CN105219478A - The preparation method of the composite lubricated material of a kind of Graphene/zirconia nanopowder - Google Patents
The preparation method of the composite lubricated material of a kind of Graphene/zirconia nanopowder Download PDFInfo
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Abstract
The invention discloses the preparation method of the composite lubricated material of a kind of Graphene/zirconia nanopowder, concrete steps are as follows: by graphite oxide solution supersound process 1 ~ 2h, be uniformly dispersed and only had the graphene oxide suspension of 1 ~ 2 layer thickness, then being diluted with ultrapure water; Eight water zirconium oxychlorides are dissolved in ultrapure water and prepare zirconyl chloride solution; By the graphene oxide suspension after dilution and zirconyl chloride solution mixing, stir, and supersound process 10 ~ 30 minutes; In mixed solution, add hydrazine hydrate, react under hydrothermal conditions, wherein temperature of reaction is 150 ~ 220 DEG C, and the reaction times is 18 ~ 24h; Reacted black solid product ultrapure water is cleaned repeatedly, and lyophilize 6 ~ 12? h, obtains zirconium oxide nano-particle at the composite lubricated material of the homodisperse Graphene/zirconia nanopowder of graphenic surface.Preparation method of the present invention has the product purity advantages of higher that technique is simple, easy to operate, cost is low, prepare.
Description
Technical field
The invention belongs to inorganic nano composite material field, relate to the preparation method of the composite lubricated material of a kind of Graphene/zirconia nanopowder.
Background technology
2004, the AndreGeim professor of Univ Manchester UK and the computer MSR Information system of doctor KostyaNovoselov leader utilize a kind of simple micromechanics stripping method to obtain the Graphene of monoatomic layer thickness first, have led a revolution in this field thus.The performance of Graphene excellence and widely application prospect cause the unprecedented research enthusiasm of researchers.
Graphene is the two-dimension nano materials that thickness only has a carbon atom, is by sp
2hydbridized carbon atoms is arranged as cellular hexaplanar crystal, have high specific surface area, intensity, hardness, Young's modulus and strong unreactiveness and structural stability, the two-dimensional nanostructure of its uniqueness, excellent mechanics, process based prediction model make it in development high performance composite and functional materials, have huge application potential.In recent years, Graphene had more wide application prospect as new and effective lubricant in tribological field.Numerous investigator demonstrates Graphene good lubrication behavior (KandanurSS, RafieeMA, YavariF, etal. by Tribological Test from microcosmic and macro-scale
carbon 2012; 50:3178-83; EswaraiahV, SankaranarayananV, RamaprabhuS.
aCSApplMaterInterfaces , 2011; 3:4221-7; FengX, KwonS, ParkJY, etal.
aCSNano 2013; 7:1718-24; HunleyDP, FlynnTJ, DodsonT, etal.
physRevB 2013; 87:035417-21).In addition, the people such as Kim (LinLY, KimDE, KimWK, etal.
surfCoatTechnol 2011; Friction force microscope (FFM) 205:4864-9) is utilized to be studied multi-layer graphene micro-tribological behavior on a silicon substrate, although find that Graphene can reduce frictional force significantly, but when load increases to 5 μ N, there is obvious wear out failure in friction after 100 weeks in needle point.In addition, the people such as Berman (BermanD, ErdemirA.SumantAV.
carbon 2013; 59:167-75) have studied its macro-tribological properties by graphene dispersion to ethanol, result shows that the interpolation of Graphene can reduce the frictional coefficient of ethanol significantly, but loses efficacy immediately when load increases to 5N.As can be seen here, the Graphene with special size, low shearing force and surface energy can play friction-reducing and antiwear action well, namely can reduce frictional coefficient significantly and have higher antiwear property.But due to the thickness that Graphene is ultra-thin, there is inevitable defect and grain boundary in macroscopical sample, under larger load, its wear resistance has much room for improvement.In addition, the Intermolecular Forces that graphene film interlayer is stronger makes it easily produce to reunite and be insoluble in water and conventional organic solvent, thus as there is the problem of dispersion stabilization difference during lubricating oil additive, as the people such as Zhang Wei (Zhang Wei, Zhu Hongwei, Di Ze are superfine.
nanosecond science and technology 2011; 8:5-9) comparative study pure 150SN lubricating oil and the tribological property after with the addition of Graphene, find that pure 150SN oil can not complete friction-wear test under experimental conditions, and add the lubricating oil that massfraction is 0.001% Graphene, its frictional coefficient is comparatively stable, but when addition is increased to 0.005%, friction coefficient of lubricating oil becomes unstable.As can be seen here, these problems above-mentioned have had a strong impact on the widespread use of Graphene.
