CN108380889B - TiC/316L composite material and preparation method thereof - Google Patents

TiC/316L composite material and preparation method thereof Download PDF

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CN108380889B
CN108380889B CN201810200246.1A CN201810200246A CN108380889B CN 108380889 B CN108380889 B CN 108380889B CN 201810200246 A CN201810200246 A CN 201810200246A CN 108380889 B CN108380889 B CN 108380889B
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composite material
temperature
stage
degreasing
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CN108380889A (en
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乔斌
尚峰
张洪涛
李化强
贺毅强
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Huaihai Institute of Techology
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Huaihai Institute of Techology
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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
    • B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
    • 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
    • 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
    • B22F3/1021—Removal of binder or filler
    • B22F3/1025—Removal of binder or filler not by heating 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
    • 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)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention provides a preparation method of a TiC/316L composite material, belonging to the field of metal materials. The invention comprises the following steps: mixing TiC and 316L stainless steel powder, and drying to obtain mixed powder; mixing the mixed powder with a binder to obtain a mixed material; sequentially granulating and injection molding the mixed materials to obtain a molded blank; and degreasing and sintering the formed blank to obtain the TiC/316L composite material. The TiC/316L composite material prepared by the method has good mechanical property, the hardness is 238-288 HV, the tensile strength is 502-508 MPa, the friction coefficient is 0.55-0.70, and the abrasion loss is reduced by 10-14% compared with that of a pure 316L stainless steel sintered test piece prepared by the same process; the corrosion current density in a 3.5% NaCl solution is 0.0079-0.0167 mA/cm2The corrosion potential is-0.706 to-0.676V.

Description

TiC/316L composite material and preparation method thereof
Technical Field
The invention relates to the field of metal materials, in particular to a TiC/316L composite material and a preparation method thereof.
Background
316L stainless steel, as a modern structural material, plays an important role in industrial development and technological advancement. The 316L stainless steel belongs to austenitic stainless steel and has excellent mechanical property. Because of its non-magnetism and excellent welding property, it has extensive application in the fields of machinery, chemical industry, sea, light industry and petroleum, etc. With the continuous development of modern industry, the requirements on the performance of 316L stainless steel materials are continuously improved, equipment using 316L stainless steel in high-temperature, high-pressure and other environments is often scrapped due to the abrasion and oxidation corrosion of the inner wall, and the service life of the equipment is seriously shortened. 316L stainless steel is an austenitic stainless steel, and because its carbon content is low, elements such as carbon are all dissolved in the crystal lattice, and no phase transformation occurs during cooling, it is not possible to increase its hardness by quenching. In recent years, people explore and develop a ceramic particle reinforced stainless steel composite material with high elastic modulus, high strength and good wear resistance and integrated structure and function by using a material compounding idea and an advanced preparation method. The ceramic particle reinforcement with low density, high strength and high hardness is added into the stainless steel matrix, so that the hardness and wear resistance of the stainless steel are improved while the density of the stainless steel is reduced, and the excellent corrosion resistance of the stainless steel matrix is kept, thereby having great application prospects in the fields of machinery, chemical engineering and the like.
The TiC particles are suitable for being used as a stainless steel composite material reinforcement, because TiC has excellent physical and chemical properties such as high hardness, oxidation resistance, corrosion resistance, small specific gravity, good thermal stability and the like, and particularly has good chemical compatibility with 316L stainless steel. High-purity TiC particles are produced commercially, the cost is low, and the TiC particles are prepared by powder injection molding, and the tendency of grain growth is small in the sintering process, so that the composite material has excellent service performance and is an ideal reinforcement material.
In the prior art, powder metallurgy technology such as die forming is often adopted to prepare TiC/316L composite material parts, and the prepared composite material has poor mechanical property.
Disclosure of Invention
In view of the above, the present invention provides a TiC/316L composite material and a method for preparing the same. The composite material prepared by the invention has excellent mechanical properties.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a TiC/316L composite material, which comprises the following steps:
(1) mixing TiC and 316L stainless steel powder, and drying to obtain mixed powder;
(2) mixing the mixed powder obtained in the step (1) with a binder to obtain a mixed material;
(3) sequentially granulating and injection molding the mixed material obtained in the step (2) to obtain a molded blank;
(4) and (4) degreasing and sintering the formed blank obtained in the step (3) to obtain the TiC/316L composite material.
