CN114480904B - Preparation method of low-content reinforcement reinforced titanium-based composite material - Google Patents
Preparation method of low-content reinforcement reinforced titanium-based composite material Download PDFInfo
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- 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
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- 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
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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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
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B22F3/24—After-treatment of workpieces or articles
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
- C22C32/0047—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 with carbides, nitrides, borides or silicides as the main non-metallic constituents
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- 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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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention discloses a preparation method of a low-content reinforcement reinforced titanium-based composite material, belonging to the technical field of metal-based composite materials. The method comprises the following specific steps: mixing Ti powder, Al powder, V powder, and B powder 4 And C, performing ball milling and mixing treatment on the powder C, then performing compression molding by adopting a cold isostatic pressing method, and performing vacuum sintering treatment after compression molding. Through the steps, the TiC + TiB reinforcement is generated in situ in the Ti-6Al-4V matrix, and then the solid solution aging treatment is carried out to obtain the low-content reinforcement reinforced titanium-based composite material. The density of the composite material can reach 95% or more, and the plate has good performance in the aspects of tensile strength, elongation and the like.
Description
Technical Field
The invention belongs to the technical field of metal matrix composite materials, and particularly relates to a preparation method of a low-content reinforcement reinforced titanium matrix composite material.
Background
The titanium alloy has the advantages of small density, high specific strength, good corrosion resistance, good heat resistance and the like, and is widely applied in the fields of aerospace, automobile, ship, chemical equipment manufacturing and the like. However, with the change of application environment, the performance requirements on the titanium alloy material are higher and higher, and the performances of the titanium alloy material such as tensile strength, elongation and the like cannot meet the application requirements. In order to improve the performance of the titanium alloy material, the performance of the titanium-based alloy is improved by adding reinforcing particles into the titanium-based alloy material at present. However, because of the active properties of titanium and its alloys, there are a series of problems to be overcome in the wetting and reaction interface of the reinforcement and the matrix alloy, the improvement of the performance of the titanium alloy material is limited, and the purpose of enhancing the performance of the titanium-based alloy material can be achieved by adding a large amount of reinforcement particles, and the manufacturing cost is high. Therefore, it is necessary to research a method capable of effectively improving the tensile strength, elongation and other properties of the titanium alloy material, and having simple operation and low preparation cost.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a preparation method of a low-content reinforcement reinforced titanium-based composite material, which adopts a preparation process of mixed powder, cold isostatic pressing and sintering to improve the performance of the titanium-based composite material through solid solution aging so as to obtain the titanium-based composite material with better comprehensive performance.
In order to achieve the purpose, the invention provides the following technical scheme:
according to one technical scheme, the preparation method of the low-content reinforcement reinforced titanium-based composite material comprises the steps of adopting a powder metallurgy method to generate a TiC + TiB reinforcement in situ in a Ti-6Al-4V matrix, and then carrying out solid solution aging treatment to obtain the low-content reinforcement reinforced titanium-based composite material.
Further, the low-content reinforcement reinforced titanium-based composite material is a (TiC + TiB)/Ti-6Al-4V composite material.
Further, the volume percentage of the TiC + TiB reinforcement in the low-content reinforcement reinforced titanium-based composite material is 3%.
Further, the molar ratio of the in-situ generated reinforcement is TiB to TiC of 4: 1.
Further, the specific operation of in-situ generation of the TiC + TiB reinforcement in the Ti-6Al-4V matrix by adopting the powder metallurgy method comprises the following steps: mixing Ti powder, Al powder, V powder, and B powder 4 And C, performing ball milling and mixing treatment on the powder C, then performing compression molding by adopting a cold isostatic pressing method, and performing vacuum sintering treatment after compression molding.
Further, the dosage of each raw material powder is as follows according to weight percentage: 8% of Al powder, 4% of V powder, and B 4 1.5% of C powder and the balance of Ti powder.
