CN113430417A - High-performance titanium alloy added with rare earth oxide and preparation method thereof - Google Patents
High-performance titanium alloy added with rare earth oxide and preparation method thereof Download PDFInfo
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 90
- 229910001404 rare earth metal oxide Inorganic materials 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 100
- 239000000843 powder Substances 0.000 claims abstract description 86
- 229910000883 Ti6Al4V Inorganic materials 0.000 claims abstract description 58
- 239000000203 mixture Substances 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 21
- 239000010439 graphite Substances 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 238000005086 pumping Methods 0.000 claims abstract description 12
- 238000000498 ball milling Methods 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 5
- 230000007547 defect Effects 0.000 abstract description 10
- 238000007493 shaping process Methods 0.000 abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 238000004663 powder metallurgy Methods 0.000 abstract description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract 1
- 229910052719 titanium Inorganic materials 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 6
- 229910000838 Al alloy Inorganic materials 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- -1 rare earth compound Chemical class 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 230000002902 bimodal effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000000386 microscopy Methods 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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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
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—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
Abstract
The invention discloses a high-performance titanium alloy added with rare earth oxide and a preparation method thereof, relating to the technical field of powder metallurgy; the method comprises the following steps: mixing spherical Ti-6Al-4V powder with nano Y2O3Mixing the powder to obtain a mixture; the mixture is loaded into a graphite mould in batches and is placed in an SPS sintering furnace for vacuum pumping treatment; sintering the mixture after the vacuum-pumping treatment in an SPS sintering furnace. In one aspect, the method is carried out by adding nano-Y2O3The addition of the powder can effectively transform the structure of Ti-6Al-4V titanium alloyThe structure improves the tensile strength, yield strength and plasticity. On the other hand, the method can avoid the oxidation of oxygen to the titanium alloy powder by sintering in a vacuum environment, and ensure that the prepared titanium alloy is not oxidized, thereby fully utilizing the wettability between the rare earth oxide and the titanium alloy, reducing the defects of a sintered product and improving the tensile strength and the shaping.
Description
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to a high-performance titanium alloy added with rare earth oxide and a preparation method thereof.
Background
The Ti-6Al-4V titanium alloy has the advantages of high specific strength, good low-temperature performance and high-temperature performance, good corrosion resistance, good biocompatibility and the like. With the continuous expansion of the application range of titanium alloy, the Ti-6Al-4V titanium alloy not only has been widely applied in the aspects of aerospace, biomedical devices and the like, but also has quietly entered the daily life. However, the Ti-6Al-4V titanium alloy can generate a defect area in the smelting process, and micro-area chemical components in the defect area are not uniform, which is mainly reflected in that the content of O is higher, the content of Al and V is lower, and oxygen-enriched inclusions are formed. Coarse phase structure is formed, the microhardness and plasticity are reduced, and shrinkage cavities and cracks are caused due to high brittleness in the deformation process, so that the mechanical properties of the Ti-6Al-4V titanium alloy are influenced. Currently, there are many methods for increasing the hardness of Ti-6Al-4V titanium alloys, such as physical vapor deposition and chemical vapor deposition. These methods have limited essential improvements, and the adhesion layer obtained is unstable and easily comes off.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a high-performance titanium alloy added with rare earth oxide and a preparation method thereof.
The invention is realized by the following steps:
in a first aspect, the present invention provides a method for preparing a high performance titanium alloy with rare earth oxide added, comprising:
mixing spherical Ti-6Al-4V powder with nano Y2O3Powder ofMixing to obtain a mixture;
the mixture is loaded into a graphite mould in batches and is placed in an SPS sintering furnace for vacuum pumping treatment;
sintering the mixture after the vacuum-pumping treatment in an SPS sintering furnace.
In an alternative embodiment, in the blend, Ti-6Al-4V powder and nano-Y2O3The mass ratio of the powder is (99-100) to (1-0.1).
