CN114411013B - Self-lubricating wear-resistant titanium-based composite material part and preparation method thereof - Google Patents
Self-lubricating wear-resistant titanium-based composite material part and preparation method thereof Download PDFInfo
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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
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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
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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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
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- 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
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0089—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with other, not previously mentioned inorganic compounds as the main non-metallic constituent, e.g. sulfides, glass
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention provides a self-lubricating wear-resistant titanium-based composite material part and a preparation method thereof, wherein the part has the structure of an alpha-Ti matrix phase of TC4, a reinforcing phase and a self-lubricating phase which are dispersedly distributed around the matrix phase; wherein the reinforcing phase is SiC particles, and the self-lubricating phase is MoS 2 Granules, WS 2 At least one of particles; and TiC particles are dispersed around the matrix phase; the friction coefficient of the product is 0.15-0.40, and the hardness is 580-950 HV. The reinforcing phase and the self-lubricating phase of the self-lubricating wear-resistant titanium-based composite material part are uniformly dispersed and distributed around the matrix phase, and the self-lubricating wear-resistant titanium-based composite material part has the advantages of fine crystal grains, high compactness, high hardness, good mechanical property, low friction coefficient, small abrasion loss, low abrasion rate and excellent wear resistance.
Description
Technical Field
The invention relates to the technical field of new material design and preparation, in particular to a self-lubricating wear-resistant titanium-based composite material part and a preparation method thereof.
Background
Titanium and its alloy are light and high-strength materials, and their density is 4507kg/m 3 ) Second only to magnesium alloys (1738 kg/m) 3 ) With aluminium alloy (2700 kg/m) 3 ) Lower than that of steel (7874 kg/m) 3 ) Copper alloy (8920 kg/m) 3 ) Tungsten alloy (19250 kg/m) 3 ) The parts with the same size are smaller in mass and higher in strength than magnesium alloy and aluminum alloy. The hardness and the toughness of the titanium and the alloy thereof are higher than those of the magnesium alloy and the aluminum alloy. The thermal expansion coefficient of titanium and the alloy thereof is low and far lower than that of materials such as steel, copper alloy, aluminum alloy and the like, and the prepared parts have high dimensional accuracy and small dimensional variable quantity under large temperature difference. And the titanium alloy have strong non-magnetism, fatigue performance and radiation resistance. In conclusion, the titanium and the alloy thereof have excellent comprehensive performance except the performances such as hardness, wear resistance and the like,therefore, the material has outstanding competitiveness in the aspects of aerospace, biomedical and advanced engineering materials. Research on powder metallurgy titanium alloy methods at home and abroad for many years shows that the titanium and the parts made of the titanium alloy by the powder metallurgy method not only have wide application prospects in aerospace and automobile industries, but also can be used for preparing various-purpose formed parts by adopting titanium and titanium alloy powder and are widely applied to various industrial departments such as food, chemical industry, medicine and the like. However, titanium and its alloy have low hardness and poor wear resistance, and its parts are easily worn in the use process, which further causes the instability of the engagement of the parts and further causes the rattling and even shaking of the instruments and equipment.
With the research and development of new material technology, the defects of titanium and alloy materials thereof can be made up by adopting a mode of doping various materials, and the structure of the titanium and alloy materials can be further improved, and the strength and other properties can be optimized. For example, the friction coefficient of the titanium alloy in contact with other materials can be reduced by adding a self-lubricating material into a titanium alloy matrix, the abrasion volume and the abrasion rate can be reduced, and the abrasion resistance of the material is increased. However, since the decomposition temperature of the added self-lubricating material is lower than the sintering temperature, the self-lubricating material decomposes in the sintering process of powder metallurgy, and the temperature rise time and the heat preservation time of the adopted atmosphere sintering or vacuum sintering are long, the self-lubricating material cannot maintain the stability of the chemical structure and further decomposes to lose the self-lubricating effect in the process, even substances which change the material structure and reduce the material performance may be introduced into the base material due to the decomposition of the added self-lubricating material, so that the structure and the performance of the base material are further deteriorated, and the doping of the composite material in the base material loses the gain effect.
Disclosure of Invention
In order to solve the technical problems of poor performances of hardness, wear resistance and the like of a titanium material and the decomposition of a self-lubricating material with a two-dimensional structure at high temperature in the prior art, the invention mainly aims to provide a self-lubricating wear-resistant titanium-based composite material part and a preparation method thereof.
