CN109554567A - A kind of Ti-Fe alloy based composites and preparation method thereof - Google Patents
A kind of Ti-Fe alloy based composites and preparation method thereof Download PDFInfo
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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
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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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
- B22F3/15—Hot isostatic pressing
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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
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
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Abstract
The present invention relates to a kind of Ti-Fe alloy based composites and preparation method thereof, belong to technical field of composite preparation.The present invention is with Ti powder, Fe powder and B4C powder is raw material, by a certain amount of Ti powder, Fe powder and B4It is packed into stainless steel capsule after the mixing of C powder, by processes such as jolt ramming, degasification, sealing, HIP sintering and machining removal jackets, obtains the Ti-Fe alloy based composites of TiC+TiB particle enhancing.The present invention guarantees that Ti-Fe alloy based composites reinforced phase is evenly distributed, consistency is high, mechanical property is good by control technological parameter and material composition.Using the preparation method of powder metallurgy, process route is simple, short preparation period, at low cost, it can be achieved that large-scale industrial application.Embodiment the results show that Ti-Fe alloy based composites provided by the invention compression strength is in 1700~1900MPa at room temperature, modulus of elasticity in comperssion is in 8~9GPa.
Description
Technical field
The present invention relates to technical field of composite preparation, and in particular to a kind of Ti-Fe alloy based composites and its
Preparation method.
Background technique
With the fast development of biomedical materials field technology, traditional pure Ti and Ti-6Al-4V alloy is increasingly difficult to
To meet the requirement of body implanting material, developing the low new titanium alloy of nontoxic, good biocompatibility, elasticity modulus is becoming
The focus on research direction in the field.Fe element is not only safe and non-toxic, cheap, but also addition can effectively improve alloy in right amount
Intensity and wearability reduce elasticity modulus, therefore are the beta stable elements of ideal biological medical titanium alloy.In recent years, Ti-Fe
It is that the research and development of alloy are increasingly subject to the concern of domestic and international researcher.Powder metallurgic method be prepare Ti-Fe alloy important channel it
One.However, since titanium and iron diffusion coefficient are widely different, and will appear Transient liquid phase during the sintering process, and therefore, conventional powder
The metallurgy sintered Ti-Fe alloy for being difficult to prepare high-compactness in end.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention includes providing a kind of Ti-Fe alloy based composites, this is compound
Material has high-compactness, preferable reinforcing effect and preferable wear-resisting property.
The purpose of the present invention further includes providing a kind of preparation method of Ti-Fe alloy based composites, the preparation method work
Skill route is simple, short preparation period, at low cost, it can be achieved that large-scale industrial application.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention proposes a kind of preparation method of Ti-Fe alloy based composites, comprising:
By Ti powder, Fe powder and B4The mixed-powder of C powder passes through vacuum outgas, then is sintered using hot isostatic pressing method.
By weight percentage, Fe powder is 1~15%, B4C powder is 0.18~1.8%, and surplus is for Ti powder and unavoidably
Impurity.
The present invention proposes a kind of Ti-Fe alloy based composites, by the preparation method of above-mentioned Ti-Fe alloy based composites
It is prepared.
The beneficial effect comprise that
The present invention is with iron powder, titanium valve and B4C powder is raw material, is prepared for Ti-Fe alloy base composite wood using powder metallurgic method
Powder densification and in-situ authigenic reaction triggering are combined by HIP sintering, are prepared TiC+TiB by material
The Ti-Fe alloy based composites of grain enhancing, composite material consistency with higher and higher compressive strength.Experiment knot
Fruit proves that for the Ti-Fe alloy based composites consistency that preparation method provided by the invention obtains up to 99.5% or more, compression is strong
Degree reaches 1860MPa, modulus of elasticity in comperssion 8.6GPa.The preparation method process route is simple, and short preparation period is at low cost,
Large-scale industrial application can be achieved.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the cross-sectional scans electron microscope for the Ti-Fe alloy based composites that the embodiment of the present invention 1 provides；
Fig. 2 is the Ti-Fe alloy based composites Fracture scan electron microscope that the embodiment of the present invention 1 provides.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Titanium composite material is obtained more higher than conventional titanium alloy by introducing the second phase reinforcement in titanium alloy substrate
Specific strength, specific stiffness, wearability and high temperature resistance, in aerospace, marine ship, automobile manufacture, derived energy chemical, biology doctor
The numerous areas such as treatment have great application prospect.From the point of view of titanium composite material preparation method, mainly there are fusion casting, machine at present
Tool alloying, self-propagating high-temperature synthesis and powder metallurgic method etc..
