CN113588390A - Method for in-situ TiC generation in titanium-based micro part - Google Patents
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- CN113588390A CN113588390A CN202110804507.2A CN202110804507A CN113588390A CN 113588390 A CN113588390 A CN 113588390A CN 202110804507 A CN202110804507 A CN 202110804507A CN 113588390 A CN113588390 A CN 113588390A
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Abstract
The invention provides a method for generating TiC in situ in a titanium-based micro part, which relates to the technical field of composite materials, wherein a titanium-based blank 4 is placed in a conductive inner sleeve 3, a graphite male die 2 applies static load to the titanium-based blank 4 for contact extrusion, the graphite male die 2, the conductive inner sleeve 3 and the titanium-based blank 4 are communicated with a circuit between a first electrode 6 and a second electrode 1, high temperature is generated by utilizing current local concentration and contact resistance, carbon in the graphite male die 2 physically permeates into the titanium-based blank 4, and the carbon and the titanium-based blank 4 are subjected to chemical reaction under the action of the high temperature to synthesize TiC particles in situ. By controlling the heating rate, the heating temperature and the heat preservation time, the carburization depth and the reaction process of carbon and titanium base are controlled, and the generation and the distribution thickness of TiC are ensured. Solves the problem of complex TiC forming process on the surface of the matrix material or in the matrix in the prior art.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a method for in-situ TiC generation in a titanium-based micro part.
Background
Under the traction of high-performance requirements of micro-weaponry, reconnaissance equipment, 5G, smart homes, medical treatment and other high-integration equipment, the micro-electro-mechanical system is rapidly developed, and the reliability and durability of a micro-electro-mechanical element serving as a 'base stone' formed by the micro-electro-mechanical system directly determine the working performance of the micro-electro-mechanical system and whether the micro-electro-mechanical system can be widely applied. The performance of the micro-part is mainly determined by the characteristics of the material, wherein the titanium alloy, which is a light structural material, has excellent comprehensive properties, such as corrosion resistance, high and low temperature resistance, good biocompatibility, excellent mechanical properties and the like, so that the titanium alloy is often applied to extreme temperature environments (such as lunar exploration) and special fluid environments (such as ocean exploration and medical instruments) and the like.
However, the wear resistance of titanium alloy is poor, and the wear resistance is a key property of titanium alloy micro parts as moving parts, so that the application of the titanium alloy is limited. Forming TiC (titanium carbide) in titanium alloy is one of effective methods for improving the hardness of materials, and the methods for forming TiC in the prior art mainly include:
liu and Hei et al (patent publication No. CN112795914A) mix Ti powder, graphite powder and NiCrBSi alloy powder, mix the powder and water glass and stir to make paste, coat on the surface of die steel and carry on the induction cladding through the induction coil, prepare in situ autogenous TiC/NiCrBSi composite coating on the surface of die steel; pueraria Roger et al (patent publication No. CN101033535A) carburizes the surface of the titanium alloy hip joint ball head in a vacuum carburizing furnace; the hemp scale and the like (patent publication number: CN110157983B) are subjected to smelting, ingot casting, heating, rolling and heat treatment to obtain the complex phase structure wear-resistant steel with the structure of lath martensite and uniformly dispersed autogenous phase TiC; yangtze et al (patent publication No. CN112342419A) disclose a method for preparing TiC reinforced titanium-based composite material based on cross-linked modified sintered titanium hydride and the composite material prepared thereby. The TiC reinforcing phase can be formed on the surface of the base material or in the base in the mode, but the process is complex and long in time consumption, and the conventional process is difficult to apply due to the small size of the characteristic structure of the micro part.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for in-situ TiC generation in a titanium-based micro-part, which solves the problem that the TiC forming process on the surface of a matrix material or in a matrix is complex in the prior art.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
provides a method for in-situ TiC generation in a titanium-based micro part, which comprises the following steps:
s1, placing the titanium-based blank in a die cavity of a conductive inner sleeve, electrically connecting the conductive inner sleeve with a first electrode, electrically connecting a graphite male die with a second electrode, and contacting the action surface of the graphite male die with the surface A of the titanium-based blank;
s2, applying a constant load of 50-80N to the titanium-based blank through the graphite male die, and simultaneously electrifying the first electrode and the second electrode to heat the graphite male die to 1000-1300 ℃ at a heating rate of 15-40 ℃/S for 120-300S;
s3, air cooling to room temperature;
s4, turning over the titanium-based blank to enable the surface B of the titanium-based blank to be in contact with the action surface of the graphite male die, and repeating the step S2;
and S5, after the heat preservation is finished, extruding the titanium-based blank by the graphite male die at the speed of 0.003-0.008 mm/S, and extruding the titanium-based blank from a forming die below to form the titanium-based micro part.
