Preparation method of yttrium oxide particle reinforced tantalum-based composite material with high tensile strength and high extensibility

Abstract

The invention discloses a preparation method of a high-tensile-strength and high-extensibility yttrium oxide particle reinforced tantalum-based composite material, and belongs to the field of refractory metal-based composite materials. The yttrium oxide particles are added, so that abnormal growth of tantalum grains in the powder metallurgy process can be effectively inhibited, and the grain size of the tantalum-based composite material is regulated and controlled. The engineering stress and deformation capacity of the tantalum-based composite material are remarkably improved in the high-temperature service process of the yttrium oxide particle reinforced tantalum-based composite material. According to the method, the content of yttrium oxide with different volume fractions can be accurately regulated and controlled in a large range. The yttrium oxide particle reinforced tantalum-based composite material prepared by the method has the advantages of fine crystal grains, inhibition of abnormal growth of the crystal grains, high engineering stress and high deformation elongation. The relative density gt of the yttrium oxide particle reinforced tantalum-based composite material; the tensile strength of the alloy is 100-650 MPa, the elongation is 98%, the room-temperature hardness is 1.6-2.1 GPa, the tensile strength is 100-650 MPa, and the ductility is 2%-27%.

Description

Technical Field

[0001] The present invention belongs to the field of refractory metal-based composite materials, and in particular relates to a method for preparing a tantalum-based composite material reinforced with yttrium oxide particles having high tensile strength and high ductility. Background Art

[0002] Tantalum metal materials have high melting points, corrosion resistance, strong chemical stability and plastic processing properties. As refractory metal materials, they have broad application prospects in extreme environments such as aviation, aerospace, chemical industry, and nuclear industry, which are subject to high temperature loads, strong corrosion, and special smelting. Tantalum metal is mainly prepared by traditional smelting or powder metallurgy methods. There is a coarse grain structure in the initial blank, and it needs to undergo a complex heat treatment process to effectively control / refine the grains to improve its plastic processing and mechanical properties. In addition, when tantalum metal materials are used in service for a long time in a high-temperature load environment, secondary recrystallization and abnormal growth of local grains are very likely to occur, resulting in rapid attenuation and loss of mechanical properties of the tantalum metal material or even complete failure. Summary of the Invention

[0003] In view of the problems existing in the prior art, the present invention provides a method for preparing a tantalum-based composite material reinforced with yttrium oxide particles having high tensile strength and high ductility.

[0004] The present invention is based on powder metallurgy technology and proposes a second-phase oxide particle dispersion strengthening method to improve / regulate the microstructure and mechanical properties of tantalum metal. Yttrium oxide generally has a body-centered cubic structure and has a variety of unique basic properties and a wide range of applications. Yttrium oxide has physical and chemical stability and chemical inertness, is not easy to react with other compounds, can work stably for a long time in harsh environments such as high temperature, strong acid, and strong alkali, and is a more ideal second-phase ceramic particle modification phase in tantalum metal. Through the ball milling mixing process, yttrium oxide is dispersed in the matrix, which can effectively hinder the movement of dislocations and grain boundaries, refine the grains, and improve the comprehensive mechanical properties of tantalum metal materials. The tantalum-based material reinforced with yttrium oxide particles prepared by the technical route of the present invention can be prepared by a powder metallurgy sintering process to produce a tantalum-based material with fine grains, uniform second phase distribution, high engineering stress, and high deformation elongation, without the need for subsequent complex heat processing. The overall process flow is significantly shortened and the preparation cost is greatly reduced. The relative density of the prepared yttrium oxide particle reinforced tantalum-based composite material is > 98 %, room temperature hardness is 1.6~2.1 GPa, tensile strength of 100~650MPa, and elongation of 2%~27%. The mechanical properties of this material are comparable to or even higher than those of traditional tantalum alloys that have undergone complex heat processing. It also features a simple and efficient process, low overall energy consumption, and controllable microstructure and properties.

[0005] A method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material comprises the following steps:

[0006] 1. Weighing ingredients:

[0007] Weighing tantalum powder and yttrium oxide powder according to a certain volume ratio to obtain a raw material;

[0008] The volume fraction of yttrium oxide powder in the raw material described in step 1 is 0.3% to 30%;

[0009] 2. Powder mixing:

[0010] After the tantalum powder and yttrium oxide powder weighed in step 1 are preliminarily mixed, they are subjected to all-round ball milling in an inert gas or vacuum environment to achieve full and uniform mixing of the powders, and are sieved in an inert gas environment through an 80-320 mesh sieve to obtain a uniformly mixed composite powder raw material;

[0011] 3. Sintering:

[0012] The uniformly mixed composite powder raw material obtained in step 2 is placed in a graphite mold and sintered in an inert gas or vacuum environment to obtain tantalum-based composite materials reinforced with yttrium oxide particles of different volume fractions.