To achieve the above objects, according to a first aspect of the present invention, there is provided a self-lubricating wear-resistant titanium-based composite article.
The structure of the self-lubricating wear-resistant titanium-based composite material part is an alpha-Ti matrix phase of TC4, and a reinforcing phase and a self-lubricating phase which are dispersedly distributed around the matrix phase; wherein, the first and the second end of the pipe are connected with each other,
the reinforced phase is SiC, and the self-lubricating phase is MoS 2 、WS 2 At least one of; and TiC is dispersed around the matrix phase;
the friction coefficient of the product is 0.15-0.40, and the hardness is 580-950 HV.
Furthermore, the abrasion volume of the workpiece is less than or equal to 0.079mm 3 The wear rate is 1.2X 10 -12 ～2.4×10 -12 m 3 The grinding crack width is 340-700 mu m.
Furthermore, the density of the product is more than or equal to 99.0 percent, the tensile strength is 700-800 MPa, the specified plastic elongation strength is 620-660 MPa, the elongation after fracture is 3.0-5.0 percent, and the reduction of area is 3.0-6.0 percent.
Furthermore, the friction coefficient of the product is 0.22, the hardness is 945HV, and the abrasion volume is less than or equal to 0.047mm 3 The wear rate is 1.39X 10 -12 m 3 N · m, grinding crack width 349.9 μm, density 99.5%, tensile strength 763MPa, specified plastic elongation 648MPa, elongation after fracture 4.2%, and reduction of area 5.4%.
Further, the work piece organization comprises: 75.0 to 97.0 mass% of an alpha-Ti matrix phase, 1.0 to 7.0 mass% of a SiC reinforcing phase, 1.5 to 14.0 mass% of a self-lubricating phase and 0.5 to 4.0 mass% of TiC.
In order to achieve the above object, according to a second aspect of the present invention, there is provided a method for preparing a self-lubricating wear-resistant titanium-based composite article.
The method for preparing the self-lubricating wear-resistant titanium-based composite material part comprises the following steps:
forming a protective film on the surface of the self-lubricating phase powder, mixing the protective film with TC4 powder and SiC powder, and then sequentially carrying out cold isostatic pressing and vacuum sintering to obtain the self-lubricating wear-resistant titanium-based composite material part; wherein, the first and the second end of the pipe are connected with each other,
the protective film is an organic film or a carbon film, the organic film is formed by a coupling agent coating method, and the carbon film is formed by a hydrothermal carbonization and emulsion template method;
the self-lubricating phase powder is MoS 2 Powder, WS 2 At least one of the powders.
Further, the raw material powder of the workpiece comprises the following components in percentage by mass: 79.0 to 97.0% of TC4 powder, 1.0 to 7.0% of SiC powder and 2.0 to 14.0% of self-lubricating phase powder.
Further, the raw material powder of the workpiece comprises the following components in percentage by mass: 79.0-90.0%, 5.0-7.0%, siC powder and 5.0-14.0% self-lubricating phase powder.
Further, a coupling agent in the coupling agent coating method adopts a silane coupling agent or a titanate coupling agent; the mass ratio of the coupling agent to the self-lubricating phase powder is 0.01-0.5: 1.
further, the mass ratio of the coupling agent to the self-lubricating phase powder is 0.1-0.5: 1.
further, in the hydrothermal carbonization and emulsion template method, a carbon source and the self-lubricating phase powder are used as raw materials, and octylamine is used as an additive; the mass ratio of the self-lubricating phase powder to the carbon source is 0.01-0.2: 1, the mass ratio of the octylamine to the carbon source is 0.05-1: 1; the carbon source is at least one of starch, glucose, citric acid and maltose.
Further, the mass ratio of the self-lubricating phase powder to the carbon source is 0.1-0.2: 1, the mass ratio of the octylamine to the carbon source is 0.5-1: 1.
further, the pressing parameters of the cold isostatic pressing are as follows: the oil pressure is 200-300 MPa, and the pressure maintaining time is 2-10 min.
Further, the process conditions of the vacuum sintering are as follows: heating at a rate of 10-20 deg.C/min, and calciningThe junction temperature is 1100-1300 ℃, the vacuum degree is 10 -2 ～10 -4 Pa, and the heat preservation time is 90-150 min.
The invention has the beneficial effects that:
1. the preparation process is simple, the flow is less, and the period is short; and the adopted raw material powder and the surface modification material have low cost and wide sources.
