CN1221645C - Hub structural nano solid lubricant and preparaton method - Google Patents
Hub structural nano solid lubricant and preparaton method Download PDFInfo
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- CN1221645C CN1221645C CN 200410020424 CN200410020424A CN1221645C CN 1221645 C CN1221645 C CN 1221645C CN 200410020424 CN200410020424 CN 200410020424 CN 200410020424 A CN200410020424 A CN 200410020424A CN 1221645 C CN1221645 C CN 1221645C
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Abstract
The present invention discloses a nanometer solid lubricant with a core-shell structure and a preparation method thereof. Particles of the lubricant are very easy to roll under the action of tangential force, and form transfer films at the surfaces of matching members which relatively move. The nanometer solid lubricant has a very strong extreme pressure resistant characteristic. A friction coefficient can be greatly lowered, and abrasion can be relieved. The nanometer solid lubricant can be suitable for severe environments of high temperature, high speed, etc. First, S or Se is coated at the surface of a spherical nanometer W particle or a nanometer Mo particle; second, coating matter S or Se, and metal Mo or W carry out vulcanization reaction in hydrogen atmosphere and at certain temperature; finally, a uniform lubrication shell layer of MoS2, MoSe2 or WS2 and WSe2 is synthesized at the surface of the nanometer Mo particle or the spherical nanometer W particle to obtain the nanometer solid lubricant. Due to the fact that the particle size of the lubricant is in a nanometer grade, the lubricant can be independently used, and can also used as an additive to be compounded with lubrication oil (ester) to be used.
Description
Technical field:
The present invention relates to the power lubrication technical field, exactly, it is that a kind of surface at nanometer molybdenum (Mo) or nanometer tungsten (W) particulate synthesizes uniform molybdenumdisulphide (MoS
2), two selenizing molybdenum (MoSe
2) or tungsten disulfide (WS
2), two selenizing tungsten (WSe
2) shell, and the Mo/MoS that obtains
2, Mo/MoSe
2Or W/WS
2, W/WSe
2Nano solid lubricant of nucleocapsid structure and preparation method thereof.
Background technology:
In mechanisms such as mechanical transmission, driving, support, no matter be sliding friction or rolling resistance, except that utilizing friction working, people always wish that the frictional coefficient between the friction pair is the smaller the better.For reaching the purpose that reduces friction, adopt the mode that between friction pair, adds lubricant usually, reduce frictional coefficient between the friction pair, alleviate friction, assurance equipment normally, operation safely.Thereby the performance of improvement lubricant can not only reduce the wearing and tearing of component effectively, and the working life of prolonged mechanical equipment can also save power, increase work efficiency, reduces operating noise; For machining equipment, can also improve the working accuracy of workpiece.
As lubricant, two kinds of liquid and solids are generally arranged, traditional solid lubricant mainly is made of soft solid and the laminate structure solid that is easy to generate layer slippage, wherein MoS
2, MoSe
2And WS
2, WSe
2Be four kinds of main raws in the sulfide-based solid lubricant.That this solid lubricant has is high temperature resistant, low temperature resistant, be difficult for evaporation, radioprotective, anticorrosive, anti-extreme pressure is strong, advantage such as free from environmental pollution.In the innovation and creation aspect solid lubricant, Chinese patent application number is: 01130864.8, publication number is: the disclosed solid lubricant of CN1337452A, its main component is MoS
2Add auxiliary agents such as Ca-S dispersion agent, ZDDP oxidation inhibitor, PIB tackifier more therein, its lubrication principle also is the laminate structure of utilizing them to have, the characteristics of easy form layers slippage, play lubricated effect at even part friction surface, and the basic structure of its particle does not change.Compare with liquid and semi-solid lubricants (lubricating ester), this class solid lubricant exists still that frictional coefficient is higher, the shortcoming of cooling heat dissipation difference; In addition, the comparatively thick sulfide-based solid lubricant of particle also is difficult to and the compound use of lubricating oil (ester), and brings influence can for the matching precision of even part.
