CN108380889A - TiC/316L composite material and preparation methods - Google Patents
TiC/316L composite material and preparation methods Download PDFInfo
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- CN108380889A CN108380889A CN201810200246.1A CN201810200246A CN108380889A CN 108380889 A CN108380889 A CN 108380889A CN 201810200246 A CN201810200246 A CN 201810200246A CN 108380889 A CN108380889 A CN 108380889A
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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
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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
- 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
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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
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—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
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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
- 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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Abstract
The present invention provides a kind of preparation methods of TiC/316L composite materials, belong to metal material field.The present invention includes the following steps：TiC is mixed with 316L powder of stainless steel, is dry, obtains mixed-powder；Mixed-powder and binder are kneaded, obtain being kneaded material；Material will be kneaded and carry out granulation and injection moulding successively, obtain forming green body；Forming green body is subjected to degreasing and sintering, obtains TiC/316L composite materials.It is 238~288HV that TiC/316L composite materials produced by the present invention, which have good mechanical property, hardness, and 502~508MPa of tensile strength, friction coefficient 0.55~0.70, wear extent 316L stainless steels pure compared with same technique, which are sintered test specimen, reduces by 10~14%；Corrosion electric current density is 0.0079~0.0167mA/cm in 3.5%NaCl solution2, 0.706~0.676V of corrosion potential.
Description
Technical field
The present invention relates to metal material field more particularly to a kind of TiC/316L composite material and preparation methods.
Background technology
316L stainless steels are played an important role as a kind of modern structure material in industrial development and scientific and technological progress.
316L stainless steels belong to austenitic stainless steel, excellent in mechanical performance.Because its nonmagnetic and excellent welding performance is in machinery, change
It is all had a wide range of applications in the various fields such as work, ocean, light industry and oil.With the continuous development of modern industry, to 316L
The requirement of stainless steel material performance is also continuously improved, in the environment such as high temperature, high pressure often using the equipment of 316L stainless steels
Because inner wall abrasion, oxidation corrosion and scrap, service life of a machine serious curtailment.316L stainless steels belong to austenitic stainless steel, due to
Its carbon content is relatively low, and the elements such as carbon are all solid-solubilized in lattice, is not undergone phase transition when cooling, therefore cannot improve it firmly by quenching
Degree.People use composition of material thinking and advanced preparation method in recent years, and it is high, resistance to explore development elasticity modulus height, intensity
Grinding the ceramic particle of the structure-function integration of better performances enhances stainless steel composite material.Low-density, high intensity and high rigidity
Ceramic particle reinforcement be added in stainless steel base, while reducing stainless steel density, improve its hardness and resistance to
Performance is ground, while remaining the excellent corrosion resistance of stainless steel base, before there is huge application in the fields such as machinery, chemical industry
Scape.
TiC particles are suitable as stainless steel composite material reinforcement, this is because TiC has, hardness is high, anti-oxidant, corrosion resistant
Erosion, the excellent physical and chemical performance such as proportion is small, thermal stability is good, especially it between 316L stainless steels with preferableization
Learn compatibility.The TiC particles of high-purity have been commercially produced, and cost is relatively low, and are prepared using powder injection forming,
Grain growth trend is smaller in sintering process, is a kind of ideal enhancing to make composite material have excellent performance
Body material.
In the prior art through preparing TiC/316L composite material parts frequently with PM technique such as die forming, prepare
Composite materials property it is poor.
Invention content
In view of this, the purpose of the present invention is to provide a kind of TiC/316L composite material and preparation methods.The present invention
Composite materials property obtained is excellent.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
The present invention provides a kind of preparation methods of TiC/316L composite materials, include the following steps：
(1) TiC is mixed with 316L powder of stainless steel, is dry, obtaining mixed-powder；
(2) mixed-powder for obtaining the step (1) is kneaded with binder, obtains being kneaded material；
(3) the mixing material that the step (2) obtains is subjected to granulation and injection moulding successively, obtains forming green body；
(4) the forming green body for obtaining the step (3) carries out degreasing and sintering, obtains TiC/316L composite materials.