Preferably, the drying temperature in the step (1) is 0-40 ℃, and the drying time is 1-2 h.
Preferably, the binder in the step (2) comprises the following components in percentage by mass: 65-75% of paraffin, 23-30% of high-density polyethylene and 2-5% of stearic acid.
Preferably, the injection molding temperature in the step (3) is 140-160 ℃.
Preferably, the pressure of injection molding in the step (3) is 60-90 MPa.
Preferably, the injection molding time in the step (3) is 1-4 s.
Preferably, the degreasing in the step (4) sequentially comprises solvent degreasing and thermal degreasing.
Preferably, the thermal degreasing sequentially comprises a first-stage thermal degreasing, a second-stage thermal degreasing and a third-stage thermal degreasing, wherein the temperature of the first-stage thermal degreasing is 100-200 ℃, the temperature of the second-stage thermal degreasing is 400-500 ℃, and the temperature of the third-stage thermal degreasing is 600-750 ℃.
Preferably, the sintering in the step (4) sequentially comprises a first stage sintering, a second stage sintering and a third stage sintering, wherein the temperature of the first stage sintering is 600-750 ℃, the temperature of the second stage sintering is 1100-1200 ℃, and the temperature of the third stage sintering is 1350-1375 ℃.
The invention also provides a TiC/316L composite material prepared by the preparation method, wherein the TiC/316L composite material has the hardness of 238-288 HV, the tensile strength of 502-508 MPa, the friction coefficient of 0.55-0.70 and the abrasion loss which is 10-14% lower than that of a pure 316L stainless steel sintered test piece in the same process; the corrosion current density in a 3.5% NaCl solution is 0.0079-0.0167 mA/cm2The corrosion potential is-0.706 to-0.676V.
The invention provides a preparation method of a TiC/316L composite material, which comprises the following steps: mixing TiC and 316L stainless steel powder, and drying to obtain mixed powder; mixing the mixed powder with a binder to obtain a mixed material; sequentially granulating and injection molding the mixed materials to obtain a molded blank; and degreasing and sintering the formed blank to obtain the TiC/316L composite material. According to the invention, TiC is added into 316L stainless steel powder, and the mixed powder is subjected to mixing, granulation, injection molding, degreasing and sintering in sequence, so that the mechanical property of the TiC/316L composite material is finally improved. Because TiC particles with excellent mechanical property are added into 316L stainless steel powderThe hardness of the particles is high, so that deformation caused by external force can be effectively resisted, and the hardness and the frictional wear performance of the test piece are improved. The embodiment shows that the hardness of the TiC/316L composite material is 238-288 HV, the tensile strength is 502-508 MPa, the friction coefficient is 0.55-0.70, and the abrasion loss is reduced by 10-14% compared with that of a pure 316L stainless steel sintered test piece in the same process; the corrosion current density in a 3.5% NaCl solution is 0.0079-0.0167 mA/cm2The corrosion potential is-0.706 to-0.676V.
Drawings
FIG. 1 is a flow chart of a TiC/316L composite material preparation method of the present invention;
FIG. 2 is a cross-sectional scan of a degreased blank of TiC/316L composite material obtained in example 1 of the present invention;
FIG. 3 is a cross-sectional scan of a TiC/316L composite material prepared in example 1 according to the present invention;
FIG. 4 is a graph showing the change in the coefficient of friction of a TiC/316L composite material obtained in example 1 of the present invention;
FIG. 5 is a Tafel plot of a TiC/316L composite material made in example 1 of the present invention;
FIG. 6 is an appearance diagram of TiC/316L composite material obtained in example 1 of the present invention.