B 4 The content of the C powder directly influences the content of the generated reinforcement particles, the reinforcing effect on the matrix material is limited when the generated reinforcement particle phase is too small, but the plasticity of the material is greatly reduced when the generated reinforcement particle phase is too much, the performance of the titanium-based composite material is hindered, and only when the content of the reinforcement is controlled to a certain value, namely B 4 When the content of the C powder is controlled at a certain value, the titanium-based composite material with excellent performance can be prepared.
Further, the Ti powder and the Al powderPowder V, powder B 4 The average grain diameter of the C powder is less than or equal to 50 mu m.
Further, the time for ball milling and mixing treatment is 24 hours, and the rotating speed is 70 r/min.
Further, the ball milling and mixing treatment is carried out on a drum mixer, and the weight ratio of balls to materials in the ball milling and mixing process is 4: 1.
Further, the cold isostatic pressing method has the pressure maintaining pressure of 180MPa and the pressure maintaining time of 20 min.
Further, the specific process of the vacuum sintering treatment comprises the following steps: heating from room temperature to 600 deg.C, maintaining for 30min, heating from 600 deg.C to 840 deg.C, maintaining for 30min, heating from 840 deg.C to 1300 deg.C, maintaining for 3h, and furnace cooling.
The invention adopts a sectional sintering mode to carry out sintering treatment, and the sectional sintering has the advantage of more full reaction.
Further, the vacuum degree of the vacuum sintering treatment is 1 × 10 -3 Pa。
Further, the process of the solution aging treatment comprises the following steps: the solid solution temperature is 940 ℃, the heat preservation is 30min, the water cooling is carried out, the aging temperature is 500 ℃, the heat preservation is carried out for 4h, and the air cooling is carried out.
In the second technical scheme of the invention, the low-content reinforcement reinforced titanium-based composite material prepared by the preparation method is provided.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention adopts a powder metallurgy method to generate TiC + TiB reinforcement in situ in a Ti-6Al-4V matrix, namely by adding B 4 C powder, which reacts with Ti in situ to generate TiB and TiC reinforcement, then carries out solid solution aging treatment to obtain the low-content reinforcement reinforced titanium-based composite material, and uses the low-content TiC + TiB reinforcement to reinforce the Ti-6Al-4V composite material. On one hand, TiB and TiC have similar density, Poisson's ratio and thermal expansion coefficient with titanium, have high melting point and do not react with the matrix, and after being added into the matrix as a reinforcing phase, the titanium-based composite material can realize effective improvement of mechanical property. By adopting TiC and TiB with lower content to reinforce the titanium-based composite material, the titanium-based composite material is improvedThe material strength reduces the adverse effect on the plasticity of the titanium-based composite material, effectively improves the practicability of the titanium-based composite material, and can obtain the titanium-based composite material with good comprehensive performance. On the other hand, the TiC + TiB reinforcement is generated by adopting an in-situ synthesis method, the matrix and the reinforcement can be well combined, the interface is clean and pollution-free, and the good combination of the interface is beneficial to the performance of the titanium-based composite material. In yet another aspect, solution aging may be used to improve properties by changing the texture of the material. After the solution treatment, the alpha phase in the matrix structure is gradually transformed into the beta phase, then the beta phase is transformed into a martensite alpha 'phase in a lattice shear mode due to the high cooling speed in the water cooling process, the alpha phase in the matrix after the aging treatment keeps the form after the solution treatment, the metastable alpha' phase is gradually decomposed into a stable beta phase, the fine beta phase can play a role in dispersion strengthening, and the comprehensive performance of the titanium-based composite material is effectively improved through the solution treatment and the aging treatment. The compactness of the titanium-based composite material prepared by the method is more than 95%, and the plate has good performances in the aspects of tensile strength, elongation and the like.
