High-strength and high-plasticity titanium matrix composite and preparation method thereof

Patent metadata

Field	Value
Publication number	US-12226826-B2
Application number	US-202017768737-A
Country	US
Kind code	B2
Filing date	Aug 17, 2020
Priority date	Jul 29, 2020
Publication date	Feb 18, 2025
Grant date	Feb 18, 2025

Abstract

The present invention provides a high-strength and high-plasticity titanium matrix composite and a preparation method thereof. The preparation method includes: preparing high-oxygen hydride-dehydride titanium powder using a high-temperature rotary ball grinding treatment process, in which the prepared hydride-dehydride titanium powder has a particle size of 10-40 μm, and has an oxygen content of 0.8-1.5 wt. %; preparing high-purity ultra-fine oxygen adsorbent powder using a wet grinding method of high-energy vibration ball grinding treatment process; in which a purity of the oxygen adsorbent powder is ≥99.9%, and a particle size of the oxygen adsorbent powder is ≤8 μm; mixing the high-oxygen hydride-dehydride titanium powder with the oxygen adsorbent powder in a protective atmosphere, and then press-forming the powder obtained after mixing to obtain a raw material blank; and performing atmosphere protective sintering treatment on the raw material blank to obtain a titanium matrix composite. The method prepares a titanium matrix composite reinforced by in-situ self-generating multi-scale Ca—Ti—O, TiC, TiB particles. The microstructure and grains are effectively refined, and the strength and plasticity of the material are significantly improved.

First claim

The invention claimed is:

1. A method for preparing a high-strength and high-plasticity titanium matrix composite, comprising the following steps:
S1: preparing high-oxygen hydride-dehydride titanium powder using a high-temperature rotary ball grinding treatment process, wherein the prepared hydride-dehydride titanium powder has a particle size of 10-40 μm, and has an oxygen content of 0.8-1.5 wt. %;
S2: preparing high-purity ultra-fine oxygen adsorbent powder using a wet grinding method of high-energy vibration ball grinding treatment process; wherein a purity of the oxygen adsorbent powder is ≥99.9%, and a particle size of the oxygen adsorbent powder is ≤8 μm; and the oxygen adsorbent is selected from at least one of CaC2 and CaB6;
S3: preparing a raw material blank, wherein the high-oxygen hydride-dehydride titanium powder is mixed with the high-purity ultra-fine oxygen adsorbent powder in a protective atmosphere, and then the powder obtained after mixing is press-formed to obtain a raw material blank; and
S4: sintering, wherein the raw material blank obtained in step S3 is subjected to atmosphere protective sintering treatment to obtain a titanium matrix composite.

2. The method for preparing the high-strength and high-plasticity titanium matrix composite according to claim 1 , wherein in step S1, the high-temperature rotary ball grinding treatment process comprises:
S1-1: putting the hydride-dehydride titanium powder and grinding balls into a protective atmosphere furnace;
S1-2: performing high-temperature rotary ball grinding treatment on the hydride-dehydride titanium powder in the protective atmosphere furnace, wherein a rotational speed of rotary ball grinding in this step is 10-60 r/min; and
S1-3: cooling the hydride-dehydride titanium powder treated in step S1-2 to room temperature, and sieving to obtain high-oxygen hydride-dehydride titanium powder.

3. The method for preparing the high-strength and high-plasticity titanium matrix composite according to claim 2 , wherein in step S1-1, the hydride-dehydride titanium powder has a median diameter D50 of the particle size of 15-50 μm, and has an oxygen content of ≤0.30 wt. %.

4. The method for preparing the high-strength and high-plasticity titanium matrix composite according to claim 2 , wherein in step S1-2, the high-temperature rotary ball grinding treatment comprises two stages; wherein in a first treatment stage, the temperature is increased to 140-200° C. at a rate of 5-10° C./min in a mixed atmosphere of argon gas and oxygen gas with an oxygen volume fraction of 10-30 vol. %, and the temperature is held for 0.5-3 h; and in a second treatment stage, the temperature is increased to 450-600° C. at a rate of 5-10° C./min in an atmosphere of high-purity argon gas, and the temperature is held for 0.5-3 h.