Detailed Description
The invention provides a preparation method of a TiC/316L composite material, which comprises the following steps:
(1) mixing and drying TiC and 316L stainless steel powder to obtain mixed powder;
(2) mixing the mixed powder obtained in the step (1) with a binder to obtain a mixed material;
(3) sequentially granulating and injection molding the mixed material obtained in the step (2) to obtain a molded blank;
(4) and (4) degreasing and sintering the formed blank obtained in the step (3) to obtain the TiC/316L composite material.
The TiC and 316L stainless steel powder are mixed and dried to obtain mixed powder. In the invention, the weight percentage of TiC in the mixed powder is preferably 5-8%, and more preferably 6-7%; the weight percentage of 316L stainless steel powder in the mixed powder is preferably 92-95%, and more preferably 93-94%.
In the invention, the 316L stainless steel powder preferably comprises the following components, by mass, 16-18% of Cr, 11-14% of Ni, 2-3% of Mo, less than or equal to 1% of Si, less than or equal to 1.5% of Mn, less than or equal to 0.38% of O, and the balance of Fe. In the invention, the median diameter of the 316L stainless steel powder is preferably 8-30 μm, and more preferably 10-20 μm; the preferable median diameter of the TiC is 8-30 mu m, and the more preferable median diameter is 10-20 mu m. The TiC and 316L stainless steel powder is not particularly limited in source, and a commercially available product known to a person skilled in the art can be adopted, and when the particle size of the product does not meet the requirement, the raw material is made to meet the requirement in a conventional mode in the art.
In the invention, the mixing time is preferably 1-2 h, and more preferably 1.5-1.8 h; the rotation speed during mixing is preferably 18-22 r/min, and more preferably 20-21 r/min. The mixing device is not particularly limited in the present invention, and may be a mixing device known to those skilled in the art, specifically, a three-dimensional powder mixer.
In the invention, the drying temperature is preferably 0-40 ℃, more preferably 10-30 ℃, and most preferably 15-20 ℃; the drying time is preferably 1-2 h, and more preferably 1.2-1.5 h. The drying equipment is not particularly limited in the present invention, and drying equipment known to those skilled in the art, specifically, a drying oven, may be used. In the invention, the drying can remove the moisture in the TiC and 316L stainless steel powder, avoid the agglomeration of the powder, ensure the uniform density distribution of the subsequent injection molding, and further avoid the defects of the TiC/316L composite material such as warping and the like in the processes of thermal degreasing and sintering.
After the mixed powder is obtained, the mixed powder and the binder are mixed to obtain a mixed material. In the invention, the weight ratio of the mixed powder to the binder is preferably 9-11, and more preferably 9.5-10.5.
In the present invention, the binder preferably comprises the following components in percentage by mass: 65-75% of paraffin, 23-30% of high-density polyethylene and 2-5% of stearic acid; more preferably, it comprises: 67-70% of paraffin, 26-29% of high-density polyethylene and 3-4% of stearic acid. In the present invention, the preparation method of the binder preferably includes the steps of: melting the high-density polyethylene to obtain a high-melting-point molten material; mixing and melting the paraffin and the stearic acid to obtain a low-melting-point molten material; and mixing the high-melting-point molten material with the low-melting-point molten material to obtain the binder.
In the invention, the melting temperature of the high-density polyethylene is preferably 140-160 ℃, and more preferably 145-150 ℃. In the invention, the mixed melting temperature of the paraffin and the stearic acid is preferably 55-70 ℃, and more preferably 60-65 ℃. In the invention, the mixing temperature of the high melting point melting material and the low melting point melting material is preferably 139-147 ℃, and more preferably 140-145 ℃.
In the present invention, the mixing is preferably carried out in a mixer. In the present invention, the loading amount of the mixer is preferably 58 to 62%, more preferably 59 to 61%, and most preferably 60%.
The binder is preferably added into a mixing roll and mixed for 10-15 min; then evenly adding the mixed powder into a mixing roll by three times; adding the first part of mixed powder into a mixing roll, and mixing for 15-20 min; adding the second part of mixed powder into a mixing roll, and mixing for 15-20 min; and adding the third part of mixed powder into a mixing roll to mix for 15-20 min. In the present invention, the kneading temperature is preferably 140 to 160 ℃ independently, and more preferably 145 to 150 ℃. In the present invention, the total time for kneading is preferably 0.5 to 1.5 hours, and more preferably 0.8 to 1.2 hours. In the invention, the mixed powder is added into the mixing mill by three times, so that the sharp increase of torque caused by too fast temperature reduction can be prevented, and the loss of equipment is reduced.