[0013] The present invention has the following beneficial effects:

[0014] This invention proposes for the first time a tantalum-based composite material reinforced with yttrium oxide particles and exhibiting high tensile strength and high ductility, and a method for preparing the same. The invention utilizes a simple process flow, significantly reducing the production cost of the tantalum-based composite material. It achieves high plasticity and deformation properties without requiring traditional heat processing or heat treatment, significantly improving the tensile strength and other mechanical properties of the tantalum-based material.

[0015] Tantalum powder and yttrium oxide powder can be fully mixed and evenly mixed by all-round planetary ball milling, and adverse factors such as powder particle agglomeration, cold welding between particles, and caking can be effectively avoided by controlling the ball milling process parameters, which can effectively improve the uniformity of the second phase distribution of the material, refine the grains and promote sintering density; using powder metallurgy solid phase sintering method, tantalum-based composite materials reinforced with yttrium oxide particles of different volume fractions are obtained; at the same time, the controllability of the production and preparation process is significantly improved, and the possibility of composite powder contamination caused by the wear of the mixing ball milling medium can be effectively reduced by controlling the ball milling process parameters, thereby ensuring the purity of the tantalum-based composite material reinforced with yttrium oxide particles. The relative density of the tantalum-based composite material reinforced with yttrium oxide particles prepared by the present invention is as follows: > 98%, room temperature hardness of 1.6~2.1GPa, tensile strength of 100~650MPa, and elongation of 2%~27%. By adjusting the volume content of yttrium oxide and the preparation process, the relative density of the prepared yttrium oxide particle reinforced tantalum-based composite material is > 99%, room temperature hardness of 1.8GPa, tensile strength of 600MPa, elongation of 22%, and comprehensive excellent performance. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 XRD patterns of tantalum-based composite materials reinforced with yttrium oxide particles of different volume fractions prepared in Comparative Example 1 and Examples 1 to 5;

[0017] Figure 2 These are SEM images of tantalum-based composite materials reinforced with yttrium oxide particles of different volume fractions prepared in Comparative Example 1 and Examples 1 to 5, where (a) is Ta prepared in Comparative Example 1, (b) is Ta-3% Y2O3 prepared in Example 1, (c) is Ta-5% Y2O3 prepared in Example 2, (d) is Ta-7% Y2O3 prepared in Example 3, (e) is Ta-10% Y2O3 prepared in Example 4, and (f) is Ta-15% Y2O3 prepared in Example 5. DETAILED DESCRIPTION

[0018] The following examples are intended to further illustrate the present invention, but should not be construed as limiting the present invention. Modifications and substitutions made to the methods, steps, or conditions of the present invention without departing from the spirit of the present invention are within the scope of the present invention.

[0019] Specific embodiment 1: This embodiment provides a method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material, comprising the following steps:

[0020] 1. Weighing ingredients:

[0021] Weighing tantalum powder and yttrium oxide powder according to a certain volume ratio to obtain a raw material;

[0022] The volume fraction of yttrium oxide powder in the raw material described in step 1 is 0.3% to 30%;

[0023] 2. Powder mixing:

[0024] After the tantalum powder and yttrium oxide powder weighed in step 1 are preliminarily mixed, they are subjected to all-round ball milling in an inert gas or vacuum environment to achieve full and uniform mixing of the powders, and are sieved in an inert gas environment through an 80-320 mesh sieve to obtain a uniformly mixed composite powder raw material;

[0025] 3. Sintering:

[0026] The uniformly mixed composite powder raw material obtained in step 2 is placed in a graphite mold and sintered in an inert gas or vacuum environment to obtain tantalum-based composite materials reinforced with yttrium oxide particles of different volume fractions.

[0027] Specific Embodiment 2: This embodiment differs from Specific Embodiment 1 in that the ball milling process described in step 2 employs an omnidirectional planetary ball mill, a ball-to-material ratio of (5-20):1, a ball mill speed of 50-500 rpm, a milling time of 12-48 hours, and the milling jar and balls are both made of zirconia. All other steps are the same as in Specific Embodiment 1.

[0028] Specific embodiment 3: This embodiment differs from specific embodiments 1 or 2 in that the ball milling process described in step 2 uses an omnidirectional planetary ball mill, a ball-to-material ratio of 10:1, a ball mill speed of 300 rpm, a milling time of 24 hours, and the milling jar and grinding balls are both made of zirconia. The other steps are the same as those in specific embodiments 1 or 2.

[0029] Specific Embodiment 4: This embodiment differs from Specific Embodiments 1 to 3 in that the ball milling process described in step 2 employs an omnidirectional planetary ball mill, a ball-to-material ratio of 5:1, a ball mill speed of 200 rpm, a milling time of 48 hours, and the milling jar and grinding balls are both made of zirconia. The remaining steps are the same as Specific Embodiments 1 to 3.