Powder metallurgic method prepares titanium composite material within the temperature range of being lower than titanium alloy fusing point, is not only avoided that founding
The high reaction problem of liquid titanium in method, and can effectively improve fusion casting bring material structure, component segregation and coarse grains
The disadvantages of, and can realize the adjusting of particulates reinforcements granularity and volume fraction in a big way, it is the titanium of great development prospect
Based composites preparation method.
From the point of view of reinforced phase addition manner, mainly there are outer addition and in-situ authigenic method.The particle of outer addition is more coarse, and
There are pollution problems with basal body interface.The chemistry that the particulates reinforcements of in-situ authigenic avoid between enhancing particle and interface is asked
Topic, and with matrix surface is pollution-free, bond strength is high, be one of the important directions of current titanium composite material research.
Although conventional powder metallurgy process can be used for preparing Ti-Fe alloy based composites, but cause obtained
Density is not still high.The present invention proposes a kind of preparation method of Ti-Fe alloy based composites, can be made with high-densit
The composite material of degree, preferable reinforcing effect and wear-resisting property.
A kind of Ti-Fe alloy based composites of the embodiment of the present invention and preparation method thereof are specifically described below.
The present invention provides a kind of Ti-Fe alloy based composites, comprising:
By Ti powder, Fe powder and B4The mixed-powder of C powder passes through vacuum outgas, then is sintered using hot isostatic pressing method；It presses
Weight percent meter, Fe powder are 1~15%, B4C powder is 0.18~1.8%, and surplus is Ti powder and inevitable impurity.
The addition of iron powder improves the intensity and hardness of composite material.But liquid is had in the too high levels sintering process of iron powder
It mutually generates, influences sintering quality.It is not in liquid phase when iron content is 1~15%, obtained composite material has preferable
Intensity and hardness.Optionally, iron content can be 2%, 3%, 4%, 11%, 13%.Further, the content of iron powder can be with
It is 5~10%, wherein the content of iron powder can be 6%, 7%, 8%, 9%.
B4C powder generates the strong of TiC+TiB particle enhancing Ti-Fe alloy based composites as reaction in-situ agent, with titanium valve
Degree and hardness.In order to guarantee being evenly distributed for reinforced phase, consistency is high, B4The content of C powder is 0.18~1.8%, wherein content
It can be 0.2%, 0.3%, 1.3%, 1.5%, 1.7%.Further, the content of iron powder can be 0.5~1.0%.Wherein,
Content can be 0.6%, 0.8%, 0.9%.In the content range, B4The addition of C powder not will lead to composite material and become fragile, and increase
The strong mechanical property of composite material.
In some embodiments of the invention, the partial size of Ti powder and Fe powder is no more than 325 mesh.Ti powder in the particle size range
Can be sufficiently mixed with Fe powder, avoiding sintering activity greatly causes consistency bad, and if partial size it is larger, sintering temperature is wanted
It asks high, improves cost and sintering condition.In order to guarantee the quality of composite material, Ti powder, Fe powder and B4The purity of C powder is all larger than
99%.
Specifically, weighing Ti powder, Fe powder and B in proportion4C powder, is loaded into three-dimensional material mixer, and mixing 3~5 hours,
Obtain mixed-powder.