Further, the diameter of the titanium-based blank is smaller than that of the action surface of the graphite male die.
Furthermore, the diameter of the titanium-based blank is 80-120 mu m smaller than that of the action surface of the graphite male die.
Further, the surface roughness Ra of the acting surface of the graphite male die and the A surface and the B surface of the titanium-based blank is more than 3.2.
Further, the conductivity of the conductive inner sleeve is smaller than that of the titanium-based blank.
Furthermore, the conductive inner sleeve is made of graphite.
Further, the resistance of the conductive inner sleeve is greater than that of the graphite male die.
Further, the titanium-based billet has a diameter of not more than 5mm and a thickness of not more than 4 mm.
Further, the extrusion ratio of the step S5 of extruding the titanium-based billet is greater than 6.5.
The principle of the method provided by the invention is that
Placing a titanium-based blank in a conductive inner sleeve, then applying a static load to the titanium-based blank by using a graphite male die which is conductive as well to perform contact extrusion, and simultaneously utilizing local current concentration and contact resistance to generate high temperature so that carbon in the graphite male die permeates into the titanium-based blank, and synthesizing the carbon and the titanium-based blank into TiC particles in situ under the action of the high temperature; the other side of the titanium-based billet is treated in the same manner as before by turning over the titanium-based billet to increase the depth of in-situ synthesis of TiC particles in the titanium-based billet.
The invention has the following beneficial effects:
1. the method provided by the invention has the advantages that the high temperature generated by local concentration of current and contact resistance is adopted to carburize the titanium-based material, carbon is subjected to chemical reaction in the titanium-based material to synthesize TiC particles in situ, the process is simple and easy to control, the cleaning is free of pollution, no subsequent treatment is needed, the process steps are saved, and the obtained titanium-based micro part is high in hardness and high in strength.
2. The forming and the carburizing of the titanium-based micro part are carried out synchronously without additional working procedures and operations, thereby greatly saving the cost and improving the productivity.
3. Because the temperature can reach 1000-1300 ℃, the volume of the titanium-based blank is small, and the carburization is to carburize the matrix of the titanium-based blank but not to carburize the surface of the material, the situation that the carburized layer is peeled off due to surface abrasion does not exist, so that the performance of the titanium-based micro part is more stable.
4. The whole set of the die used in the invention has simple and reasonable structure and few parts, and the internal forming die can be replaced randomly according to the processing shape, for example, the extrusion forming of the gear and shaft parts can be replaced by the forming die with the inner hole in the shape of a gear or a shaft correspondingly, the operation is convenient, and the technical requirement is low.
Drawings
Fig. 1 is a vertical sectional view of the entire set of molds used in the present invention.
FIG. 2 is a cross-sectional axial view of a titanium-based billet in accordance with the present invention.
FIG. 3 is the phase diagram of the in situ synthesis of TiC in a TC4 titanium-based micro-part in example 1.
Fig. 4 is a diagram illustrating detection of an element at F in fig. 3.
FIG. 5 is a phase diagram of gold after single-sided carburization of a TA2 titanium base billet in example 2.
FIG. 6 is a scanning electron micrograph of in situ synthesized TiC in TA2 titanium-based micro part in example 2.
Wherein, 1, a second electrode; 2. a graphite male die; 21. a convex portion; 3. a conductive inner sleeve; 31. a mold cavity; 4. a titanium-based billet; 5. forming a mold; 6. a first electrode.
Detailed Description
The embodiment of the invention solves the problem of complex TiC forming process on the surface of a matrix material or in a matrix in the prior art by providing a method for in-situ generating TiC in a titanium-based micro-part.
The general idea for solving the technical problems in the embodiment of the application is as follows:
the method comprises the steps of changing a male die in a die for extruding a titanium-based blank 4 in the prior art into a graphite male die 2, placing the titanium-based blank 4 in a conductive inner sleeve 3, applying static load to the titanium-based blank 4 by the graphite male die 2 for contact extrusion, communicating the graphite male die 2, the conductive inner sleeve 3 and the titanium-based blank 4 with a circuit between a first electrode 6 and a second electrode 1, utilizing local current concentration and contact resistance to generate high temperature, enabling carbon in the graphite male die 2 to physically permeate into the titanium-based blank 4, and enabling the carbon to chemically react with the titanium-based blank 4 under the action of the high temperature to synthesize TiC particles in situ. The other surfaces of the titanium-based blank 4 are treated by turning the titanium-based blank 4 in the same way so as to increase the depth of in-situ synthesis of TiC particles in the titanium-based blank 4, and the carburization depth and the reaction process of carbon and the titanium-based are controlled by controlling the heating rate, the heating temperature and the heat preservation time so as to ensure the generation and the distribution thickness of TiC.