[0030] Specific embodiment 5: This embodiment differs from specific embodiments 1 to 4 in that the sintering in step 3 is hot pressing sintering. The other steps are the same as those in specific embodiments 1 to 4.

[0031] Specific embodiment 6: This embodiment differs from specific embodiments 1 to 5 in that the sintering in step 3 is spark plasma sintering. The other steps are the same as those in specific embodiments 1 to 5.

[0032] Specific embodiment seven: The difference between this embodiment and specific embodiments one to six is ​​that the hot pressing sintering process is: heating from room temperature to 1600℃~ 2200°C, keep at 1500°C~2200°C for 1min~60min, cool to room temperature, heating rate is 10°C / min~30°C / min, cooling rate is 10°C / min~30°C / min, and the pressure is maintained at 10MPa~50MPa during sintering. Other steps are the same as those in Specific Embodiments 1 to 6.

[0033] Specific embodiment eight: The difference between this embodiment and specific embodiments one to seven is that the spark plasma sintering process is: heating from room temperature to 1600℃~ 2200℃, at 1600℃ ~2200 Keep warm at 1min~3 min, cooled to room temperature, the heating rate is 50℃ / min~150℃ / min, the cooling rate is 50℃ / min~150℃ / min, and the pressure is maintained at 10MPa~50MPa during the sintering process. Other steps are the same as those in specific embodiments 1 to 7.

[0034] Specific embodiment 9: This embodiment differs from specific embodiments 1 to 8 in that when the sintering atmosphere in step 3 is an inert gas, the inert gas is argon, helium or krypton. The other steps are the same as specific embodiments 1 to 8.

[0035] Specific Embodiment 10: This embodiment differs from Specific Embodiments 1 to 9 in that the sintering described in step 3 can be a multi-step sintering process; the multi-step sintering process is as follows: heating from room temperature to a temperature range of 1000°C to 1600°C, providing a holding period at 1000°C to 1600°C for 10 to 120 minutes at a pressure of 10 MPa to 100 MPa, then continuing to heat to 1600°C to 2200°C and holding for 30 to 300 minutes at a pressure of 10 MPa to 100 MPa. The other steps are the same as Specific Embodiments 1 to 9.

[0036] The following examples are used to verify the beneficial effects of the present invention:

[0037] Example 1: A method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material (Ta-3% Y2O3), comprising the following steps:

[0038] 1. Weighing ingredients:

[0039] Weighing tantalum powder and yttrium oxide powder according to a certain volume ratio to obtain a raw material;

[0040] The volume fraction of yttrium oxide powder in the raw material described in step 1 is 3%;

[0041] 2. Powder mixing:

[0042] After the tantalum powder and yttrium oxide powder weighed in step 1 are preliminarily mixed, they are subjected to all-round ball milling in a vacuum environment to achieve full and uniform mixing of the powders, and then sieved in an argon atmosphere through an 80-mesh sieve to obtain a uniformly mixed raw material;

[0043] The ball milling process in step 2 is as follows: a full-scale planetary ball mill is used, the ball-to-material ratio is 20:1, the speed of the ball mill is 200 r / min, the ball milling time is 24 h, and the ball mill jar and the grinding balls are both made of zirconia;

[0044] 3. Sintering:

[0045] The uniformly mixed raw materials obtained in step 2 are placed in a graphite mold and hot-pressed and sintered in an argon atmosphere to obtain a tantalum-based composite material reinforced with yttrium oxide particles (Ta-3% Y2O3);

[0046] The hot pressing sintering process is as follows: heating from room temperature to 2100°C, keeping at 2100°C for 60 minutes, cooling to room temperature, heating rate of 20°C / min, cooling rate of 20°C / min, and maintaining the pressure at 30MPa during the sintering process.

[0047] The yttrium oxide reinforced tantalum-based composite material prepared in Example 1 has uniform distribution of elements, a density of 98.64%, a hardness of 1.89 GPa, a tensile strength of 602 MPa, a yield strength of 477 MPa, and an elongation of 21.54%.

[0048] Example 2: A method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material (Ta-5% Y2O3), comprising the following steps:

[0049] 1. Weighing ingredients:

[0050] Weighing tantalum powder and yttrium oxide powder according to a certain volume ratio to obtain a raw material;

[0051] The volume fraction of yttrium oxide powder in the raw material described in step 1 is 5%;

[0052] 2. Powder mixing:

[0053] After the tantalum powder and yttrium oxide powder weighed in step 1 are preliminarily mixed, they are subjected to all-round ball milling in a vacuum environment to achieve full and uniform mixing of the powders, and then sieved in an argon atmosphere through an 80-mesh sieve to obtain a uniformly mixed raw material;

[0054] The ball milling process in step 2 is as follows: a full-scale planetary ball mill is used, the ball-to-material ratio is 20:1, the speed of the ball mill is 200 r / min, the ball milling time is 24 h, and the ball mill jar and the grinding balls are both made of zirconia;

[0055] 3. Sintering:

[0056] The uniformly mixed raw materials obtained in step 2 are placed in a graphite mold and hot-pressed and sintered in an argon atmosphere to obtain a tantalum-based composite material reinforced with yttrium oxide particles (Ta-5% Y2O3);

[0057] The hot pressing sintering process is as follows: heating from room temperature to 2100°C, keeping at 2100°C for 60 minutes, cooling to room temperature, heating rate of 20°C / min, cooling rate of 20°C / min, and maintaining the pressure at 30MPa during the sintering process.

