CN105950914B - A kind of new Ni using hollow over spherical powder as lubrication phase3Al based self-lubricating materials and preparation method - Google Patents
A kind of new Ni using hollow over spherical powder as lubrication phase3Al based self-lubricating materials and preparation method Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
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Abstract
The present invention relates to a kind of new Ni using hollow over spherical powder as lubrication phase3Al based self-lubricating materials, it is prepared by Ni powder, Al powder and hollow over spherical powder, and the main chemical compositions of the hollow over spherical powder are lubrication phase MoS2With glass phase;Wherein Ni:Al mol ratio=3:1, the quality of hollow over spherical powder is Ni powder, (1.0 2.0) wt.% of Al powder gross masses.The self-lubricating material is by hollow over spherical powder In-situ reaction in Ni3In Al matrixes, the coefficient of friction and wear rate of the self-lubricating material of gained in process of friction and wear are relatively low, have excellent tribological property, and preparation method is simply novel, and technological parameter is easily controlled in preparation process.
Description
Technical field
The present invention relates to a kind of new Ni using hollow over spherical powder as lubrication phase3Al based self-lubricating materials and its preparation side
Method.
Background technology
With developing rapidly for modern industrial technology especially Aeronautics and Astronautics technology, some extreme operating condition condition such as high temperature,
Moving component under the environment such as high load, intense radiation proposes more and more higher for high temperature resistant, the performance such as wear-resistant of lubriation material
Requirement, there is an urgent need to develop solid lubrication technology, new self-lubricating antifriction high-abrasive material is researched and developed, to efficiently solve tradition
Lubrication failure problem of the lubriation material under harsh operating mode.Ni3Al intermetallic compounds are because with fusing point height, creep strength
Greatly, the features such as corrosion-resistant and stability is high, high-temperature oxidation resistance is strong, aviation, metallurgy, machinery, ring have been widely used in it
Protect the fields such as industry, and the potentiality to make further progress and demand ([1] Dong Hongxing, the He Yue brightness .Ni for expanding application3Al metals
Between compound progress [J] Materials Science and Engineering of Powder Metallurgies, 2009 (14):83-88.).But Ni3Change between Al metals
The temperature-room type plasticity of compound is low, fracture toughness is poor, and these features limit its application industrially.Thus, how further to carry
High Ni3The tribological property of Al intermetallic compounds under severe conditions meets that the requirement of industrial application becomes extremely important.
In recent years, many researchers are to Ni3The tribological property of Al intermetallic compounds has carried out a series of research
([2]Qingshuai Zhu,Xiaoliang Shi,WenzhengZhai,Kang Yang,Ahmed Mohamed Mahmoud
Ibrahim,Zengshi Xu,Long Chen,Yecheng Xiao,Ao Zhang,Qiaoxin Zhang.Influence of
subsurface micro/nano-structural evolution on macroscopic tribological
behavior of Ni3Al matrix composites[J].Tribology letters,2015,57(3):1-13;[3]
WenzhengZhai,Xiaoliang Shi,Zengshi Xu,Ao Zhang.Investigation of the friction
layer of Ni3Al matrix composites[J].Wear,2015,328-329:39- 49;[4] Xu Jianlin, Yan Cheng
Flag, Zhu Shengyu, Yang Jun, Bi Qinling .Ni3Research [J] tribology journals of Al based self lubricated composite material tribological properties,
2012(12):584-591.).Further to improve Ni3The tribological property of Al intermetallic compounds, domestic and foreign scholars do not turn off
Zhan Xin research work.And for the trend of China's energy-saving and emission-reduction, reduction pollution, not only to the anti-friction wear-resistant of advanced engineering material
Performance, and higher requirement it is also proposed to the processing technology of preparing of material.Therefore, researcher actively seeks tribology
Energy lubrication phase that is excellent, being readily produced preparation, to meet the needs of solid self lubricant material is growing, this kind of lubrication phase is not only
Possesses good properties of antifriction and wear resistance, and manufacture craft is easy, is easy to produce in batches, reduces energy resource consumption.Therefore, it is necessary to
The technology of preparing of novel self-lubricating composite is further studied, to improve Ni3The tribological property of Al intermetallic compounds, together
When be applied to large-scale production.