2. According to the invention, the self-lubricating phase powder is subjected to surface modification, so that the surface of the self-lubricating phase powder reacts in situ to generate a TiC protective layer in the high-temperature sintering process, ti and C of the protective layer are combined in a covalent bond manner, the decomposition temperature is high, the melting point is high, the thermal conductivity is poor, the influence of heat on the self-lubricating phase powder in the sintering process can be effectively isolated, and the self-lubricating phase powder is further protected from decomposition; meanwhile, tiC generated by the reaction can play a role in enhancing mechanical properties such as hardness, strength and toughness of the matrix, and the comprehensive performance of the material is further improved; and, the decomposition of the self-lubricating phase powder during the temperature rise can be further reduced by increasing the temperature rise rate. Through the organic matter coating on the surface of the powder, the generation of the in-situ TiC protective layer and the improvement of the heating rate, the decomposition of the two-dimensional structure type self-lubricating material at high temperature can be effectively reduced, and the completeness, stability and self-lubricating effect of the chemical structure of the material are ensured.
3. The reinforcing phase and the self-lubricating phase of the self-lubricating wear-resistant titanium-based composite material part prepared by the method are in dispersed and uniform distribution in a matrix, and the doped MoS 2 Powder, WS 2 Powder and MoS 2 +WS 2 The powder is not decomposed after sintering, the grain size of the composite material part is smaller, the compactness is higher, the mechanical properties such as hardness and strength are excellent, the friction coefficient is far lower than that of a titanium alloy base material, the abrasion loss under the same working condition is smaller, and the abrasion resistance is optimized and improved.
4. The self-lubricating wear-resistant titanium-based composite material part can be used for parts such as gear parts, transmission parts, combined parts and the like, and a small amount of lubricating oil can be added or even no lubricating oil is used in the service process.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a flow chart of a process for preparing a self-lubricating wear-resistant titanium-based composite material part according to an embodiment of the invention;
FIG. 2a is an SEM morphology (metallographic morphology) of a TC4 material article prepared in comparative example 1;
FIG. 2b is an SEM morphology (metallographic morphology) of the titanium matrix composite article prepared in comparative example 4;
FIG. 2c is an SEM image (metallographic image) of the self-lubricating wear-resistant titanium-based composite material manufactured in example 1 of the invention;
FIG. 2d is an SEM image (metallographic image) of the self-lubricating wear-resistant titanium-based composite material manufactured in example 3 of the invention;
FIG. 3 shows the Electron Probe (EPMA) results of a self-lubricating wear-resistant titanium-based composite article according to example 1 of the present invention; wherein, fig. 3a is a selected EPMA analysis area; FIG. 3b is the EPMA result of Ti element distributed inside the grains and between the slabs, distinguished from the position of the reinforcing and self-lubricating phases; FIG. 3c shows EPMA results of Al elements distributed inside the grains and along the lath features in a direction similar to the lath features; FIG. 3d shows EPMA results of V elements, which are dispersed and uniformly distributed in the lath shape; FIG. 3e shows EPMA results for Si distributed inside the reinforcing phase; FIG. 3f shows EPMA results of C element, which is located close to Si and uniformly distributed in the enhanced phase; FIG. 3g is the EPMA result of Mo element, which is dispersed and uniformly distributed around the self-lubricating phase, different from the positions of Si and C elements; FIG. 3h shows EPMA results of S element, which is uniformly dispersed around the self-lubricating phase at the same position as Mo element.
FIG. 4 is a graph comparing the coefficient of friction of the TC4 material article prepared in comparative example 1 and the self-lubricating wear-resistant titanium-based composite article prepared in the example of the invention;
FIG. 5a is an SEM topography of the wear scar of the TC4 material article made in comparative example 1;
FIG. 5b is an SEM topography of the wear scar of the titanium matrix composite article made in comparative example 4;
FIG. 5c is an SEM image of the wear scar of the self-lubricating wear-resistant titanium-based composite material manufactured in the embodiment 1 of the invention;
FIG. 5d is an SEM image of the wear scar of the self-lubricating wear-resistant titanium-based composite product prepared in the embodiment 3 of the invention.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
According to the specific embodiment of the invention, a preparation method of a self-lubricating wear-resistant titanium-based composite material part is provided.
As shown in FIG. 1, the preparation method of the self-lubricating wear-resistant titanium-based composite material product comprises the following steps:
(1) And weighing the matrix powder, the reinforcing phase powder and the self-lubricating phase powder according to the proportion. Wherein, the mass percentages of the matrix powder, the reinforcing phase powder and the self-lubricating phase powder in the total are respectively 79.0-97.0%, 1.0-7.0% and 2.0-14.0%.
