CN108893645B - Containing polynary lubrication phase TiAl based self lubricated composite material and preparation method thereof - Google Patents
Containing polynary lubrication phase TiAl based self lubricated composite material and preparation method thereof Download PDFInfo
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Abstract
One kind belonging to technical field of composite materials containing polynary lubrication phase TiAl based self lubricated composite material and preparation method thereof.Containing polynary lubrication phase TiAl based self lubricated composite material, the mass percent of chemical component are as follows: TiCx: 10-30wt.%, Ti3SiC2With OLC mixture: 10-30wt.%, Cr:1-5wt.%, remaining is Ti powder and Al powder；The TiCxIn 0.4≤x≤1.1；Preparation method are as follows: mentioned component is carried out ball and is mixed, mixed-powder is made；Then it is dried, pre-molding；Sintering, polishing.TiAl based self lubricated composite material produced by the present invention not only has lower high/low temperature coefficient of friction and wear rate, but also has the performances such as high-mechanic, high intensity, is suitable for the materials such as mass production self-lubricating bearing.
Description
Technical field
The present invention relates to technical field of composite materials, more particularly to one kind to contain polynary lubrication phase TiAl base self-lubricating composite wood
Material and preparation method thereof.
Background technique
With the rapid development of machinery industry, TiAl alloy is widely applied in many fields, but the height of TiAl alloy
Coefficient of friction and abrasion loss limit its extensive use.In order to improve the friction and wear behavior of TiAl alloy, the human hairs such as Zhang Qiaoxin
A kind of TiAl- graphene-Ti is illustrated3SiC2Self-lubricating composite, obtained composite material is with high purity, crystal grain is tiny, consistency
Height, and [Zhang Qiaoxin, Xu Zengshi, Shi Xiaoliang wait a kind of TiAl- graphene-of with excellent mechanical property and tribological property
Ti3SiC2The Hubei self-lubricating composite and preparation method thereof [P]: CN103882257A, 2014]；Shi Xiaoliang et al. invention one
Kind contains Ti3SiC2、Ti2The TiAl intermetallic compound base solid self-lubricating of AlC and C ternary composite lubricating phase and reinforced phase TiC
Composite material.The self-lubricating composite consistency of synthesis is high, tribological property is good, technological parameter is stable, and preparation process is quick
It is simply, easy to operate that [Shi Xiaoliang, Peng Meichao, Zhang Qiaoxin wait a kind of TiAl intermetallic compound base solid self-lubricating composite material of
And preparation method thereof the Hubei [P]: CN102492871A, 2012]；Zhai W et al. then passes through the Ti of addition different content3SiC2
And MoS2Lubrication mutually prepares TiAl based self lubricated composite material (TMC).Studies have shown that addition 10wt.% (Ti3SiC2-MoS2) profit
The TMC of sliding phase has good tribological property [Zhai W, Shi X, Wang since friction surface generates unique layered structure
M,et al.Friction and Wear Properties of TiAl-Ti3SiC2-MoS2Composites Prepared
by Spark Plasma Sintering[J].Tribology Transactions,2014,57(3):416-424].However,
After the variation that wider range occurs for temperature, general lubricant easily fails, therefore prepares a kind of in wide temperature variation model
The TiAl based self lubricated composite material that self-lubricating effect can be generated in enclosing is imperative.
Summary of the invention
The object of the present invention is to provide one kind containing polynary lubrication phase TiAl based self lubricated composite material and preparation method thereof, more
Member lubrication phase TiAl based self lubricated composite material not only has lower high/low temperature coefficient of friction and wear rate, but also has Gao Cheng
The performances such as load, high intensity are suitable for the materials such as mass production self-lubricating bearing.
The technical solution of the present invention is as follows:
One kind containing polynary lubrication phase TiAl based self lubricated composite material, the mass percent of chemical component are as follows: TiCx:
10-30wt.%, Ti3SiC2With OLC (carbon onion) mixture: 10-30wt.%, Cr:1-5wt.%, remaining is Ti powder and Al
Powder；The TiCxIn 0.4≤x≤1.1.
The Ti3SiC2In OLC mixture, Ti3SiC2Mass ratio with OLC (carbon onion) is 3:1；It is described compound
Ti and Al molar ratio is 1:0.85-0.95 in material.
The TiCxGranularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC (carbon onion) is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm；It is Nano diamond that the OLC (carbon onion), which prepares raw material,.