The content of the invention
The technical problems to be solved by the invention are to provide one kind for above-mentioned the shortcomings of the prior art with hollow
Spherical powder is the new Ni of lubrication phase3Al based self-lubricating materials and preparation method thereof, hollow over spherical powder In-situ reaction is existed
Ni3In Al matrixes, the self-lubricating material of gained has excellent tribological property, and preparation method is simply novel, and technique is easily-controllable
System.
The present invention is to solve the problems, such as that used technical scheme set forth above is:
A kind of new Ni using hollow over spherical powder as lubrication phase3Al based self-lubricating materials, it is by Ni powder, Al powder and hollow
Spherical powder is prepared, wherein Ni:Al mol ratio=3:1, the quality of hollow over spherical powder is Ni powder, Al powder gross masses
(1.0-2.0) wt.%.
In such scheme, the hollow over spherical powder is by lubrication phase MoS2With glass phase composition.Specifically preparation method is:
Choose MoS2Powder, which is added in the sodium silicate aqueous solution containing auxiliary reagent, forms mixed liquor, by gained mixed liquor through drying, molten
After melting, the droplet-like reactant of gained melting, which is ejected into water, to be condensed, and collects the particulate matter of water surface upper strata floating, drying
Afterwards, it is required hollow over spherical powder.Wherein, the concentration of sodium metasilicate is 15- in the sodium silicate aqueous solution containing auxiliary reagent
20wt.%, auxiliary reagent addition are the 5-10% of sodium metasilicate addition, and auxiliary reagent is boric acid, urea, ammonium pentaborate press matter
Measure ratio 1:(1-1.5):The mixture of (0.5-1);Melting uses oxygen-acetylene welding torch device;Drying temperature is no more than 80 DEG C.
In such scheme, the hollow over spherical powder is the hollow over spherical powder for possessing individual particle structure, individual particle it is straight
Footpath is 20 μm of 5-, and wall thickness is the 8%~10% of its diameter.
In such scheme, the hollow over spherical powder is a kind of spheric granules of outward appearance for grey, with rigid shell, and
And there is the characteristics of hollow light.
The above-mentioned new Ni using hollow over spherical powder as lubrication phase3The preparation method of Al based self-lubricating materials, it is included such as
Lower step:
1) Ni is pressed:Al mol ratio=3:1 chooses Ni powder and Al powder, by Ni powder, (1.0-2.0) of Al powder gross masses
Wt.% chooses hollow over spherical powder, and hollow over spherical powder is mixed with Ni powder, Al powder, obtains dispensing;
2) dispensing obtained by step 1) is well mixed, obtains sintered material;
3) sintered material obtained by step 2) is subjected to discharge plasma sintering, obtained using hollow over spherical powder as lubrication phase
New Ni3Al based self-lubricating materials.
In such scheme, the mixing described in step 2), using vibration batch mixing.Wherein, vibration frequency 45-55Hz, vibration
Power is 10000-12000N, and duration of oscillation is 15-25 minutes.
In such scheme, the discharge plasma sintering process described in step 3) is:Sintering temperature is 1100-1200 DEG C, risen
Warm speed is 90-110 DEG C/min, sintering pressure 20-25MPa, vacuum are 1 × 10-2-1×10-1Pa, soaking time are
10- 15min。
The present invention is able to new Ni of the hollow over spherical powder for lubrication phase3Al based self-lubricating materials, in fretting wear
Excellent tribological property is embodied in journey, coefficient of friction is smaller (average value about 0.27-0.33), and fluctuating range is smaller, mill
Loss rate is 4.5-5.1 × 10-5mm3/(Nm)。
To sum up, the present invention chooses MoS2Powder is added in the sodium silicate aqueous solution containing auxiliary reagent, using dry mixed
Liquid, the technology that prepared by high temperature, condensation is collected, prepare a kind of hollow over spherical powder material for possessing individual particle structure, and
Using this hollow over spherical powder as lubrication phase, new Ni is prepared using discharge plasma sintering3Al based self-lubricating materials.In addition,
It is this to use the new Ni using hollow over spherical powder as lubrication phase prepared by discharge plasma sintering technique3Al base self-lubricating materials
Material, its purity is high, compactness is good, has excellent tribological property, coefficient of friction and wear rate in process of friction and wear
It is relatively low;And the step method involved by preparation process is simple and convenient, suitable for large-scale production.