After the mixed material is obtained, the mixed material is sequentially granulated and injection molded to obtain a molded blank. In the invention, the particle size of the granular material obtained by granulating the mixed material is preferably 1-5 mm, and more preferably 1.5-2.5 mm. The granulation method of the present invention is not particularly limited, and granulation methods known to those skilled in the art may be used.
In the invention, the injection molding temperature is preferably 140-160 ℃, and more preferably 150-157 ℃; the injection molding pressure is preferably 60-90 MPa, and more preferably 75-82 MPa; the injection molding time is preferably 1 to 4 seconds, and more preferably 2 to 3 seconds. In the invention, the pressure maintaining pressure of the injection molding is preferably 30-50 MPa, and more preferably 35-43 MPa; the dwell time for the injection molding is preferably 1 to 4 seconds, and more preferably 2 to 3 seconds.
In the present invention, the temperature of the injection molding mold is preferably 20 to 40 ℃, and more preferably 30 to 38 ℃.
According to the technical scheme, the injection molding parameters are adopted to prepare a molded blank, and the density difference of a near gate and a far gate of the molded blank is 0.001-0.003 g-cm-3The density gradient of the formed blank is ensured to be in a reasonable range, the defects of subsequent processing are avoided, and the formed blank has no defects such as insufficient injection, cracks, flash and the like.
After a formed blank is obtained, the formed blank is degreased and sintered to obtain the TiC/316L composite material. In the present invention, the degreasing preferably includes solvent degreasing and thermal degreasing in this order. In the invention, the temperature of solvent degreasing is preferably 45-65 ℃, and more preferably 50-55 ℃; the degreasing time of the solvent is preferably 6-8 h, and more preferably 6.5-7.0 h. In the present invention, the degreasing solvent for solvent degreasing is preferably trichloroethylene. In the invention, the mass ratio of the total use amount of the degreasing solvent to the formed blank is preferably 12-18: 1, more preferably 14 to 17: 1, most preferably 15 to 16: 1. in the present invention, the solvent degreasing aims to remove most of paraffin and a small part of stearic acid in the binder.
In the present invention, the thermal degreasing is preferably performed by sequentially performing a first-stage thermal degreasing, a second-stage thermal degreasing, and a third-stage thermal degreasing. In the invention, the first-stage thermal degreasing is preferably carried out by raising the temperature from room temperature to 100-200 ℃ for first-stage heat preservation, and the time for raising the temperature to the first-stage thermal degreasing temperature is preferably 150-200 min, and more preferably 160-180 min; the heat preservation time of the first-stage thermal degreasing is preferably 80-100 min, and more preferably 85-95 min. In the present invention, the purpose of the first stage thermal degreasing is to remove residual paraffin and stearic acid in solvent degreasing. The solvent degreasing removes the paraffin and the stearic acid on the surface of the blank, but the paraffin and the stearic acid cannot be completely removed inside the blank, if the temperature is too high and too fast in the first stage, the pore in the blank is closed quickly, and the aim of completely removing the paraffin and the stearic acid cannot be achieved.
In the invention, the second-stage thermal degreasing is preferably carried out by raising the temperature of the first-stage thermal degreasing to 400-500 ℃ for second-stage heat preservation, and the time for raising the temperature to the second-stage thermal degreasing temperature is preferably 80-110 min, and more preferably 85-100 min; the heat preservation time of the second-stage thermal degreasing is preferably 80-100 min, and more preferably 90-95 min. In the present invention, the purpose of the second stage of thermal degreasing is to remove the high density polyethylene.