The present invention also provides the preparation methods containing polynary lubrication phase TiAl based self lubricated composite material comprising following step
It is rapid:
(1) first TiC using planetary ball mill in argon atmospherexPowder, Cr powder, Ti powder and Al powder carry out uniform ball and mix,
Alcohol uses WC sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 200-350r/min, Ball-milling Time 2-3h as dispersing agent, abrading-ball；
Ti is then added3SiC2With OLC (carbon onion) mixture, then with same rotational speed ball milling 0.5h, mixed-powder is made；
The mass percent of the chemical component of the composite material are as follows: TiCx: 10-30wt.%, Ti3SiC2(carbon is received with OLC
Rice green onion) mixture: 10-30wt.%, Cr:1-5wt.%, remaining is Ti powder and Al powder；The TiCxIn 0.4≤x≤1.1；
(2) mixed-powder of above-mentioned steps (1) is dried in argon atmosphere, and is fitted into pre-molding in graphite jig,
Pressure is 15-30MPa, dwell time 10-30s；
(3) mold of step (2) is put into furnace, discharge plasma sintering is carried out in argon atmosphere, sintering temperature is
1000-1250 DEG C, heating rate is 60-90 DEG C/min, sintering pressure 30-50MPa, vacuum degree 15-40Pa, keeps the temperature 10-
30min obtains blank test specimen；
(4) the blank test specimen by step (3) preparation carries out surface polishing treatment, obtains with TiCx、Ti3SiC2With OLC (carbon
Nanometer green onion) it is the TiAl based self lubricated composite material for lubricating phase.
The Ti3SiC2In OLC (carbon onion) mixture, Ti3SiC2Mass ratio with OLC (carbon onion) is 3:
1；Ti and Al molar ratio is 1:0.85-0.95 in the composite material.
The TiCxGranularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC (carbon onion) is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm；It is Nano diamond that the OLC, which prepares raw material,.
Compared with the prior art, the present invention has the following advantages:
1, the present invention uses TiAl alloy as matrix, in TiCx、Ti3SiC2With a variety of lubrication phases of OLC (carbon onion)
Under synergistic effect, the mechanical performance of TiAl based self lubricated composite material is not only enhanced, moreover it is possible to generate in wide temperature range
Lubricant effect reduces its coefficient of friction, reduces wear rate.
2, added OLC is lubrication phase, improves the defect of TiAl higher dry friction coefficient and wear rate, in friction process
In can generate graphite scrap, amorphous carbon or even diamond-like carbon film-coating, further enrich lubrication mechanism；Secondly, OLC has gold
The wear resistance of matrix can be enhanced in hard rock core.
3, TiAl based self lubricated composite material produced by the present invention not only has lower high/low temperature coefficient of friction and abrasion
Rate, and there are the performances such as high-mechanic, high intensity, it is suitable for the materials such as mass production self-lubricating bearing.
Detailed description of the invention
The HRTEM figure that Fig. 1 is OLC of the present invention with diamond core.
Specific embodiment
Embodiment 1
By TiC0.4For 15wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 10wt.%, Cr are
1wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.9), by TiC0.4Powder, Cr powder, Ti powder and Al powder
It is mixed using uniform ball is carried out in planetary ball mill in argon atmosphere, absolute alcohol is added as dispersing agent, abrading-ball uses WC
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 250r/min, mixing time 2.5h；Ti is then added3SiC2(80 mesh) and OLC particle,
Again with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 15MPa, when pressure maintaining
Between 18s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1100 DEG C, heating rate is 70 DEG C/
Min, sintering pressure 30MPa, vacuum degree 30Pa keep the temperature 10min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.4、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm；
Embodiment 2
By TiC0.6For 15wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 20wt.%, Cr are
2wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.85), by TiC0.6Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 200r/min, mixing time 2h；Ti is then added3SiC2(120 mesh) and OLC particle,
Again with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 20MPa, when pressure maintaining
Between 10s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1100 DEG C, heating rate is 70 DEG C/
Min, sintering pressure 40MPa, vacuum degree 30Pa keep the temperature 15min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.6、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm；
Embodiment 3
By TiC0.4For 30wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 10wt.%, Cr are
1wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.95), by TiC0.4Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 200r/min, mixing time 2.5h；Ti is then added3SiC2(130 mesh) and OLC
Grain, then with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 15MPa, when pressure maintaining
Between 20s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1100 DEG C, heating rate is 90 DEG C/
Min, sintering pressure 30MPa, vacuum degree 20Pa keep the temperature 10min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.4、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm；
Embodiment 4
By TiC0.8For 10wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 30wt.%, Cr are
5wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.86), by TiC0.8Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 350r/min, mixing time 2.2h；Ti is then added3SiC2(160) and OLC particle,
Again with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 21MPa, when pressure maintaining
Between 12s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1250 DEG C, heating rate is 60 DEG C/
Min, sintering pressure 45MPa, vacuum degree 17Pa keep the temperature 25min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.8、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm；
Embodiment 5
By TiC0.9For 11wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 17wt.%, Cr are
4wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.89), by TiC0.9Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 220r/min, mixing time 2.1h；Ti is then added3SiC2(170) and OLC particle,
Again with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 25MPa, when pressure maintaining
Between 22s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1060 DEG C, heating rate is 80 DEG C/
Min, sintering pressure 50MPa, vacuum degree 35Pa keep the temperature 14min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.9、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm；
Embodiment 6
By TiC1.1For 27wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 28wt.%, Cr are
2wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.91), by TiC1.1Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 290r/min, mixing time 2.2h；Ti is then added3SiC2(180 mesh) and OLC
Grain, then with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 17MPa, when pressure maintaining
Between 15s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1150 DEG C, heating rate is 90 DEG C/
Min, sintering pressure 42MPa, vacuum degree 37Pa keep the temperature 28min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC1.1、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm；
Embodiment 7
By TiC0.7For 17wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 19wt.%, Cr are
3wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.85), by TiC0.7Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 310r/min, mixing time 2.7h；Ti is then added3SiC2(90 mesh) and OLC particle,
Again with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 28MPa, when pressure maintaining
Between 28s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1220 DEG C, heating rate is 60 DEG C/
Min, sintering pressure 32MPa, vacuum degree 19Pa keep the temperature 17min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.7、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm；
Embodiment 8
By TiC0.5For 30wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 25wt.%, Cr are
1wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.93), by TiC0.5Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 320r/min, mixing time 2.6h；Ti is then added3SiC2(130 mesh) and OLC
Grain, then with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 16MPa, when pressure maintaining
Between 17s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1000 DEG C, heating rate is 70 DEG C/
Min, sintering pressure 35MPa, vacuum degree 35Pa keep the temperature 22min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.5、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm；
Embodiment 9
By TiC0.9For 10wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 13wt.%, Cr are
3wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.9), by TiC0.9Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 260r/min, mixing time 2h；Ti is then added3SiC2(140 mesh) and OLC particle,
Again with same rotational speed mixing 0.5h, mixed-powder is made；It is Nano diamond that OLC, which prepares raw material,.
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 18MPa, when pressure maintaining
Between 13s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1040 DEG C, heating rate is 80 DEG C/
Min, sintering pressure 40MPa, vacuum degree 37Pa keep the temperature 13min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.9、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm；
Embodiment 10
By TiC1.1For 29wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 12wt.%, Cr are
1wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.89), by TiC1.1Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 290r/min, mixing time 2.5h；Ti is then added3SiC2(100 mesh) and OLC
Grain, then with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 28MPa, when pressure maintaining
Between 30s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1200 DEG C, heating rate is 80 DEG C/
Min, sintering pressure 36MPa, vacuum degree 20Pa keep the temperature 20min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC1.1、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm；
Embodiment 11
By TiC0.5For 10wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 26wt.%, Cr are
5wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.85), by TiC0.5Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 330r/min, mixing time 2h；Ti is then added3SiC2(110 mesh) and OLC particle,
Again with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 17MPa, when pressure maintaining
Between 15s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1050 DEG C, heating rate is 70 DEG C/
Min, sintering pressure 45MPa, vacuum degree 25Pa keep the temperature 21min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.5、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm；
Embodiment 12
By TiC0.5For 20wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 22wt.%, Cr are
4wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.92), by TiC0.5Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 270r/min, mixing time 2.8h；Ti is then added3SiC2(140 mesh) and OLC
Grain, then with same rotational speed mixing 0.5h, mixed-powder is made；It is Nano diamond that OLC, which prepares raw material,.
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 21MPa, when pressure maintaining
Between 10s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1180 DEG C, heating rate is 80 DEG C/
Min, sintering pressure 30MPa, vacuum degree 15Pa keep the temperature 24min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.5、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm；
Embodiment 13
By TiC1.1For 10wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 12wt.%, Cr are
5wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.9), by TiC1.1Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 320r/min, mixing time 3h；Ti is then added3SiC2(180 mesh) and OLC particle,
Again with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 30MPa, when pressure maintaining
Between 25s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1200 DEG C, heating rate is 90 DEG C/
Min, sintering pressure 44MPa, vacuum degree 22Pa keep the temperature 13min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC1.1、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm.