The self-lubricating phase powder is MoS 2 Powder, WS 2 At least one of the powders.
The matrix powder is TC4 powder.
The reinforcing phase powder is SiC powder.
(2) And carrying out surface modification on the self-lubricating phase powder to obtain the modified self-lubricating phase powder with the surface attached with the protective film.
The protective film is an organic film or a carbon film, the organic film is formed by a coupling agent coating method, and the carbon film is formed by a hydrothermal carbonization and emulsion template method.
The coupling agent coating method specifically comprises the following steps:
firstly, weighing a coupling agent, wherein the mass ratio of the coupling agent to self-lubricating phase powder is 0.01-0.5: 1; then putting the coupling agent into the volatile organic matter solution, and fully and uniformly mixing to form a mixed solution, wherein the solid-to-liquid ratio of the mixed solution is 1.0-5.0 g/mL; then, putting the self-lubricating phase powder into the mixed solution, and continuously stirring to ensure that the mixed solution is fully contacted with the self-lubricating phase powder and uniformly mixed; then heating the mixture in a blast oven at the temperature of between 60 and 90 ℃ for 12 to 48 hours until the organic solution is fully volatilized and only dry self-lubricating phase powder with the modified surface is left; and finally, grinding the modified self-lubricating phase powder in a mortar to obtain the modified self-lubricating phase powder with clear granularity.
The coupling agent can be silane coupling agent and titanate coupling agent; among them, the silane coupling agent may be aminosilane (e.g., 3-aminopropyltriethoxysilane), vinylsilane (e.g., vinyltriethoxysilane), acylsilane (e.g., 3-methacryloxypropyltrimethoxysilane), octylsilane (e.g., octyltriethoxysilane), or alkylsilane;
the titanate coupling agent can be isopropyl tristearate, isopropyl dioleate acyloxy (dioctyl phosphate acyloxy) titanate or isopropyl trioleate acyloxy titanate.
The volatile organic solution can be absolute ethyl alcohol, methanol, toluene and xylene.
The hydrothermal carbonization and emulsion template method comprises the following specific steps:
self-lubricating phase powder and a carbon source are used as raw materials, and octylamine is used as an additive. Dissolving self-lubricating phase powder and a carbon source in distilled water respectively to obtain a mixed solution, wherein the mass ratio of the self-lubricating phase powder to the carbon source is (0.01-0.2): 1; adding octylamine into the mixed solution, wherein the mass ratio of the octylamine to the carbon source is 0.05-1: 1, oscillating to be uniform; putting the mixed liquid into a hydrothermal reaction kettle, and preserving the heat for 1-50 hours at the temperature of 50-200 ℃; and (3) taking out the reaction kettle, cooling to room temperature, opening the container, pouring out the precipitate, and cleaning with distilled water and ethanol to obtain the modified self-lubricating phase powder.
The carbon source may be at least one of starch, glucose, citric acid, and maltose.
(3) And mechanically mixing the matrix powder, the reinforcing phase powder and the modified self-lubricating phase powder to obtain uniformly mixed composite material powder. Wherein, the mechanical mixing adopts a multi-axis roller mill or a planetary ball mill, the ball milling medium is titanium balls, agate balls, stainless steel balls or zirconia balls, the ball milling speed is 50-150 r/min, and the ball milling time is 12-24 h.
(4) Placing the composite material powder in a soft die for cold isostatic pressing, wherein the pressing parameters are as follows: the oil pressure is 200-300 MPa, and the pressure maintaining time is 2-10 min.
(5) Vacuum sintering, wherein the process conditions are as follows: the heating rate is 10-20 ℃/min, the sintering temperature is 1100-1300 ℃, and the vacuum degree is 10 -2 ～10 -4 Pa, and keeping the temperature for 90-150 min to obtain the self-lubricating wear-resistant titanium-based composite material product.
(6) And (4) carrying out mechanical processing treatment on the prepared self-lubricating wear-resistant titanium-based composite material part to obtain the required self-lubricating wear-resistant titanium-based composite material part.
The invention also provides a self-lubricating wear-resistant titanium-based composite material part, which has the structure of an alpha-Ti matrix phase of TC4, a reinforcing phase and a self-lubricating phase, wherein the reinforcing phase and the self-lubricating phase are dispersedly distributed around the matrix phase; wherein the reinforcing phase is SiC, and the self-lubricating phase is MoS 2 、WS 2 At least one of (a); and TiC is dispersed around the matrix phase; the friction coefficient of the product is 0.15-0.30, and the hardness is 580-950 HV.