In an alternative embodiment, in the blend, Ti-6Al-4V powder and nano-Y2O3The mass ratio of the powder is (99.2-99.5) to (0.8-0.5).
In an alternative embodiment, the particle size of the Ti-6Al-4V powder is 15-45 μm; nanometer Y2O3The particle size of the powder is 20-30 nm.
In an alternative embodiment, the mix is composed of spherical Ti-6Al-4V powder and nano-Y2O3Mixing the powder under a ball milling condition, wherein the ball-material ratio of ball milling is (3-4): 1, ball milling rotation speed is 200-400 r/min, and ball milling time is 2-5 h;
alternatively, the first and second electrodes may be,
the mixture is prepared from spherical Ti-6Al-4V powder and nano Y2O3Mixing the powder under the condition of ball milling, and then stirring and mixing the powder in a mixer to obtain the powder; wherein the ball-material ratio of ball milling is (3-4): 1, ball milling rotation speed is 200-400 r/min, and ball milling time is 2-5 h; the stirring speed is 30-45 rpm, and the stirring time is 2-3 h.
In an alternative embodiment, in the step of batch charging the mixture into the graphite mold:
the amount of the mixture added into the graphite die with the diameter of 20mm is 15g each time.
In an alternative embodiment, in the step of placing the mixture in an SPS sintering furnace for vacuuming:
and the step of vacuumizing treatment is to vacuumize the SPS sintering furnace to be below 500 Pa.
In an alternative embodiment, in the step of sintering in an SPS sintering furnace:
the sintering temperature is 1000-1200 ℃; the sintering heat preservation time is 2-10 mim; the sintering pressure is 25-35 MPa; the sintering rate is 80-120 ℃/min.
In an alternative embodiment, in the step of sintering in an SPS sintering furnace:
the sintering temperature is 1100 ℃; the sintering heat preservation time is 5 mim; the sintering pressure is 30 MPa; the sintering rate was 100 ℃/min.
In a second aspect, the present invention provides a high performance titanium alloy with rare earth oxide added, which is prepared by the method for preparing the high performance titanium alloy with rare earth oxide added according to any one of the foregoing embodiments.
The embodiment of the invention has at least the following advantages or beneficial effects:
the embodiment of the invention provides a preparation method of a high-performance titanium alloy added with rare earth oxide, which comprises the following steps: mixing spherical Ti-6Al-4V powder with nano Y2O3Mixing the powder to obtain a mixture; the mixture is loaded into a graphite mould in batches and is placed in an SPS sintering furnace for vacuum pumping treatment; sintering the mixture after the vacuum-pumping treatment in an SPS sintering furnace. In one aspect, the method is carried out by adding nano-Y2O3The powder can obviously improve the tensile strength, the yield strength and the elongation percentage of the Ti-6Al-4V titanium alloy, so that the structure of the Ti-6Al-4V titanium alloy is converted from a Widmannstatten structure to a bimodal structure, and the crystal grains are obviously refined; and nano Y2O3The powder is mainly distributed at the grain boundary to inhibit further growth of grains; and a small part of the titanium alloy is distributed in the crystal to generate dislocation pinning so as to effectively transform the tissue structure of the Ti-6Al-4V titanium alloy, so that the tensile strength, the yield strength and the plasticity of the titanium alloy are improved. On the other hand, the method can avoid the oxidation of oxygen to the titanium alloy powder by sintering in a vacuum environment, and ensure that the prepared titanium alloy is not oxidized, thereby fully utilizing the wettability between the rare earth oxide and the titanium alloy, reducing the defects of a sintered product and improving the tensile strength and the shaping.
The embodiment of the invention provides a high-performance titanium alloy added with rare earth oxide, which is prepared by the method. Therefore, the steel has the advantages of high strength and good toughness.
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 metallographic micrograph of a high performance titanium alloy with added rare earth oxide prepared according to examples 1 to 4 of the present invention;
FIG. 2 is a tensile fracture morphology of the high performance titanium alloy with rare earth oxide added prepared in examples 1-4 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 features and properties of the present invention are described in further detail below with reference to examples.
