CN113652569B - Preparation method of gradient-enhanced titanium-based composite material - Google Patents
Preparation method of gradient-enhanced titanium-based composite material Download PDFInfo
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- CN113652569B CN113652569B CN202110961086.4A CN202110961086A CN113652569B CN 113652569 B CN113652569 B CN 113652569B CN 202110961086 A CN202110961086 A CN 202110961086A CN 113652569 B CN113652569 B CN 113652569B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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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
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
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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
- B22F3/20—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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
Abstract
The invention provides a preparation method of a gradient reinforced titanium-based composite material, which comprises the following steps: mixing titanium ball powder and TiB2Mixing alcohol, and carrying out low-energy ball milling in a ball milling tank with inert protective gas; drying the mixed powder subjected to ball milling in a vacuum drying furnace; carrying out gradient composite compaction on the mixed powder by using a hydraulic press; then welding the steel sheath cover to the top end of the steel sheath; putting the steel ingot into a high-temperature box for presintering, taking out the steel ingot, and placing the steel ingot in air for cooling to room temperature; and (3) placing the pre-sintered steel ingot in a high-temperature furnace for heat preservation, taking out the steel ingot and then rapidly extruding the steel ingot in an extruder to obtain an extrusion bar of the titanium-based composite material. The preparation method of the gradient reinforced titanium-based composite material provided by the invention can quickly prepare the gradient reinforced titanium-based composite material, eliminates the interface between the two composite materials, exerts the toughness advantage of the titanium alloy and the high temperature resistance and high strength advantages of the titanium-based composite material, and improves the heat resistance and the mechanical property.
Description
Technical Field
The invention belongs to the technical field of preparation of metal matrix composites, and particularly relates to a preparation method of a gradient reinforced titanium matrix composite.
Background
Titanium and titanium alloys have excellent comprehensive mechanical properties, and are highly valued and widely applied in the industries of aviation, aerospace, ships, petroleum, chemical engineering, weapons, electronics, biomedical and the like. However, the strength and heat resistance of titanium alloy are much lower than those of titanium-based composite materials, and the toughness of titanium-based composite materials is much lower than that of titanium alloy, so that titanium materials with strong external strength and tough internal strength are extremely needed in common application background. Therefore, it is necessary to continuously control the change of the internal composition and the fine structure, eliminate the interface between the two, make the titanium-based composite material strong in external strength and tough in internal strength, and improve the heat resistance and mechanical properties. Therefore, how to adopt a proper process to realize the technical requirement becomes a technical problem which needs to be solved urgently.
Disclosure of Invention
The invention aims to provide a preparation method of a gradient reinforced titanium-based composite material, which solves the technical problem of how to quickly prepare the gradient reinforced titanium-based composite material, eliminates an interface between the titanium alloy and the composite material, exerts the toughness of the titanium alloy and the high strength and high temperature resistance of the titanium-based composite material, and improves the heat resistance and the mechanical property.
A preparation method of a gradient reinforced titanium-based composite material comprises the following steps:
step S1: titanium ball powder (50-350 meshes) + TiB2Mixing (not more than 4 μm) and alcohol, and performing low-energy ball milling in a ball milling tank with inert protective gas;
step S2: drying the mixed powder subjected to ball milling in a vacuum drying furnace;
step S3: putting titanium ball powder into a detachable die, pressing the titanium ball powder into a compact by using a hydraulic press, taking out the pressed ball powder, putting the pressed ball powder into a No. 45 steel ladle sleeve, and overlapping the centers of the titanium ball powder and the 45 steel ladle sleeve;
step S4: placing the dried mixed powder into a space between the ball powder blank and the steel sheath, pressing the blank under the condition of maintaining the pressure of the central blank by using a combined type pressure head, welding a steel sheath cover to the top end of the steel sheath, and sealing the sheath;
step S5: putting the steel ingot into a high-temperature box for presintering, taking out the steel ingot, and placing the steel ingot in air for cooling to room temperature;
step S6: and (3) placing the pre-sintered steel ingot in a high-temperature furnace for heat preservation, taking out after a period of time, and quickly extruding in an extruder to obtain an extruded bar of the titanium-based composite material.
In the step S3, the detachable die is H25# steel, and is composed of an upper die 1 and a bottom die 2, the inner diameter of which is 30mm, the outer diameter of which is 40mm, and the height of which is 40mm, the x 40mm, and the x 10 mm; the inner diameter of the steel sheath is 39mm, and the height of the steel sheath is 45 mm.