The self-lubricating wear-resistant titanium-based composite material part and the preparation process thereof are described in detail with reference to specific embodiments.
Example 1
A self-lubricating wear-resistant Ti-based composite material product is prepared from TC4 powder and granularity D 50 =27.0 μm, 90.0wt.%; the reinforcing material is SiC powder with a particle size D 50 5.0 μm, 5.0wt.%; the lubricating material is MoS 2 Powder, particle size D 50 =2.6 μm, accounting for 5.0wt%.
Firstly, moS 2 Carrying out coupling agent coating surface modification treatment on the powder, wherein the coupling agent is a titanate coupling agent, the mass ratio of the coupling agent to the self-lubricating phase powder is 0.1, the solid-liquid ratio is 2.0g/mL, the temperature of an oven is 75 ℃, and the time is 24min, so as to obtain a modified lubricating material with an organic matter protective film attached to the surface; then mechanically mixing the materials by using a multi-axis roller mill to obtain composite material powder, wherein the mixed medium is zirconia balls, the ball milling speed is 100r/min, and the ball milling time is 24 hours; then placing the composite material powder in a soft rubber mold for cold isostatic pressing, wherein the pressure is 250MPa, and the pressure maintaining time is 5min; and finally, placing the blank subjected to cold isostatic pressing in a vacuum sintering furnace for sintering, wherein the sintering process comprises the following steps: the heating rate is 15 ℃/min, the sintering temperature is 1250 ℃, and the sintering vacuum degree is 2.0 multiplied by 10 -3 Pa, and the heat preservation time is 120min.
Examples 2 to 3 adopt the same preparation process as example 1, except that the raw material powder and specification, mechanical mixing and spark plasma sintering process parameters, etc. are used, and the process parameters in the preparation method of the self-lubricating wear-resistant titanium-based composite material parts of examples 1 to 3 are summarized as shown in tables 1 to 4.
TABLE 1 EXAMPLES 1 TO 3 raw material powders and their specifications are summarized
TABLE 2 summary of mechanical mixing Process parameters in examples 1-3
TABLE 3 summary of mechanical mixing Process parameters in examples 1-3
TABLE 4 summary of cold isostatic pressing and vacuum sintering process parameters in examples 1-3
Meanwhile, the mechanical properties and frictional wear properties of the self-lubricating wear-resistant titanium-based composite material parts obtained in the embodiments 1 to 3 are also detected, and the results are detailed in tables 5 and 6.
TABLE 5 summary of mechanical Properties of self-lubricating wear-resistant Ti-based composite articles of examples 1-3
TABLE 6 summarization of the Friction and wear properties of the self-lubricating wear-resistant titanium-based composite material of examples 1-3
The combination of table 6 and table 7 shows that the self-lubricating wear-resistant titanium-based composite material product prepared in the embodiment of the invention has a compact and uniform structure, the compactness reaches more than 99.0%, the full-compact state can be achieved, the hardness can reach 580-950 HV, the tensile strength can reach 760-800 MPa, the specified plastic elongation strength can reach 620-660 MPa, the elongation after fracture can reach 3.0% -5.0%, the reduction of area can reach 3.0% -6.0%, the friction coefficient can be optimized to 0.20-0.40, and the wear volume can be reduced to 0.079mm 3 The wear rate was optimized to 1.2X 10 -12 ～2.4×10 -12 m 3 /N·m。
FIG. 3 shows the EPMA results of the self-lubricating wear-resistant Ti-based composite material prepared in example 1 of the present invention, and it can be seen from the combination of FIG. 3a, FIG. 3b, FIG. 3c, FIG. 3d, FIG. 3e, FIG. 3f, FIG. 3g and FIG. 3h that the Ti, al and V elements are uniformly distributed around and in the crystal grains of the TC4 matrix, and the added MoS 2 The elements Mo and S contained in the powder can be detected; meanwhile, the positions of the Mo and the S are the same, which indicates that the added self-lubricating phase powder is in the vacuum sintering processThe integrity and the stability of a two-dimensional structure are still maintained without complete decomposition or decomposition; the added SiC powder contains elements Si and C which can be detected, the Si element exists in the reinforcing phase structure, the C element exists in the position same as the Si element on one hand, and exists around the lubricating phase structure on the other hand, the annular distribution shape surrounding the lubricating phase structure is presented, the existence of the Ti element can be detected at the annular shape at the same time, and a TiC protective layer can be generated on the surface of the self-lubricating material after the surface modification.