The embodiment of the invention provides a preparation method of a high-performance titanium alloy added with rare earth oxide, which specifically comprises the following steps:
s1: mixing spherical Ti-6Al-4V powder with nano Y2O3Mixing the powder to obtain a mixture;
s2: the mixture is loaded into a graphite mould in batches and is placed in an SPS sintering furnace for vacuum pumping treatment;
s3: sintering the mixture after the vacuum-pumping treatment in an SPS sintering furnace.
In detail, in the above step, one of the twoFlour by adding nano-Y2O3The powder can obviously improve the tensile strength, the yield strength and the elongation percentage of the Ti-6Al-4V titanium alloy, so that the structure of the Ti-6Al-4V titanium alloy is converted from a Widmannstatten structure to a bimodal structure, and the crystal grains are obviously refined; and nano Y2O3The powder is mainly distributed at the grain boundary to inhibit further growth of grains; and a small part of the titanium alloy is distributed in the crystal to generate dislocation pinning so as to effectively transform the tissue structure of the Ti-6Al-4V titanium alloy, so that the tensile strength, the yield strength and the plasticity of the titanium alloy are improved. On the other hand, the method can avoid the oxidation of oxygen to the titanium alloy powder by sintering in a vacuum environment, and ensure that the prepared titanium alloy is not oxidized, thereby fully utilizing the wettability between the rare earth oxide and the titanium alloy, reducing the defects of a sintered product and improving the tensile strength and the shaping. In addition, through the three steps, the titanium alloy finished product can be obtained by sintering in vacuum, and compared with the prior art, the titanium alloy finished product has the advantages of simple and convenient preparation process, low production cost and formability without subsequent treatment, so that the titanium alloy finished product can be used for producing small-sized devices and is widely applied to the manufacturing field of aerospace and precise medical devices.
In more detail, in step S1, in the mixture, Ti-6Al-4V powder and nano Y2O3The mass ratio of the powder is (99-100) to (1-0.1). Mixing Ti-6Al-4V powder and nano Y2O3The use amount of the powder is controlled within the range, so that the compactness of the sintered sample can be effectively ensured to be better, and the sintered sample has fine crystal grains and excellent mechanical property. When the proportion of the usage amount of the silicon carbide and the silicon carbide is less than the proportion, the sintered crystal grains are relatively large, the structure is hardly transformed, and the purposes of improving the tensile strength, the yield strength and the plasticity are difficult to achieve; when the proportion of the rare earth compound and the rare earth compound exceeds the proportion, the added rare earth compound is agglomerated to a certain extent in a sintered product, so that some defects are generated, and the mechanical property is reduced.
Alternatively, in the examples of the present invention, in the mixed material, Ti-6Al-4V powder and nano Y powder2O3Powder ofThe mass ratio of (99.2-99.5) to (0.8-0.5). For the same reason as above, the ratio of the two is controlled within the range, so that the nano Y can be better ensured2O3The powder can effectively transform the structure of Ti-6Al-4V titanium alloy, thereby obviously improving the tensile strength, yield strength and plasticity of the alloy.
Meanwhile, in step S1, the particle size of the Ti-6Al-4V powder is 15-45 μm; nanometer Y2O3The particle size of the powder is 20-30 nm. The particle size and the nanometer Y of Ti-6Al-4V powder2O3The particle diameters of the powders are respectively controlled within the ranges, so that the Ti-6Al-4V powder and the Y powder can be effectively ensured2O3The powder can be tightly combined in the sintering process, and meanwhile, the good combination interface is ensured, and the mechanical property of the prepared titanium alloy can be effectively improved through the good combination interface.
In addition, it should be noted that, in step S1, the mixed material is composed of spherical Ti-6Al-4V powder and nano Y2O3The powder is mixed under the condition of ball milling and then stirred and mixed in a mixer. Of course, in other embodiments of the present invention, ball milling and mixing or stirring may be performed separately, but when a certain mixing operation is performed separately, the time for the operation needs to be prolonged to ensure the uniformity of the mixture.