In the step S4, the combined ram is composed of an inner ram 6 and an outer ram 7, the inner ram 6 is connected with the combined ram upper end cover 3 by a high-strength spring 4, the outer ram 7 is connected with the combined body 5 as a whole, the diameter of the inner ram 6 is 30mm, and the inner diameter of the outer ram 7 is 30mm and the outer diameter thereof is 39 mm.
In the step S5, the temperature of the high temperature chamber is 900-.
In the step S6, the extrusion direction distribution of the extrusion bar is studied along the whisker length direction under the action of the extruder, and the extrusion ratio of the extruder is 7-25.
The invention achieves the following remarkable effects:
(1) post-composite-green-compact TiB2TiB in the middle of the titanium alloy sphere and the mixed powder sphere at the particle distribution interface in the pre-sintering process2The B atoms in the titanium alloy powder can be diffused to the titanium balls of the mixed powder and the unmixed titanium alloy balls at the same time, the B atoms at the interface react with the Ti atoms to generate new-phase TiB, and the generated TiB grows into the titanium matrix to preliminarily eliminate the interface.
(2) In the extrusion process, TiB rotates towards the extrusion direction, the substrate flows towards the whisker, dislocation is accumulated, dynamic recrystallization is promoted, and the interface is eliminated finally.
(3) The composite material has strong external strength and internal toughness, has no interface, and the whiskers are distributed along the extrusion direction under the action of extrusion force, so that the external strength and the internal toughness of the composite material are improved, and the performance of the material is fully exerted.
(4) The heat resistance of the outer part of the bar is improved to be higher than that of the inner part by 100-150 ℃, and the high-temperature application range of the material is expanded.
Drawings
FIG. 1 is an organization chart of an interface disclosed in an embodiment of the invention.
Fig. 2 is a structural diagram of a detachable compact die according to an embodiment of the present invention.
Figure 3 is a combined drawing of the combined pressure head disclosed by the embodiment of the invention.
Detailed Description
In order to clearly illustrate the technical features of the present solution, the present solution is described below by way of specific embodiments.
A preparation method of a gradient reinforced titanium-based composite material comprises the following steps:
step S1: titanium ball powder (50-350 meshes) + TiB2Mixing (not more than 4 μm) and alcohol, and performing low-energy ball milling in a ball milling tank with inert protective gas;
step S2: drying the mixed powder subjected to ball milling in a vacuum drying furnace;
step S3: putting titanium ball powder into a detachable die, pressing the titanium ball powder into a blank by using a hydraulic press, taking out the ball powder after pressing the blank, putting the ball powder into a No. 45 steel ladle sleeve, and overlapping the centers of the ball powder and the steel ladle sleeve;
step S4: placing the dried mixed powder into a space between the ball powder blank and the steel sheath, pressing the blank under the condition of maintaining the pressure of the central blank by using a combined type pressure head, welding a steel sheath cover to the top end of the steel sheath, and sealing the sheath;
step S5: putting the steel ingot into a high-temperature box for presintering, taking out the steel ingot, and placing the steel ingot in air for cooling to room temperature;
step S6: and (3) placing the pre-sintered steel ingot in a high-temperature furnace for heat preservation, taking out after a period of time, and quickly extruding in an extruder to obtain an extruded bar of the titanium-based composite material.
In step S1, the rotation speed of ball milling is 50-300r/min, and the ball milling time is 4-10 h.
In step S3, the detachable die is H25# steel and consists of an upper die 1 with the inner diameter of 30mm, the outer diameter of 40mm and the height of 40mm and a steel plate with the bottom die 2 of 40mm multiplied by 10 mm; the inner diameter of the steel sheath is 39mm, and the height of the steel sheath is 45 mm.
In the step S4, the combined pressure head is composed of an inner pressure head 6 and an outer pressure head 7, the inner pressure head 6 is connected with the upper end cover 3 of the combined pressure head through a high-strength spring 4, the outer pressure head 7 is integrally connected with the combined pressure head body 5, the diameter of the inner pressure head 6 is 30mm, and the inner diameter and the outer diameter of the outer pressure head 7 are 30mm and 39 mm.