The mechanical properties and frictional wear properties of the self-lubricating wear-resistant titanium-based composite material prepared in the examples of the invention will be described in detail through comparative examples.
Comparative example 1
The matrix material is TC4 powder with a particle size D 50 =27.0 μm, and the ratio of TC4 powder is 100%. Firstly, mechanically mixing by using a multi-axis roller mill, wherein a mixing medium is zirconia balls, the ball milling speed is 100r/min, and the ball milling time is 24 hours; then placing the mechanically mixed TC4 powder in a soft rubber mold for cold isostatic pressing, wherein the pressure is 250MPa, and the pressure maintaining time is 5min; and finally, sintering the blank subjected to cold isostatic pressing in a vacuum sintering furnace, wherein the sintering process comprises the following steps: the heating rate is 15 ℃/min, the sintering temperature is 1250 ℃, and the sintering vacuum degree is 2.0 multiplied by 10 -3 Pa, and the heat preservation time is 120min.
Comparative example 2
A Ti-based composite material product is prepared from TC4 powder and granularity D 50 =27.0 μm, 90.0wt.%; the reinforcing material is SiC powder with a particle size D 50 =5.0 μm, 10.0wt.%; no lubricating material.
Firstly, mechanically mixing by using a multi-axis roller mill to obtain composite material powder, wherein the mixed medium is zirconia balls, the ball milling speed is 100r/min, and the ball milling time is 24 hours; then placing the composite material powder in a soft rubber mold for cold isostatic pressing, wherein the pressure is 250MPa, and the pressure maintaining time is 5min; and finally, sintering the blank subjected to cold isostatic pressing in a vacuum sintering furnace, wherein the sintering process comprises the following steps: the heating rate is 15 ℃/min, the sintering temperature is 1250 ℃, and the sintering vacuum degree is 2.0 multiplied by 10 -3 Pa, and the heat preservation time is 120min.
Comparative example 3
A Ti-based composite material product is prepared from TC4 powder and granularity D 50 =27.0 μm, 90.0wt.%; no reinforcing material; the lubricating material is MoS 2 Powder, particle size D 50 =2.6 μm, accounting for 10.0wt%.
Firstly, mechanically mixing by using a multi-axis roller mill to obtain composite material powder, wherein a mixing medium is zirconia balls, the ball milling speed is 100r/min, and the ball milling time is 24 hours; then placing the composite material powder in a soft rubber mold for cold isostatic pressing, wherein the pressure is 250MPa, and the pressure maintaining time is 5min; and finally, placing the composite material powder blank subjected to cold isostatic pressing in a vacuum sintering furnace for sintering, wherein the sintering process comprises the following steps: the heating rate is 15 ℃/min, the sintering temperature is 1250 ℃, and the sintering vacuum degree is 2.0 multiplied by 10 -3 Pa, and the heat preservation time is 120min.
Comparative example 4
A self-lubricating wear-resistant Ti-based composite material product is prepared from TC4 powder and granularity D 50 =27.0 μm, 90.0wt.%; the reinforcing material is SiC powder with a particle size D 50 5.0 μm, 5.0wt.%; the lubricating material is MoS 2 Powder, particle size D 50 =2.6 μm, accounting for 5.0wt%. Firstly, mechanically mixing by using a multi-axis roller mill to obtain composite material powder, wherein a mixing medium is zirconia balls, the ball milling speed is 100r/min, and the ball milling time is 24 hours; then placing the composite material powder in a soft rubber mold for cold isostatic pressing, wherein the pressure is 250MPa, and the pressure maintaining time is 5min; and finally, sintering the blank subjected to cold isostatic pressing in a vacuum sintering furnace, wherein the sintering process comprises the following steps: the heating rate is 15 ℃/min, the sintering temperature is 1250 ℃, and the sintering vacuum degree is 2.0 multiplied by 10 -3 Pa, and the heat preservation time is 120min.
Meanwhile, the invention also detects the mechanical property and the frictional wear property of the titanium-based composite material parts obtained in the comparative examples 1 to 4, wherein the frictional wear property is tested by adopting a ball-disk frictional wear tester and an industry standard method, and the results are detailed in tables 7 and 8.