In the invention, the third-stage thermal degreasing is preferably carried out by raising the temperature of the second-stage thermal degreasing to 600-750 ℃ and carrying out third-stage heat preservation, and the time for raising the temperature to the third-stage thermal degreasing temperature is preferably 120-180 min, and more preferably 150-170 min; the heat preservation time of the third-stage thermal degreasing is preferably 60-80 min, and more preferably 70-75 min. In the invention, the main purpose of the third stage of thermal degreasing is to primarily improve the relative density of the blank, and the binder in the blank is completely removed through the action of the first two stages of thermal degreasing. If the blank is taken out without further heating, the blank can be broken, mainly because the blank loses the adhesive and has low relative density, and the third stage of thermal degreasing can ensure that the subsequent process can be carried out to avoid the blank from being broken.
After degreasing is complete, the present invention preferably includes cooling the degreased body to room temperature. The cooling method is not limited in any way, and the cooling method known to those skilled in the art can be adopted, specifically, the cooling method is carried out in a furnace.
After the degreased blank body is cooled, the cooled product is sintered to obtain the TiC/316L composite material. In the present invention, the sintering is preferably performed under vacuum conditions. In the present invention, in the case of the present invention,the degree of vacuum of the vacuum condition is preferably 3X 10-3～4×10-3Pa。
In the present invention, the sintering is preferably performed by sequentially performing the first-stage sintering, the second-stage sintering, and the third-stage sintering. In the invention, the first-stage sintering is preferably carried out by heating from room temperature to 600-750 ℃, and the time for heating to the first-stage sintering temperature is preferably 350-500 min, and more preferably 400-450 min; the time for the first stage sintering is preferably 60-80 min, and more preferably 70-75 min.
In the invention, the second-stage sintering is preferably carried out by heating the first-stage sintering temperature to 1100-1200 ℃, and the time for heating to the second-stage sintering temperature is preferably 120-180 min, and more preferably 140-160 min; the time for the second-stage sintering is preferably 60-70 min.
In the invention, the third-stage sintering is preferably carried out by heating the second-stage sintering temperature to 1350-1375 ℃, and the time for heating to the third-stage sintering temperature is preferably 50-100 min, and more preferably 60-90 min; the time for the third-stage sintering is preferably 40-60 min.
According to the invention, the relative density, hardness and wear resistance of the composite material can be effectively improved through sintering; meanwhile, the sintering reduces the influence of the reduction of the tensile strength of the composite material caused by adding TiC; in addition, the sintering also avoids the defect that the composite material is oxidized under the high-temperature condition.
In the invention, after the sintering is finished, the sintered product is preferably cooled along with a furnace to obtain the TiC/316L composite material.
The invention also provides a TiC/316L composite material prepared by the preparation method. In the invention, the TiC/316L composite material preferably comprises the following components, by weight, 5-8% of TiC and 92-95% of 316L stainless steel powder; more preferably, the alloy comprises 5-6% of TiC and 94-95% of 316L stainless steel powder.
In the invention, the TiC/316L composite material has the hardness of more than or equal to 238HV, the tensile strength of more than or equal to 502MPa, the friction coefficient of more than or equal to 0.55, and the abrasion loss is reduced under the same condition10 percent; the corrosion current density in 3.5 percent NaCl solution is more than or equal to 0.0079mA/cm2The corrosion potential is more than or equal to-0.706V.
The TiC/316L composite material and the preparation method thereof provided by the present invention will be described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
FIG. 1 is a flow chart of the preparation of TiC/316L composite material of the present invention. Mixing TiC and 316L stainless steel powder to obtain mixed powder; mixing the mixed powder with a binder for mixing to obtain a mixed material; sequentially granulating and injection molding the mixed materials to obtain a molded blank; and degreasing and sintering the obtained formed blank to finally obtain the TiC/316L composite material.