Compared with prior art, the beneficial effects of the invention are as follows:
1st, self-lubricating material of the present invention by hollow over spherical powder In-situ reaction in Ni3In Al matrixes, gained moistens certainly
Sliding material property is excellent, and purity is high, can effectively reduce coefficient of friction and wear rate of the material in sliding process, excellent with stablizing
Good tribological property.
2nd, the present invention prepares self-lubricating material using discharge plasma sintering process, improves combined coefficient, sintering reaction
Stable, the cycle is short, saves the energy, and on the basis of synthesis cost is reduced, effectively prevent can because adding hollow over spherical powder
Dephasign caused by energy produces.
3rd, preparation method of the present invention is simply novel, and technological parameter is easily controlled in preparation process, and quick and feasibility is high;This
The prices of raw materials are moderate needed for invention, wide material sources, and equipment cost needed for preparation lubrication phase hollow over spherical powder is relatively low, prepares work
Skill is easy, energy-conserving and environment-protective, suitable scale extensive use easy to operate.
Brief description of the drawings
Fig. 1 is the preparation technology flow chart of the present invention.
Fig. 2 is the field emission scanning electron microscope photo of the hollow over spherical powder prepared by the embodiment of the present invention 1, and multiplication factor is
500 times.
Fig. 3 is the field emission scanning electron microscope photo of the hollow over spherical powder prepared by the embodiment of the present invention 1, and multiplication factor is
5000 times.
Fig. 4 is the obtained new Ni using hollow over spherical powder as lubrication phase of the embodiment of the present invention 23Al based self-lubricating materials
The electron probe photo of the polishing scratch obtained after friction-wear test.
Fig. 5 is under room temperature condition, is tested a kind of using hollow over spherical powder as lubrication obtained by the embodiment of the present invention 1,2,3
The new Ni of phase3The friction coefficient curve of Al based self-lubricating materials, test condition are:Load 10N, sliding speed 0.2m/s, when
Between 50min, friction radius 5mm.
Fig. 6 is under room temperature condition, is tested a kind of using hollow over spherical powder as lubrication obtained by the embodiment of the present invention 1,2,3
The new Ni of phase3The wear rate test result of Al based self-lubricating materials, test condition are:Load 10N, sliding speed 0.2m/s,
Time 50min, friction radius 5mm.
Embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention is not
It is limited only to the following examples.
In following embodiments, the hollow over spherical powder is by MoS2Powder and the sodium silicate aqueous solution system containing auxiliary reagent
It is standby to form.The present invention provides a kind of specific preparation method, but does not limit its preparation method, and what other method was prepared meets
The hollow spherical powder of condition needed for the present invention is also applied for the present invention.
The present invention provide hollow over spherical powder preparation method be:Choose MoS2Powder is added to the silicic acid containing auxiliary reagent
Mixed liquor is formed in sodium water solution, by gained mixed liquor through being dried to obtain powder particle;High-temperature fusion is carried out to powder particle, will
The droplet-like reactant of gained, which is ejected into water, to be condensed, and collects the particulate matter of water surface upper strata floating, is required after drying
The hollow over spherical powder wanted.Wherein, the concentration of sodium metasilicate is 15-20wt.% in the sodium silicate aqueous solution containing auxiliary reagent, auxiliary
Reagent addition is the 5-10% of sodium metasilicate addition, and auxiliary reagent is boric acid, urea, ammonium pentaborate in mass ratio 1:(1-
1.5):The mixture of (0.5-1);Melting uses oxygen-acetylene welding torch device;Drying temperature is no more than 80 DEG C.