TABLE 7 summary of mechanical Properties of Ti-based composite articles of comparative examples 1-4
The metallographic morphology of the TC4 material product obtained after sintering in the comparative example 1 is shown in fig. 2a, and as can be seen by combining table 7 and fig. 2a, the density of the TC4 material product is high and can reach a fully dense state; and the crystal grain appearance of the material is lath-shaped, and the crystal boundary of the material is clear and visible.
The metallographic morphology of the sintered titanium-based composite product obtained in comparative example 4 is shown in fig. 2b, and as can be seen by combining table 7 and fig. 2b, the compactness of the titanium-based composite product is low, and obvious holes exist; and the grain morphology and the grain boundary of the material are unclear.
Fig. 2c and fig. 2d show the metallographic morphology of the self-lubricating wear-resistant titanium-based composite material manufactured in the embodiments 1 and 3 of the present invention, respectively, and it can be seen from table 5 that the density of the self-lubricating wear-resistant titanium-based composite material manufactured in the present invention is high, a fully dense state can be achieved, the lath morphology and the grain boundary are clearly visible, and the doped reinforcement phase material and the self-lubricating phase material are uniformly dispersed and distributed in the matrix material.
TABLE 8 summary of tribological wear properties of titanium-based composite articles of comparative examples 1-4
In general, the smaller the friction coefficient, the wider the wear scar width, the smaller the wear volume, the lower the wear rate, and the better the wear resistance of the material.
As can be seen from Table 8, the TC4 material of comparative example 1 and the titanium matrix composite of comparative examples 2-4 both had coefficients of friction greater than 0.5; wherein, the friction coefficient of the TC4 material product in the comparative example 1 is 0.70, the friction coefficient of the titanium-based composite material product in the comparative example 4 is 0.60, and the abrasion process can be divided into two stages, namely an initial abrasion stage (0-50 s) and a stable abrasion stage (50-600 s).
FIGS. 5a and 5b show the wear scar topography of a TC4 material piece and a titanium matrix composite material piece, respectively, wherein the TC4 material piece has a wear scar width of 1030.1 mu m and a wear volume of 0.139mm 3 The wear rate is 4.07 x 10 -12 m 3 N.m, the width of the grinding crack of the titanium-based composite material part is 983.6 mu m, and the abrasion volume is 0.130mm 3 The wear rate is 3.30X 10 -12 m 3 The existence of furrows, scratches, sticking points and abrasive dust can be obviously observed, and the use requirement of the self-lubricating wear-resistant titanium-based composite material product cannot be met.
In the embodiment of the invention, the surface of the self-lubricating phase powder is modified, so that the self-lubricating phase powder can keep the stability of a chemical structure in a sintering process, further plays a self-lubricating role in a friction and wear process, and reduces the friction coefficient of a material; and the base powder is doped with the reinforcing phase powder and the self-lubricating phase powder to play the roles of fine grain strengthening and dispersion strengthening, so that the hardness of the material is increased.
It can be seen from table 6, fig. 4, fig. 5c and fig. 5d that the friction coefficient of the self-lubricating wear-resistant titanium-based composite material product prepared in the embodiment of the present invention is not more than 0.38, which is smaller than the friction coefficients of the material products prepared in comparative examples 1 to 4, and compared with comparative example 1, the hardness of the self-lubricating wear-resistant titanium-based composite material product in example 3 is improved by about 150%, the friction coefficient is reduced by about 70%, the wear volume is reduced by about 75%, and the wear resistance is increased by about 70%. Compared with comparative examples 2-4, the hardness of the self-lubricating wear-resistant titanium-based composite material part in example 3 is increased by about 100%, the friction coefficient is reduced by about 60%, the wear volume is reduced by about 65%, the wear resistance is increased by about 60%, the wear volume is greatly reduced, the wear resistance is greatly improved, and the self-lubricating and wear-resistant requirements are met.
In addition, although the strength and the plasticity of the self-lubricating wear-resistant titanium-based composite material prepared in the embodiment of the invention are reduced relative to the strength and the plasticity of the TC4 material prepared in the comparative example 1 and are better than those of the titanium-based composite material prepared in the comparative examples 2-4, the use requirement of the titanium-based composite material can be met.
The invention avoids thermal decomposition in the sintering process of powder metallurgy by modifying the surface of the self-lubricating phase powder with the two-dimensional structure, and can keep the integrity of the two-dimensional self-lubricating material by further increasing the heating rate, thereby improving the frictional wear performance of the prepared material.