Mixed-powder is packed into pre-fabricated stainless steel capsule, by jolt ramming, is lower than 10 in vacuum degree-1Pa, temperature
Fruit storage is carried out under conditions of being 600~700 DEG C.Jacket is sealed again.
The jacket of sealing is put into hot isostatic pressing, is sintered using hot isostatic pressing method.960~1050 DEG C are warming up to, 120
Heat-insulation pressure keeping is sintered 1~3 hour under the pressure condition of~150MPa, then furnace cooling.It should be noted that heating rate is not
Higher than 10 DEG C/min, guarantee the abundant reaction of mixed-powder, so that reinforced phase is evenly distributed, consistency is high, mechanical property is good.It can
Choosing, sintering temperature is 970 DEG C, 980 DEG C, 990 DEG C, 1000 DEG C.Sintering pressure is 130~140MPa.
The stainless steel capsule in surface is removed using machining to get Ti-Fe alloy based composites are arrived.
The present invention is by using B4C powder is raw material, controls the proportion of each raw material, while controlling technological parameter, passes through heat etc.
Powder densification and in-situ authigenic reaction triggering are combined, the Ti- of TiC+TiB particle enhancing are prepared by static pressure sintering
Fe alloy-base composite material, composite material consistency with higher and higher compressive strength.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of Ti-Fe alloy based composites are present embodiments provided, are mainly prepared by following steps:
According to Ti-5wt%Fe-0.9wt%B4C quality proportioning, by hydrogenation dehydrogenation titanium powder, carbonyl iron dust and B4C powder is packed into
It is mixed in three-dimensional material mixer, mixes 3~5 hours, obtain mixed-powder；
Mixed-powder is packed into pre-fabricated stainless steel capsule, artificial jolt ramming, by being taken off at 600~700 DEG C of vacuum
Gas is vacuumized lower than 10-1Then jacket mouth is welded sealing by Pa；
The jacket of sealing is put into hot isostatic pressing, is heated up with the rate of 10 DEG C/min, is 960~1050 DEG C in temperature,
Air pressure is then furnace cooling heat-insulation pressure keeping 1~3 hour under 120~150MPa；
The stainless steel capsule in surface is removed using machining to get Ti-Fe alloy based composites are arrived.
Micro-structural test is carried out to Ti-Fe alloy based composites, the section of consistency 99.5%, composite material is aobvious
Micro-assembly robot is referring to attached drawing 1, and fracture section is referring to attached drawing 2.Microstructure of composite is fine and close as seen from the figure, and crystallite dimension is tiny, matrix
For (alpha+beta) Ti, reinforced phase is evenly distributed, without apparent hole.
Mechanics Performance Testing is carried out to Ti-Fe alloy based composites, room temperature compressive strength is 1860MPa, the elasticity of compression
Modulus is 8.6GPa.
Embodiment 2
A kind of Ti-Fe alloy based composites are present embodiments provided, are mainly prepared by following steps:
According to Ti-1wt%Fe-0.18wt%B4C quality proportioning, by hydrogenation dehydrogenation titanium powder, carbonyl iron dust and B4C powder dress
Enter in three-dimensional material mixer and mix, mixes 3 hours, obtain mixed-powder；
Mixed-powder is packed into pre-fabricated stainless steel capsule, artificial jolt ramming, by deaerating at 600 DEG C of vacuum, is taken out
Vacuum is lower than 10-1Then jacket mouth is welded sealing by Pa；
The jacket of sealing is put into hot isostatic pressing, is heated up with the rate of 8 DEG C/min, is 960 DEG C in temperature, air pressure is
Heat-insulation pressure keeping 1 hour under 120MPa, then furnace cooling；
The stainless steel capsule in surface is removed using machining to get Ti-Fe alloy based composites are arrived.
Micro-structural test, consistency 98% are carried out to Ti-Fe alloy based composites.It is compound to Ti-Fe alloy base
Material carries out Mechanics Performance Testing, and room temperature compressive strength is 1730MPa, modulus of elasticity in comperssion 8.1GPa.
