CN108913974A - A kind of sulfur-bearing self-lubricating high-entropy alloy and preparation method thereof - Google Patents
A kind of sulfur-bearing self-lubricating high-entropy alloy and preparation method thereof Download PDFInfo
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0089—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with other, not previously mentioned inorganic compounds as the main non-metallic constituent, e.g. sulfides, glass
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Abstract
The invention discloses a kind of sulfur-bearing self-lubricating high-entropy alloy, the ingredient of the self-lubricating high-entropy alloy is MxCoCrFeNiSy, one or more of M Al, Ti, Mo, V, Nb, Mn, W, Zr, the atomic ratio x of content is that the atomic ratio y value of 0 ~ 2, S element is 0.05 ~ 3, and the atomic ratio of other elements is 0.5 ~ 1.5.The invention also discloses the preparation methods of the self-lubricating high-entropy alloy.Sulfur-bearing self-lubricating high-entropy alloy disclosed by the invention has both good mechanical property and wide temperature range（Room temperature ~ 800 DEG C）Self-lubricating property, and it is at low cost, high reliablity can be used for being difficult in the operating conditions such as oil-poor, high temperature, heavy duty having a good application prospect on the mechanical equipment using conventional fat lubrication in fields such as metallurgy, mine, the energy, automobile, war industry and nuclear industry.
Description
Technical field
The present invention relates to a kind of sulfur-bearing self-lubricating high-entropy alloys and preparation method thereof, belong to high-entropy alloy and the wear-resistant material of anti-attrition
Material field.
Background technique
Taiwan Kexue man Ye Junwei professor in China first proposed the concept of high-entropy alloy in nineteen ninety-five, by more than two decades
Development, the design theory and technology of preparing of high-entropy alloy have tended to be perfect at present.Different from conventional metal material, high entropy closes
Gold is usually by a variety of metals for waiting atomic ratios or connecing near atomic ratio（Or it is nonmetallic）Element composition, has simple face-centered cubic
（FCC）, body-centered cubic（BCC）Or the phase structure of FCC+BCC, but the intensity, hardness, anti-to hardly match with conventional metal material
Radiation, high temperature resistant, anticorrosive and wear-resistant etc. excellent performance are the best times in the harsh operating condition such as heavy duty, high temperature, thump
Material selection has good in the fields such as mine, metallurgy, automobile, aerospace, equipment manufacturing, war industry and nuclear industry
Application prospect.Although high-entropy alloy all has good wearability under normal circumstances, its autogamy it is secondary or with other metal materials
Coefficient of friction is usually higher when material is with pair, is difficult to provide good lubrication in the operating conditions such as oil-poor, heavily loaded, high speed and high temperature, holds
It easily causes moving component to fail, causes catastrophic consequence.Therefore, there is the high-entropy alloy of good self-lubricating property to have for exploitation
Important engineering application value.
Under normal circumstances, S element is considered as a kind of harmful impurity element in Conventional alloys.Because of S element activity
Higher, the elements such as easy Ti, Mn, Nb and Cr with alloy react, and form metal sulfide in the alloy.And metal sulphur
The intensity of compound is generally lower, and plasticity and toughness are poor, can significantly deteriorate its mechanical property when forming sulfide in alloy, especially
It is that the effect of the deterioration to plasticity and toughness is the most obvious.Therefore, in Conventional alloys, S content is generally strictly controlled at extremely low
Level.
Summary of the invention
It is an object of the invention to overcome the problems, such as that conventional high-entropy alloy tribological property is poor, a kind of sulfur-bearing is provided from moistening
Sliding high-entropy alloy and preparation method thereof, the self-lubricating high-entropy alloy have both good mechanical property and wide temperature range self-lubricating property,
It has a good application prospect in the operating conditions such as oil-poor, high temperature and heavy duty.
A kind of sulfur-bearing self-lubricating high-entropy alloy, it is characterised in that the ingredient of the self-lubricating high-entropy alloy is MxCoCrFeNiSy,
M is one or more of Al, Ti, Mo, V, Nb, Mn, W, Zr, and the atomic ratio x of content is the atomic ratio of 0 ~ 2, S element
Example y value is 0.05 ~ 3, and the atomic ratio of other elements is 0.5 ~ 1.5.
Select MxBasis material of the CoCrFeNi series high-entropy alloy as self-lubricating high-entropy alloy, is based primarily upon with lower section
The reason of face：Firstly, the excellent in mechanical performance such as series high-entropy alloy intensity, plasticity and the toughness, can be effectively reduced S element
The deterioration degree to alloy mechanical property is added；Secondly, the S element being added can be anti-with Ti, Cr, Mo, the elements such as w in alloy
It answers, forms the metal sulfide with good friction-reducing and antiwear action；Third, series high-entropy alloy surface shape in the high temperature environment
At oxide have good greasy property, can further improve the High Temperature Tribological Behavior of alloy.