Example 1
Mixing 5% of TiC and 95% of 316L stainless steel powder in a three-dimensional powder mixing machine for 1.5h at a rotation speed of 20 r/min; drying the TiC/316L mixture in a drying oven to obtain mixed powder; wherein the drying temperature is 20 ℃, and the drying time is 1.5 h;
the paraffin wax comprises the following components in percentage by weight: high density polyethylene: stearic acid 65%: 30%: 5% of prepared binder, firstly putting the binder into a mixing cavity for mixing for 10min, adding one third of TiC/316L mixed powder after the binder is completely melted, continuing mixing for 15min, continuing adding one third of TiC/316L mixed powder after mixing uniformly, continuing mixing for 20min, and obtaining mixed material; wherein the total mixing time is 1 h; the mixing temperature is 145 ℃;
granulating the mixed material to obtain a granular material with the particle size of 4 mm; carrying out injection molding on the granular material to obtain a molded blank; wherein the temperature of the injection molding die is 35 ℃, the temperature of the injection molding is 156 ℃, the injection molding pressure is 75MPa, the injection molding time is 2s, the pressure maintaining pressure of the injection molding is 37MPa, and the pressure maintaining time of the injection molding is 3 s;
carrying out solvent degreasing on the formed blank, wherein the solvent is trichloroethylene, the solvent degreasing temperature is 55 ℃, and the degreasing time is 6 h; carrying out thermal degreasing treatment on the solvent degreasing product, wherein the thermal degreasing process comprises the following steps: heating from room temperature to 180 deg.C for 180 min; keeping the temperature at 180 ℃ for 90 min; heating from 180 deg.C to 450 deg.C for 90 min; keeping the temperature at 450 ℃ for 90 min; heating to 750 deg.C at 450 deg.C for 150 min; keeping the temperature at 750 ℃ for 60 min; finally cooling to room temperature to obtain a thermal degreasing product; the cross section scanning diagram of the degreased blank is shown in FIG. 2; as can be seen from fig. 2: after the thermal degreasing is finished, communicating pores appear in the test piece, and the binder is completely removed.
Sintering the thermal degreased product under vacuum condition with vacuum degree of 3.5 × 10-3Pa; the sintering process comprises the following steps: heating from room temperature to 750 ℃ within 450min, and carrying out first-stage sintering, wherein the sintering time is 80 min; then heating from 750 ℃ to 1200 ℃ in 150min and carrying out second-stage sintering, wherein the sintering time is 60 min; heating from 1200 ℃ to 1375 ℃ within 90min, and carrying out third-stage sintering for 45 min; and cooling the sintered product along with a furnace to obtain the TiC/316L composite material.
The TiC/316L composite material obtained is subjected to section microscopic analysis, and the test result is shown in figure 3. FIG. 3 shows that the TiC/316L composite material of the present invention has transgranular fracture at the fracture surface.
Testing the hardness of the composite material by using GB/T230-; the friction wear of the composite material was tested using ASTM G99-04 and the corrosion resistance of the composite material was tested using GB/T24196-2009. The performance test result of the TiC/316L composite material is as follows: relative density 93.72%, tensile strength Rm508MPa, 288 HV; coefficient of friction 0.55, as shown in FIG. 4; the abrasion loss of the TiC/316L composite material is 0.109mm3The abrasion loss of the pure 316L test piece under the same frictional abrasion test condition is 0.124mm3It can be seen that the addition of TiC reduces the amount of wear by 14%.
The corrosion current density in a NaCl solution with the mass fraction of 3.5 percent is 0.0079mA/cm2Corrosion potential-0.676V, Tafel curve of the composite material is shown in FIG. 5Shown in the figure. As can be seen from fig. 5: under the process parameters of example 1, the final corrosion potential of the sintered test piece is-0.676V, and the corrosion current density is 0.0079mA/cm2。
The appearance of the TiC/316L composite material is shown in FIG. 6; as can be seen from fig. 6: under the process parameters of the example 1, the final sintered test piece has good appearance and appearance, and does not have the defects of warping, deformation and the like. The TiC/316L composite material prepared under the process parameters is improved in mechanical property and guaranteed in design shape.