5. The method for preparing the high-strength and high-plasticity titanium matrix composite according to claim 1 , wherein in step S2, the wet grinding method of high-energy vibration ball grinding treatment process comprises:
S2-1: loading the oxygen adsorbent raw material and zirconia grinding balls into a ball grinding tank in a protective atmosphere, adding a protective liquid to the ball grinding tank, and then sealing the ball grinding tank;
S2-2: loading the sealed ball grinding tank into a high-energy vibration ball grinding mill for wet grinding to obtain an oxygen adsorbent slurry; and
S2-3: drying the oxygen adsorbent slurry obtained after wet grinding under a protective atmosphere condition or vacuum condition at 40-60° C. for 1-4 h, and then sieving to obtain high-purity ultra-fine oxygen adsorbent powder.

6. The method for preparing the high-strength and high-plasticity titanium matrix composite according to claim 5 , wherein in step S2-1, a ball-to-material ratio of the zirconia grinding balls to the oxygen adsorbent raw material is 5-10:1, and the protective liquid is an anhydrous and oxygen-free volatile organic solvent.

7. The method for preparing the high-strength and high-plasticity titanium matrix composite according to claim 5 , wherein in step S2-2, a vibration frequency of the wet grinding is 1000-1400 times/min, and the wet grinding is performed for 3-6 h according to the ball grinding mode of ball grinding for 2-4 min and shutdown for 4-8 min.

8. The method for preparing the high-strength and high-plasticity titanium matrix composite according to claim 1 , wherein in step S3, a mass fraction percentage of the oxygen adsorbent powder during mixing is 0.4-2.0 wt. %.

9. The method for preparing the high-strength and high-plasticity titanium matrix composite according to claim 1 , wherein in step S4, a sintering temperature of the sintering treatment is 1100-1300° C., a heating rate is 2-8° C./min, and a temperature-holding time is 30-180 min.

10. A high-strength and high-plasticity titanium matrix composite, which is prepared by the method according to claim 1 , wherein the titanium matrix composite has a micro-fine equiaxed grain microstructure, with a grain size being 20-100 μm.

11. The method for preparing the high-strength and high-plasticity titanium matrix composite according to claim 2 , wherein in step S2, the wet grinding method of high-energy vibration ball grinding treatment process comprises:
S2-1: loading the oxygen adsorbent raw material and zirconia grinding balls into a ball grinding tank in a protective atmosphere, adding a protective liquid to the ball grinding tank, and then sealing the ball grinding tank;
S2-2: loading the sealed ball grinding tank into a high-energy vibration ball grinding mill for wet grinding to obtain an oxygen adsorbent slurry; and
S2-3: drying the oxygen adsorbent slurry obtained after wet grinding under a protective atmosphere condition or vacuum condition at 40-60° C. for 1-4 h, and then sieving to obtain high-purity ultra-fine oxygen adsorbent powder.

12. The method for preparing the high-strength and high-plasticity titanium matrix composite according to claim 3 , wherein the grinding balls are zirconia with a particle size of 6-8 mm; and a mass ratio of the grinding balls to the hydride-dehydride titanium powder is 0.5-2:1.

13. The method for preparing the high-strength and high-plasticity titanium matrix composite according to claim 8 , wherein the mixing is carried out on a mechanical mixer, a rotational speed of the mixer is 60-100 r/min, and the time is 4-8 h.

14. The high-strength and high-plasticity titanium matrix composite according to claim 10 , wherein a granular Ca—Ti—O reinforcing phase and TiC, TiB reinforcing phase are generated in-situ in the titanium matrix composite, with a particle size of the Ca—Ti—O reinforcing phase being 100-300 nm, and a particle size of the TIC, TiB reinforcing phase being 1-5 μm.

Assignees

• Univ Beijing Science & Technology

Inventors

• Lu Xin
• Pan Yu
• Yang Yucheng
• Zhang Jiazhen
• Xu Wei
• Liu Bowen
• Zhang Ce
• Sun Jianzhuo
• Liu Yanjun
• Qu Xuanhui

Classifications

• B22F2303/45

  Part of a final mixture to be processed further · CPC title

• B22F2301/205

  Titanium, zirconium or hafnium · CPC title

• B22F2203/11

  temperature, temperature profile · CPC title

• B22F2201/11

  Argon · CPC title

• B22F2009/049

  by pulverising at particular temperature · CPC title