The high-entropy alloy of self-lubricating containing S is mainly by the high entropy solid solution phase and metal and sulphur of FCC, BCC or FCC+BCC
Compound phase composition.
The compound of the metal and S mutually mainly include TiS, TiS2、MoS2、VS、WS2、NbS2、MnS2、FeS、FeS2、
ZrS、NiS、NiS2、Ni3S2、CoS、CoS2、CrS、Cr2S3、Cr3S4And CrxSyEtc. one such or several.
The preparation method of the high-entropy alloy of self-lubricating containing S, it is characterised in that the preparation method used is smelting process or powder
Last metallurgy method.
The smelting process is induction melting, electric arc melting, plasma melting, electron-beam smelting, electromagnetic levitation-melt or swashs
Light cladding.
The powder metallurgic method is pressureless sintering, hot pressed sintering, discharge plasma sintering, induction sintering or microwave sintering.
The raw material for preparing sulfur-bearing self-lubricating high-entropy alloy mainly include Co, Cr, Fe, Ni, Al, Ti, Mo, V, Nb, Mn,
W、Zr、S、TiS、TiS2、MoS2、VS、WS2、NbS2、MnS2、FeS、FeS2、ZrS、NiS、NiS2、Ni3S2、CoS、CoS2、CrS、
Cr2S3、Cr3S4Deng powder or block, also include intermediate alloy, such as Ni-Cr, Ni-Co, Co-Cr-Ni, Fe-Ni, Fe-Cr
Powder or block.
The method using the smelting process preparation high-entropy alloy of self-lubricating containing S, it is characterised in that this method mainly includes such as
Lower step：
1）Raw material are measured according to the composition proportion of sulfur-bearing self-lubricating high-entropy alloy；
2）Raw material are packed into smelting equipment, melt back 3 ~ 5 times, the ingredient of alloy are made to reach uniform；
3）It comes out of the stove after cooling, removes surface impurity, obtain sulfur-bearing self-lubricating high-entropy alloy finished product.
The method using the powder metallurgic method preparation high-entropy alloy of self-lubricating containing S, it is characterised in that this method is mainly wrapped
Include following steps：
1）Raw material powder is measured according to the composition proportion of sulfur-bearing self-lubricating high-entropy alloy；
2）Raw material powder is uniformly mixed；
3）Pre-molding is directly loadable into graphite jig and is sintered on agglomerating plant；
4）5 ~ 200 DEG C/min of heating rate, 600 ~ 1800 DEG C of sintering temperature, 5 ~ 120 min of soaking time, pressure sintering
When pressure be 5 ~ 40 MPa, furnace cooling after the completion of sintering；
5）After the completion of sintering, surface impurity is removed, obtains sulfur-bearing self-lubricating high-entropy alloy finished product.
In terms of technology of preparing, if preparing high-entropy alloy containing S using smelting process, the S element of low melting point is easy to be burnt
Damage causes the content of S element to deviate design value, and sulfide is easy segregation.In addition, SO easy to form when high melt2Deng
Sulfide gas pollutes the environment.Therefore, in order to avoid the scaling loss of S element and uniform tissue is obtained, when melting is preferential
Select FeS, FeS2, the higher melting-point sulfide such as NiS replace pure S element as raw material.If, can using PM technique
To select pure S element as raw material, FeS, FeS can also be used2, the higher melting-point sulfide such as NiS is as raw material.Meanwhile
It is preferential to select raw material powder of the partial size less than 150 microns in order to obtain uniform institutional framework.
Metal sulfide generally all has good tribological property, shows in the operating conditions such as oil-poor, heavily loaded, high speed and high temperature
Excellent antifriction antiwear characteristic is shown.Based on this, the present invention in high-entropy alloy by adding S element, the shape in alloy structure
At a large amount of metal sulfide with friction-reducing and antiwear action.On the one hand, the formation of sulfide solves high-entropy alloy tribology
The poor problem of performance；On the other hand, have benefited from the good obdurability of high-entropy alloy matrix, overcome the formation pairing of sulfide
The deterioration of golden mechanical property acts on, to obtain the self-lubricating high-entropy alloy for having both good mechanics and tribological property.It is setting
In terms of counting thinking, this high-entropy alloy of self-lubricating containing S disclosed by the invention is the high-entropy alloy and tool that will have good obdurability
There is the metal sulfide of good self-lubricating property to be organically combined, this mentality of designing at home and abroad disclosed documents and materials
In be not reported；In terms of material property, this self-lubricating high-entropy alloy has both good tribology and power in wide temperature range
Performance is learned, and technology of preparing is simple, high reliablity, there is good industrial applications prospect.
