CN109554567B - Ti-Fe alloy based composite material and preparation method thereof - Google Patents
Ti-Fe alloy based composite material and preparation method thereof Download PDFInfo
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- 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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- B22F3/14—Both compacting and sintering simultaneously
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- 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 invention relates to a Ti-Fe alloy based composite material and a preparation method thereof, belonging to the technical field of composite material preparation. The invention uses Ti powder, Fe powder and B4C powder is used as raw material, and a certain amount of Ti powder, Fe powder and B powder are mixed4And C powder is mixed and then is loaded into a stainless steel sheath, and the TiC + TiB particle reinforced Ti-Fe alloy base composite material is obtained through the processes of compacting, degassing, sealing, hot isostatic pressing sintering, machining, sheath removal and the like. The invention ensures that the Ti-Fe alloy based composite material has even distribution of the reinforcing phase, high density and good mechanical property by controlling the process parameters and the material components. The preparation method of powder metallurgy is adopted, the process route is simple, the preparation period is short, the cost is low, and large-scale industrial application can be realized. The embodiment results prove that the compressive strength of the Ti-Fe alloy-based composite material provided by the invention is 1700-1900 MPa at room temperature, and the compressive elastic modulus is 8-9 GPa.
Description
Technical Field
The invention relates to the technical field of composite material preparation, and particularly relates to a Ti-Fe alloy based composite material and a preparation method thereof.
Background
With the rapid development of the technology in the field of biomedical materials, the traditional pure Ti and Ti-6Al-4V alloys are more and more difficult to meet the requirements of human body implant materials, and the development of novel titanium alloys which are non-toxic, good in biocompatibility and low in elastic modulus is becoming the key research direction in the field.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a Ti-Fe alloy based composite material which has high compactness, better reinforcing effect and better wear resistance.
The invention also aims to provide a preparation method of the Ti-Fe alloy based composite material, which has the advantages of simple process route, short preparation period and low cost and can realize large-scale industrial application.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a preparation method of a Ti-Fe alloy based composite material, which comprises the following steps:
mixing Ti powder, Fe powder and B4And degassing the mixed powder of the C powder in vacuum, and sintering by adopting a hot isostatic pressing method.
1-15% of Fe powder and B40.18-1.8% of C powder, and the balance of Ti powder and inevitable impurities.
The invention provides a Ti-Fe alloy based composite material, which is prepared by the preparation method of the Ti-Fe alloy based composite material.
The beneficial effects of the invention include:
the invention uses iron powder, titanium powder and B4The powder C is used as a raw material, a Ti-Fe alloy based composite material is prepared by a powder metallurgy method, powder densification and in-situ authigenic reaction triggering are combined through hot isostatic pressing sintering, and the TiC + TiB particle reinforced Ti-Fe alloy based composite material is prepared and has high density and high compression strength. Experimental results prove that the density of the Ti-Fe alloy-based composite material obtained by the preparation method provided by the invention reaches over 99.5%, the compression strength reaches 1860MPa, and the compression elastic modulus is 8.6 GPa. The preparation method has the advantages of simple process route, short preparation period and low cost, and can realize large-scale industrial application.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a sectional scanning electron microscope of a Ti-Fe alloy-based composite material provided in example 1 of the present invention;
FIG. 2 is a scanning electron microscope view of a fracture of the Ti-Fe alloy-based composite material provided in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The titanium-based composite material has higher specific strength, specific stiffness, wear resistance and high temperature resistance than the traditional titanium alloy by introducing the second-phase reinforcement into the titanium alloy matrix, and has great application prospect in various fields such as aerospace, marine ships, automobile manufacturing, energy chemical industry, biomedical treatment and the like. From the view of the preparation method of the titanium-based composite material, at present, a fusion casting method, a mechanical alloying method, a self-propagating high-temperature synthesis method, a powder metallurgy method and the like are mainly adopted.
The powder metallurgy method for preparing the titanium-based composite material in the temperature range lower than the melting point of the titanium alloy can not only avoid the problem of high reaction of liquid titanium in the casting method, but also effectively improve the defects of material organization, component segregation, large crystal grains and the like caused by the casting method, can realize the adjustment of the particle size and the volume fraction of the particle reinforced phase in a larger range, and is a preparation method of the titanium-based composite material with great development prospect.
From the aspect of the enhanced phase adding mode, the external addition method and the in-situ self-generation method are mainly used. The particles of the external addition method are relatively coarse, and the pollution problem exists between the particles and the interface of the matrix. The in-situ self-generated particle reinforced phase avoids the chemical problem between reinforced particles and an interface, has no pollution with the surface of a matrix and high bonding strength, and is one of the important directions of the research of the titanium-based composite material at present.