Preferably, the drying temperature in the step (1) is 0~40 DEG C, and drying time is 1~2h.
Preferably, the binder in the step (2) includes the following components'mass percentage：65~75% paraffin,
23~30% high density polyethylene (HDPE), 2~5% stearic acid.
Preferably, the temperature of injection moulding is 140~160 DEG C in the step (3).
Preferably, the pressure of injection moulding is 60~90MPa in the step (3).
Preferably, the time of injection moulding is 1~4s in the step (3).
Preferably, degreasing includes solvent degreasing and thermal debinding successively in the step (4).
Preferably, the thermal debinding includes that first stage thermal debinding, second stage thermal debinding and phase III heat are de- successively
The temperature of fat, the first stage thermal debinding is 100~200 DEG C, and the temperature of the second stage thermal debinding is 400~500 DEG C,
The temperature of the phase III thermal debinding is 600~750 DEG C.
Preferably, the sintering in the step (4) includes first stage sintering, second stage sintering and phase III successively
The temperature of sintering, the first stage sintering is 600~750 DEG C, and the temperature of the second stage sintering is 1100~1200 DEG C,
The temperature of the phase III sintering is 1350~1375 DEG C.
The present invention also provides TiC/316L composite materials made from preparation method described above, the TiC/316L is compound
The hardness of material is 238~288HV, 502~508MPa of tensile strength, friction coefficient 0.55~0.70, the more same technique of wear extent
Pure 316L stainless steels sintering test specimen reduces by 10~14%；In 3.5%NaCl solution corrosion electric current density be 0.0079~
0.0167mA/cm2, corrosion potential is -0.706~-0.676V.
The present invention provides a kind of preparation methods of TiC/316L composite materials, include the following steps：Not by TiC and 316L
Powdered steel of becoming rusty mixing, drying, obtain mixed-powder；Mixed-powder and binder are kneaded, obtain being kneaded material；Material will be kneaded
Granulation and injection moulding are carried out successively, obtain forming green body；Forming green body is subjected to degreasing and sintering, it is compound to obtain TiC/316L
Material.TiC is added in 316L powder of stainless steel in the present invention, is kneaded, be granulated, is injected into successively to above-mentioned mixed-powder
Shape, degreasing and sintering finally improve the mechanical property of TiC/316L composite materials.Due to being added in 316L powder of stainless steel
The TiC particles of excellent in mechanical performance, TiC particles hardness itself is higher, is deformed caused by external force so as to effectively resist, and improves
The hardness and friction and wear behavior of test specimen.From embodiment as can be seen that the hardness of TiC/316L composite materials provided by the invention
For 238~288HV, 502~508MPa of tensile strength, friction coefficient 0.55~0.70, wear extent 316L pure compared with same technique be stainless
Steel, which is sintered test specimen, reduces by 10~14%；Corrosion electric current density is 0.0079~0.0167mA/cm in 3.5%NaCl solution2, rotten
Erosion current potential is -0.706~-0.676V.
Figure of description
Fig. 1 is the preparation method flow chart of TiC/316L composite materials of the present invention；
Fig. 2 is the profile scanning figure for the degreasing blank that TiC/316L composite materials are made in the embodiment of the present invention 1；
Fig. 3 is the profile scanning figure that TiC/316L composite materials are made in the embodiment of the present invention 1；
Fig. 4 is the friction coefficient variation diagram that TiC/316L composite materials are made in the embodiment of the present invention 1；
Fig. 5 is the Tafel curve figure that TiC/316L composite materials are made in the embodiment of the present invention 1；
Fig. 6 is the outside drawing that TiC/316L composite materials are made in the embodiment of the present invention 1.
Specific implementation mode
The present invention provides a kind of preparation methods of TiC/316L composite materials, include the following steps：
(1) TiC and 316L powder of stainless steel is mixed, is dry, obtaining mixed-powder；
(2) mixed-powder for obtaining step (1) is kneaded with binder, obtains being kneaded material；
(3) the mixing material that step (2) obtains is subjected to granulation and injection moulding successively, obtains forming green body；
(4) the forming green body for obtaining step (3) carries out degreasing and sintering, obtains TiC/316L composite materials.