Sulfur-bearing self-lubricating high-entropy alloy disclosed by the invention has both good mechanical property and wide temperature range（Room temperature ~ 800
℃）Self-lubricating property, and at low cost, high reliablity can be used in the operating conditions such as oil-poor, high temperature, heavy duty being difficult to using conventional oil
On the mechanical equipment of grease lubrication, there is good application in fields such as metallurgy, mine, the energy, automobile, war industry and nuclear industry
Prospect.
Detailed description of the invention
Fig. 1 is the CoCrFeNiS of arc melting method preparation0.25The X-ray diffraction of self-lubricating high-entropy alloy（XRD）Spectrogram.
Fig. 2 is the CoCrFeNiS of arc melting method preparation0.25The backscattered electron of self-lubricating high-entropy alloy microscopic structure
Picture.
Fig. 3 is the CoCrFeNiS of arc melting method preparation0.25Self-lubricating high-entropy alloy is in room temperature within the scope of 800 DEG C
Coefficient of friction.
Fig. 4 is the Al of applied powder metallurgy method preparation0.2CoCrFeNiS0.75The XRD spectra of self-lubricating high-entropy alloy.
Fig. 5 is the Al of applied powder metallurgy method preparation0.2CoCrFeNiS0.75The back of self-lubricating high-entropy alloy microscopic structure dissipates
Penetrate charge pattern.
Fig. 6 is the Al of powder metallurgic method preparation0.2CoCrFeNiS0.75Self-lubricating high-entropy alloy is in room temperature to 800 DEG C of ranges
Interior coefficient of friction.
Specific embodiment
Elaborate below to the embodiment of the present invention, the present embodiment be under the premise of the technical scheme of the present invention into
Row is implemented, and the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following realities
Example is applied, it is all to be all belonged to the scope of the present invention based on the technology that the content of present invention is realized.
Embodiment 1
It selects Co, Cr, Fe, Ni and FeS block materials as raw material, is prepared using non-consumable vacuum arc melting technology
CoCrFeNiS0.25Self-lubricating high-entropy alloy.Main implementation steps are as follows：
1）According to CoCrFeNiS0.25The atomic percent of self-lubricating high-entropy alloy converses required Co, Cr, Fe, Ni and FeS
The mass percent of equal raw materials measures raw material according to mass percent.
2）The raw material surface of block to be polished, scale removal is then charged into dehydrated alcohol, it is cleaned by ultrasonic 10 min,
After the impurity for removing surface, drying is stand-by.
3）The block material cleaned up is fitted into the water jacketed copper crucible of arc-melting furnace, is evacuated to 10-3Pa with
Under, being then charged with high-purity argon gas to furnace pressure is 10 ~ 20 Pa, then is evacuated to 10-3Pa hereinafter, repeatedly three times,
Ensure that the foreign gas in furnace is excluded completely, being finally filled with high-purity argon gas makes the pressure in furnace in 10 ~ 20 Pa.
4）Melting electric current is adjusted to 10 ~ 60 A, melting voltage is adjusted to 5 ~ 30 V, then starting the arc melting, for guarantee at
Divide uniformly, at least melting 5 times applies manipulator that alloy pig is overturn 180 degree after the completion of each melting, is then carrying out next time
Melting.
5）After the completion of melting, alloy sample is taken out, removes the impurity on surface, obtains sulfur-bearing self-lubricating high-entropy alloy sample.
Using the object phase composition of the high-entropy alloy of X-ray diffractometer analysis preparation, result is as shown in Figure 1, it is seen that alloy
In only FCC phase and CrxSyPhase.Using its microscopic structure of sem analysis, Fig. 2 gives CoCrFeNiS0.25The high entropy of self-lubricating closes
The backscattered electron image of golden microscopic structure, wherein the object of black is mutually CrxSyPhase, and white object is mutually FCC phase.Using HT-1000
Type high temperature friction and wear testing machine tests its tribological property, and antithesis is Si when test3N4Ball, 5 N of load, sliding speed are
0.28 m/s, coefficient of friction are as shown in Figure 3, it is seen that the alloy in the range of room temperature is to 800 DEG C coefficient of friction 0.31 ~
Between 0.43, there is good wide temperature range self-lubricating property.