Embodiment 14
By TiC0.8For 20wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 29wt.%, Cr are
4wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.87), by TiC0.8Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 350r/min, mixing time 2.1h；Ti is then added3SiC2(190 mesh) and OLC
Grain, then with same rotational speed mixing 0.5h, mixed-powder is made；It is Nano diamond that OLC, which prepares raw material,.
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 20MPa, when pressure maintaining
Between 20s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1210 DEG C, heating rate is 60 DEG C/
Min, sintering pressure 50MPa, vacuum degree 40Pa keep the temperature 12min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.8、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm.
Embodiment 15
By TiC0.6For 13wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 15wt.%, Cr are
1wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.95), by TiC0.6Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 350r/min, mixing time 3h；Ti is then added3SiC2(150 mesh) and OLC particle,
Again with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 22MPa, when pressure maintaining
Between 19s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1150 DEG C, heating rate is 60 DEG C/
Min, sintering pressure 30MPa, vacuum degree 33Pa keep the temperature 27min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.6、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm.
Embodiment 16
By TiC0.4For 25wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 24wt.%, Cr are
2wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.86), by TiC0.4Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 200r/min, mixing time 2h；Ti is then added3SiC2(120 mesh) and OLC particle,
Again with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 19MPa, when pressure maintaining
Between 27s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1000 DEG C, heating rate is 90 DEG C/
Min, sintering pressure 39MPa, vacuum degree 18Pa keep the temperature 24min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.4、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm.
Embodiment 17
By TiC0.7For 19wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 30wt.%, Cr are
3wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.91), by TiC0.7Powder, Cr powder, Ti powder and Al powder
It is mixed that (10-30 μm) carries out uniform ball to it using planetary ball mill in argon atmosphere, absolute alcohol is added as dispersing agent,
Abrading-ball uses sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 270r/min, mixing time 2.3h；Ti is then added3SiC2(200 mesh)
With OLC particle, then with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 25MPa, when pressure maintaining
Between 30s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1050 DEG C, heating rate is 70 DEG C/
Min, sintering pressure 47MPa, vacuum degree 20Pa keep the temperature 10min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.7、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm.
Embodiment 18
By TiC0.6For 22wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 15wt.%, Cr are
4wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.94), by TiC0.6Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 210r/min, mixing time 2.3h；Ti is then added3SiC2(160 mesh) and OLC
Grain, then with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 22MPa, when pressure maintaining
Between 28s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1220 DEG C, heating rate is 80 DEG C/
Min, sintering pressure 38MPa, vacuum degree 40Pa keep the temperature 30min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.6、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm.
Embodiment 19
By TiC0.9For 25wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 24wt.%, Cr are
5wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.88), by TiC0.9Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 290r/min, mixing time 2.8h；Ti is then added3SiC2(120 mesh) and OLC
Grain, then with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 26MPa, when pressure maintaining
Between 21s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1080 DEG C, heating rate is 90 DEG C/
Min, sintering pressure 35MPa, vacuum degree 28Pa keep the temperature 27min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.9、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200
Mesh；The granularity of OLC is 3-8nm, and the granularity of Ti, Al, Cr are 10-30 μm.
Embodiment 20
By TiC0.4For 27wt.%, Ti3SiC2With OLC (Ti3SiC2It is 3:1 with OLC mass ratio) it is that 27wt.%, Cr are
3wt.%, remaining is the ratio of Ti powder and Al powder (Ti and Al molar ratio is 1:0.86), by TiC0.4Powder, Cr powder, Ti powder and Al powder
Uniform ball is carried out to it using planetary ball mill in argon atmosphere to mix, and absolute alcohol is added as dispersing agent, abrading-ball uses
Sintered carbide ball, ratio of grinding media to material 6:1, revolving speed 220r/min, mixing time 2.5h；Ti is then added3SiC2(80 mesh) and OLC particle,
Again with same rotational speed mixing 0.5h, mixed-powder is made；
Mixed-powder is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure 30MPa, when pressure maintaining
Between 29s；Then it putting it into furnace and to carry out SPS sintering in argon atmosphere, sintering temperature is 1240 DEG C, heating rate is 60 DEG C/
Min, sintering pressure 34MPa, vacuum degree 24Pa keep the temperature 29min, obtain blank test specimen；
The blank test specimen of above-mentioned preparation is carried out surface polishing treatment to obtain with TiC0.4、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
TiC described in the present embodiment0.4Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is
The granularity of 3-8nm, Ti, Al, Cr are 10-30 μm.