[0058] The yttrium oxide reinforced tantalum-based composite material prepared in Example 2 has uniform distribution of elements, a density of 98.93%, a hardness of 1.54 GPa, a tensile strength of 475 MPa, a yield strength of 336 MPa, and an elongation of 23.33%.

[0059] Example 3: A method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material (Ta-7% Y2O3), comprising the following steps:

[0060] 1. Weighing ingredients:

[0061] Weighing tantalum powder and yttrium oxide powder according to a certain volume ratio to obtain a raw material;

[0062] The volume fraction of yttrium oxide powder in the raw material described in step 1 is 7%;

[0063] 2. Powder mixing:

[0064] After the tantalum powder and yttrium oxide powder weighed in step 1 are preliminarily mixed, they are subjected to all-round ball milling in a vacuum environment to achieve full and uniform mixing of the powders, and then sieved in an argon atmosphere through an 80-mesh sieve to obtain a uniformly mixed raw material;

[0065] The ball milling process in step 2 is as follows: a full-scale planetary ball mill is used, the ball-to-material ratio is 20:1, the speed of the ball mill is 200 r / min, the ball milling time is 24 h, and the ball mill jar and the grinding balls are both made of zirconia;

[0066] 3. Sintering:

[0067] The uniformly mixed raw materials obtained in step 2 are placed in a graphite mold and hot-pressed and sintered in an argon atmosphere to obtain a tantalum-based composite material reinforced with yttrium oxide particles (Ta-7% Y2O3);

[0068] The hot pressing sintering process is as follows: heating from room temperature to 2100°C, keeping at 2100°C for 60 minutes, cooling to room temperature, heating rate of 20°C / min, cooling rate of 20°C / min, and maintaining the pressure at 30MPa during the sintering process.

[0069] The yttrium oxide reinforced tantalum-based composite material prepared in Example 3 has uniform distribution of elements, a density of 99.01%, a hardness of 1.62 GPa, a tensile strength of 472 MPa, a yield strength of 337 MPa, and an elongation of 19.81%.

[0070] Example 4: A method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material (Ta-10% Y2O3), comprising the following steps:

[0071] 1. Weighing ingredients:

[0072] Weighing tantalum powder and yttrium oxide powder according to a certain volume ratio to obtain a raw material;

[0073] The volume fraction of yttrium oxide powder in the raw material described in step 1 is 10%;

[0074] 2. Powder mixing:

[0075] After the tantalum powder and yttrium oxide powder weighed in step 1 are preliminarily mixed, they are subjected to all-round ball milling in a vacuum environment to achieve full and uniform mixing of the powders, and then sieved in an argon atmosphere through an 80-mesh sieve to obtain a uniformly mixed raw material;

[0076] The ball milling process in step 2 is as follows: a full-scale planetary ball mill is used, the ball-to-material ratio is 20:1, the speed of the ball mill is 200 r / min, the ball milling time is 24 h, and the ball mill jar and the grinding balls are both made of zirconia;

[0077] 3. Sintering:

[0078] The uniformly mixed raw materials obtained in step 2 are placed in a graphite mold and hot-pressed and sintered in an argon atmosphere to obtain a tantalum-based composite material reinforced with yttrium oxide particles (Ta-10% Y2O3);

[0079] The hot pressing sintering process is as follows: heating from room temperature to 2100°C, keeping at 2100°C for 60 minutes, cooling to room temperature, heating rate of 20°C / min, cooling rate of 20°C / min, and maintaining the pressure at 30MPa during the sintering process.

[0080] The yttrium oxide reinforced tantalum-based composite material prepared in Example 4 has uniform distribution of elements, a density of 99.16%, a hardness of 1.71 GPa, a tensile strength of 441 MPa, a yield strength of 307 MPa, and an elongation of 12.58%.