In step S5, post-compaction TiB2TiB in the middle of the titanium alloy sphere and the mixed powder sphere at the particle distribution interface in the pre-sintering process2B atoms in the titanium alloy powder can diffuse into titanium balls mixed with the powder and unmixed titanium alloy balls at the same time, the B atoms at the interface react with the Ti atoms to generate new-phase TiB, and the generated TiB is transformed into titanium baseIn vivo growth, and initial elimination of the interface.
In step S6, the TiB rotates towards the extrusion direction, dislocation is accumulated, dynamic recrystallization is promoted, and the matrix flows along with the rotation of the whisker, so that the interface problem is solved.
The technical features of the present invention which are not described in the above embodiments may be implemented by or using the prior art, and are not described herein again, of course, the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and variations, modifications, additions or substitutions which may be made by those skilled in the art within the spirit and scope of the present invention should also fall within the protection scope of the present invention.
Claims (4)
1. A preparation method of a gradient reinforced titanium-based composite material is characterized by comprising the following steps:
1) composite green compact
Titanium ball powder of 50 to 350 meshes and TiB with the grain diameter not more than 4 mu m2Mixing with alcohol, and performing low-energy ball milling in a ball milling tank with inert protective gas;
drying the mixed powder subjected to ball milling in a vacuum drying furnace;
putting titanium ball powder into a detachable die with the inner diameter of 30mm and the height of 40mm, and pressing the titanium ball powder into a blank by using a hydraulic press;
taking out the titanium ball powder after compacting, putting the titanium ball powder into a steel ladle sleeve with the inner diameter of 39mm and the height of 45mm, and overlapping the centers;
finally, placing the dried mixed powder into a space between the titanium ball powder blank and the steel sheath, and pressing the blank under the condition of maintaining the pressure of the central blank by using a combined type pressure head;
2) presintering and extruding
Placing the blank sheath welded with the upper cover into a high-temperature furnace for presintering, taking out and then placing into air for cooling;
and putting the pre-sintered blank into a high-temperature furnace with expected extrusion temperature for heat preservation, taking out the blank and putting the blank into a hydraulic extruder for extrusion to obtain the gradient-enhanced titanium-based composite material.
2. The method for preparing a gradient reinforced Ti-based composite material as claimed in claim 1, wherein in the step 1), the detachable mold is made of H25# steel and is composed of an upper mold with an inner diameter of 30mm, an outer diameter of 40mm and a height of 40mm and a steel plate with a bottom mold of 40mm x 10 mm.
3. The method for preparing a gradient reinforced titanium-based composite material as claimed in claim 1, wherein in the step 1), the combined pressing head is composed of an inner pressing head and an outer pressing head, the inner pressing head is connected with an upper end cover of the combined pressing head through a high-strength spring, the outer pressing head is integrally connected with the combined pressing head body, the diameter of the inner pressing head is 30mm, and the inner diameter and the outer diameter of the outer pressing head are 30mm and 39mm respectively.
4. The method as claimed in claim 1, wherein the pre-sintering temperature in the high temperature furnace in step 2) is 900-1200 ℃, and the pre-sintering time is 1-4 h.
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CN105234404A (en) * | 2015-11-06 | 2016-01-13 | 哈尔滨工业大学(威海) | Compound titanium powder and titanium-based composite material and preparation methods thereof |
CN108796264A (en) * | 2018-06-28 | 2018-11-13 | 北京理工大学 | A kind of preparation method of oriented alignment TiB whisker-reinforced titanium-based composite materials |
CN108796265A (en) * | 2018-06-28 | 2018-11-13 | 北京理工大学 | A kind of preparation method of TiB nanometers of enhancing titanium matrix composite |
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US20080029186A1 (en) * | 2006-02-14 | 2008-02-07 | Stanley Abkowitz | Homogeneous titanium tungsten alloys produced by powder metal technology |
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CN105234404A (en) * | 2015-11-06 | 2016-01-13 | 哈尔滨工业大学(威海) | Compound titanium powder and titanium-based composite material and preparation methods thereof |
CN108796264A (en) * | 2018-06-28 | 2018-11-13 | 北京理工大学 | A kind of preparation method of oriented alignment TiB whisker-reinforced titanium-based composite materials |
CN108796265A (en) * | 2018-06-28 | 2018-11-13 | 北京理工大学 | A kind of preparation method of TiB nanometers of enhancing titanium matrix composite |
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