TiC and 316L powder of stainless steel is mixed, is dry by the present invention, obtains mixed-powder.In the present invention, the mixing
The weight percent of TiC is preferably 5~8% in powder, and more preferably 6~7%；316L powder of stainless steel in the mixed-powder
Weight percent be preferably 92~95%, more preferably 93~94%.
In the present invention, the 316L powder of stainless steel preferably includes 16~18%Cr of component of following mass percent,
11~14%Ni, 2~3%Mo, Si≤1%, Mn≤1.5%, O≤0.38%, surplus Fe.In the present invention, the 316L
The meso-position radius of powder of stainless steel is preferably 8~30 μm, more preferably 10~20 μm；The meso-position radius of the TiC is preferably 8~30 μ
M, more preferably 10~20 μm.The present invention does not have special restriction to the source of the TiC and 316L powder of stainless steel, using this
Commercial goods known to field technology personnel, when the grain size of commodity is unsatisfactory for above-mentioned requirements, conventional by this field
Mode makes raw material reach above-mentioned requirements.
In the present invention, the time of the mixing is preferably 1~2h, more preferably 1.5~1.8h；Turn when the mixing
Speed is preferably 18~22r/min, more preferably 20~21r/min.The present invention does not have the equipment of the mixing special restriction,
Using mixing apparatus well known to those skilled in the art, specifically, such as three-dimensional mixed powder machine.
In the present invention, the temperature of the drying is preferably 0~40 DEG C, more preferably 10~30 DEG C, most preferably 15~
20℃；The time of the drying is preferably 1~2h, more preferably 1.2~1.5h.The present invention is to the equipment of the drying without spy
Different restriction, using drying equipment well known to those skilled in the art, specifically, such as drying box.It is described dry in the present invention
The dry moisture that can be removed in TiC and 316L powder of stainless steel, avoids the reunion of powder, it is ensured that subsequent injections shape close
Degree is evenly distributed, and then the TiC/316L composite materials in thermal debinding and sintering process is avoided the defects of warpage occur.
After obtaining mixed-powder, mixed-powder and binder are kneaded by the present invention, obtain being kneaded material.In the present invention, institute
The weight ratio for stating mixed-powder and binder is preferably 9~11, and more preferably 9.5~10.5.
In the present invention, the binder preferably includes the component of following mass percent：65~75% paraffin, 23~
30% high density polyethylene (HDPE), 2~5% stearic acid；More preferably include：67~70% paraffin, 26~29% high density
Polyethylene and 3~4% stearic acid.In the present invention, the preparation method of the binder preferably includes following steps：By the height
Density polyethylene melts, and obtains high-melting-point fused materials；By the paraffin and stearic acid mixed melting, molten low melting point object is obtained
Material；The high-melting-point fused materials are mixed with molten low melting point material, obtain binder.
In the present invention, the fusion temperature of the high density polyethylene (HDPE) is preferably 140~160 DEG C, more preferably 145~
150℃.In the present invention, the paraffin and stearic mixed melting temperature are preferably 55~70 DEG C, more preferably 60~65
℃.In the present invention, the mixing temperature of the high-melting-point fused materials and molten low melting point material is preferably 139~147 DEG C, more
Preferably 140~145 DEG C.
In the present invention, the mixing carries out preferably in kneading machine.In the present invention, the useful load of the kneading machine is excellent
58~62%, more preferably 59~61% are selected as, optimal is 60%.
The binder is preferably added in kneading machine by the present invention, is kneaded 10~15min；Then by the mixed-powder
It is average to be added in kneading machine in three times；First part of mixed-powder is added in kneading machine, is kneaded 15~20min；Second part mixed
It closes powder to be added in kneading machine, is kneaded 15~20min；Third part mixed-powder is added to 15~20min of mixing in kneading machine.
In the present invention, the temperature of the mixing is preferably independently 140~160 DEG C, more preferably 145~150 DEG C.In the present invention, institute
It is preferably 0.5~1.5h to state mixing total time, more preferably 0.8~1.2h.In the present invention, the mixed-powder is divided into three times
Kneading machine is added, torque suddenly increases caused by cooling can be prevented too fast, reduces equipment loss.