Embodiment 2
Selection pure metal powder Al, Co, Cr, Fe, Ni and FeS powder is raw material, the preparation of applied powder metallurgy method
Al0.2CoCrFeNiS0.75The high-entropy alloy of self-lubricating containing S, main implementation steps are as follows：
1）According to Al0.2CoCrFeNiS0.75Atomic percent converse the raw materials such as required Al, Co, Cr, Fe, Ni and FeS
Mass percent measures raw material powder according to mass percent.
2）Raw material powder is packed into planetary ball mill mixing, ratio of grinding media to material is 3 when mixing:1, drum's speed of rotation is 150 r/
Min, mixing time are 2 hours.
3）Uniformly mixed raw material is packed into graphite jig, hot pressed sintering is carried out in discharge plasma sintering sintering furnace,
50 DEG C/min of heating rate when sintering, 1200 DEG C of sintering temperature, 30 MPa of sintering pressure, the sintered heat insulating time is 10 min, is burnt
Furnace cooling after the completion of knot.
4）The impurity on the sample removal surface that sintering is obtained, obtains self-lubricating high-entropy alloy sample.
The object phase composition of alloy is analyzed using X-ray diffractometer, as a result as shown in Figure 4, it is seen that this alloy mainly by
FCC phase and CrxSyPhase composition.Fig. 5 is the Al of applied powder metallurgy method preparation0.2CoCrFeNiS0.75Self-lubricating high-entropy alloy is micro-
The backscattered electron image of tissue, it is seen that the wherein Cr of blackxSyIt is mutually uniformly distributed on FCC phase matrix.It is high using HT-1000 type
Warm friction wear testing machine tests its tribological property, and antithesis is Si when test3N4Ball, 5 N of load, sliding speed 0.28
m/s.Fig. 6 gives this room temperature of high-entropy alloy containing self-lubricating to the coefficient of friction within the scope of 800 DEG C, it is seen that it is in wide temperature range
With good self-lubricating property.
Above-described embodiment is only enumerated two kinds of sulfur-bearing self-lubricating high-entropy alloys and two different preparation methods, here without
Method enumerates all embodiments, all various changes extended out in technical solution disclosed by the invention
Or it changes still in the scope of protection of the present invention.
Claims (10)
1. a kind of sulfur-bearing self-lubricating high-entropy alloy, it is characterised in that the ingredient of the self-lubricating high-entropy alloy is MxCoCrFeNiSy, M
It is the atomic ratio of 0 ~ 2, S element for one or more of Al, Ti, Mo, V, Nb, Mn, W, Zr, the atomic ratio x of content
Example y value is 0.05 ~ 3, and the atomic ratio of other elements is 0.5 ~ 1.5.
2. self-lubricating high-entropy alloy as described in claim 1, it is characterised in that the sulfur-bearing self-lubricating high-entropy alloy mainly by
The high entropy solid solution phase and metal of FCC, BCC or FCC+BCC and the compound phase composition of sulphur.
3. self-lubricating high-entropy alloy as claimed in claim 2, it is characterised in that the compound of the metal and sulphur be mutually TiS,
TiS2、MoS2、VS、WS2、NbS2、MnS2、FeS、FeS2、ZrS、NiS、NiS2、Ni3S2、CoS、CoS2、CrS、Cr2S3、Cr3S4With
CrxSyOne or more of.
4. the preparation method of sulfur-bearing self-lubricating high-entropy alloy as described in any one of claims 1 to 3, it is characterised in that use
Preparation method is smelting process or powder metallurgic method.
5. preparation method as claimed in claim 4, it is characterised in that the smelting process be induction melting, electric arc melting, etc. from
Sub- melting, electron-beam smelting, electromagnetic levitation-melt or laser melting coating.
6. preparation method as claimed in claim 4, it is characterised in that the powder metallurgic method be pressureless sintering, hot pressed sintering,
Discharge plasma sintering, induction sintering or microwave sintering.
7. preparation method as claimed in claim 5, it is characterised in that prepare sulfur-bearing self-lubricating high-entropy alloy using smelting process
Key step is as follows：
1）Raw material are measured according to the composition proportion of sulfur-bearing self-lubricating high-entropy alloy；
2）Raw material are packed into smelting equipment, melt back 3 ~ 5 times, the ingredient of alloy are made to reach uniform；
3）It comes out of the stove after cooling, removes surface impurity, obtain sulfur-bearing self-lubricating high-entropy alloy finished product.
8. preparation method as claimed in claim 7, it is characterised in that cannot be using S as raw material.
