CN110732665B - Preparation method of gradient titanium material - Google Patents

Preparation method of gradient titanium material Download PDF

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CN110732665B
CN110732665B CN201911021724.3A CN201911021724A CN110732665B CN 110732665 B CN110732665 B CN 110732665B CN 201911021724 A CN201911021724 A CN 201911021724A CN 110732665 B CN110732665 B CN 110732665B
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titanium
gradient
carrying
extrusion
hardness
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CN110732665A (en
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高洪亮
朱心昆
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Kunming University of Science and Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • 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
    • 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
    • B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
    • 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
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • 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
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • B22F2003/208—Warm or hot extruding
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps

Abstract

The invention discloses a preparation method of a gradient titanium material, and belongs to the technical field of metal material processing. The method comprises the steps of firstly, carrying out compression molding on titanium powder, and carrying out vacuum sintering, heat preservation and cooling after molding; and then respectively carrying out variable-channel extrusion forming at different temperatures to obtain a gradient-structure titanium material, and finally changing the gradient from the rotary swaging processing surface of the titanium rod to the center of the titanium rod, so that the hardness value is effectively improved through rotary swaging processing. The hardness curve shows that the hardness value of the titanium material prepared by the method changes along with the change of the distance from the surface to the core; the titanium is formed into the gradient structure material by the simple preparation method, and the titanium gradient structure material has important value and application space in the fields of rapidly developed medical treatment, aerospace and the like.