For better understanding of the above technical solutions, the following detailed descriptions will be provided in conjunction with the drawings and the detailed description of the embodiments.
The whole set of mold structure used in this embodiment is as shown in fig. 1, the cavity 31 of the conductive inner sleeve 3 is a cylindrical cavity along the vertical direction, the top end of the cavity 31 is open, and is used for inserting the convex part 21 of the graphite male mold 2 and abutting against the titanium-based blank 4, and the end face of the convex part 21 is the active surface of the graphite male mold 2. At the bottom end of the cavity 31 is mounted a forming die 5, the titanium base billet 4, before being extruded, being generally cylindrical in shape, with an axial cross-section as shown in fig. 2. The titanium-based blank 4 is placed between the forming die 5 and the convex part 21, and a forming hole which penetrates through the forming die 5 along the axial direction is processed on the forming die, for example, the forming hole of the gear forming die is an internal gear hole. The bottom end of the conductive inner sleeve 3 and the top end of the graphite male die 2 are respectively and electrically connected with a first electrode 6 and a second electrode 6 of the gleeble 1500D thermal simulator, and electrical parameter regulation and control are carried out through the gleeble 1500D thermal simulator.
The method for in-situ generation of TiC in the titanium-based micro part comprises the following steps:
s1, placing the titanium-based blank 4 in the die cavity 31 of the conductive inner sleeve 3, electrically connecting the conductive inner sleeve 3 with the first electrode 6, electrically connecting the graphite male die 2 with the second electrode 1, and contacting the action surface of the graphite male die 2 with the surface A of the titanium-based blank 4.
S2, applying a vertical downward load to the graphite male die 2 by the thermal simulator, and transferring the vertical downward load to the titanium-based blank 4 through the graphite male die 2, wherein the load is a constant load of 50-80N, so that the graphite male die 2 is fully contacted with the titanium-based blank 4 due to extrusion.
Meanwhile, the first electrode 6 and the second electrode 1 are electrified, and the graphite male die 2 is heated to 1000-1300 ℃ at a heating rate of 15-40 ℃/s and is kept warm for 120-300 s by using alternating current of 20000-30000A at 3-5V. Under the action of high temperature, carbon on the graphite male die 2 permeates into the titanium-based blank 4, and along with the heat preservation process, the carbon gradually permeates and reacts with the titanium base to generate TiC (titanium carbide) in situ.
And S3, cutting off the power and cooling to room temperature after the heat preservation time is over.
S4, turning the titanium-based blank 4, enabling the B surface of the titanium-based blank 4 to be in contact with the action surface of the graphite male die 2, applying a constant load to the graphite male die for 250-80N, raising the temperature to 1000-1300 ℃ through a thermal simulation machine according to the heating rate of 15-40 ℃/S, preserving the temperature for 120-300S, enabling carbon to penetrate from the B surface, and then generating TiC with a certain thickness in the titanium-based blank 4 in situ, so that the distribution range of the TiC in the titanium-based blank 4 is up to more than 80%. In this embodiment, the A-side and the B-side are both end faces of the cylindrical titanium base material 4, as shown in FIG. 2.
And S5, after the heat preservation is finished, extruding the titanium-based blank 4 by the graphite male die 2 at the speed of 0.003-0.008 mm/S, and extruding and molding the titanium-based blank 4 from the lower molding die 5 to form the titanium-based micro part.
As a preferable scheme of the embodiment, the diameter of the titanium-based blank 4 is smaller than the diameter of the acting surface of the graphite male die 2, that is, the diameter of the titanium-based blank 4 is smaller than the diameter of the convex part 21, so that the convex part 21 can completely cover the a surface and the B surface of the titanium-based blank 4, carbon can be ensured to smoothly permeate into the titanium-based blank 4, and simultaneously the permeation depth and the breadth of the carbon are enlarged.
In a preferred embodiment of this embodiment, the diameter of the titanium base billet 4 is 80 to 120 μm smaller than the diameter of the active surface of the graphite male mold 2. By controlling the size of the action surface of the graphite male die 2, the structure of the die can be more compact, and meanwhile, the loss of graphite materials caused by high temperature and the waste of energy can be reduced.