From Fig. 2 and Fig. 3:Prepared hollow over spherical powder overall structure is spherical for individual particle, individual particle it is straight
Footpath is 5-20 μm;Through being checked under actual perforate electron microscope, hollow ball is confirmed as, outward appearance is grey, shell is hard;Enter one
Step determines that the wall of hollow ball is by lubrication phase MoS2With glass phase composition, according to the close of quality, volume and solid section
Degree, the wall thickness for estimating hollow ball are the 8%~10% of its diameter.
Embodiment 1
A kind of new Ni using hollow over spherical powder as lubrication phase3Al based self-lubricating materials, it is by Ni powder, Al powder and hollow
Spherical powder is prepared, wherein Ni:Al mol ratio=3:1, the quality of hollow over spherical powder is Ni powder, Al powder gross masses
1.0wt.%, the hollow over spherical powder are by lubrication phase MoS2With glass phase composition.
As shown in figure 1, the above-mentioned new Ni using hollow over spherical powder as lubrication phase3The preparation side of Al based self-lubricating materials
Method, it comprises the following steps:
1) Ni is pressed:Al mol ratio=3:1 chooses 13.0 grams of Ni powder, 7.0 grams of Al powder and the hollow ball shape powder of above-mentioned preparation
0.2 gram of end;Ni powder, Al powder and hollow over spherical powder are mixed, obtain dispensing;
2) above-mentioned dispensing is placed in dry-mixed in vibration batch mixer, vibration batch mixing outer tank is cylinder of steel, built-in polytetrafluoroethyltank tank,
Vibration frequency is 45Hz, and vibration force 10000N, duration of oscillation is 15 minutes, obtains sintered material;
3) sintered material obtained by step 2) is subjected to discharge plasma sintering, discharge plasma sintering process is:Sintering temperature
To spend for 1100 DEG C, heating rate be 90 DEG C/min, sintering pressure 20MPa, vacuum are 1 × 10-1Pa, soaking time are
10min, obtain the new Ni using hollow over spherical powder as lubrication phase3Al based self-lubricating materials.
Tested by HVS-1000 type digital display microhardnesses instrument, prepared by embodiment 1 it is a kind of using hollow over spherical powder as
Lubricate the new Ni of phase3Al based self-lubricating materials, its hardness are 6.27GPa, relative density 99.4%.Fig. 5 (a) and 6 (a)
Show:Ni manufactured in the present embodiment3The coefficient of friction of Al based self lubricated composite materials is smaller (average value about 0.33), and fluctuates width
Degree is smaller, and wear rate is 5.1 × 10-5mm3/ (Nm), embodies excellent tribological property.
Embodiment 2
A kind of new Ni using hollow over spherical powder as lubrication phase3Al based self-lubricating materials, it is by Ni powder, Al powder and hollow
Spherical powder is prepared, wherein Ni:Al mol ratio=3:1, the quality of hollow over spherical powder is Ni powder, Al powder gross masses
1.5wt.%, the hollow over spherical powder are by lubrication phase MoS2With glass phase composition.
The above-mentioned new Ni using hollow over spherical powder as lubrication phase3The preparation method of Al based self-lubricating materials, it is included such as
Lower step:
1) Ni is pressed:Al mol ratio=3:1 chooses 13.0 grams of Ni powder, 7.0 grams of Al powder and the hollow ball shape powder of above-mentioned preparation
0.3 gram of end;Ni powder, Al powder and hollow over spherical powder are mixed, obtain dispensing;
2) above-mentioned dispensing is placed in dry-mixed in vibration batch mixer, vibration batch mixing outer tank is cylinder of steel, built-in polytetrafluoroethyltank tank,
Vibration frequency is 50Hz, and vibration force 11000N, duration of oscillation is 20 minutes, obtains sintered material;
3) sintered material obtained by step 2) is subjected to discharge plasma sintering, discharge plasma sintering process is:Sintering temperature
To spend for 1150 DEG C, heating rate be 100 DEG C/min, sintering pressure 25MPa, vacuum are 5 × 10-2Pa, soaking time are
12min, obtain a kind of new Ni of hollow over spherical powder for lubrication phase3Al based self-lubricating materials.
