is that 1:20 weighs raw material according to medical glucose solution and the mass ratio of pure titanium powder, in dehydrated alcohol as dispersing liquid
Metal mud is fitted into the graphite jig of Φ 30 × 60 after vacuum drying by mechanical stirring and ultrasonic disperse 60min
Carry out vacuum hotpressing and sintering.
The fire box temperature of hot-pressed sintering furnace is first raised to 600 DEG C with the heating rate of 5 DEG C/min, is that 20MPa is protected with pressure
Warm pressure 40min；The fire box temperature of hot-pressed sintering furnace is raised to by 1250 DEG C of guarantor 20min with 10 DEG C/min heating rate again, then
Fast cooling to 1200 DEG C, etc. fire box temperatures stablize at 1200 DEG C, pressure rise to 30MPa, heat preservation hot pressed sintering
60min, after to be sintered, sintered sample cools to room temperature with the furnace, takes out sample.
It is 4mm/s, mould heating-up temperature according to extrusion speed finally sintered sample in the extrusion die of designed, designed
It is 500 DEG C, extrusion ratio 16:1, squeezes temperature and squeezed for 1200 DEG C.Finally obtained sample is machined again
And carry out correlated performance detection.
The extrusion die of designed, designed is as shown in Figure 1,2 upper end of mould sleeve connects pressure head 1, the connection of 2 lower end of mould sleeve
Pedestal 5, wing base upper end is equipped with extrusion cup in mould sleeve, and extrusion cup upper end and pressure head lower end are equipped with sample.
Embodiment 2
It is that 1:10 weighs raw material according to medical glucose solution and the mass ratio of pure titanium powder, in dehydrated alcohol as dispersing liquid
Metal mud is fitted into the graphite jig of Φ 30 × 60 after vacuum drying by mechanical stirring and ultrasonic disperse 60min
Carry out vacuum hotpressing and sintering.
The fire box temperature of hot-pressed sintering furnace is first raised to 600 DEG C with the heating rate of 5 DEG C/min, is that 20MPa is protected with pressure
Warm pressure 40min；The fire box temperature of hot-pressed sintering furnace is raised to by 1250 DEG C of guarantor 20min with 10 DEG C/min heating rate again, then
Fast cooling to 1200 DEG C, etc. fire box temperatures stablize at 1200 DEG C, pressure rise to 30MPa, heat preservation hot pressed sintering
60min, after to be sintered, sintered sample cools to room temperature with the furnace, takes out sample.
It is 4mm/s, mould heating-up temperature according to extrusion speed finally sintered sample in the extrusion die of designed, designed
It is 500 DEG C, extrusion ratio 16:1, squeezes temperature and squeezed for 1200 DEG C.Finally obtained sample is machined again
And carry out correlated performance detection.
Claims (3)
1. the synthetic method that a kind of ultravacuum fabricated in situ prepares graphene enhancing stone titanium composite material, it is characterised in that main
Steps are as follows:
(1) it weighs pure titanium valve and medical glucose solution prepares mixing, prepared composite sludge is added into appropriate anhydrous second
The method combined under conditions of alcohol by mechanical stirring and ultrasonic disperse is evenly dispersed；
(2) above-mentioned dispersing liquid is subjected to vacuum drying 2h at 80 DEG C, target is to remove most of dehydrated alcohol；
(3) composite sludge that dispersion obtains is shaped by vacuum warm, specifically obtains φ 30 with 30PMa pressure at 600 DEG C
Prefabricated section；The prefabricated section that forming obtains is entered into sinter molding in vacuum sintering funace again；
(4) by the prefabricated section sample of step (3), temperature is 1200 DEG C in vacuum sintering funace and pressure is that 30MPa hot pressing is burnt
60min is tied, sintering graphite alkene enhancing stone titanium composite material sample cools to room temperature with the furnace, takes out sample；
It (5) is 4mm/ according to extrusion speed by the sintering graphite alkene enhancing stone titanium composite material of step (4) in extrusion die
S, mould heating-up temperature are 500 DEG C, extrusion ratio 16:1, squeeze temperature and are squeezed for 1200 DEG C.
2. the synthesis that a kind of ultravacuum fabricated in situ according to claim 1 prepares graphene enhancing stone titanium composite material
Method, it is characterised in that: pure titanium valve granularity is 50m, and medical glucose solution content is the 0wt%-20wt% of overall quality,
The atomic ratio of Ti and C is between 0-0.5；Dehydrated alcohol is as dispersion machine.
3. a kind of synthesis side of ultravacuum in-situ sintering graphene enhancing stone titanium composite material according to claim 1
Method, it is characterised in that: hot forming and hot pressed sintering are two stages realized in same sintering furnace；The temperature of hot forming
It is 600 DEG C, hot pressing pressure 20MPa, hot pressing time 40min.
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| CN201811380037.6A CN109317678A (en) | 2018-11-20 | 2018-11-20 | A kind of synthetic method of ultra-vacuum in-situ hot-pressing sintering graphene-reinforced stone-titanium-based composite material |
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| CN201811380037.6A CN109317678A (en) | 2018-11-20 | 2018-11-20 | A kind of synthetic method of ultra-vacuum in-situ hot-pressing sintering graphene-reinforced stone-titanium-based composite material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115534494A (en) * | 2022-10-13 | 2022-12-30 | 合肥工业大学 | Cu/graphene film laminated composite material and preparation method thereof |
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2018
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Patent Citations (7)
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| US20130130112A1 (en) * | 2011-11-17 | 2013-05-23 | Byung-joo Chung | Silicon based shape memory alloy negative active material, negative active material composition including same, rechargeable lithium battery including same, and method of preparing same |
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| CN115534494A (en) * | 2022-10-13 | 2022-12-30 | 合肥工业大学 | Cu/graphene film laminated composite material and preparation method thereof |
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