It obtains after being kneaded material, the present invention will be kneaded material and be granulated successively and injection moulding, obtain shaping green body.
In the present invention, the mixing material is preferably 1~5mm through being granulated obtained granule materials grain size, more preferably 1.5~2.5mm.
The present invention does not have the mode of the granulation special restriction, using granulation mode well known to those skilled in the art.
In the present invention, the temperature of the injection moulding is preferably 140~160 DEG C, more preferably 150~157 DEG C；The note
The pressure for penetrating forming is preferably 60~90MPa, more preferably 75~82MPa；The time of the injection moulding is preferably 1~4s,
More preferably 2~3s.In the present invention, the dwell pressure of the injection moulding is preferably 30~50MPa, more preferably 35~
43MPa；The dwell time of the injection moulding is preferably 1~4s, more preferably 2~3s.
In the present invention, the mold temperature of the injection moulding is preferably 20~40 DEG C, more preferably 30~38 DEG C.
In the present invention, forming green body, the forming is prepared according to the parameter of injection moulding described in above-mentioned technical proposal
The nearly remote cast gate density contrast of green body is 0.001~0.003gcm-3, ensure that forming blank density gradient in rational range
It is interior, avoid following process from defect occur, make forming green body without short, crackle, overlap the defects of.
After obtaining forming green body, the forming green body is carried out degreasing and sintering by the present invention, obtains TiC/316L composite woods
Material.In the present invention, the degreasing preferably includes solvent degreasing and thermal debinding successively.In the present invention, the solvent degreasing
Temperature is preferably 45~65 DEG C, more preferably 50~55 DEG C；The time of the solvent degreasing is preferably 6~8h, and more preferably 6.5
~7.0h.In the present invention, the solvent degreasing is preferably trichloro ethylene with degreasing solvent.In the present invention, the degreasing is molten
Total dosage of agent and the mass ratio of forming green body are preferably 12~18：1, more preferably 14~17：1, most preferably 15~16：1.
In the present invention, the purpose of the solvent degreasing is most of paraffin and fraction stearic acid in removing binder.
In the present invention, the thermal debinding preferably carries out first stage thermal debinding, second stage thermal debinding and third successively
Stage thermal debinding.In the present invention, the first stage thermal debinding is preferably by room temperature to 100~200 DEG C of first ranks of progress
Duan Baowen, the heating-up time for being warming up to the first stage thermal debinding temperature is preferably 150~200min, more preferably 160~
180min；The soaking time of the first stage thermal debinding is preferably 80~100min, more preferably 85~95min.In this hair
In bright, the purpose of the first stage thermal debinding is to remove paraffin and stearic acid remaining in solvent degreasing.Solvent degreasing is by base
Part is removed by the paraffin and stearic acid of near surface, but inside can not thoroughly remove, if it is too fast excessively high to heat up in the first stage,
It can lead in blank that the closing of pores is very fast, be unable to reach removing paraffin and stearic purpose completely.
In the present invention, the second stage thermal debinding is preferably that first stage thermal debinding temperature is warming up to 400~500 DEG C
Second stage heat preservation is carried out, the heating-up time for being warming up to the second stage thermal debinding temperature is preferably 80~110min, more excellent
It is selected as 85~100min；The soaking time of the second stage thermal debinding is preferably 80~100min, more preferably 90~
95min.In the present invention, the purpose of the second stage thermal debinding is removing high density polyethylene (HDPE).
In the present invention, the phase III thermal debinding is preferably warming up to 600~750 by second stage thermal debinding temperature
DEG C carry out phase III heat preservation, the time for being warming up to the phase III thermal debinding temperature is preferably 120~180min, more preferably
For 150~170min；The soaking time of the phase III thermal debinding is preferably 60~80min, more preferably 70~75min.
In the present invention, the main purpose of the phase III thermal debinding is the preliminary relative density for improving blank, by preceding two benches
The effect of thermal debinding, the binder inside blank remove completely.If not continuing heating but taking out blank, blank meeting
It is broken, this is primarily due to that blank loses binder and relative density is relatively low, and phase III thermal debinding can ensure
Follow-up process carries out and blank is avoided to be broken.