Summary of the invention:
The objective of the invention is to utilize the electrical explosion technology to obtain the particulate of nano-level sphere W and Mo, again through the coating and the sulfuration of sulphur (S) or selenium (Se), preparing a kind of inside is that hard solid nuclear, surface are nano level micro mist for lubricated shell, mean diameter, and then overcome the deficiency that prior art exists, provide a kind of being easy to form transfer film, have stronger anti-extreme pressure property on the even part surface of relative movement, can reduce friction system significantly, alleviate wearing and tearing, be applicable to nuclear shell structure nano solid lubricant lubricated under the severe rugged environments such as high temperature, high speed.
Nucleocapsid structure solid lubricant of the present invention is microparticle surfaces coating S or the Se at ball shaped nano W or nanometer Mo, under nitrogen atmosphere and certain temperature, make coating S or Se and metal W or Mo carry out vulcanization reaction then, finally synthesize uniform MoS on the surface of W or Mo particulate
2, MoSe
2Or WS
2, WSe
2Lubricated shell obtain.
The particle diameter of described ball shaped nano W or nanometer Mo micro mist is 60nm--90nm, and coating is S or Se; The solvent of S or Se is tetracol phenixin (CCl
4) and dithiocarbonic anhydride (CS
2) mixed solution; Vulcanization reaction carries out in hydrogen; The explosion chamber gaseous media is an argon gas.
Ball shaped nano W of the present invention or nanometer Mo micropowder preparing process are: the raw material of W or Mo micro mist is that purity is higher than 99.95% silk material.Electrical explosion chamber (8) are evacuated to below the 1Pa, in explosion chamber (8), charge into high purity (99.999%) argon gas to 0.25MPa--0.35Mpa; Diameter is that W or the Mo silk of 0.3mm--0.36mm sent in the electrical explosion district (5) continuously by wire drive feeder (7); In electrical explosion district (5) length is that 7cm--9cm, working direct current high-voltage power supply (1) are under the condition of 1.6 μ F--2.4 μ F for 30KV--36KV, capacitor bank (2) total capacitance, prepares nanometer W or nanometer Mo spherical particle powder that diameter is 60nm--90nm.
The S of nanometer W of the present invention or nanometer Mo particulate or the method for coating of Se are: with volume ratio is 1: the ratio of 1--1.5, and with tetracol phenixin (CCl
4) and dithiocarbonic anhydride (CS
2) make mixed solvent; Be blended into 150--200 gram S or 130--180 gram Se in every liter solvent; Me/X=1.4--1.9 (Me:W, Mo in molar ratio; X:S Se), gets nanometer W or nanometer Mo and adds in the above-mentioned mixing liquid of dissolved, stirs 10--20 minute; With ultrasonic concussion dispersing nanometer powder, kept 15-30 minute; Solvent is removed in underpressure distillation again; Obtain nanometer W or nanometer Mo powder that the surface coats S or Se.In the mixing solutions of converting that contains S or Se, add the nanometer W or the nanometer Mo powder of different amounts, can obtain different nanometer W of S or Se covering amount or nanometer Mo powder.
The nanometer W that S of the present invention or Se coat or the vulcanization reaction method of nanometer Mo powder are: the nanometer W or the nanometer Mo powder of an amount of S or Se coating are encased in the vulcanization reaction chamber, reaction chamber is evacuated to below the 1pa, charge into hydrogen to 0.05Mpa--0.09Mpa to reaction chamber, reaction chamber is heated to 360 ℃--and 560 ℃, it is constant to keep the reaction chamber hydrogen-pressure, constant temperature 2 hours--and 4 hours.Cool to room temperature then with the furnace, acquisition be Me/Me X
2(Me:W or Mo, X:S or Se) nuclear shell structure nano solid lubricant.
Solid lubricant of the present invention, its inside are hard solid nuclear, and the surface is lubricated shell, and micro powder granule is spherical, and mean diameter is below 100nm, thereby this lubricant is equivalent to numerous Miniature ball.Compare with existing solid lubricant, this lubricant particulate under the effect of tangential force very easily produces rolling, not only can make even part in relative movement, realize rolling resistance, but also be easy to form transfer film, and have stronger anti-extreme pressure property on even part surface by this lubricant.Thereby can reduce frictional coefficient significantly, alleviate wearing and tearing, improve the serviceability of even parts such as gear, the working life of prolonged mechanical component.Because the particle size of this lubricant is at nano level, so it can also be as additive and the compound use of lubricating oil (ester), this also improves its over-all properties greatly.In addition, the wearing and tearing that the present invention can obviously alleviate the abrasive particle mating plate under the situation that has abrasive particle to exist.The present invention can demonstrate its good lubricating property especially under severe rugged environments such as high temperature, high speed.