Tested by HVS-1000 type digital display microhardnesses instrument, prepared by embodiment 2 it is a kind of using hollow over spherical powder as
Lubricate the new Ni of phase3The hardness of Al based self-lubricating materials is 6.36GPa, relative density 99.3%.Fig. 5 (b) and 6 (b) table
Bright Ni manufactured in the present embodiment3The coefficient of friction of Al based self lubricated composite materials is smaller (average value about 0.29), and fluctuates width
Spend it is small, wear rate be 4.5 × 10-5mm3/ (Nm), embodies excellent tribological property.
Embodiment 3
A kind of new Ni using hollow over spherical powder as lubrication phase3Al based self-lubricating materials, it is by Ni powder, Al powder and hollow
Spherical powder is prepared, wherein Ni:Al mol ratio=3:1, the quality of hollow over spherical powder is Ni powder, Al powder gross masses
2.0wt.%, the hollow over spherical powder are by lubrication phase MoS2With glass phase composition.
The above-mentioned new Ni using hollow over spherical powder as lubrication phase3The preparation method of Al based self-lubricating materials, it is included such as
Lower step:
1) Ni is pressed:Al mol ratio=3:1 chooses 13.0 grams of Ni powder, 7.0 grams of Al powder and the hollow ball shape powder of above-mentioned preparation
0.4 gram of end;Ni powder, Al powder and hollow over spherical powder are mixed, obtain dispensing;
2) above-mentioned dispensing is placed in dry-mixed in vibration batch mixer, vibration batch mixing outer tank is cylinder of steel, built-in polytetrafluoroethyltank tank,
Vibration frequency is 55Hz, and vibration force 12000N, duration of oscillation is 25 minutes, obtains sintered material;
3) sintered material obtained by step 2) is subjected to discharge plasma sintering, discharge plasma sintering process is:Sintering temperature
To spend for 1200 DEG C, heating rate be 110 DEG C/min, sintering pressure 25MPa, vacuum are 1 × 10-2Pa, soaking time are
15min, obtain a kind of new Ni using hollow over spherical powder as lubrication phase3Al based self-lubricating materials.
Tested by HVS-1000 type digital display microhardnesses instrument, prepared by embodiment 3 using hollow over spherical powder to lubricate
The new Ni of phase3The hardness of Al based self-lubricating materials is 6.48GPa, relative density 99.1%.Fig. 5 (c) is under room temperature condition,
Test the obtained new Ni using hollow over spherical powder as lubrication phase of the embodiment of the present invention 33The friction system of Al based self-lubricating materials
Number curve, it is known that the coefficient of friction of the self-lubricating composite is smaller (average value about 0.27), and fluctuating range is small.Fig. 6 (c)
Show the new Ni that embodiment 3 is prepared3The wear rate of Al based self-lubricating materials is 4.8 × 10-5mm3/(Nm).Understand this implementation
New Ni prepared by example3Al based self lubricated composite materials show excellent tribological property.
According to the result of the test of above three embodiment, show that the present invention is able to hollow over spherical powder as the new of lubrication phase
Type Ni3Al based self-lubricating materials embody excellent tribological property in process of friction and wear, and coefficient of friction is smaller, average
It is worth about 0.27-0.33, and fluctuating range is smaller, wear rate is 4.5-5.1 × 10-5mm3/(Nm)。
Each raw material cited by the present invention can realize the present invention, and the bound value of each raw material, interval value can
Realize the present invention, the bound value and interval value of technological parameter (such as frequency, temperature, time, vacuum) of the invention
The present invention, embodiment numerous to list herein can be realized.
Described above is only the preferred embodiment of the present invention, it is noted that is come for one of ordinary skill in the art
Say, without departing from the concept of the premise of the invention, some modifications and variations can also be made, these belong to the present invention's
Protection domain.