While the invention has been described with reference to specific preferred embodiments, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the following claims. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (6)
1. A self-lubricating wear-resistant titanium-based composite material part is characterized in that the tissue of the part is an alpha-Ti matrix phase of TC4, a reinforcing phase and a self-lubricating phase which are dispersedly distributed around the matrix phase; wherein the content of the first and second substances,
the reinforced phase is SiC, and the self-lubricating phase is MoS 2 、WS 2 At least one of; and TiC is dispersed around the matrix phase;
the friction coefficient of the product is 0.15-0.40, and the hardness is 580-950 HV;
the self-lubricating wear-resistant titanium-based composite material part is prepared by the method comprising the following steps of:
forming a protective film on the surface of the self-lubricating phase powder, mixing the protective film with TC4 powder and SiC powder, and then sequentially carrying out cold isostatic pressing and vacuum sintering to obtain the self-lubricating wear-resistant titanium-based composite material part; wherein, the first and the second end of the pipe are connected with each other,
the protective film is an organic film or a carbon film, the organic film is formed by a coupling agent coating method, and the carbon film is formed by a hydrothermal carbonization and emulsion template method;
the self-lubricating phase powder is MoS 2 Powder, WS 2 At least one of a powder;
the coupling agent in the coupling agent coating method adopts a silane coupling agent or a titanate coupling agent; the mass ratio of the coupling agent to the self-lubricating phase powder is 0.01 to 0.5:1;
in the hydrothermal carbonization and emulsion template method, a carbon source and the self-lubricating phase powder are used as raw materials, and octylamine is used as an additive; the mass ratio of the self-lubricating phase powder to the carbon source is 0.01 to 0.2:1, the mass ratio of the octylamine to the carbon source is 0.05 to 1:1;
the carbon source is at least one of starch, glucose, citric acid and maltose;
the product organization is composed of the following parts: 75.0 to 97.0 percent of alpha-Ti matrix phase, 1.0 to 7.0 percent of SiC reinforcing phase, 1.5 to 14.0 percent of self-lubricating phase and 0.5 to 4.0 percent of TiC by mass percentage.
2. The self-lubricating wear-resistant titanium-based composite article of claim 1, wherein the article has a wear volume of 0.079mm or less 3 The wear rate is 1.2X 10 -12 ~2.4×10 -12 m 3 The wear scar width is 340 to 700 mu m.
3. The self-lubricating wear-resistant titanium-based composite material part as claimed in claim 1 or 2, wherein the compactness of the part is equal to or greater than 99.0%, the tensile strength is 700-800MPa, the specified plastic elongation is 620-660 MPa, the elongation after fracture is 3.0% -5.0%, and the reduction of area is 3.0% -6.0%.
4. A method for preparing the self-lubricating wear-resistant titanium-based composite article according to any one of claims 1 to 3, comprising the steps of:
forming a protective film on the surface of the self-lubricating phase powder, mixing the protective film with TC4 powder and SiC powder, and then sequentially carrying out cold isostatic pressing and vacuum sintering to obtain the self-lubricating wear-resistant titanium-based composite material part; wherein the content of the first and second substances,
the protective film is an organic film or a carbon film, the organic film is formed by a coupling agent coating method, and the carbon film is formed by a hydrothermal carbonization and emulsion template method;
the above-mentionedThe self-lubricating phase powder is MoS 2 Powder, WS 2 At least one of a powder;
the coupling agent in the coupling agent coating method adopts a silane coupling agent or a titanate coupling agent; the mass ratio of the coupling agent to the self-lubricating phase powder is 0.01 to 0.5:1;
in the hydrothermal carbonization and emulsion template method, a carbon source and the self-lubricating phase powder are used as raw materials, and octylamine is used as an additive; the mass ratio of the self-lubricating phase powder to the carbon source is 0.01 to 0.2:1, the mass ratio of the octylamine to the carbon source is 0.05 to 1:1;
the carbon source is at least one of starch, glucose, citric acid and maltose.
5. The method of claim 4, wherein the pressing parameters of the cold isostatic pressing are: the oil pressure is 200 to 300MPa, and the dwell time is 2 to 10min.
6. The method according to claim 4, wherein the process conditions of the vacuum sintering are as follows: the heating rate is 10 to 20 ℃/min, the sintering temperature is 1100 to 1300 ℃, and the vacuum degree is 10 -2 ~10 -4 Pa, and the heat preservation time is 90 to 150min.
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