Description of drawings:
Fig. 1 is the principle schematic that the present invention is used to prepare the electrical explosion device of ball shaped nano W or nanometer Mo powder.
Among the figure: the 1st, DC high-voltage power supply, the 2nd, electrical condenser group, the 3rd, plasma discharge tube, the 4th, plate target, the 5th, blast area, the 6th, negative electrode, the 7th, W or Mo raw material thread are supplied with drive system, the 8th, explosion chamber, the 9th, ground wire.
Embodiment:
Embodiment 1:
The preparation of nanometer W or nanometer Mo micro mist: the mean diameter of ball shaped nano W or nanometer Mo is relevant with the total capacitance of selected material filament diameter, plate target and cloudy interpolar electrical explosion section length, the high direct voltage that is provided and electrical condenser group.
Electrical explosion chamber 8 is evacuated to below the 1Pa, in explosion chamber 8, charge into the argon gas of high purity (99.999%), ar pressure is that 0.28Mpa, electrical explosion section length are that 8cm, working direct current high pressure are that 35KV, capacitor bank total capacitance are under the condition of 2.4 μ F in electrical explosion chamber 8, the W silk that purity is higher than 99.95%, diameter is 0.33mm is sent in the electrical explosion district 5 continuously by wire drive feeder 7, and the ball shaped nano W particulate mean diameter of preparing is 80nm.
Electrical explosion chamber 8 is evacuated to below the 1Pa, in explosion chamber 8, charge into the argon gas of high purity (99.999%), ar pressure is 0.25Mpa in electrical explosion chamber 8,, the electrical explosion section length is that 8cm, working direct current high pressure are that 33KV, capacitor bank total capacitance are under the condition of 2.0 μ F, the Mo silk that purity is higher than 99.95%, diameter is 0.33mm is sent in the electrical explosion district 5 continuously by wire drive feeder 7, and the ball shaped nano Mo particulate mean diameter of preparing is 65nm.
Embodiment 2:
The S of nanometer W or nanometer Mo or Se coat:
Respectively get the CS of 500ml
2And CCl
4Solvent is made mixed solvent, gets 160 gram S and joins in the solvent, stirs S is dissolved fully, makes mixed solution; Get 1.5 kilograms of nanometer W or 0.8 kilogram of nanometer Mo joins in the mixed solution, stirred 15 minutes; Disperseed 25 minutes with ultrasonic concussion then; Solvent is removed in underpressure distillation again; Obtain the powder of S clad nano W or S clad nano Mo.
Respectively get the CS of 500ml
2And CCl
4Solvent is made mixed solvent, gets 150 gram Se and joins in the solvent, stirs Se is dissolved fully, makes mixed solution; Get 0.6 kilogram of nanometer W or 0.3 kilogram of nanometer Mo joins in the mixed solution, stirred 15 minutes; Disperseed 25 minutes with ultrasonic concussion then; Solvent is removed in underpressure distillation again; Obtain the powder of Se clad nano W or Se clad nano Mo.
In the mixing solutions of converting that contains S or Se, add the nanometer W or the nanometer Mo of different amounts, can obtain S or the different nano-powder of Se covering amount.
Embodiment 3:
Vulcanization reaction
Nanometer W or nanometer Mo that the S that packs in reaction chamber coats, reaction chamber is evacuated to below the 1pa, charges into hydrogen to 0.07Mpa to reaction chamber, and reaction chamber is heated to 390 ℃, and it is constant to keep the reaction chamber hydrogen-pressure, constant temperature 4 hours.Cool to room temperature then with the furnace, obtain W/WS
2Or Mo/MoS
2The nuclear shell structure nano solid lubricant.
Embodiment 4:
Nanometer W or nanometer Mo that the Se that packs in reaction chamber coats, reaction chamber is evacuated to below the 1pa, charges into hydrogen to 0.08Mpa to reaction chamber, and reaction chamber is heated to 490 ℃, and it is constant to keep the reaction chamber hydrogen-pressure, constant temperature 4 hours.Cool to room temperature then with the furnace, promptly obtain W/WSe
2Or Mo/MoSe
2The nuclear shell structure nano solid lubricant.