Specifically, the ball-material ratio of ball milling is (3-4): 1, preferably 4: 1. The ball milling speed is 200-400 r/min, preferably 300 r/min. The ball milling time is 2-5 h, preferably 4 h. Meanwhile, the powder is mixed on a ZX-0.5 type double-cone efficient mixer by stirring, the stirring speed is 30-45 rpm, preferably 30-35 rpm, and the stirring time is 2-3 h, preferably 2 h. The ball milling operation and the stirring powder mixing operation are matched for use, which is beneficial to the homogenization of the mixture and the uniform distribution of the added powder, thereby being more beneficial to the homogenization of the components of the sintered product and leading the spherical Ti-6Al-4V powder and the nano Y powder to be used2O3After the powder is mixed and sintered, the compactness of the titanium alloy can be improved, the defects can be reduced, and the strength and the shaping can be improved.
In detail, in step S2, in the step of charging the mixed material into the graphite mold in batches, the amount of the mixed material charged into the Φ 20mm graphite mold at a time was 15g, and of course, less than 15g of the mixed material remained in total at once. By such an arrangement, the amount of powder added during sintering can be controlled, and the influence on the properties of the material when the powder leaks or runs short of the mold can be avoided. Of course, in other embodiments of the present invention, the amount of the mixture used for a single time may also be adjusted according to the use of graphite molds with different sizes, and the embodiments of the present invention are not limited thereto.
Meanwhile, in step S2, in the step of placing the mixed material in the SPS sintering furnace to perform the vacuum-pumping treatment, the vacuum-pumping treatment is performed by vacuum-pumping the SPS sintering furnace to 500Pa or less. The titanium alloy powder is prevented from being oxidized in the sintering process under the definite vacuum state, and the vacuum degree is controlled within the range, so that the titanium alloy powder is prevented from being oxidized in the sintering process, the normal operation of the sintering operation can be effectively ensured, and the sintering efficiency and the quality of a product obtained by sintering are ensured.
In detail, in step S3, the sintering temperature for sintering in the SPS sintering furnace is 1000-1200 ℃, and 1100 ℃ is preferred; the sintering heat preservation time is 2-10 mim, preferably 5 min; the sintering pressure is 25-35 MPa, preferably 30 MPa; the sintering rate is 80-120 ℃/min, preferably 100 ℃/min. The sintering temperature is adopted for the purpose of effectively controlling the sintering temperature, if the sintering temperature is lower than 1100 ℃, a sintered product cannot be completely compact, contains a plurality of pores and holes, and influences the mechanical property, and when the sintering temperature is higher than 1100 ℃, the compactness and the performance of the sintered product are similar to those of the sintered product sintered at 1100 ℃, so that the sintering temperature is set to be 1100 ℃ for saving energy consumption and improving the performance of the composite material.
Through the setting and parameter selection of the three steps, the prepared titanium alloy has the advantages of small grain size, uniform component distribution and higher density, and the relative density is more than 99%. Meanwhile, the titanium alloy prepared by the above method has the advantages of higher hardness, large tensile strength and good ductility, and for further illustrating the technical effects of the present invention, the following will describe in detail the high performance titanium alloy with rare earth oxide added and the preparation method thereof with reference to the examples, but they should not be construed as limiting the scope of the present invention.
Example 1
The embodiment provides a high-performance titanium alloy added with rare earth oxide, which is prepared by the following method:
s1: mixing spherical Ti-6Al-4V powder and nano Y2O3The powder is prepared from the following components in percentage by mass of 99.3: 0.7, and the ball-to-material ratio during ball milling is 4:1, the rotating speed is 300r/min, and then the materials are mixed for 1 hour on a mixer at the speed of 30rpm to obtain a mixture;
s2: weighing 15g of the mixture, putting the mixture into a graphite mold, putting the graphite mold into an SPS sintering furnace for sintering, and vacuumizing to below 500 Pa;
s3: sintering at the temperature rising rate of 80 ℃/min, the sintering pressure of 30MPa and the sintering temperature of 1100 ℃ for 5min, and cooling to room temperature along with the furnace to obtain the high-performance Ti-6Al-4V titanium alloy.