[0081] Example 5: A method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material (Ta-15% Y2O3), comprising the following steps:

[0082] 1. Weighing ingredients:

[0083] Weighing tantalum powder and yttrium oxide powder according to a certain volume ratio to obtain a raw material;

[0084] The volume fraction of yttrium oxide powder in the raw material described in step 1 is 15%;

[0085] 2. Powder mixing:

[0086] After the tantalum powder and yttrium oxide powder weighed in step 1 are preliminarily mixed, they are subjected to all-round ball milling in a vacuum environment to achieve full and uniform mixing of the powders, and then sieved in an argon atmosphere through an 80-mesh sieve to obtain a uniformly mixed raw material;

[0087] The ball milling process in step 2 is as follows: a full-scale planetary ball mill is used, the ball-to-material ratio is 20:1, the speed of the ball mill is 200 r / min, the ball milling time is 24 h, and the ball mill jar and the grinding balls are both made of zirconia;

[0088] 3. Sintering:

[0089] The uniformly mixed raw materials obtained in step 2 are placed in a graphite mold and hot-pressed and sintered in an argon atmosphere to obtain a tantalum-based composite material reinforced with yttrium oxide particles (Ta-15% Y2O3);

[0090] The hot pressing sintering process is as follows: heating from room temperature to 2100°C, keeping at 2100°C for 60 minutes, cooling to room temperature, heating rate of 20°C / min, cooling rate of 20°C / min, and maintaining the pressure at 30MPa during the sintering process.

[0091] The yttrium oxide reinforced tantalum-based composite material prepared in Example 5 has uniform distribution of elements, a density of 99.38%, a hardness of 1.83 GPa, a tensile strength of 335 MPa, a yield strength of 295 MPa, and an elongation of 6.38.

[0092] Example 6: A method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material (Ta-20% Y2O3), comprising the following steps:

[0093] 1. Weighing ingredients:

[0094] Weighing tantalum powder and yttrium oxide powder according to a certain volume ratio to obtain a raw material;

[0095] The volume fraction of yttrium oxide powder in the raw material described in step 1 is 20%;

[0096] 2. Powder mixing:

[0097] After the tantalum powder and yttrium oxide powder weighed in step 1 are preliminarily mixed, they are subjected to all-round ball milling in a vacuum environment to achieve full and uniform mixing of the powders, and then sieved in an argon atmosphere through an 80-mesh sieve to obtain a uniformly mixed raw material;

[0098] The ball milling process in step 2 is as follows: a full-scale planetary ball mill is used, the ball-to-material ratio is 20:1, the speed of the ball mill is 200 r / min, the ball milling time is 24 h, and the ball mill jar and the grinding balls are both made of zirconia;

[0099] 3. Sintering:

[0100] The uniformly mixed raw materials obtained in step 2 are placed in a graphite mold and hot-pressed and sintered in an argon atmosphere to obtain a tantalum-based composite material reinforced with yttrium oxide particles (Ta-20% Y2O3);

[0101] The hot pressing sintering process is as follows: heating from room temperature to 2100°C, keeping at 2100°C for 60 minutes, cooling to room temperature, heating rate of 20°C / min, cooling rate of 20°C / min, and maintaining the pressure at 30MPa during the sintering process.

[0102] The yttrium oxide reinforced tantalum-based composite material prepared in Example 6 has uniform distribution of elements, a density of 99.06%, a hardness of 2.25 GPa, a tensile strength of 308 MPa, a yield strength of 239 MPa, and an elongation of 4.16%.

[0103] Example 7: A method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material (Ta-3% Y2O3), comprising the following steps:

[0104] 1. Weighing ingredients:

[0105] Weighing tantalum powder and yttrium oxide powder according to a certain volume ratio to obtain a raw material;

[0106] The volume fraction of yttrium oxide powder in the raw material described in step 1 is 3%;

[0107] 2. Powder mixing:

[0108] After the tantalum powder and yttrium oxide powder weighed in step 1 are preliminarily mixed, they are subjected to all-round ball milling in a vacuum environment to achieve full and uniform mixing of the powders, and then sieved in an argon atmosphere through an 80-mesh sieve to obtain a uniformly mixed raw material;

[0109] The ball milling process in step 2 is as follows: a full-scale planetary ball mill is used, the ball-to-material ratio is 20:1, the speed of the ball mill is 200 r / min, the ball milling time is 24 h, and the ball mill jar and the grinding balls are both made of zirconia;

[0110] 3. Sintering:

[0111] The uniformly mixed raw materials obtained in step 2 are placed in a graphite mold and hot-pressed and sintered in an argon atmosphere to obtain a tantalum-based composite material reinforced with yttrium oxide particles (Ta-3% Y2O3);

[0112] The hot pressing sintering process is as follows: heating from room temperature to 2000°C, keeping at 2000°C for 60 minutes, cooling to room temperature, heating rate of 20°C / min, cooling rate of 20°C / min, and maintaining the pressure at 30MPa during the sintering process.

[0113] The yttrium oxide reinforced tantalum-based composite material prepared in Example 7 has uniform distribution of elements, a density of 98.81%, a hardness of 1.81 GPa, a tensile strength of 516 MPa, a yield strength of 406 MPa, and an elongation of 22.67%.