Embodiment 3
A kind of Ti-Fe alloy based composites are present embodiments provided, are mainly prepared by following steps:
According to Ti-15wt%Fe-1.8wt%B4C quality proportioning, by hydrogenation dehydrogenation titanium powder, carbonyl iron dust and B4C powder dress
Enter in three-dimensional material mixer and mix, mixes 5 hours, obtain mixed-powder；
Mixed-powder is packed into pre-fabricated stainless steel capsule, artificial jolt ramming, by deaerating at 700 DEG C of vacuum, is taken out
Vacuum is lower than 10-1Then jacket mouth is welded sealing by Pa；
The jacket of sealing is put into hot isostatic pressing, is heated up with the rate of 9 DEG C/min, is 1050 DEG C in temperature, air pressure is
Heat-insulation pressure keeping 3 hours under 150MPa, then furnace cooling；
The stainless steel capsule in surface is removed using machining to get Ti-Fe alloy based composites are arrived.
Micro-structural test, consistency 99% are carried out to Ti-Fe alloy based composites.It is compound to Ti-Fe alloy base
Material carries out Mechanics Performance Testing, and room temperature compressive strength is 1902MPa, modulus of elasticity in comperssion 8.9GPa.
Embodiment 4
A kind of Ti-Fe alloy based composites are present embodiments provided, are mainly prepared by following steps:
According to Ti-5wt%Fe-0.5wt%B4C quality proportioning, by hydrogenation dehydrogenation titanium powder, carbonyl iron dust and B4C powder is packed into
It is mixed in three-dimensional material mixer, mixes 3 hours, obtain mixed-powder；
Mixed-powder is packed into pre-fabricated stainless steel capsule, artificial jolt ramming, by deaerating at 650 DEG C of vacuum, is taken out
Vacuum is lower than 10-1Then jacket mouth is welded sealing by Pa；
The jacket of sealing is put into hot isostatic pressing, is heated up with the rate of 10 DEG C/min, is 1000 DEG C in temperature, air pressure is
Heat-insulation pressure keeping 2 hours under 130MPa, then furnace cooling；
The stainless steel capsule in surface is removed using machining to get Ti-Fe alloy based composites are arrived.
Micro-structural test, consistency 99.2% are carried out to Ti-Fe alloy based composites.It is multiple to Ti-Fe alloy base
Condensation material carries out Mechanics Performance Testing, and room temperature compressive strength is 1800MPa, modulus of elasticity in comperssion 8.2GPa.
Embodiment 5
A kind of Ti-Fe alloy based composites are present embodiments provided, are mainly prepared by following steps:
According to Ti-10wt%Fe-1.0wt%B4C quality proportioning, by hydrogenation dehydrogenation titanium powder, carbonyl iron dust and B4C powder dress
Enter in three-dimensional material mixer and mix, mixes 4 hours, obtain mixed-powder；
Mixed-powder is packed into pre-fabricated stainless steel capsule, artificial jolt ramming, by being taken off at 600~700 DEG C of vacuum
Gas is vacuumized lower than 10-1Then jacket mouth is welded sealing by Pa；
The jacket of sealing is put into hot isostatic pressing, is heated up with the rate of 10 DEG C/min, is 980 DEG C in temperature, air pressure is
Heat-insulation pressure keeping 1~3 hour under 140MPa, then furnace cooling；
The stainless steel capsule in surface is removed using machining to get Ti-Fe alloy based composites are arrived.
Micro-structural test, consistency 99.2% are carried out to Ti-Fe alloy based composites.It is multiple to Ti-Fe alloy base
Condensation material carries out Mechanics Performance Testing, and room temperature compressive strength is 1890MPa, modulus of elasticity in comperssion 8.7GPa.