Example 2
The embodiment provides a high-performance titanium alloy added with rare earth oxide, which is prepared by the following method:
s1: spherical Ti-6Al-4V powder and nano Y with the same mass as in example 12O3The powder is prepared from the following components in percentage by mass of 99.5: 0.5, and the ball-material ratio during ball milling is 4:1, the rotating speed is 400r/min, and then the materials are mixed for 2 hours on a mixer at the speed of 35rpm to obtain a mixture;
s2: weighing 15g of the mixture, putting the mixture into a graphite mold, putting the graphite mold into an SPS sintering furnace for sintering, and vacuumizing to below 500 Pa;
s3: sintering at a temperature rise rate of 100 ℃/min, a sintering pressure of 30MPa and a sintering temperature of 1100 ℃ for 5min, and cooling to room temperature along with the furnace to obtain the high-performance Ti-6Al-4V titanium alloy.
Example 3
The embodiment provides a high-performance titanium alloy added with rare earth oxide, which is prepared by the following method:
s1: spherical Ti-6Al-4V powder and nano Y with the same mass as in example 12O3The powder is prepared from the following components in percentage by mass of 99.3: 0.7, and the ball-to-material ratio during ball milling is 4:1, the rotating speed is 200r/min, and then the materials are mixed for 3 hours on a mixer at the speed of 40rpm to obtain a mixture;
s2: weighing 15g of the mixture, putting the mixture into a graphite mold, putting the graphite mold into an SPS sintering furnace for sintering, and vacuumizing to below 500 Pa;
s3: sintering at the temperature rising rate of 120 ℃/min, the sintering pressure of 30MPa and the sintering temperature of 1000 ℃ for 10min, and cooling to room temperature along with the furnace to obtain the high-performance Ti-6Al-4V titanium alloy.
Example 4
The embodiment provides a high-performance titanium alloy added with rare earth oxide, which is prepared by the following method:
s1: spherical Ti-6Al-4V powder and nano Y with the same mass as in example 12O3The powder is prepared from the following components in percentage by mass of 99.3: 0.7, the ball-material ratio during ball milling is 3: 1, the rotating speed is 300r/min, and then the materials are mixed for 2 hours on a mixer at the speed of 45rpm to obtain a mixture;
s2: weighing 15g of the mixture, putting the mixture into a graphite mold, putting the graphite mold into an SPS sintering furnace for sintering, and vacuumizing to below 500 Pa;
s3: sintering at a temperature rise rate of 100 ℃/min, a sintering pressure of 35MPa and a sintering temperature of 1000 ℃ for 5min, and cooling to room temperature along with the furnace to obtain the high-performance Ti-6Al-4V titanium alloy.
Experimental example 1
The grain size of the high-performance titanium alloy added with rare earth oxide provided in examples 1-4 was measured by metallographic microscopy, and the results are shown in the grain refinement and structure transformation diagram under the metallographic microscope in fig. 1 and the tensile fracture morphology diagram in fig. 2, wherein (1) is example 1, (2) is example 2, (3) is example 3, and (4) is example 4. The compactness of the high-performance Ti-6Al-4V titanium alloy is tested by using an Archimedes drainage method, and the test result is shown in Table 1. The Vickers hardness of the high-performance Ti-6Al-4V titanium alloy is measured by a microhardness meter, the tensile strength and the ductility of the high-performance Ti-6Al-4V titanium alloy are measured by a universal machine, and the test results are shown in Table 2. The grain refinement and the structure transformation under a metallographic microscope are shown in figure 1, and the tensile fracture morphology is shown in figure 2.