[0114] Example 8: A method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material (Ta-3% Y2O3), comprising the following steps:

[0115] 1. Weighing ingredients:

[0116] Weighing tantalum powder and yttrium oxide powder according to a certain volume ratio to obtain a raw material;

[0117] The volume fraction of yttrium oxide powder in the raw material described in step 1 is 3%;

[0118] 2. Powder mixing:

[0119] After the tantalum powder and yttrium oxide powder weighed in step 1 are preliminarily mixed, they are subjected to all-round ball milling in a vacuum environment to achieve full and uniform mixing of the powders, and then sieved in an argon atmosphere through an 80-mesh sieve to obtain a uniformly mixed raw material;

[0120] The ball milling process in step 2 is as follows: a full-scale planetary ball mill is used, the ball-to-material ratio is 20:1, the speed of the ball mill is 200 r / min, the ball milling time is 24 h, and the ball mill jar and the grinding balls are both made of zirconia;

[0121] 3. Sintering:

[0122] The uniformly mixed raw materials obtained in step 2 are placed in a graphite mold and hot-pressed and sintered in an argon atmosphere to obtain a tantalum-based composite material reinforced with yttrium oxide particles (Ta-3% Y2O3);

[0123] The hot pressing sintering process is as follows: heating from room temperature to 1800°C, keeping at 1800°C for 60 minutes, cooling to room temperature, heating rate of 20°C / min, cooling rate of 20°C / min, and maintaining the pressure at 30MPa during the sintering process.

[0124] The yttrium oxide reinforced tantalum-based composite material prepared in Example 8 has uniform distribution of elements, a density of 98.03%, a hardness of 1.36 GPa, a tensile strength of 492 MPa, a yield strength of 384 MPa, and an elongation of 19.56%.

[0125] Example 9: A method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material (Ta-3% Y2O3), comprising the following steps:

[0126] 1. Weighing ingredients:

[0127] Weighing tantalum powder and yttrium oxide powder according to a certain volume ratio to obtain a raw material;

[0128] The volume fraction of yttrium oxide powder in the raw material described in step 1 is 3%;

[0129] 2. Powder mixing:

[0130] After the tantalum powder and yttrium oxide powder weighed in step 1 are preliminarily mixed, they are subjected to all-round ball milling in a vacuum environment to achieve full and uniform mixing of the powders, and then sieved in an argon atmosphere through an 80-mesh sieve to obtain a uniformly mixed raw material;

[0131] The ball milling process in step 2 is as follows: a full-scale planetary ball mill is used, the ball-to-material ratio is 20:1, the speed of the ball mill is 200 r / min, the ball milling time is 24 h, and the ball mill jar and the grinding balls are both made of zirconia;

[0132] 3. Sintering:

[0133] The uniformly mixed raw materials obtained in step 2 are placed in a graphite mold and hot-pressed and sintered in an argon atmosphere to obtain a tantalum-based composite material reinforced with yttrium oxide particles (Ta-3% Y2O3);

[0134] The hot pressing sintering process is as follows: heating from room temperature to 1600°C, keeping at 1600°C for 60 minutes, cooling to room temperature, heating rate of 20°C / min, cooling rate of 20°C / min, and maintaining the pressure at 30MPa during the sintering process.

[0135] The yttrium oxide reinforced tantalum-based composite material prepared in Example 9 has uniform distribution of elements, a density of 91.76%, a hardness of 1.18 GPa, a tensile strength of 301 MPa, a yield strength of 271 MPa, and an elongation of 2.2%.

[0136] Example 10: A method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material (Ta-3% Y2O3), comprising the following steps:

[0137] 1. Weighing ingredients:

[0138] Weighing tantalum powder and yttrium oxide powder according to a certain volume ratio to obtain a raw material;

[0139] The volume fraction of yttrium oxide powder in the raw material described in step 1 is 3%;

[0140] 2. Powder mixing:

[0141] After the tantalum powder and yttrium oxide powder weighed in step 1 are preliminarily mixed, they are subjected to all-round ball milling in a vacuum environment to achieve full and uniform mixing of the powders, and then sieved in an argon atmosphere through an 80-mesh sieve to obtain a uniformly mixed raw material;

[0142] The ball milling process in step 2 is as follows: using a full-scale planetary ball mill, a ball-to-material ratio of 10:1, a ball mill speed of 150 r / min, a ball milling time of 48 h, and the ball milling jar and grinding balls are made of zirconia;

[0143] 3. Sintering:

[0144] The uniformly mixed raw materials obtained in step 2 are placed in a graphite mold and hot-pressed and sintered in an argon atmosphere to obtain a tantalum-based composite material reinforced with yttrium oxide particles (Ta-3% Y2O3);

[0145] The hot pressing sintering process is as follows: heating from room temperature to 2100°C, keeping at 2100°C for 30 minutes, cooling to room temperature, heating rate of 30°C / min, cooling rate of 30°C / min, and maintaining the pressure at 50MPa during the sintering process.