Example 2
Mixing 5.5 percent of TiC and 94.5 percent of 316L stainless steel powder in a three-dimensional powder mixing machine for 2 hours at a rotating speed of 21 r/min; drying the TiC/316L mixture in a drying oven to obtain mixed powder; wherein the drying temperature is 20 ℃, and the drying time is 1.2 h;
the paraffin wax comprises the following components in percentage by weight: high density polyethylene: stearic acid 70%: 28%: 2% of the binder is prepared, the binder is firstly placed into a mixing cavity for mixing for 15min, one third of the mixed powder is added after the binder is completely melted and is continuously mixed for 15min, one third of the mixed powder is continuously added after the mixing is uniform and is continuously mixed for 10min, one third of the mixed powder is continuously added after the mixing is uniform and is continuously mixed for 20min, and a mixed material is obtained; wherein the total mixing time is 1 h; the mixing temperature is 145 ℃;
granulating the mixed material to obtain a granular material with the particle size of 4 mm; carrying out injection molding on the granular material to obtain a molded blank; wherein the temperature of the injection molding die is 37 ℃, the temperature of the injection molding is 155 ℃, the injection molding pressure is 78MPa, the injection molding time is 3s, the pressure maintaining pressure of the injection molding is 40MPa, and the pressure maintaining time of the injection molding is 3 s;
carrying out solvent degreasing on the formed blank, wherein the solvent is trichloroethylene, the solvent degreasing temperature is 55 ℃, and the degreasing time is 6 h; carrying out thermal degreasing treatment on the solvent degreasing product, wherein the thermal degreasing process comprises the following steps: heating from room temperature to 180 deg.C for 180 min; keeping the temperature at 180 ℃ for 90 min; heating from 180 deg.C to 450 deg.C for 90 min; keeping the temperature at 450 ℃ for 90 min; heating to 750 deg.C at 450 deg.C for 150 min; keeping the temperature at 750 ℃ for 60 min; finally cooling to room temperature to obtain a thermal degreasing product;
sintering the thermal degreased product under vacuum condition with vacuum degree of 3.5 × 10-3Pa; the sintering process comprises the following steps: heating from room temperature to 700 ℃ within 400min, and sintering at the first stage for 70 min; then heating from 700 ℃ to 1150 ℃ within 160min and carrying out second-stage sintering for 70 min; heating to 1350 deg.C from 1150 deg.C within 80min, and sintering for 60 min; and cooling the sintered product along with a furnace to obtain the TiC/316L composite material.
The mechanical properties and corrosion resistance of the TiC/316L composite material prepared in example 2 are tested by adopting the test standard of example 1, and the test results are as follows: relative density of 90.25%, tensile strength Rm502MPa, 238HV of Vickers hardness and 0.70 of friction coefficient; the abrasion loss is reduced by 10 percent compared with that of a pure 316L stainless steel sintered test piece in the same process.
The corrosion current density in a 3.5% NaCl solution was 0.0167mA/cm2The corrosion potential is-0.706V. Comparative example 1
Selecting gas atomized 316L stainless steel powder with a median diameter D5012.01 μm, Fe-17Cr-12Ni-2.5Mo-1Si-2 Mn-0.03C-0.045P-0.003S; TiC middle diameter D501 μm; mixing 3% by mass of TiC and 97% by mass of gas atomized 316L stainless steel powder in a mixer for 8 hours to obtain mixed powder;
preparing a binder by taking paraffin, polypropylene, carnauba wax and stearic acid as raw materials; putting the binder into an internal mixer until the binder is melted, and then gradually and progressively putting the TiC/316L mixed powder into the internal mixer until the TiC/316L mixed powder and the binder are uniformly mixed to obtain a mixed material; wherein the loading of the mixed powder is 62.5%;
manually granulating the mixed material to obtain a granular material; performing injection molding on the granular material to obtain an injection molding blank; wherein, the injection molding uses a 12.5MPa type injection molding machine, and a standard tensile test piece (MPIF50) can be produced; wherein the injection molding temperature is 175 ℃, the injection molding mold temperature is 35 ℃, and the cycle period of the injection molding is 20 s;
sequentially carrying out solvent degreasing and thermal degreasing on the injection molding blank: wherein the solvent degreasing adopts an n-heptane solvent, the solvent degreasing temperature is 60 ℃, and the solvent degreasing time is 4 h; carrying out thermal degreasing after solvent degreasing is finished; the thermal degreasing is divided into two stages: the first stage is that the temperature is raised from room temperature to 600 ℃, the temperature raising rate is 1.8 ℃/min, and the temperature is kept at 600 ℃ for 1 h; the second stage is that the temperature is raised from 600 ℃ to 900 ℃, the temperature raising rate is 4 ℃/min, the temperature is maintained for 1h at 900 ℃, and the process is carried out under the hydrogen protection state;
sintering the degreased blank to obtain a TiC/316L composite material; wherein, a tubular sintering furnace is adopted in the sintering stage; the sintering process is mainly divided into two stages: in the first stage, the temperature is increased to 1100 ℃ from 900 ℃, the temperature increase rate is 10 ℃/min, and the temperature is maintained at 1100 ℃ for 5 min; in the second stage, the temperature is raised to 1385 ℃ from 1100 ℃, the temperature raising rate is 5 ℃/min, and the temperature is kept for 1h at 1385 ℃; the sintering process takes place under hydrogen protection.