(2) The components and the proportion of the preparation method are easy to control, the interface between the reinforcement and the matrix is clean, the reinforcement is uniformly distributed, the comprehensive performance of the titanium-based composite material is improved, and the preparation cost of the titanium-based composite material is reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a metallographic structure of a low-reinforcement-content reinforced titanium-based composite material prepared in example 1 of the present invention, wherein (a) is a metallographic structure with a scale of 50 μm, and (b) is a metallographic structure with a scale of 10 μm, which is further enlarged;
FIG. 2 is a metallographic structure of a low-reinforcement-content reinforced titanium-based composite material prepared in comparative example 1 of the present invention;
FIG. 3 is a graph of tensile fractures of a low reinforcement content reinforced titanium matrix composite made in accordance with example 1 of the present invention.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. It is intended that the specification and examples be considered as exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
Example 1
Firstly, weighing Ti powder, Al powder, V powder and B powder by adopting a balance with the precision of 0.001g according to the proportion of raw materials 4 C powder (by weight percent, Al powder 8%, V powder 4%, B powder 4 1.5% of C powder and the balance of Ti powder), then filling the weighed powder into a mixing bottle, and filling weighed stainless steel grinding balls into the mixing bottle in advance, wherein the diameters of the grinding balls are respectively 5mm, 10mm and 15mm, and the weight ratio of the grinding balls with three diameters is 5 mm: 10 mm: 15mm ═ 4: 3: 3, the weight ratio of the ball material is 4: 1. And putting the filled mixing bottle on a drum mixer for ball milling and mixing for 24 hours at the rotating speed of 70 r/min. And taking out the uniformly mixed powder, putting the powder into a rubber mold, sealing two ends by adopting a thin iron wire, putting the sealed powder into a cold isostatic press for press forming after sealing, and performing pressure maintaining pressing for 20min at the pressure maintaining of 180 MPa. Taking out the pressed sample, sintering in a vacuum sintering furnace with vacuum degree of 1 × 10 -3 Pa, the sintering process is to heat the temperature from room temperature to 600 ℃, preserve heat for 30min, heat the temperature from 600 ℃ to 840 ℃, preserve heat for 30min, heat the temperature from 840 ℃ to 1300 ℃, preserve heat for 3h, then cool the sample along with the furnace to obtain a cylindrical titanium-based composite material sample with the size of 40mm multiplied by 120mm (diameter multiplied by height), and carry out solid solution aging treatment on the titanium-based composite material, wherein the solid solution aging process is as follows: the solution temperature is 940 ℃, the temperature is kept for 30min, the water is cooled to the room temperature, the aging temperature is 500 ℃, the temperature is kept for 4h, and the air is cooled to the room temperature, so that the low-content reinforcement reinforced titanium-based composite material, namely the (TiC + TiB)/Ti-6Al-4V composite material, is obtained.
Comparative example 1
The difference from example 1 is that the solution aging treatment process was omitted.
Effect verification
(1) Metallographic image analysis
The metallographic structure of the low-reinforcement-content reinforced titanium-based composite material prepared in example 1 is shown in fig. 1, wherein (a) is a metallographic structure with a scale of 50 μm, and (b) is a further enlarged metallographic structure with a scale of 10 μm, and as can be seen from fig. 1, the metallographic structure after solution aging treatment is an α phase, a β phase, and a martensite α 'phase, and the martensite α' phase decomposes into the β phase during aging treatment, with only a small amount of residue, so that (b) is not shown.
The metallographic structure diagram of the low-content reinforcement reinforced titanium-based composite material prepared in the comparative example 1 is shown in fig. 2, and it can be known from fig. 2 and fig. 1 that the matrix structure before solution treatment is alpha + beta phase, the alpha phase in the matrix structure gradually changes into beta phase after solution treatment, then the beta phase changes into martensite alpha 'phase in a lattice shear manner due to the fast cooling speed in the water cooling process, the alpha phase in the matrix after aging treatment retains the form after solution treatment, the metastable alpha' phase gradually decomposes into stable beta phase, and the fine beta phase can play a role in dispersion strengthening.