Claims (8)
- A kind of 1. new Ni using hollow over spherical powder as lubrication phase3Al based self-lubricating materials, it is characterised in that it is by Ni powder, Al Powder and hollow over spherical powder are prepared, and the main chemical compositions of the hollow over spherical powder are lubrication phase MoS2With glass phase; The mol ratio of Ni powder and Al powder is 3:1, the quality of hollow over spherical powder is Ni powder, Al powder gross masses(1.0-2.0)wt.%;Institute It is the hollow over spherical powder for possessing individual particle structure to state hollow over spherical powder, and a diameter of 5-20 μm of individual particle, wall thickness is straight for its The % of 8 % in footpath~10.
- A kind of 2. new Ni using hollow over spherical powder as lubrication phase according to claim 13Al based self-lubricating materials, its The preparation method for being characterised by the hollow over spherical powder is:Choose MoS2It is water-soluble that powder is added to the sodium metasilicate containing auxiliary reagent Mixed liquor is formed in liquid, by gained mixed liquor after drying, melting, the droplet-like reactant of gained melting, which is ejected into water, to be carried out Condensation, the particulate matter of water surface upper strata floating is collected, be required hollow over spherical powder after drying.
- A kind of 3. new Ni using hollow over spherical powder as lubrication phase according to claim 23Al based self-lubricating materials, its The concentration for being characterised by sodium metasilicate in the sodium silicate aqueous solution containing auxiliary reagent is 15-20wt.%, and auxiliary reagent addition is silicon The 5-10% of sour sodium addition, auxiliary reagent are boric acid, urea, ammonium pentaborate in mass ratio 1:(1-1.5):(0.5-1)Mixing Thing.
- A kind of 4. new Ni using hollow over spherical powder as lubrication phase according to claim 33Al based self-lubricating materials, its It is characterised by that the melting is melted using oxygen-acetylene welding;Drying temperature is no more than 80 DEG C.
- A kind of 5. new Ni using hollow over spherical powder as lubrication phase3The preparation method of Al based self-lubricating materials, it is characterised in that it Comprise the following steps:1)By Ni:Al mol ratio=3:1 choose Ni powder and Al powder, by Ni powder, Al powder gross masses(1.0-2.0)Wt.% chooses Hollow over spherical powder, hollow over spherical powder is mixed with Ni powder, Al powder, obtains dispensing;2)By step 1)Gained dispensing is well mixed, and obtains sintered material;3)By step 2)Gained sintered material carries out discharge plasma sintering, obtains using hollow over spherical powder as the new of lubrication phase Ni3Al based self-lubricating materials;The main chemical compositions of the hollow over spherical powder are lubrication phase MoS2With glass phase;The hollow over spherical powder is to possess The hollow over spherical powder of individual particle structure, a diameter of 5-20 μm of individual particle, wall thickness for its diameter the % of 8 %~10.
- A kind of 6. new Ni using hollow over spherical powder as lubrication phase according to claim 53The system of Al based self-lubricating materials Preparation Method, it is characterised in that step 2)Described mixing, using vibration batch mixing.
- A kind of 7. new Ni using hollow over spherical powder as lubrication phase according to claim 63The system of Al based self-lubricating materials Preparation Method, it is characterised in that the vibration frequency is 45-55Hz, and vibration force 10000-12000N, duration of oscillation is 15-25 points Clock.
- A kind of 8. new Ni using hollow over spherical powder as lubrication phase according to claim 53The system of Al based self-lubricating materials Preparation Method, it is characterised in that step 3)Described discharge plasma sintering process is:Sintering temperature is 1100-1200 DEG C, heating Speed is 90-110 DEG C/min, sintering pressure 20-25MPa, vacuum are 1 × 10-2-1×10-1Pa, soaking time 10- 15min。
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CN106906427B (en) * | 2017-02-20 | 2019-05-24 | 武汉理工大学 | A kind of M50 based self-lubricating material and preparation method thereof |
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