Claims (3)
1, nuclear shell structure nano is characterized in that because of the body lubricant: the diameter that the electrical explosion method produces is that the W of 60nm-90nm or the spherical particle surface of Mo coat S or Se, behind the vulcanization reaction, produces MoS at W or Mo microparticle surfaces
2, MoSe
2Or WS
2, WSe
2The micro mist of evenly lubricated shell.
2, nuclear shell structure nano solid lubricant according to claim 1 is characterized in that: the explosion chamber gaseous media is an argon gas, and the solvent of coating S or Se is tetracol phenixin CCl
4With dithiocarbonic anhydride CS
2Mixed solution, vulcanization reaction carries out in hydrogen.
3, the preparation method of a kind of nuclear shell structure nano solid lubricant as claimed in claim 1 is as follows, it is characterized in that:
(a) preparation of ball shaped nano W or nanometer Mo micro mist: the raw material of W or Mo micro mist is that purity is higher than 99.95% silk material, electrical explosion chamber (8) are evacuated to below the 1Pa, in explosion chamber (8), charge into purity and be higher than 99.999% argon gas to 0.25MPa-0.35MPa, diameter is that W or the Mo silk of 0.3mm-0.36mm sent in the electrical explosion district (5) continuously by wire drive feeder (7), length is 7cm-9cm in electrical explosion district (5), working direct current high-voltage power supply (1) is 30KV-36KV, capacitor bank (2) total capacitance is under the condition of 1.6 μ F-2.4 μ F, prepares nanometer W or nanometer Mo spherical particle powder that diameter is 60nm-90nm;
(b) nanometer W or the S of nanometer Mo particulate or the coating of Se: with volume ratio is 1: 1-1: 5 ratio, and with tetracol phenixin CCl
4With dithiocarbonic anhydride CS
2Make mixed solvent, every liter solvent is converted sulphur 150-200 gram or selenium 130-180 gram, Me/X=1.4-1.9 in molar ratio, and Me is W, Mo; X is S, and Se gets nanometer W or nanometer Mo and adds in the above-mentioned mixing liquid of dissolved, stirs 10-20 minute, with ultrasonic concussion dispersing nanometer powder, keeps 15-30 minute; Solvent is removed in underpressure distillation again;
(c) the nanometer W of S or Se coating or the vulcanization reaction of nanometer Mo powder: the nanometer W or the nanometer Mo powder of S or Se coating are encased in the vulcanization reaction chamber, reaction chamber is evacuated to below the 1Pa, charge into hydrogen to 0.05MPa-0.09MPa to reaction chamber, reaction chamber is heated to 360 ℃--and 560 ℃, it is constant to keep the reaction chamber hydrogen-pressure, constant temperature 2 hours-4 hours cools to room temperature then with the furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410020424 CN1221645C (en) | 2004-04-20 | 2004-04-20 | Hub structural nano solid lubricant and preparaton method |
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|---|---|---|---|
| CN 200410020424 CN1221645C (en) | 2004-04-20 | 2004-04-20 | Hub structural nano solid lubricant and preparaton method |
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|---|---|
| CN1563299A CN1563299A (en) | 2005-01-12 |
| CN1221645C true CN1221645C (en) | 2005-10-05 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7632788B2 (en) * | 2005-12-12 | 2009-12-15 | Afton Chemical Corporation | Nanosphere additives and lubricant formulations containing the nanosphere additives |
| CN101993759A (en) * | 2009-08-12 | 2011-03-30 | 吉林师范大学 | Nanoscale lubricating oil additive and application thereof |
| CN101898750B (en) * | 2009-10-28 | 2012-05-23 | 无锡润鹏复合新材料有限公司 | Solid lubricating oil additive MoSe2 nanosheet and preparation method thereof |
| CN104128612B (en) * | 2014-08-20 | 2017-01-11 | 武汉科技大学 | W@WS2 core/shell nano-powder and preparation method thereof |
| CN112899060B (en) * | 2021-03-03 | 2022-03-25 | 中国科学院兰州化学物理研究所 | Preparation and application of molybdenum disulfide/zinc sulfide hybrid lubricating additive |
| CN115502393A (en) * | 2022-08-10 | 2022-12-23 | 中国第一汽车股份有限公司 | Application of core-shell structure nanoparticles in surface coating of gear steel and cold spraying method thereof |
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