Although the conventional powder metallurgy method can be used for preparing Ti-Fe alloy based composite materials, the obtained compactness is still not high. The invention provides a preparation method of a Ti-Fe alloy-based composite material, which can be used for preparing the composite material with high density, better reinforcing effect and wear resistance.
The Ti-Fe alloy-based composite material and the method for preparing the same according to the embodiments of the present invention will be described in detail below.
The invention provides a Ti-Fe alloy based composite material, which comprises the following components:
mixing Ti powder, Fe powder and B4Vacuum degassing is carried out on the mixed powder of the C powder, and then sintering is carried out by adopting a hot isostatic pressing method; 1-15% of Fe powder and B40.18-1.8% of C powder, and the balance of Ti powder and inevitable impurities.
The addition of the iron powder improves the strength and hardness of the composite material. However, when the content of the iron powder is too high, a liquid phase is generated in the sintering process, and the sintering quality is affected. When the content of the iron powder is 1-15%, no liquid phase occurs, and the obtained composite material has good strength and hardness. Alternatively, the iron powder content may be 2%, 3%, 4%, 11%, 13%. Further, the content of the iron powder may be 5 to 10%, wherein the content of the iron powder may be 6%, 7%, 8%, 9%.
B4The C powder is used as an in-situ reactant and generates TiC + TiB particles with the titanium powder to enhance the strength and hardness of the Ti-Fe alloy matrix composite material. In order to ensure even distribution and high density of the reinforcing phase, B4The content of the C powder is 0.18-1.8%, wherein the content can be 0.2%, 0.3%, 1.3%, 1.5% and 1.7%. Further, the content of the iron powder may be 0.5 to 1.0%. Wherein the content can be 0.6%, 0.8%, 0.9%. Within this content range, B4The addition of the powder C can not cause the composite material to become brittle, and the mechanical property of the composite material is enhanced.
In some embodiments of the invention, Ti powder andthe grain diameter of the Fe powder is not larger than 325 meshes. The Ti powder and the Fe powder in the particle size range can be fully mixed, the problem of poor density caused by high sintering activity is avoided, the requirement on sintering temperature is high if the particle size is large, and the cost and the sintering condition are improved. In order to ensure the quality of the composite material, Ti powder, Fe powder and B4The purity of the C powder is more than 99 percent.
Specifically, Ti powder, Fe powder and B powder are weighed according to the proportion4And C, putting the powder C into a three-dimensional mixer, and mixing for 3-5 hours to obtain mixed powder.
Filling the mixed powder into a prepared stainless steel ladle sleeve, compacting, and keeping the vacuum degree below 10-1Pa, and the temperature is 600-700 ℃ for vacuum degassing treatment. And sealing the sheath.
And (4) placing the sealed sheath into hot isostatic pressing, and sintering by adopting the hot isostatic pressing method. Heating to 960-1050 ℃, carrying out heat preservation and pressure maintaining sintering for 1-3 hours under the pressure condition of 120-150 MPa, and then cooling along with the furnace. It should be noted that the heating rate is not higher than 10 ℃/min, so as to ensure the sufficient reaction of the mixed powder, and to make the reinforcing phase distributed uniformly, the density high, and the mechanical property good. Optionally, the sintering temperature is 970 ℃, 980 ℃, 990 ℃ and 1000 ℃. The sintering pressure is 130-140 MPa.
And removing the stainless steel sheath on the surface by machining to obtain the Ti-Fe alloy based composite material.
The invention is realized by adopting B4The powder C is used as a raw material, the proportion of the raw materials is controlled, the process parameters are controlled, and the powder densification and the in-situ spontaneous reaction triggering are combined through hot isostatic pressing sintering to prepare the TiC + TiB particle reinforced Ti-Fe alloy based composite material which has higher density and higher compression strength.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a Ti-Fe alloy based composite material, which is mainly prepared by the following steps:
according to Ti-5wt% Fe-0.9wt% B4C mass ratio, removing hydrogenationTitanium hydride powder, carbonyl iron powder and B4C, putting the powder C into a three-dimensional mixer for mixing for 3-5 hours to obtain mixed powder;
the mixed powder is filled into a prefabricated stainless steel ladle sleeve, is manually compacted, is degassed at the temperature of 600-700 ℃ in vacuum, and is vacuumized to be lower than 10 DEG C-1Pa, and then welding the sheath opening to seal;
placing the sealed sheath into hot isostatic pressing, heating at the speed of 10 ℃/min, keeping the temperature and the pressure for 1-3 hours at the temperature of 960-1050 ℃ and the air pressure of 120-150 MPa, and then cooling along with a furnace;
and removing the stainless steel sheath on the surface by machining to obtain the Ti-Fe alloy based composite material.