Description

Preparation method of gradient titanium material
Technical Field
The invention relates to a preparation method of a gradient titanium material, belonging to the technical field of metal material processing.
Background
Titanium has a number of excellent combinations of properties: the titanium alloy has the advantages of low density, high melting point (the melting point of titanium is 1668 ℃, slightly higher than that of iron and nickel, and higher than that of aluminum and magnesium by more than 1000 ℃), high specific strength (the strength is equivalent to or higher than that of common structural steel, and the specific strength of titanium is the highest in metal structural materials), good corrosion resistance (titanium forms a firm oxide film with oxygen on the surface in an oxidizing atmosphere, and has strong corrosion resistance on atmosphere, seawater, soil and a plurality of chemical media), good process performance and the like, and is an ideal structural material for aerospace engineering. Titanium has small heat conductivity and no magnetism, and some titanium alloys also have the functions of superconductivity, memory performance, hydrogen storage performance and the like. Meanwhile, the demand growth point of the high-tech industries such as computers on titanium is emerging continuously, and the continuous development of the titanium field is promoted.
The existing preparation method of the gradient structure material comprises the following steps: the mechanical grinding treatment (SMAT) of the surface causes severe plastic deformation of the material surface, thereby causing obvious refinement of the crystal grains or change of the substructure of the material surface. The structure which shows gradient change from the surface layer to the core part of the material is obtained. The SMAT method is used for preparing a gradient sample, and multidirectional plastic deformation occurs on the surface of the sample when a bullet impacts the surface of a material. The surface mechanical rolling technology (SMGT) is a plastic deformation technology which adopts a spherical rolling head to press into the surface layer of a material to be processed for grinding or rolling to generate large shearing deformation on the surface layer of the material to generate grain refinement and form a gradient nano structure. SMAT has the disadvantages that columnar metal cannot be processed, SMGT has the disadvantages that the processing period is long and the processing cannot be fast and massively carried out; these disadvantages limit the mass production and use of the materials.
Disclosure of Invention
The invention aims to provide a preparation method of a gradient titanium material, which comprises the steps of carrying out powder compression molding, processing the titanium material through variable-channel extrusion to form a gradient from a surface layer to a center part of a titanium rod, and carrying out treatment by combining a rotary forging process to obtain the titanium rod; finally, the gradient from the rotary swaging processing surface of the titanium rod to the center part is changed, and the hardness value is effectively improved; the gradient structure titanium material prepared by the invention has gradient hardness value change from the surface to the core (namely, the grain layer which is gradually transited from the outermost surface to the sub-surface is transited to the core layer finally), and the gradient structure titanium material with high hardness value is obtained, and the method specifically comprises the following steps:
(1) carrying out compression molding on titanium powder to obtain a block material;
(2) carrying out vacuum sintering on the block obtained in the step (1), and then cooling to room temperature under a gas protection device;
(3) carrying out hot extrusion molding on the titanium sample obtained in the step (2) by using a variable channel extrusion method to form a titanium rod with the diameter of 20 mm;
(4) and (4) carrying out rotary swaging on the titanium rod in the step (3) at room temperature to form a titanium rod with the diameter of 4.5 mm.
Preferably, in the step (1) of the invention, the purity of the titanium powder is more than or equal to 99.6%, and the granularity is-150 to-250 meshes.
Preferably, the extrusion force of the compression molding in the step (1) is 300-500 MPa.
Preferably, the vacuum sintering condition in the step (2) is 1250-1300 ℃, the heat preservation time is 1-2 h, and the temperature rising speed is 10 ℃/min.
Preferably, the hot extrusion molding conditions of the variable channel extrusion method in step (3) of the present invention are as follows: the extrusion temperature is 600-700 ℃, the temperature rise speed is 150-180 ℃/min, and the extrusion ratio is 8: 1-9: 1.
The rotary swaging equipment disclosed by the invention is a conventional process.
The invention has the beneficial effects that:
(1) the method combines a variable channel extrusion technology with rotary forging to prepare a gradient structure material with a hardness value from high to low from a surface layer to a core part, so as to obtain a gradient titanium material with high strength; the method has the advantages of low cost, simple processing technology, easy production and stable product quality.
(2) The invention obtains the titanium material with high strength gradient by controlling the hot pressing temperature and the processing method, which is more than 2 times of the annealed titanium.
Drawings
FIG. 1 is a graph of Vickers hardness of a gradient titanium material prepared by channel-variable extrusion at different temperatures according to examples 1 and 2 of the present invention.
FIG. 2 shows the Vickers hardness of the gradient titanium material obtained by the swaging process of the gradient titanium material according to the embodiment of the present invention.
Detailed Description
The invention will be further described with reference to the drawings and the detailed description, but the scope of the invention is not limited thereto.
Example 1
A preparation method of a high-hardness gradient structure titanium material specifically comprises the following steps:
(1) controlling the granularity of titanium powder (with the purity of 99.6 percent), sieving the titanium powder on a-200-mesh sieve, and taking undersize for later use.
(2) And (2) performing compression molding (400 MPa) on the titanium powder obtained in the step (1) to form a block body with the diameter of 60mm (the density is 85%).
(3) And (3) sintering the block obtained in the step (2) in vacuum at 1300 ℃, preserving heat for 1.5h, and then cooling to room temperature (the density is 93%) under a gas protection device.
(4) Performing thermal extrusion molding (600 ℃) on the titanium sample obtained in the step (3) by using a variable channel extrusion method to form a titanium rod with the diameter of 20mm, performing hardness experiment test at the temperature rising speed of 150 ℃/min and the extrusion ratio of 8: 1; the hardness value of the titanium material can reach 2630MPa, the thickness of the gradient layer is about 150 mu m, the hardness value of the core part is 2100MPa, and the titanium material has obvious gradient difference and can obviously improve the surface hardness.
(5) And (4) carrying out room temperature rotary swaging on the titanium rod with the diameter of 4.5mm in the step (4) to form a titanium rod with the diameter of 4.5mm, and carrying out a hardness experiment test.
The hardness value of the gradient titanium material prepared by the embodiment can reach about 3100MPa in the range of 0-600 μm, and then the hardness value is reduced to 2700MPa in the range of 600-1400 μm, and the hardness value of the core part is 3100 MPa. The method has obvious gradient change, the hardness value is reduced and improved from high, the method has the gradient structural characteristic, and the hardness value from the surface to the core is obviously improved after the rotary swaging processing.
Example 2
A preparation method of a high-hardness gradient structure titanium material specifically comprises the following steps:
(1) controlling the granularity of titanium powder (with the purity of 99.7 percent), screening the titanium powder on a-200-mesh screen, and taking undersize for later use.
(2) And (2) carrying out compression molding on the titanium powder obtained in the step (1) to form a block body with the diameter of 60mm (the density is 85%).
(3) And (3) sintering the block obtained in the step (2) in vacuum at 1300 ℃, preserving heat for 2 hours, and then cooling to room temperature under a gas protection device.
(4) And (3) performing hardness test on the titanium sample obtained in the step (3) by using a variable channel extrusion method to perform hot extrusion molding (700 ℃) to form a titanium rod with the diameter of 20mm, wherein the temperature rise speed is 180 ℃/min, the extrusion ratio is 9:1, and the hardness value of the gradient titanium material can reach 2700MPa, the thickness of the gradient layer is about 150 mu m, the hardness value of the core part is 2100MPa, so that the obvious gradient difference is realized, and the surface hardness can be obviously improved.
(5) And (4) carrying out room temperature rotary swaging on the titanium rod with the diameter of 4.5mm in the step (4) to form a titanium rod with the diameter of 4.5mm, and carrying out a hardness experiment test.
The hardness value of the gradient titanium material prepared by the embodiment can reach about 3150MPa in the range of 0 mu m to 600 mu m, and then the hardness value is reduced to 2800MPa in the range of 600 mu m to 1400 mu m, and the hardness value of the center is 3100 MPa. The method has obvious gradient change, the hardness value is reduced and improved from high, the method has the gradient structural characteristic, and the hardness value from the surface to the core is obviously improved after the rotary swaging processing.
Example 3
A preparation method of a high-hardness gradient structure titanium material specifically comprises the following steps:
(1) controlling the granularity of titanium powder (with the purity of 99.7 percent), screening the titanium powder on a-200-mesh screen, and taking undersize for later use.
(2) And (2) carrying out compression molding on the titanium powder obtained in the step (1) to form a block body with the diameter of 60mm (the density is 85%).
(3) And (3) sintering the block obtained in the step (2) in vacuum at 1250 ℃, preserving heat for 1h, and then cooling to room temperature under a gas protection device.
(4) And (3) performing a hardness experiment test on the titanium sample obtained in the step (3) by using a variable channel extrusion method to perform hot extrusion molding (650 ℃) to form a titanium rod with the diameter of 20mm, wherein the temperature rise speed is 170 ℃/min, and the extrusion ratio is 9: 1.
(5) And (4) carrying out room temperature rotary swaging on the titanium rod with the diameter of 4.5mm in the step (4) to form a titanium rod with the diameter of 4.5mm, and carrying out a hardness experiment test.
The hardness value of the gradient titanium material prepared by the embodiment can reach about 3000MPa in the range of 0-600 μm, and then the hardness value is reduced to 2800MPa in the range of 600-1400 μm, and the hardness value of the center is 3000 MPa. The hardness value is obviously improved from the high degree, and the surface hardness value to the center after the rotary swaging processing is obviously improved, as shown in figure 2.