(2) Compactness test
The density of the low-content reinforcement reinforced titanium-based composite materials prepared in the example 1 and the comparative example 1 is tested according to an Archimedes drainage method, and the test result is as follows: the density of example 1 was 96.6% and that of comparative example 1 was 96%.
(3) Mechanical Property test
The low-content reinforcement reinforced titanium-based composite materials prepared in the example 1 and the comparative example 1 are taken to be subjected to a room temperature tensile test, an Shimadzu AG-I250 type precision universal tester is adopted in the room temperature tensile test, the gauge length of a sample is 15mm, the width of the sample is 5mm, the thickness of the sample is 2mm (the low-content reinforcement reinforced titanium-based composite materials prepared in the example and the comparative example are subjected to cutting processing according to the standard), the tensile test of each group is carried out for three times, the experimental environment during the tensile process is kept consistent, and the average value of the results is taken. The stretch breaking pattern of example 1 is shown in fig. 3, and it can be seen from fig. 3 that the reinforcement can take the load during the stretching process, thereby increasing the tensile strength. The results for specific tensile strength and elongation are shown in table 1:
TABLE 1
| Tensile strength/MPa | Elongation/percent | |
| Example 1 | 758.6 | 2.1 |
| Comparative example 1 | 619.53 | 1.79 |
As can be seen from Table 1, the titanium matrix composite material after the solution aging treatment had a tensile strength of 758.6MPa and an elongation of 2.1%, the tensile strength was increased by 22% compared to 619.53MPa before the solution aging treatment, and the elongation was increased by 17.3% compared to 1.79% before the solution aging treatment.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A preparation method of a low-content reinforcement reinforced titanium-based composite material is characterized in that a powder metallurgy method is adopted to generate TiC + TiB reinforcement in situ in a Ti-6Al-4V matrix, and then solid solution aging treatment is carried out to obtain the low-content reinforcement reinforced titanium-based composite material;
the specific operation of in-situ generation of the TiC + TiB reinforcement in the Ti-6Al-4V matrix by adopting a powder metallurgy method is as follows: mixing Ti powder, Al powder, V powder, and B powder 4 Performing ball milling and mixing treatment on the powder C, then performing compression molding by adopting a cold isostatic pressing method, and performing vacuum sintering treatment after compression molding;
according to weight percentageThe use amount of each raw material powder is as follows: 8% of Al powder, 4% of V powder, and B 4 1.5% of C powder and the balance of Ti powder;
the pressure maintaining pressure of the cold isostatic pressing method is 180MPa, and the pressure maintaining time is 20 min;
the volume percentage of TiC + TiB reinforcement in the low-content reinforcement reinforced titanium-based composite material is 3%;
the specific process of the vacuum sintering treatment comprises the following steps: heating from room temperature to 600 deg.C, maintaining for 30min, heating from 600 deg.C to 840 deg.C, maintaining for 30min, heating from 840 deg.C to 1300 deg.C, maintaining for 3h, and furnace cooling;
the process of the solid solution aging treatment comprises the following steps: the solid solution temperature is 940 ℃, the heat preservation is 30min, the water cooling is carried out, the aging temperature is 500 ℃, the heat preservation is carried out for 4h, and the air cooling is carried out.
2. The method of claim 1, wherein the Ti powder, Al powder, V powder, B powder are selected from the group consisting of Ti powder, Al powder, V powder 4 The average grain diameter of the C powder is less than or equal to 50 mu m.
3. The method for preparing the titanium-based composite material reinforced with low content of reinforcements according to claim 1, wherein the ball milling mixing treatment time is 24 hours and the rotating speed is 70 r/min.
4. The method of claim 1, wherein the vacuum sintering process is performed at a vacuum of 1 x 10 -3 Pa。
5. A low reinforcement content reinforced titanium-based composite material prepared by the method of any one of claims 1 to 4.
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