The microstructure test of the Ti-Fe alloy based composite material shows that the compactness is 99.5%, the section microstructure of the composite material is shown in figure 1, the fracture section is shown in figure 2, the figure shows that the composite material has compact structure and fine grain size, the matrix is (α + β) Ti, the reinforced phase is uniformly distributed, and no obvious holes exist.
The mechanical property test is carried out on the Ti-Fe alloy based composite material, the room temperature compression strength is 1860MPa, and the compression elastic modulus is 8.6 GPa.
Example 2
The embodiment provides a Ti-Fe alloy based composite material, which is mainly prepared by the following steps:
according to Ti-1 wt% Fe-0.18 wt% B4C, mixing hydrogenated dehydrogenated titanium powder, carbonyl iron powder and B4C, putting the powder into a three-dimensional mixer for mixing for 3 hours to obtain mixed powder;
loading the mixed powder into a stainless steel jacket prepared in advance, manually compacting, degassing at 600 deg.C, and vacuumizing to below 10 ℃-1Pa, and then welding the sheath opening to seal;
putting the sealed sheath into hot isostatic pressing, heating at the speed of 8 ℃/min, keeping the temperature and the pressure for 1 hour at the temperature of 960 ℃ and the air pressure of 120MPa, and then cooling along with the furnace;
and removing the stainless steel sheath on the surface by machining to obtain the Ti-Fe alloy based composite material.
And microstructure test is carried out on the Ti-Fe alloy-based composite material, and the density is 98%. The mechanical property test is carried out on the Ti-Fe alloy-based composite material, the room temperature compressive strength is 1730MPa, and the compressive elastic modulus is 8.1 GPa.
Example 3
The embodiment provides a Ti-Fe alloy based composite material, which is mainly prepared by the following steps:
according to Ti-15 wt% Fe-1.8 wt% B4C, mixing hydrogenated dehydrogenated titanium powder, carbonyl iron powder and B4C, putting the powder into a three-dimensional mixer for mixing for 5 hours to obtain mixed powder;
loading the mixed powder into a stainless steel jacket prepared in advance, manually compacting, degassing at 700 deg.C, and vacuumizing to below 10 ℃-1Pa, and then welding the sheath opening to seal;
putting the sealed sheath into hot isostatic pressing, heating at the speed of 9 ℃/min, keeping the temperature and pressure for 3 hours at 1050 ℃ and 150MPa, and then cooling along with the furnace;
and removing the stainless steel sheath on the surface by machining to obtain the Ti-Fe alloy based composite material.
And microstructure test is carried out on the Ti-Fe alloy-based composite material, and the compactness is 99%. The Ti-Fe alloy based composite material is subjected to mechanical property test, the room temperature compression strength is 1902MPa, and the compression elastic modulus is 8.9 GPa.
Example 4
The embodiment provides a Ti-Fe alloy based composite material, which is mainly prepared by the following steps:
according to Ti-5wt% Fe-0.5 wt% B4C, mixing hydrogenated dehydrogenated titanium powder, carbonyl iron powder and B4C, putting the powder into a three-dimensional mixer for mixing for 3 hours to obtain mixed powder;
loading the mixed powder into a stainless steel jacket prepared in advance, manually compacting, degassing at 650 deg.C, and vacuumizing to less than 10 ℃-1Pa, and then welding the sheath opening to seal;
putting the sealed sheath into hot isostatic pressing, heating at the speed of 10 ℃/min, keeping the temperature and the pressure for 2 hours at the temperature of 1000 ℃ and the air pressure of 130MPa, and then cooling along with the furnace;
and removing the stainless steel sheath on the surface by machining to obtain the Ti-Fe alloy based composite material.
And microstructure test is carried out on the Ti-Fe alloy-based composite material, and the density is 99.2%. The mechanical property test is carried out on the Ti-Fe alloy based composite material, the room temperature compressive strength is 1800MPa, and the compressive elastic modulus is 8.2 GPa.
Example 5
The embodiment provides a Ti-Fe alloy based composite material, which is mainly prepared by the following steps:
according to Ti-10 wt% Fe-1.0 wt% B4C, mixing hydrogenated dehydrogenated titanium powder, carbonyl iron powder and B4C, putting the powder into a three-dimensional mixer for mixing for 4 hours to obtain mixed powder;
the mixed powder is filled into a prefabricated stainless steel ladle sleeve, is manually compacted, is degassed at the temperature of 600-700 ℃ in vacuum, and is vacuumized to be lower than 10 DEG C-1Pa, and then welding the sheath opening to seal;
putting the sealed sheath into hot isostatic pressing, heating at the speed of 10 ℃/min, keeping the temperature and the pressure at 980 ℃ and 140MPa for 1-3 hours, and then cooling along with a furnace;
and removing the stainless steel sheath on the surface by machining to obtain the Ti-Fe alloy based composite material.