[0146] The yttrium oxide reinforced tantalum-based composite material prepared in Example 10 has uniform distribution of elements, a density of 99.86%, a hardness of 1.95 GPa, a tensile strength of 605 MPa, a yield strength of 245 MPa, and an elongation of 21.87%.

[0147] Example 11: A method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material (Ta-1% Y2O3), comprising the following steps:

[0148] 1. Weighing ingredients:

[0149] Weighing tantalum powder and yttrium oxide powder according to a certain volume ratio to obtain a raw material;

[0150] The volume fraction of yttrium oxide powder in the raw material described in step 1 is 1%;

[0151] 2. Powder mixing:

[0152] After the tantalum powder and yttrium oxide powder weighed in step 1 are preliminarily mixed, they are subjected to all-round ball milling in a vacuum environment to achieve full and uniform mixing of the powders, and then sieved in an argon atmosphere through an 80-mesh sieve to obtain a uniformly mixed raw material;

[0153] The ball milling process in step 2 is as follows: using a full-scale planetary ball mill, a ball-to-material ratio of 10:1, a ball mill speed of 120 r / min, a ball milling time of 48 h, and the ball milling jar and grinding balls are made of zirconia;

[0154] 3. Sintering:

[0155] The uniformly mixed raw materials obtained in step 2 are placed in a graphite mold and hot-pressed and sintered in an argon atmosphere to obtain a tantalum-based composite material reinforced with yttrium oxide particles (Ta-1% Y2O3);

[0156] The hot pressing sintering process is as follows: heating from room temperature to 2100°C, keeping at 2100°C for 10 minutes, cooling to room temperature, heating rate of 100°C / min, cooling rate of 100°C / min, and maintaining the pressure at 50MPa during the sintering process.

[0157] The yttrium oxide reinforced tantalum-based composite material prepared in Example 11 has uniform distribution of elements, a density of 99.75%, a hardness of 1.75 GPa, a tensile strength of 595 MPa, a yield strength of 215 MPa, and an elongation of 25.16%.

[0158] Example 12: A method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material (Ta-2%Y2O3), comprising the following steps:

[0159] 1. Weighing ingredients:

[0160] Weighing tantalum powder and yttrium oxide powder according to a certain volume ratio to obtain a raw material;

[0161] The volume fraction of yttrium oxide powder in the raw material described in step 1 is 2%;

[0162] 2. Powder mixing:

[0163] After the tantalum powder and yttrium oxide powder weighed in step 1 are preliminarily mixed, they are subjected to all-round ball milling in a vacuum environment to achieve full and uniform mixing of the powders, and then sieved in an argon atmosphere through an 80-mesh sieve to obtain a uniformly mixed raw material;

[0164] The ball milling process in step 2 is as follows: using a full-scale planetary ball mill, a ball-to-material ratio of 10:1, a ball mill speed of 150 r / min, a ball milling time of 48 h, and the ball milling jar and grinding balls are made of zirconia;

[0165] 3. Sintering:

[0166] The uniformly mixed raw materials obtained in step 2 are placed in a graphite mold and hot-pressed and sintered in an argon atmosphere to obtain a tantalum-based composite material reinforced with yttrium oxide particles (Ta-2% Y2O3);

[0167] The hot pressing sintering process is as follows: heating from room temperature to 2200°C, keeping at 2200°C for 5 minutes, cooling to room temperature, heating rate of 100°C / min, cooling rate of 100°C / min, and maintaining the pressure at 50MPa during the sintering process.

[0168] The yttrium oxide reinforced tantalum-based composite material prepared in Example 12 has uniform distribution of elements, a density of 99.67%, a hardness of 1.72 GPa, a tensile strength of 618 MPa, a yield strength of 228 MPa, and an elongation of 26.74%.

[0169] Comparative Example 1: The preparation of pure tantalum material is carried out according to the following steps:

[0170] 1. Weigh the required powder:

[0171] Weigh tantalum powder to obtain raw materials;

[0172] 2. Mixing initial powder:

[0173] The tantalum powder weighed in step 1 is subjected to full-scale planetary ball milling in a vacuum environment, and sieved in an argon atmosphere to pass through an 80-mesh sieve;

[0174] The high-energy ball milling process parameters in step 2 are: ball-to-material ratio of 20:1, ball mill speed of 200 r / min, and ball milling time of 24 h;

[0175] 3. Sintering:

[0176] The powder obtained in step 2 is placed in a graphite mold and hot-pressed and sintered under argon protection to obtain the corresponding pure tantalum material, namely Ta;

[0177] The sintering process in step 3 is as follows: heating from room temperature to 2100°C, keeping the temperature at 2100°C for 10 min, then cooled to room temperature at a heating rate of 20 ℃ / min, the cooling rate is 20℃ / min, and the pressure is maintained at 30MPa during the sintering process.

[0178] The pure tantalum material prepared in Comparative Example 1 has a density of 99.82%, a hardness of 2.34 GPa, a tensile strength of 108 MPa, a yield strength of 108 MPa, and an elongation of 0.5%.