After the completion of degreasing, present invention preferably comprises be cooled to room temperature degreasing blank.Mode of the present invention to the cooling
There is no any special limitation, using the type of cooling well known to those skilled in the art, specifically, such as furnace cooling.
After degreasing blank cooling, product after cooling is sintered by the present invention, obtains TiC/316L composite materials.At this
In invention, the sintering preferably carries out under vacuum.In the present invention, the vacuum degree of the vacuum condition be preferably 3 ×
10-3~4 × 10-3Pa。
In the present invention, the sintering preferably carries out first stage sintering, second stage sintering and phase III burning successively
Knot.In the present invention, first stage sintering is warming up to preferably by room temperature to 600~750 DEG C of progress first stage sintering
The time of the first stage sintering temperature is preferably 350~500min, more preferably 400~450min；The first stage
The time of sintering is preferably 60~80min, more preferably 70~75min.
In the present invention, second stage sintering is preferably warming up to 1100~1200 DEG C of progress by first stage sintering temperature
Second stage is sintered, and the time for being warming up to the second stage sintering temperature is preferably 120~180min, more preferably 140~
160min；The time of the second stage sintering is preferably 60~70min.
In the present invention, phase III sintering is preferably warming up to 1350~1375 DEG C of progress by second stage sintering temperature
Phase III is sintered, and the time for being warming up to phase III sintering temperature is preferably 50~100min, more preferably 60~90min；
The time of the phase III sintering is preferably 40~60min.
In the present invention, the relative density, hardness and wear-resisting property of composite material are can effectively improve by sintering；It burns simultaneously
Knot reduces the influence that the composite material tensile strength caused by TiC is added reduces；In addition, sintering also avoids composite material and exists
The defect aoxidized under hot conditions.
In the present invention, TiC/316L composite materials are obtained preferably by sintered product furnace cooling after the sintering.
The present invention also provides TiC/316L composite materials made from preparation method described above.In the present invention, described
TiC/316L composite materials preferably include following components in percentage by weight 5~8%TiC, 92~95%316L powder of stainless steel；
More preferably include 5~6%TiC, 94~95%316L powder of stainless steel.
In the present invention, the TiC/316L composite hardnesses >=238HV, tensile strength >=502MPa, friction coefficient >=
0.55, wear extent under equal conditions reduces >=10%；Corrosion electric current density >=0.0079mA/ in 3.5%NaCl solution
cm2, corrosion potential >=-0.706V.
TiC/316L composite material and preparation methods provided by the invention are carried out specifically with reference to embodiment
It is bright, but they cannot be interpreted as limiting the scope of the present invention.
Fig. 1 is the preparation flow figure of TiC/316L composite materials of the present invention.TiC and 316L powder of stainless steel is mixed to get
Mixed-powder；Mixed-powder is mixed with binder and is kneaded, and obtains being kneaded material；It is granulated and is noted successively to being kneaded material
Forming is penetrated, forming green body is obtained；Degreasing and sintering are carried out to obtained forming green body, finally obtain TiC/316L composite materials.