Claims (3)

1. The preparation method of the gradient titanium material is characterized by comprising the following steps:
(1) carrying out compression molding on titanium powder to obtain a block material;
(2) carrying out vacuum sintering on the block obtained in the step (1), and then cooling to room temperature under a gas protection device;
(3) carrying out hot extrusion molding on the titanium sample obtained in the step (2) by using a variable channel extrusion method to form a titanium rod with the diameter of 20 mm;
(4) performing room-temperature rotary swaging on the titanium rod in the step (3) to form a titanium rod with the diameter of 4.5 mm;
the vacuum sintering condition in the step (2) is 1250-1300 ℃, and the heat preservation time is 1-2 h;
the hot extrusion molding conditions of the variable channel extrusion method in the step (3) are as follows: the extrusion temperature is 600-700 ℃, the temperature rise speed is 150-180 ℃/min, and the extrusion ratio is 8: 1-9: 1.
2. The method for preparing a gradient titanium material according to claim 1, wherein: in the step (1), the purity of the titanium powder is more than or equal to 99.6 percent, and the granularity is-150 to-250 meshes.
3. The method for preparing a gradient titanium material according to claim 1, wherein: the extrusion force of the compression molding in the step (1) is 300-500 MPa.
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Citations (3)

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Publication number Priority date Publication date Assignee Title
CN105302955A (en) * 2015-10-22 2016-02-03 上海理工大学 Hardness and hardness distribution design method for rotary swaged shaft of sedan
CN105483419A (en) * 2016-01-25 2016-04-13 江西省科学院应用物理研究所 Preparation method of high-strength and high-conductivity aluminum oxide dispersion-strengthened copper-based composite
CN107881447A (en) * 2017-11-22 2018-04-06 四川大学 Pure titanium of a kind of thread crystal grain of high-strength tenacity and preparation method thereof

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US20110223053A1 (en) * 2008-03-06 2011-09-15 Commonwealth Scientific And Industrial Research Organisation Manufacture of pipes

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105302955A (en) * 2015-10-22 2016-02-03 上海理工大学 Hardness and hardness distribution design method for rotary swaged shaft of sedan
CN105483419A (en) * 2016-01-25 2016-04-13 江西省科学院应用物理研究所 Preparation method of high-strength and high-conductivity aluminum oxide dispersion-strengthened copper-based composite
CN107881447A (en) * 2017-11-22 2018-04-06 四川大学 Pure titanium of a kind of thread crystal grain of high-strength tenacity and preparation method thereof

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