The mechanical properties of the obtained TiC/316L composite material were tested using the same test standards as in example 1, and the test results were as follows: the relative density is 91.8 percent, the tensile strength is 270MPa, the hardness is 305HV, and the wear rate is 3.35E-8.
By comparison, it can be found that: the maximum tensile strength of the TiC/316L composite material prepared by the method is 508MPa, which is far greater than the maximum tensile strength of 270MPa of the composite material prepared by the comparative example, and the tensile strength of the TiC/316L composite material can be further improved by adopting the process.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (8)

1. A preparation method of TiC/316L composite material comprises the following steps:
(1) mixing TiC and 316L stainless steel powder, and drying to obtain mixed powder;
(2) mixing the mixed powder obtained in the step (1) with a binder to obtain a mixed material;
(3) sequentially granulating and injection molding the mixed material obtained in the step (2) to obtain a molded blank;
(4) degreasing and sintering the formed blank obtained in the step (3) to obtain a TiC/316L composite material;
the weight percentage of TiC in the mixed powder is 5-8%; the weight percentage of 316L stainless steel powder in the mixed powder is 92-95%;
the binder in the step (2) comprises the following components in percentage by mass: 65-75% of paraffin, 23-30% of high-density polyethylene and 2-5% of stearic acid;
the sintering in the step (4) sequentially comprises a first stage sintering, a second stage sintering and a third stage sintering, wherein the temperature of the first stage sintering is 600-750 ℃, the temperature of the second stage sintering is 1100-1200 ℃, and the temperature of the third stage sintering is 1350-1375 ℃.
2. A TiC/316L composite material preparation method according to claim 1, wherein the drying temperature in step (1) is 0-40 ℃ and the drying time is 1-2 h.
3. The TiC/316L composite material preparation method of claim 1, wherein the temperature of injection molding in step (3) is 140-160 ℃.
4. A TiC/316L composite material preparation method according to claim 1 or 3, wherein the pressure of injection molding in step (3) is 60-90 MPa.
5. A TiC/316L composite material preparation method according to claim 4, wherein the time of injection molding in step (3) is 1-4 s.
6. A TiC/316L composite preparation method according to claim 1, wherein said degreasing in step (4) comprises solvent degreasing and thermal degreasing in sequence.
7. A TiC/316L composite material preparation method according to claim 6, wherein said thermal degreasing sequentially comprises a first stage thermal degreasing, a second stage thermal degreasing and a third stage thermal degreasing, the temperature of said first stage thermal degreasing is 100-200 ℃, the temperature of said second stage thermal degreasing is 400-500 ℃, and the temperature of said third stage thermal degreasing is 600-750 ℃.
8. The TiC/316L composite material prepared by the preparation method of any one of claims 1 to 7, which is characterized in that the TiC/316L composite material has the hardness of 238 to 288HV, the tensile strength of 502 to 508MPa, the friction coefficient of 0.55 to 0.70 and the abrasion loss of 10 to 14 percent lower than that of a pure 316L stainless steel sintered test piece in the same process; the corrosion current density in a 3.5% NaCl solution is 0.0079-0.0167 mA/cm2The corrosion potential is-0.706 to-0.676V.
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