Embodiment 1
By the TiC that mass percent is 5% and the 316L powder of stainless steel that mass percent is 95% in three-dimensional hybrid powder
Last machine is mixed, incorporation time 1.5h, and mixed rotating speed is 20r/min；By TiC/316L mixtures in drying box into
Row is dried to obtain mixed-powder；Wherein dry temperature is 20 DEG C, and the dry time is 1.5h；
It is paraffin according to weight percent：High density polyethylene (HDPE)：Stearic acid=65%：30%：5% is configured to binder,
First binder is put into and is kneaded intracavitary mixing 10min, the TiC/316L mixed-powders of one third are added after it is completely melt
Continue to be kneaded 15min, one third TiC/316L mixed-powders are continuously added after being kneaded uniformly and continue to be kneaded 15min, when mixed
One third TiC/316L mixed-powders are continuously added after refining uniformly to continue to be kneaded 20min, obtain being kneaded material；Wherein, described
The total time of mixing is 1h；The melting temperature is 145 DEG C；
Material will be kneaded to be granulated, obtain the granule materials that grain size is 4mm；Granule materials progress injection moulding is obtained
Shape green body；Wherein, the mold temperature of injection moulding is 35 DEG C, and the temperature of injection moulding is 156 DEG C, and injecting forming pressure is
75MPa, injection moulding time are 2s, and the dwell pressure of injection moulding is 37MPa, and the dwell time of injection moulding is 3s；
Solvent degreasing is carried out to forming green body, solvent is trichloro ethylene, and solvent degreasing temperature is 55 DEG C, and degreasing time is
6h；Thermal debinding processing is carried out to solvent degreasing product, the technique of the thermal debinding is：First 180 DEG C are heated to from room temperature, when heating
Between 180min；90min is kept the temperature at 180 DEG C；450 DEG C are heated to by 180 DEG C, heating time 90min；It is kept the temperature at 450 DEG C
90min；450 DEG C are heated to 750 DEG C, heating time 150min；60min is kept the temperature at 750 DEG C；It is finally down to room temperature, is obtained
Thermal debinding product；Degreasing blank profile scanning figure is as shown in Figure 2；As seen from Figure 2：After thermal debinding, inside test specimen
There is interconnected pore, binder removes completely.
Thermal debinding product is sintered under vacuum, vacuum degree is 3.5 × 10-3Pa；The sintering process is：
To 750 DEG C and first stage sintering, sintering time 80min are carried out by room temperature in 450min；Then in 150min by 750
It DEG C is warming up to 1200 DEG C and carries out second segment sintering, sintering time 60min；In 90min 1375 DEG C are warming up to by 1200 DEG C
And phase III sintering is carried out, sintering time 45min；Furnace cooling obtains TiC/316L composite materials after sintering.
Section microscopic analysis is carried out to obtained TiC/316L composite materials, test results are shown in figure 3.It can be with by Fig. 3
Find out that the TiC/316L composite materials of the present invention transgranular fracture phenomenon occur in section part.
The hardness of composite material is tested using GB/T 230-2009, using GB/T 10423-2002 to composite wood
The tensile strength of material is tested；The fretting wear of composite material is tested using ASTM G99-04, using GB/T
24196-2009 tests the corrosion resistance of composite material.The performance test results of TiC/316L composite materials are as follows：Phase
It is 93.72% to density, tensile strength Rm=508MPa, Vickers hardness=288HV；Friction coefficient 0.55, as shown in Figure 4；
The wear extent of TiC/316L composite materials is 0.109mm3, wear extent of pure 316L test specimens under the conditions of identical frictional wear experiment
For 0.124mm3, it can be seen that the addition of TiC makes wear extent reduce 14%.
Corrosion electric current density is 0.0079mA/cm in mass fraction is 3.5%NaCl solution2, corrosion potential-
The Tafel curve of 0.676V, composite material are as shown in Figure 5.As shown in Figure 5：It is finally to burn under the technological parameter of embodiment 1
The corrosion potential for tying test specimen is -0.676V, corrosion electric current density 0.0079mA/cm2。
The appearance of TiC/316L composite materials is as shown in Figure 6；As shown in Figure 6：Under the technological parameter of embodiment 1, finally
Being sintered test specimen has good exterior appearance, the defects of warpage does not occur, deforms.Illustrate to prepare under the technological parameter
TiC/316L composite materials ensure that design shape while mechanical property is promoted.