[0179] Figure 1 XRD patterns of tantalum-based composite materials reinforced with yttrium oxide particles having different volume fractions prepared in Comparative Example 1 and Examples 1 to 5;

[0180] from Figure 1It can be seen that the yttrium oxide reinforced tantalum-based composite material with the chemical formula Ta-3%Y2O3 prepared in Example 1 contains two phases, the main phase is tantalum and the second phase is yttrium oxide, and there is no impurity phase. This proves that the technical solution can obtain a yttrium oxide reinforced tantalum-based composite material of Ta-3%Y2O3, effectively avoiding the introduction of impurities and the generation of impurity phases.

[0181] Figure 2 These are SEM images of tantalum-based composite materials reinforced with yttrium oxide particles of different volume fractions prepared in Comparative Example 1 and Examples 1 to 5, where (a) is Ta prepared in Comparative Example 1, (b) is Ta-3% Y2O3 prepared in Example 1, (c) is Ta-5% Y2O3 prepared in Example 2, (d) is Ta-7% Y2O3 prepared in Example 3, (e) is Ta-10% Y2O3 prepared in Example 4, and (f) is Ta-15% Y2O3 prepared in Example 5.

[0182] from Figure 2 It can be seen that the yttrium oxide reinforced tantalum-based composite material with the chemical formula Ta-3%Y2O3 prepared in Example 1 has high density, uniform distribution of the second phase, and no obvious segregation.

Claims

1. A method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material, characterized in that The preparation method comprises the following steps:

1. Weighing ingredients: Weighing tantalum powder and yttrium oxide powder according to a certain volume ratio to obtain a raw material; The volume fraction of yttrium oxide powder in the raw material described in step 1 is 0.3% to 30%; 2. Powder mixing: After the tantalum powder and yttrium oxide powder weighed in step 1 are preliminarily mixed, they are subjected to all-round ball milling in an inert gas or vacuum environment to achieve full and uniform mixing of the powders, and are sieved in an inert gas environment through an 80-320 mesh sieve to obtain a uniformly mixed composite powder raw material; 3. Sintering: The uniformly mixed composite powder raw material obtained in step 2 is placed in a graphite mold and sintered in an inert gas or vacuum environment to obtain tantalum-based composite materials reinforced with yttrium oxide particles of different volume fractions.

2. The method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material according to claim 1, characterized in that The ball milling process described in step 2 is: using a full-scale planetary ball mill, the ball-to-material ratio is (5~20):1, the ball mill speed is 50r / min~500r / min, the ball milling time is 12h~48h, and the ball mill jar and grinding balls are both made of zirconia.

3. The method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material according to claim 1, characterized in that The ball milling process described in step 2 is: using a full-scale planetary ball mill, a ball-to-material ratio of 10:1, a ball mill speed of 300 r / min, a ball milling time of 24 h, and the ball mill jar and grinding balls are both made of zirconia.

4. The method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material according to claim 1, characterized in that The ball milling process described in step 2 is: using a full-scale planetary ball mill, a ball-to-material ratio of 5:1, a ball mill speed of 200 r / min, a ball milling time of 48 h, and the ball mill jar and grinding balls are both made of zirconia.

5. The method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material according to claim 1, characterized in that The sintering described in step three is hot pressing sintering.

6. The method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material according to claim 1, characterized in that The sintering in step three is spark plasma sintering.

7. The method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material according to claim 5, characterized in that The hot pressing sintering process is as follows: heating from room temperature to 1600°C~2200°C, keeping at 1500°C~2200°C for 1min~60min, cooling to room temperature, heating rate of 10°C / min~30°C / min, cooling rate of 10°C / min~30°C / min, and maintaining pressure of 10MPa~50MPa during sintering.

8. The method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material according to claim 6, characterized in that The spark plasma sintering process is as follows: heating from room temperature to 1600°C~2200°C, keeping the temperature at 1600°C~2200°C for 1min~3min, cooling to room temperature, the heating rate is 50°C / min~150°C / min, the cooling rate is 50°C / min~150°C / min, and the pressure is maintained at 10MPa~50MPa during the sintering process.

9. The method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material according to claim 1, characterized in that When the sintering atmosphere in step 3 is an inert gas, the inert gas is argon, helium or krypton.

10. The method for preparing a high tensile strength and high ductility yttrium oxide particle reinforced tantalum-based composite material according to claim 1, characterized in that The sintering described in step three can be a multi-step sintering process; the process of the multi-step sintering is: heating from room temperature to a temperature range of 1000℃~1600℃, setting a holding stage in the temperature range of 1000℃~1600℃, the holding time is 10min~120min, maintaining the pressure at 10MPa~100MPa, and then continuing to heat to 1600℃~2200℃, and keeping it for 30min~300min, maintaining the pressure at 10MPa~100MPa.

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