TABLE 1 compactness and grain size test results of Ti-6Al-4V titanium alloy composite materials
TABLE 2 hardness, tensile strength and shape test results for Ti-6Al-4V titanium alloy composites
| Numbering | Hardness (HV) | Tensile strength (MPa) | Elongation (%) |
| Example 1 | 392 | 1088 | 7.9 |
| Example 2 | 386 | 1060 | 6.8 |
| Example 3 | 374 | 1024 | 4.3 |
| Example 4 | 371 | 1015 | 3.9 |
According to the data in the table 1, the grain size of the high-performance Ti-6Al-4V titanium alloy prepared by the method and the formula is obviously refined, the compactness is higher, and the high-performance titanium alloy prepared by the method and the formula has uniform component distribution and no more defects, and can be used for preparing small-sized precise instruments. Meanwhile, according to the comparison between example 1 and examples 2-4, it can be seen that when Ti-6Al-4V powder and nano Y are used2O3The mass ratio of the powder is 99.3: 0.7, the aluminum alloy obtained at the sintering temperature of 1100 ℃, the sintering rate of 100 ℃/min and the sintering pressure of 30MPa has higher density and lower grain size. As can be seen from the comparison between example 1 and example 2, when Ti-6Al-4V powder and nano-Y powder were used2O3The mass ratio of the powder is 99.3: the density is better when the density is 0.7, and the comparison between the example 1 and the examples 3 and 4 shows that the aluminum alloy with better density can be obtained when the sintering temperature is 1100 ℃, the sintering rate is 100 ℃/min and the sintering pressure is 30 MPa. In contrast, the comparison between example 3 and example 4 shows that the ball-to-feed ratio is 4:1 is more favorable for obtaining compact aluminum alloy.
According to the data in table 2, the high-performance titanium alloy prepared by the method and the formula of the invention has better comprehensive mechanical properties of hardness, tensile strength and ductility. Meanwhile, according to the comparison between example 1 and examples 2-4, it can be seen that when Ti-6Al-4V powder and nano Y are used2O3The mass ratio of the powder is 99.3: 0.7, the sintering temperature is 1100 ℃, the sintering rate is 100 ℃/min and the sintering pressure is 30MPa, the strength and the comprehensive shaping performance are better, and are 1088MPa and 7.9 percent respectively, and the method can be used for preparing some fine parts. Meanwhile, when Ti-6Al-4V powder and nano Y are used, it can be seen from the comparison between example 1 and example 22O3The mass ratio of the powder is 99.3: the hardness and tensile strength were more excellent at 0.7, and a comparison of example 1 with examples 3 and 4 revealed that an aluminum alloy having more excellent hardness and tensile strength was more obtained at a sintering temperature of 1100 deg.C, a sintering rate of 100 deg.C/min and a sintering pressure of 30 MPa. In contrast, the comparison between example 3 and example 4 shows that the ball-to-feed ratio is 4:1 is more favorable for obtaining the aluminum alloy with higher strength and hardness.
As shown in FIG. 1, the high performance Ti-6Al-4V titanium alloy produced by sintering at 1100 ℃ is almost free of defects, has uniform component distribution, and has significantly refined grains. As shown in FIG. 2, the fracture of the prepared high performance titanium alloy contains a large amount of dimples, Y2O3Mainly distributed in the fossa, has less microscopic defects and obviously improved toughness.
Therefore, according to the above structure, the high performance titanium alloy with the addition of the rare earth oxide provided by the embodiment of the present invention can increase the maximum tensile strength to 1088MPa, which is 16.9% higher than the prior art; the elongation of the material can be improved to 7.9%. The improvement effect of the titanium alloy is obviously better than the strengthening effect of other materials for strengthening the Ti-6Al-4V titanium alloy. Nanometer Y2O3The addition of the titanium alloy transforms the structure of the Ti-6Al-4V titanium alloy, so that the tensile strength, the yield strength and the plasticity of the titanium alloy are improved.