Embodiment 2
The 316L powder of stainless steel for being 94.5% with mass percent by the TiC that mass percent is 5.5% is mixed in three-dimensional
It closes and is mixed in powder machine, incorporation time 2h, mixed rotating speed is 21r/min；By TiC/316L mixtures in drying box
It is inside dried to obtain mixed-powder；Wherein, dry temperature is 20 DEG C, and the dry time is 1.2h；
It is paraffin according to weight percent：High density polyethylene (HDPE)：Stearic acid=70%：28%：2% is configured to binder,
First binder is put into and is kneaded intracavitary mixing 15min, the mixed-powder that one third is added after it is completely melt continues to be kneaded
15min continuously adds one third mixed-powder after being kneaded uniformly and continues to be kneaded 10min, continuously added after being kneaded uniformly
One third mixed-powder continues to be kneaded 20min, obtains being kneaded material；Wherein, the total time of the mixing is 1h；The mixing
Temperature is 145 DEG C；
Material will be kneaded to be granulated, obtain the granule materials that grain size is 4mm；Granule materials progress injection moulding is obtained
Shape green body；Wherein, the mold temperature of injection moulding is 37 DEG C, and the temperature of injection moulding is 155 DEG C, and injecting forming pressure is
78MPa, injection moulding time are 3s, and the dwell pressure of injection moulding is 40MPa, and the dwell time of injection moulding is 3s；
Solvent degreasing is carried out to forming green body, solvent is trichloro ethylene, and solvent degreasing temperature is 55 DEG C, and degreasing time is
6h；Thermal debinding processing is carried out to solvent degreasing product, the technique of the thermal debinding is：First 180 DEG C are heated to from room temperature, when heating
Between 180min；90min is kept the temperature at 180 DEG C；450 DEG C are heated to by 180 DEG C, heating time 90min；It is kept the temperature at 450 DEG C
90min；450 DEG C are heated to 750 DEG C, heating time 150min；60min is kept the temperature at 750 DEG C；It is finally down to room temperature, is obtained
Thermal debinding product；
Thermal debinding product is sintered under vacuum, vacuum degree is 3.5 × 10-3Pa；The sintering process is：
It to 700 DEG C and is carried out and first stage sintering, sintering time 70min by room temperature in 400min；Then in 160min
It is warming up to 1150 DEG C by 700 DEG C and carries out second segment sintering, sintering time 70min；It is warming up to by 1150 DEG C in 80min
1350 DEG C and phase III sintering is carried out, sintering time 60min；Furnace cooling obtains TiC/316L composite materials after sintering.
Using the testing standard of embodiment 1 to the mechanical property and corrosion resistant of TiC/316L composite materials made from embodiment 2
Corrosion can be tested, and experimental result is as follows：Relative density is 90.25%, tensile strength Rm=502MPa, Vickers hardness=
238HV, friction coefficient 0.70；Wear extent 316L stainless steels sintering test specimen pure compared with same technique reduces by 10%.
Corrosion electric current density is 0.0167mA/cm in 3.5%NaCl solution2, corrosion potential -0.706V.Comparative example 1
Aerosolization 316L powder of stainless steel is selected, the meso-position radius of the powder of stainless steel is D50=12.01 μm, ingredient is
Fe-17Cr-12Ni-2.5Mo-1Si-2Mn-0.03C-0.045P-0.003S；The meso-position radius D of TiC50=1 μm；By quality percentage
8h is mixed in mixing machine than the TiC for 3% with the aerosolization 316L powder of stainless steel that mass percent is 97% to be mixed
Powder；
Using paraffin, polypropylene, Brazil wax and stearic acid binder is configured to as raw material；Binder is put into mixing
Machine is until melt, then be gradually incrementally put into TiC/316L mixed-powders, until TiC/316L mixed-powders and binder are mixed
It closes uniformly, obtains being kneaded material；Wherein the useful load of mixed-powder is 62.5%；
Manual granulating is carried out to being kneaded material, obtains granule materials；Injection moulding is carried out to granule materials, is injected
Shape green body；Wherein, injection moulding uses 12.5MPa type injection molding machines, can produce standard tensile test specimen (MPIF
50)；Wherein, the temperature of injection moulding is 175 DEG C, and the mold temperature of injection moulding is 35 DEG C, and the cycle period of injection moulding is
20s；
Solvent degreasing and thermal debinding are carried out successively to injection moulding green body：Wherein solvent degreasing uses normal heptane solvent, molten
The temperature of agent degreasing is 60 DEG C, and the time of solvent degreasing is 4h；Thermal debinding is carried out after solvent degreasing；The thermal debinding is divided into
Two stages：First stage is temperature from room temperature to 600 DEG C, and heating rate is 1.8 DEG C/min, and 1h is kept the temperature at 600 DEG C；The
Two-stage is that temperature is warming up to 900 DEG C from 600 DEG C, and heating rate is 4 DEG C/min, and 1h is kept the temperature at 900 DEG C, which is happened at hydrogen
Under gas shielded state；
Green body after degreasing is sintered to obtain TiC/316L composite materials；Wherein, sintering stage is sintered using tubular type
Stove；Sintering process is broadly divided into two stages：900 DEG C of first stage is warming up to 1100 DEG C, and heating rate is 10 DEG C/min, and 1100
DEG C heat preservation 5min；1100 DEG C of second stage is warming up to 1385 DEG C, and heating rate is 5 DEG C/min, 1385 DEG C of heat preservation 1h；Sintering process
It is happened under hydrogen shield state.