In a preferred embodiment of the present invention, the surface roughness Ra of the active surface of the graphite male die 2 and the a-and B-surfaces of the titanium base billet 4 is greater than 3.2. The roughness Ra is more than 3.2, so that the sliding of a contact surface caused by uneven stress can be avoided when the graphite male die is loaded to extrude the titanium-based blank 4; meanwhile, a gap with the height of not less than 3.2 microns is formed between the graphite male die 2 and the titanium-based blank 4 through the roughness, so that the graphite has enough contact surface area with the blank 4 under the action of high temperature and enters the titanium-based blank under the driving of high temperature, thereby reducing the difficulty of carbon infiltration into the titanium-based blank and improving the carburization effect.
As a preferable aspect of the present embodiment, the electrical conductivity of the conductive inner sleeve 3 is smaller than that of the titanium base material 4. After the same time of electrification, the temperature of the conductive inner sleeve 3 is higher than that of the titanium-based blank 4, so that free carbon in the die cavity 31 can enter the titanium-based blank 4 under the action of temperature difference, and the carburization effect is improved.
As a preferable solution of this embodiment, the material of the conductive inner sleeve 3 may be other conductive metal materials, such as carbon steel; the conductive inner sleeve 3 may be made of graphite.
As a preferable scheme of the present embodiment, the resistance of the conductive inner sleeve 3 is greater than that of the graphite male die 2. The outer part of the conductive inner sleeve 3 is contacted with a working cavity of a thermal simulator, the temperature difference between the outer wall and the inner wall of the conductive inner sleeve is usually about 100 ℃, and the resistance of the conductive inner sleeve 3 is larger than that of the graphite male die 2, so that the graphite male die 2 has higher current density, and the carburization of the graphite male die 2 on the titanium-based blank 4 is facilitated.
As a preferable aspect of the present embodiment, the titanium base billet 4 has a diameter of not more than 5mm and a thickness of not more than 4 mm. The method in the embodiment has good effect on TiC in-situ generation of the titanium-based micro-part, but the effect is not ideal for the titanium-based micro-part with the diameter larger than 5mm and/or the thickness larger than 4 mm.
As a preferable aspect of the present embodiment, the extrusion ratio of the extruded titanium base billet 4 in step S5 is formed to be larger than 6.5. When the extrusion ratio is more than 6.5, the recrystallized grains of the titanium-based blank 4 in the extrusion process can be more refined, and the forming quality of the titanium-based micro part is improved.
Example 1, the surface A of a TC4 titanium-based blank 4 with the diameter of 4mm and the height of 3mm is contacted and electrified with the action surface of a graphite male die 2, the parameters of a thermal simulator are adjusted to heat to 1300 ℃ at the heating rate of 10 ℃/s, then the temperature is kept for 180s, and then the temperature is cooled to the room temperature; then the surface B of the titanium-based blank 4 is contacted with the action surface of the graphite male die 2, the thermal simulator is adjusted to the same parameters after being reassembled, the temperature is raised to 1300 ℃ at the heating rate of 10 ℃/s, and then the temperature is preserved for 180 s; the forming shaft hole of the forming die 5 is hollow cylindrical, the graphite male die 2 extrudes the titanium-based blank 4 at the speed of 0.005mm/s, the extrusion ratio is 6.5, and the process is finished when the extrusion stroke is 1.5 mm. Polishing and corroding the middle part of the axial length of the extrusion part, and finding that uniformly distributed TiC particles exist, wherein the average grain size of the TiC particles is 3.16 mu m as shown in a figure 3; and the distribution of the elements inside is shown in fig. 4.
Example 2, the A surface of a TA2 titanium-based blank 4 with the diameter of 5mm and the height of 2mm is contacted and electrified with the action surface of a graphite male die 2, the temperature is heated to 1200 ℃ at the heating rate of 30 ℃/s, then the temperature is preserved for 120s, and then the blank is air-cooled to the room temperature; then contacting the surface B of the titanium-based blank 4 with the action surface of the graphite male die 2, reassembling, heating to 1200 ℃ by the same parameters, and preserving heat for 120 s; and replacing the forming die 5 with a die with a forming shaft hole in an internal tooth shape, extruding the titanium-based blank by the graphite male die 2 at the speed of 0.008mm/s, wherein the extrusion ratio is 8, and the process is finished when the extrusion stroke is 1mm to obtain the titanium-based micro gear. From the metallographic phase diagram of the titanium base ingot after carburization on one side as shown in FIG. 5, it can be seen that the TiC particles are distributed at a thickness of 917 μm. The middle part of the axial length of the titanium-based micro gear is polished and corroded, and the existence of evenly distributed TiC particles is found through the observation of a scanning electron microscope, wherein the average particle size is 4.08 mu m, as shown in figure 6.