In summary, the embodiment of the invention provides a high-performance titanium alloy added with rare earth oxide and having high strength and good toughness and a preparation method thereof, and the prepared titanium alloy has the advantages of light weight, high specific strength, high density, good shaping and the like. And the preparation process is simple and convenient, the titanium alloy can be formed without subsequent treatment, the production cost is reduced, and the comprehensive mechanical property of the Ti-6Al-4V titanium alloy is improved.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a high-performance titanium alloy added with rare earth oxide is characterized by comprising the following steps:
mixing spherical Ti-6Al-4V powder with nano Y2O3Mixing the powder to obtain a mixture;
putting the mixture into a graphite mold in batches, and placing the graphite mold into an SPS sintering furnace for vacuumizing treatment;
and sintering the mixture subjected to the vacuum-pumping treatment in the SPS sintering furnace.
2. The method for preparing a high-performance titanium alloy with addition of rare earth oxide according to claim 1, wherein:
in the mixture, the Ti-6Al-4V powder and the nano Y2O3The mass ratio of the powder is (99-100) to (1-0.1).
3. The method for preparing a high-performance titanium alloy with addition of rare earth oxide according to claim 2, wherein:
in the mixture, the Ti-6Al-4V powder and the nano Y2O3The mass ratio of the powder is (99.2-99.5) to (0.8-0.5).
4. The method for producing a high-performance titanium alloy added with a rare earth oxide according to any one of claims 1 to 3, characterized in that:
the particle size of the Ti-6Al-4V powder is 15-45 mu m; the nano Y2O3The particle size of the powder is 20-30 nm.
5. The method for producing a high-performance titanium alloy added with a rare earth oxide according to any one of claims 1 to 3, characterized in that:
the mixture is composed of the spherical Ti-6Al-4V powder and the nano Y2O3Mixing the powder under a ball milling condition, wherein the ball-material ratio of ball milling is (3-4): 1, ball millingThe rotating speed is 200-400 r/min, and the ball milling time is 2-5 h;
alternatively, the first and second electrodes may be,
the mixture is composed of the spherical Ti-6Al-4V powder and the nano Y2O3Mixing the powder under the condition of ball milling, and then stirring and mixing the powder in a mixer to obtain the powder; wherein the ball-material ratio of ball milling is (3-4): 1, ball milling rotation speed is 200-400 r/min, and ball milling time is 2-5 h; the stirring speed is 30-45 rpm, and the stirring time is 2-3 h.
6. The method for producing a high-performance titanium alloy with addition of rare earth oxide according to any one of claims 1 to 3, wherein in the step of charging the mixture into the graphite mold in batches:
the amount of the mixture added into the graphite die with the diameter of 20mm is 15g each time.
7. The method for producing a high-performance titanium alloy with addition of rare earth oxide according to any one of claims 1 to 3, wherein in the step of placing the mixture in the SPS sintering furnace for vacuuming:
and the step of vacuumizing treatment is to vacuumize the SPS sintering furnace to be below 500 Pa.
8. The method for producing a high-performance titanium alloy added with a rare earth oxide according to any one of claims 1 to 3, wherein in the step of sintering in the SPS sintering furnace:
the sintering temperature is 1000-1200 ℃; the sintering heat preservation time is 2-10 mim; the sintering pressure is 25-35 MPa; the sintering rate is 80-120 ℃/min.
9. The method for producing a high-performance titanium alloy added with a rare earth oxide according to claim 8, wherein in the step of sintering in the SPS sintering furnace:
the sintering temperature is 1100 ℃; the sintering heat preservation time is 5 mim; the sintering pressure is 30 MPa; the sintering rate was 100 ℃/min.
10. A high-performance titanium alloy added with rare earth oxide is characterized in that:
the high-performance titanium alloy added with the rare earth oxide is prepared by the preparation method of the high-performance titanium alloy added with the rare earth oxide as claimed in any one of claims 1 to 9.
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