And microstructure test is carried out on the Ti-Fe alloy-based composite material, and the density is 99.2%. The mechanical property test is carried out on the Ti-Fe alloy-based composite material, the room temperature compressive strength is 1890MPa, and the compressive elastic modulus is 8.7 GPa.
Example 6
The embodiment provides a Ti-Fe alloy based composite material, which is mainly prepared by the following steps:
according to Ti-8 wt% Fe-0.8 wt% B4C, mixing hydrogenated dehydrogenated titanium powder, carbonyl iron powder and B4C, putting the powder into a three-dimensional mixer for mixing for 4 hours to obtain mixed powder;
loading the mixed powder into a stainless steel jacket prepared in advance, manually compacting, degassing at 700 deg.C, and vacuumizing to below 10 ℃-1Pa, and then welding the sheath opening to seal;
putting the sealed sheath into hot isostatic pressing, heating at the speed of 10 ℃/min, keeping the temperature and pressure for 2 hours at 1050 ℃ and 150MPa, and then cooling along with the furnace;
and removing the stainless steel sheath on the surface by machining to obtain the Ti-Fe alloy based composite material.
And microstructure test is carried out on the Ti-Fe alloy-based composite material, and the density is 99.4%. The mechanical property test is carried out on the Ti-Fe alloy-based composite material, the room temperature compression strength is 1840MPa, and the compression elastic modulus is 8.4 GPa.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (2)
1. A preparation method of a Ti-Fe alloy based composite material is characterized by comprising the following steps:
according to Ti-5wt% Fe-0.9wt% B4C, mixing hydrogenated dehydrogenated titanium powder, carbonyl iron powder and B4C, putting the powder C into a three-dimensional mixer for mixing for 3-5 hours to obtain mixed powder;
the mixed powder is filled into a prefabricated stainless steel ladle sleeve, is manually compacted, is degassed at the temperature of 600-700 ℃ in vacuum, and is vacuumized to be lower than 10 DEG C-1Pa, and then welding the sheath opening to seal;
placing the sealed sheath into hot isostatic pressing, heating at the speed of 10 ℃/min, keeping the temperature and the pressure for 1-3 hours at the temperature of 960-1050 ℃ and the air pressure of 120-150 MPa, and then cooling along with a furnace;
and removing the stainless steel sheath on the surface by machining to obtain the Ti-Fe alloy-based composite material, wherein the density of the Ti-Fe alloy-based composite material reaches over 99.5 percent, the compressive strength reaches 1860MPa, and the compressive elastic modulus is 8.6 GPa.
2. The Ti-Fe alloy-based composite material is characterized by being prepared by the preparation method of the Ti-Fe alloy-based composite material according to claim 1, wherein the compactness of the Ti-Fe alloy-based composite material reaches more than 99.5 percent, the compressive strength reaches 1860MPa, and the compressive elastic modulus is 8.6 GPa.
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| CN1122114C (en) * | 2001-03-23 | 2003-09-24 | 中国科学院金属研究所 | High-strnegth Ti-base composition reinforced by in-situ combination of crystal whiskers with particles |
| CN105088014B (en) * | 2015-09-15 | 2017-04-05 | 北京工业大学 | A kind of low-cost high-strength Ti Fe alloy blanks and its preparation technology |
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| CN101921930A (en) * | 2010-09-16 | 2010-12-22 | 上海交通大学 | Multicomponent microalloyed titanium alloy and preparation method thereof |
| CN103305781A (en) * | 2013-07-09 | 2013-09-18 | 上海交通大学 | Multi-element microalloyed titanium alloy processing method |
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Address after: 510000 363 Changxin Road, Tianhe District, Guangzhou, Guangdong. Patentee after: Institute of materials and processing, Guangdong Academy of Sciences Address before: 510000 363 Changxin Road, Tianhe District, Guangzhou, Guangdong. Patentee before: Guangdong Institute Of Materials And Processing |
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Effective date of registration: 20221110 Address after: 510651 No. 363, Changxin Road, Guangzhou, Guangdong, Tianhe District Patentee after: Institute of new materials, Guangdong Academy of Sciences Address before: 510000 363 Changxin Road, Tianhe District, Guangzhou, Guangdong. Patentee before: Institute of materials and processing, Guangdong Academy of Sciences |