The mechanical property of obtained TiC/316L composite materials is surveyed using testing standard same as Example 1
Examination, test result is as follows：Relative density is 91.8%, tensile strength 270MPa, hardness 305HV, wear rate 3.35E-8.
It is can be found that by comparison：The tensile strength of TiC/316L composite materials prepared by method using the present invention is maximum
It is far longer than the composite material the maximum tensile strength 270MPa of comparative example preparation for 508MPa, illustrating can be into one using this technique
Step improves the tensile strength of TiC/316L composite materials.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of TiC/316L composite materials, includes the following steps：
(1) TiC is mixed with 316L powder of stainless steel, is dry, obtaining mixed-powder；
(2) mixed-powder for obtaining the step (1) is kneaded with binder, obtains being kneaded material；
(3) the mixing material that the step (2) obtains is subjected to granulation and injection moulding successively, obtains forming green body；
(4) the forming green body for obtaining the step (3) carries out degreasing and sintering, obtains TiC/316L composite materials.
2. the preparation method of TiC/316L composite materials according to claim 1, which is characterized in that in the step (1)
Drying temperature be 0~40 DEG C, drying time be 1~2h.
3. the preparation method of TiC/316L composite materials according to claim 1, which is characterized in that in the step (2)
Binder include the following components'mass percentage：65~75% paraffin, 23~30% high density polyethylene (HDPE), 2~5%
Stearic acid.
4. the preparation method of TiC/316L composite materials according to claim 1, which is characterized in that in the step (3)
The temperature of injection moulding is 140~160 DEG C.
5. the preparation method of TiC/316L composite materials according to claim 1 or 4, which is characterized in that the step (3)
The pressure of middle injection moulding is 60~90MPa.
6. the preparation method of TiC/316L composite materials according to claim 5, which is characterized in that in the step (3)
The time of injection moulding is 1~4s.
7. the preparation method of TiC/316L composite materials according to claim 1, which is characterized in that in the step (4)
Degreasing includes solvent degreasing and thermal debinding successively.
8. the preparation method of TiC/316L composite materials according to claim 7, which is characterized in that the thermal debinding is successively
Including first stage thermal debinding, second stage thermal debinding and phase III thermal debinding, the temperature of the first stage thermal debinding is
100~200 DEG C, the temperature of the second stage thermal debinding is 400~500 DEG C, and the temperature of the phase III thermal debinding is 600
~750 DEG C.
9. the preparation method of TiC/316L composite materials according to claim 1, which is characterized in that in the step (4)
Sintering include first stage sintering, second stage sintering and phase III sintering, the temperature of first stage sintering successively
It it is 600~750 DEG C, the temperature of the second stage sintering is 1100~1200 DEG C, and the temperature of the phase III sintering is
1350~1375 DEG C.
10. TiC/316L composite materials made from any one of claim 1~9 preparation method, which is characterized in that described
The hardness of TiC/316L composite materials is 238~288HV, 502~508MPa of tensile strength, friction coefficient 0.55~0.70, mill
Damage amount 316L stainless steels sintering test specimen pure compared with same technique reduces by 10~14%；Corrosion electric current density is in 3.5%NaCl solution
0.0079~0.0167mA/cm2, corrosion potential is -0.706~-0.676V.
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