Embodiment 6
A kind of Ti-Fe alloy based composites are present embodiments provided, are mainly prepared by following steps:
According to Ti-8wt%Fe-0.8wt%B4C quality proportioning, by hydrogenation dehydrogenation titanium powder, carbonyl iron dust and B4C powder is packed into
It is mixed in three-dimensional material mixer, mixes 4 hours, obtain mixed-powder；
Mixed-powder is packed into pre-fabricated stainless steel capsule, artificial jolt ramming, by deaerating at true 700 DEG C, is taken out true
Sky is lower than 10-1Then jacket mouth is welded sealing by Pa；
The jacket of sealing is put into hot isostatic pressing, is heated up with the rate of 10 DEG C/min, is 1050 DEG C in temperature, air pressure is
Heat-insulation pressure keeping 2 hours under 150MPa, then furnace cooling；
The stainless steel capsule in surface is removed using machining to get Ti-Fe alloy based composites are arrived.
Micro-structural test, consistency 99.4% are carried out to Ti-Fe alloy based composites.It is multiple to Ti-Fe alloy base
Condensation material carries out Mechanics Performance Testing, and room temperature compressive strength is 1840MPa, modulus of elasticity in comperssion 8.4GPa.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of Ti-Fe alloy based composites characterized by comprising
By Ti powder, Fe powder and B4The mixed-powder of C powder passes through vacuum outgas, then is sintered using hot isostatic pressing method；
By weight percentage, the Fe powder is 1~15%, the B4C powder is 0.18~1.8%, and surplus is for the Ti powder and not
Evitable impurity.
2. the preparation method of Ti-Fe alloy based composites according to claim 1, which is characterized in that the Fe powder is 5
~10%, the B4C powder is 0.5~1.0%.
3. the preparation method of Ti-Fe alloy based composites according to claim 1, which is characterized in that the Ti powder and
The partial size of the Fe powder is no more than 325 mesh.
4. the preparation method of Ti-Fe alloy based composites according to claim 1, which is characterized in that the B4C powder
Grain is not more than 325 mesh.
5. the preparation method of Ti-Fe alloy based composites according to claim 1, which is characterized in that the mixed powder
The preparation method at end includes: using three-dimensional material mixer to the Ti powder, the Fe powder and the B4C powder mixing 3~5 hours.
6. the preparation method of Ti-Fe alloy based composites according to claim 1, which is characterized in that the mixing
The method of powder under vacuum degassing includes: to be packed into the mixed-powder in pre-fabricated jacket, low in vacuum degree by jolt ramming
In 10-1Pa, temperature carry out Fruit storage under conditions of being 600~700 DEG C.
7. the preparation method of Ti-Fe alloy based composites according to claim 1, which is characterized in that the mixing
The method that powder is sintered using hot isostatic pressing method includes:
The mixed-powder Jing Guo vacuum outgas is put into furnace, is warming up to 960~1050 DEG C, in the pressure of 120~150MPa
Heat-insulation pressure keeping is sintered 1~3 hour under the conditions of power, then furnace cooling.
8. the preparation method of Ti-Fe alloy based composites according to claim 7, which is characterized in that in temperature-rise period
Heating rate be not higher than 10 DEG C/min.
9. the preparation method of Ti-Fe alloy based composites according to claim 7, which is characterized in that sintering temperature is
960~1050 DEG C, sintering pressure is 130~140MPa.
10. a kind of Ti-Fe alloy based composites, which is characterized in that closed by Ti-Fe as described in any one of claim 1 to 9
The preparation method of auri composite material is prepared.
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Cited By (1)
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| CN114250379A (en) * | 2021-12-14 | 2022-03-29 | 北京科技大学 | Preparation method of in-situ particle reinforced metal matrix composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114250379A (en) * | 2021-12-14 | 2022-03-29 | 北京科技大学 | Preparation method of in-situ particle reinforced metal matrix composite material |
| CN114250379B (en) * | 2021-12-14 | 2022-07-08 | 北京科技大学 | Preparation method of in-situ particle reinforced metal matrix composite material |
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