9. preparation method as claimed in claim 6, it is characterised in that prepare the high entropy of sulfur-bearing self-lubricating using powder metallurgic method and close
The key step of gold is as follows：
1）Raw material powder is measured according to the composition proportion of sulfur-bearing self-lubricating high-entropy alloy；
2）Raw material powder is uniformly mixed；
3）Pre-molding is directly loadable into graphite jig and is sintered on agglomerating plant；5 ~ 200 DEG C/min of heating rate is burnt
600 ~ 1800 DEG C of junction temperature, 5 ~ 120 min of soaking time, pressure is 5 ~ 40 MPa when pressure sintering, after the completion of sintering
Furnace cooling；
4）After the completion of sintering, surface impurity is removed, obtains sulfur-bearing self-lubricating high-entropy alloy finished product.
10. the preparation method as described in claim 7 or 9, it is characterised in that the partial size of the raw material and raw material powder is small
In 150 microns.
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Cited By (8)
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|---|---|---|---|---|
| CN109702199A (en) * | 2019-02-26 | 2019-05-03 | 中国科学院兰州化学物理研究所 | A kind of high-entropy alloy-base self-lubricating oily bearing material |
| CN109913732A (en) * | 2019-03-21 | 2019-06-21 | 大连理工大学 | A kind of radiation resistance FCC configuration high-entropy alloy and preparation method thereof |
| CN110527869A (en) * | 2019-09-30 | 2019-12-03 | 沈阳大陆激光工程技术有限公司 | A kind of the self-lubricating abrasion-resistant phase material and its preparation process of laser manufacture guide ruler liner plate |
| CN111001799A (en) * | 2019-09-30 | 2020-04-14 | 安阳工学院 | TiNiCrNb-based self-lubricating pin shaft material with multilayer structure and preparation method thereof |
| CN112647009A (en) * | 2021-01-15 | 2021-04-13 | 中国科学院兰州化学物理研究所 | High-strength high-wear-resistance medium-entropy alloy and preparation method thereof |
| CN112723862A (en) * | 2020-12-29 | 2021-04-30 | 太原理工大学 | Method for preparing high-entropy oxide ceramic material simply and low in consumption |
| CN115341127A (en) * | 2022-09-20 | 2022-11-15 | 中国科学院兰州化学物理研究所 | Self-lubricating high-entropy alloy and preparation method and application thereof |
| CN115404387A (en) * | 2022-09-20 | 2022-11-29 | 中国科学院兰州化学物理研究所 | High-temperature wear-resistant high-entropy alloy and preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109702199A (en) * | 2019-02-26 | 2019-05-03 | 中国科学院兰州化学物理研究所 | A kind of high-entropy alloy-base self-lubricating oily bearing material |
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| CN110527869A (en) * | 2019-09-30 | 2019-12-03 | 沈阳大陆激光工程技术有限公司 | A kind of the self-lubricating abrasion-resistant phase material and its preparation process of laser manufacture guide ruler liner plate |
| CN111001799A (en) * | 2019-09-30 | 2020-04-14 | 安阳工学院 | TiNiCrNb-based self-lubricating pin shaft material with multilayer structure and preparation method thereof |
| CN110527869B (en) * | 2019-09-30 | 2021-06-15 | 沈阳大陆激光工程技术有限公司 | Self-lubricating wear-resistant phase material for laser-manufactured guide ruler lining plate and preparation process thereof |
| CN111001799B (en) * | 2019-09-30 | 2021-10-19 | 安阳工学院 | TiNiCrNb-based self-lubricating pin shaft material with multilayer structure and preparation method thereof |
| CN112723862A (en) * | 2020-12-29 | 2021-04-30 | 太原理工大学 | Method for preparing high-entropy oxide ceramic material simply and low in consumption |
| CN112647009A (en) * | 2021-01-15 | 2021-04-13 | 中国科学院兰州化学物理研究所 | High-strength high-wear-resistance medium-entropy alloy and preparation method thereof |
| CN115341127A (en) * | 2022-09-20 | 2022-11-15 | 中国科学院兰州化学物理研究所 | Self-lubricating high-entropy alloy and preparation method and application thereof |
| CN115404387A (en) * | 2022-09-20 | 2022-11-29 | 中国科学院兰州化学物理研究所 | High-temperature wear-resistant high-entropy alloy and preparation method and application thereof |
| CN115404387B (en) * | 2022-09-20 | 2023-08-22 | 中国科学院兰州化学物理研究所 | High-temperature wear-resistant high-entropy alloy and preparation method and application thereof |
| CN115341127B (en) * | 2022-09-20 | 2023-12-15 | 中国科学院兰州化学物理研究所 | Self-lubricating high-entropy alloy and preparation method and application thereof |
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