It should be apparent to those skilled in the art that while the preferred embodiments of the present invention have been described, additional variations and modifications in these embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention. It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the machine equivalent technology of the claims of the present invention, it is intended that the present invention also include such modifications and variations.
Claims (9)
1. A method for in-situ TiC generation in a titanium-based micro part is characterized by comprising the following steps:
s1, placing the titanium-based blank in a die cavity of a conductive inner sleeve, electrically connecting the conductive inner sleeve with a first electrode, electrically connecting a graphite male die with a second electrode, and contacting the action surface of the graphite male die with the surface A of the titanium-based blank;
s2, applying a constant load of 50-80N to the titanium-based blank through the graphite male die, and simultaneously electrifying the first electrode and the second electrode to heat the graphite male die to 1000-1300 ℃ at a heating rate of 15-40 ℃/S for 120-300S;
s3, air cooling to room temperature;
s4, turning over the titanium-based blank to enable the surface B of the titanium-based blank to be in contact with the action surface of the graphite male die, and repeating the step S2;
and S5, after the heat preservation is finished, extruding the titanium-based blank by the graphite male die at the speed of 0.003-0.008 mm/S, and extruding the titanium-based blank from a forming die below to form the titanium-based micro part.
2. A method of in situ TiC synthesis in a titanium-based micro part as claimed in claim 1, wherein the diameter of said titanium-based blank is smaller than the diameter of the active face of said graphite male die.
3. A method of in situ TiC synthesis in titanium-based micro-parts as claimed in claim 1 or 2, wherein the diameter of said titanium-based blank is 80-120 μm smaller than the diameter of the active face of said graphite male mold.
4. A method of in situ TiC synthesis in titanium-based micro-parts according to claim 1, characterized in that the surface roughness Ra of the active face of said graphite male die and of the a and B faces of said titanium-based blank is > 3.2.
5. The method of in situ TiC in titanium-based micro-parts of claim 1, wherein said inner conductive sleeve has an electrical conductivity less than that of said titanium-based blank.
6. The method of in-situ TiC in titanium-based micro-part of claim 1, wherein said inner conductive sleeve is made of graphite.
7. The method of in situ TiC in titanium-based micro-parts of claim 1, wherein said inner conductive sleeve has a resistance greater than that of said male graphite mold.
8. The method of in situ TiC in a titanium-based micro-part of claim 1, wherein said titanium-based billet has a diameter no greater than 5mm and a thickness no greater than 4 mm.
9. The method of in situ TiC in titanium-based micro-parts of claim 1, wherein said step S5 extrudes a titanium-based billet to form an extrusion ratio greater than 6.5.
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| JP2012238733A (en) * | 2011-05-12 | 2012-12-06 | Thermo Graphitics Co Ltd | Anisotropic thermally-conductive element and manufacturing method thereof |
| CN103447530A (en) * | 2013-08-27 | 2013-12-18 | 四川大学 | Method for preparing pure titanium miniature parts on basis of multi-physical-field activated sintering |
| CN103862049A (en) * | 2014-04-02 | 2014-06-18 | 四川大学 | Ni-Ti porous material mini-sized part and sintering method thereof |
| CN103865496A (en) * | 2012-12-14 | 2014-06-18 | 深圳市纳宇材料技术有限公司 | Electricity-insulation heat-conduction powder and material, and preparation methods thereof |
| CN111672925A (en) * | 2020-07-21 | 2020-09-18 | 四川大学 | Electric field assisted titanium alloy micro-gear extrusion forming die and method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012238733A (en) * | 2011-05-12 | 2012-12-06 | Thermo Graphitics Co Ltd | Anisotropic thermally-conductive element and manufacturing method thereof |
| CN103865496A (en) * | 2012-12-14 | 2014-06-18 | 深圳市纳宇材料技术有限公司 | Electricity-insulation heat-conduction powder and material, and preparation methods thereof |
| CN103447530A (en) * | 2013-08-27 | 2013-12-18 | 四川大学 | Method for preparing pure titanium miniature parts on basis of multi-physical-field activated sintering |
| CN103862049A (en) * | 2014-04-02 | 2014-06-18 | 四川大学 | Ni-Ti porous material mini-sized part and sintering method thereof |
| CN111672925A (en) * | 2020-07-21 | 2020-09-18 | 四川大学 | Electric field assisted titanium alloy micro-gear extrusion forming die and method thereof |
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