The performance for the product that above-described embodiment obtains is detected, performance indicator is as shown in table 1.Fig. 1 is the present invention
Composite material HRTEM figure, as shown in Figure 1, composite material of the invention have the diamond nuclei heart, matrix can be significantly increased
Wear resistance.
The above is the preferred implementation case column in the present invention, is also not listed one by one herein.It particularly points out, in the field
Technical staff without departing from the concept of the premise of the invention, can also make a variety of modifications and variations, therefore these are all answered
It belongs to the scope of protection of the present invention.
The performance of composite material is made in 1 the various embodiments described above of table
Claims (3)
1. one kind contains polynary lubrication phase TiAl based self lubricated composite material, it is characterised in that: the mass percent of its chemical component
Are as follows: TiCx: 10-30wt.%, Ti3SiC2With OLC mixture: 10-30wt.%, Cr:1-5wt.%, remaining is Ti powder and Al powder；
The TiCxIn 0.4≤x≤1.1, the Ti3SiC2In OLC mixture, Ti3SiC2Mass ratio with OLC is 3:1；It is described multiple
Ti and Al molar ratio is 1:0.85-0.95 in condensation material；
The composite material is prepared by following steps:
(1) first TiC in argon atmospherexPowder, Cr powder, Ti powder and Al powder carry out uniform ball and mix, and alcohol is as dispersing agent, ratio of grinding media to material
6:1, revolving speed 200-350r/min, Ball-milling Time 2-3h；Ti is then added3SiC2With OLC mixture, then with same rotational speed ball milling
Mixed-powder is made in 0.5h；
The mass percent of the chemical component of the composite material are as follows: TiCx: 10-30wt.%, Ti3SiC2With OLC mixture:
10-30wt.%, Cr:1-5wt.%, remaining is Ti powder and Al powder；The TiCxIn 0.4≤x≤1.1；
(2) mixed-powder of above-mentioned steps (1) is dried in argon atmosphere, and is fitted into pre-molding in graphite jig, pressure
For 15-30MPa, dwell time 10-30s；
(3) mold of step (2) is put into furnace, discharge plasma sintering, sintering temperature 1000- is carried out in argon atmosphere
1250 DEG C, heating rate is 60-90 DEG C/min, sintering pressure 30-50MPa, vacuum degree 15-40Pa, keeps the temperature 10-30min, obtains
To blank test specimen；
(4) the blank test specimen by step (3) preparation carries out surface polishing treatment, obtains with TiCx、Ti3SiC2It is lubrication phase with OLC
TiAl based self lubricated composite material.
2. according to claim 1 contain polynary lubrication phase TiAl based self lubricated composite material, it is characterised in that: the TiCx
Granularity be 20-45 μm；Ti3SiC2Granularity be 80-200 mesh；The granularity of OLC is 3-8nm, and the granularity of Ti, Al, Cr are 10-30
μm；It is Nano diamond that the OLC, which prepares raw material,.
3. according to claim 1 contain polynary lubrication phase TiAl based self lubricated composite material, it is characterised in that: the step
(1) ball milling is carried out using planetary ball mill in, abrading-ball uses WC sintered carbide ball.
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| CN102492871A (en) * | 2011-12-19 | 2012-06-13 | 武汉理工大学 | TiAl intermetallic compound-based solid seif-lubricating composite material and preparation method thereof |
| CN102888549A (en) * | 2012-10-19 | 2013-01-23 | 武汉理工大学 | TiAl-C-Ag-Ti2AlC-TiC self-lubricating composite material and preparation method thereof |
| CN107021761A (en) * | 2017-04-26 | 2017-08-08 | 燕山大学 | A kind of silicon nitride based self lubricated composite material |
| CN107916349A (en) * | 2017-11-10 | 2018-04-17 | 燕山大学 | A kind of TiAl based high-temp-resistants self-lubricating composite and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102492871A (en) * | 2011-12-19 | 2012-06-13 | 武汉理工大学 | TiAl intermetallic compound-based solid seif-lubricating composite material and preparation method thereof |
| CN102888549A (en) * | 2012-10-19 | 2013-01-23 | 武汉理工大学 | TiAl-C-Ag-Ti2AlC-TiC self-lubricating composite material and preparation method thereof |
| CN107021761A (en) * | 2017-04-26 | 2017-08-08 | 燕山大学 | A kind of silicon nitride based self lubricated composite material |
| CN107916349A (en) * | 2017-11-10 | 2018-04-17 | 燕山大学 | A kind of TiAl based high-temp-resistants self-lubricating composite and preparation method |
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