CN110732665A - Preparation method of gradient titanium materials - Google Patents
Preparation method of gradient titanium materials Download PDFInfo
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- CN110732665A CN110732665A CN201911021724.3A CN201911021724A CN110732665A CN 110732665 A CN110732665 A CN 110732665A CN 201911021724 A CN201911021724 A CN 201911021724A CN 110732665 A CN110732665 A CN 110732665A
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000010936 titanium Substances 0.000 title claims abstract description 40
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000001125 extrusion Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000000748 compression moulding Methods 0.000 claims abstract description 8
- 238000000465 moulding Methods 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000004321 preservation Methods 0.000 claims abstract description 3
- 238000005242 forging Methods 0.000 claims description 8
- 238000001192 hot extrusion Methods 0.000 claims description 6
- 238000012545 processing Methods 0.000 abstract description 8
- 239000007769 metal material Substances 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 239000002344 surface layer Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910000746 Structural steel Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000009702 powder compression Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
- Forging (AREA)
Abstract
The invention discloses a preparation method of gradient titanium materials, which belongs to the technical field of metal material processing, the method comprises the steps of carrying out compression molding on titanium powder, carrying out vacuum sintering, heat preservation and cooling after molding, carrying out channel-changing extrusion molding at different temperatures respectively to obtain a gradient structure titanium material, carrying out rotary swaging on a titanium rod to process the gradient from the surface to the core, and effectively improving the hardness value after rotary swaging, wherein the hardness value of the prepared titanium material is changed along with the change of the distance from the surface to the core, and the invention forms the titanium into the gradient structure material by a simple preparation method, thereby having important value and application space in the fields of rapidly developing medical treatment, aerospace and the like.
Description
Technical Field
The invention relates to a preparation method of gradient titanium materials, belonging to the technical field of metal material processing.
Background
Titanium has many excellent comprehensive properties, i.e. 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, and 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 layers of firm oxide films with oxygen on the surface in an oxidizing atmosphere, and has strong corrosion resistance to atmosphere, seawater, soil and many chemical media), good technological properties and the like, thus being an ideal aerospace engineering structural material.
The surface mechanical grinding treatment (SMAT) is adopted to cause the surface of the material to generate severe plastic deformation so as to cause the crystal grains on the surface of the material to be obviously refined or the substructure to be changed, and a structure presenting gradient change from the surface layer to the center of the material is obtained.
Disclosure of Invention
The invention aims to provide a preparation method of gradient titanium materials, which comprises the following steps of performing powder compression molding, processing the titanium materials by variable channel extrusion to form a gradient from the surface layer to the center of a titanium rod, combining a rotary forging process to obtain the titanium rod, and finally changing the gradient from the rotary forging processing surface to the center of the titanium rod to effectively improve the hardness value, wherein the hardness value of the gradient-structure titanium material prepared by the invention is changed in a gradient manner from the surface to the center (namely, the gradient-structure titanium material gradually transits from the grain layer on the outermost surface to the grain layer on the subsurface and finally transits to the grain layer on the center), and the gradient-structure titanium material with high hardness value is obtained, and the preparation 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 room-temperature rotary forging on the titanium rod in the step (3) 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 now be described with reference to the drawings and the detailed description, but the scope of the invention is not limited to the description.
Example 1
The preparation method of titanium materials with high-hardness gradient structures 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 forging on the 20mm titanium rod in the step (4) to form a titanium rod with the diameter of 4.5mm, and carrying out 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
The preparation method of titanium materials with high-hardness gradient structures 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 forging on the 20mm titanium rod in the step (4) to form a titanium rod with the diameter of 4.5mm, and carrying out 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
The preparation method of titanium materials with high-hardness gradient structures 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 forging on the 20mm titanium rod in the step (4) to form a titanium rod with the diameter of 4.5mm, and carrying out 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 (5)
- The preparation method of the gradient titanium materials of 1 and 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) and (4) carrying out room-temperature rotary forging on the titanium rod in the step (3) to form a titanium rod with the diameter of 4.5 mm.
- 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.
- 4. The method for preparing a gradient titanium material according to claim 1, wherein: the vacuum sintering condition in the step (2) is 1250-1300 ℃, and the heat preservation time is 1-2 h.
- 5. The method for preparing a gradient titanium material according to claim 1, wherein: 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.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113941831A (en) * | 2021-09-23 | 2022-01-18 | 哈尔滨理工大学 | Method for rapidly preparing gradient titanium plate based on vacuum hot pressing process |
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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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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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US20110223053A1 (en) * | 2008-03-06 | 2011-09-15 | Commonwealth Scientific And Industrial Research Organisation | Manufacture of pipes |
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 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113941831A (en) * | 2021-09-23 | 2022-01-18 | 哈尔滨理工大学 | Method for rapidly preparing gradient titanium plate based on vacuum hot pressing process |
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