Zirconium white is a kind of important structure and function material, have that thermal conductivity is little, hardness and chemical stability and thermostability high, be widely used in the multiple fields such as pottery, refractory materials, machinery, photoelectricity, electronics, aerospace, biological and chemical.Based on zirconic above-mentioned excellent properties, the tribological property of investigator to zirconium white and matrix material thereof has carried out large quantity research.Such as, nano zircite joins in PAO-6 as lubricating oil additive by the people such as Battez, demonstrates zirconium oxide nano-particle suspension have good tribological property (BattezAH, GonzalezR, ViescaJL, etal. by rub(bing)test
wear , 2008; 265:422-8).The people such as the Zheng Shaohua zirconia/silica nano composite material that utilized Method in situ modification to prepare, the nano composite material of this surface modification has good diffusional stability in lubricating oil, thus improves tribological property (LiW, the ZhengSH of lubricating oil significantly, CaoBQ, etal.
jNanopartRes , 2011; 13:2129-37).
Metal oxide/graphene nanocomposite material can show the performance even characteristic of novelty of enhancing usually because of the synergistic effect between component; namely graphenic surface is carried on uniformly by inorganic nanoparticles; not only can solve the easy agglomeration of Graphene; the lubricity that grapheme material is good can be kept simultaneously; the high supporting capacity of Zirconium oxide can being made full use of again, making zirconium white/graphene nanometer composite as showing excellent tribological property during lubricating oil additive.But although researcher has carried out the preparation method of zirconium white/graphene complex, and be applied to different field, these preparation methods are only limitted to electrochemical deposition method and atomic layer deposition method.Recently, the people such as Wang Zonghua uses Na in water-Isopropanol Solvent
2s has prepared Graphene/zirconia composite as precipitation agent and reductive agent, but the method preparation process is more loaded down with trivial details.Up to the present, prepare zirconium white/graphene nanocomposite material by a step hydrothermal synthesis method and have no open report as the applied research of lubricating oil additive.
Summary of the invention
The object of the present invention is to provide the preparation method of the composite lubricated material of a kind of Graphene/zirconia nanopowder, this matrix material has the features such as dispersion stabilization in straight lubrication oil is good, tribological property is excellent, its preparation process simple and fast, can repetitive operation, is easy to scale operation.
The nanoscale zirconia particle that the composite lubricated material of Graphene/zirconia nanopowder prepared by the present invention is disperseed by Graphene and its surface uniform of laminated structure forms, wherein the median size of nano zirconia particles is about 5nm, and graphene film generation gauffer illustrates to only have the Graphene of several individual layer stacking.
The preparation method of the composite lubricated material of Graphene/zirconia nanopowder proposed in the present invention, concrete steps are as follows:
1) by graphite oxide solution supersound process 1 ~ 2h, be uniformly dispersed and only had the graphene oxide suspension of 1 ~ 2 layer thickness, then being diluted with ultrapure water;
2) eight water zirconium oxychlorides are dissolved in ultrapure water prepare zirconyl chloride solution;
3) by the graphene oxide suspension after dilution and zirconyl chloride solution mixing, stir, and supersound process 10 ~ 30 minutes;
4) in the mixed solution of step 3), add hydrazine hydrate, react under hydrothermal conditions, wherein temperature of reaction is 150 ~ 220 DEG C, and the reaction times is 18 ~ 24h;
5) reacted black solid product ultrapure water is cleaned, and lyophilize 6 ~ 12h, obtain zirconium oxide nano-particle at the composite lubricated material of the homodisperse Graphene/zirconia nanopowder of graphenic surface.
The concentration of the graphene oxide suspension after described step 1) dilution is 2.0 ~ 2.8mg/mL.
The concentration of described zirconyl chloride solution is 10 ~ 25mM.
The volume of hydrazine hydrate used accounts for 0.15 ~ 0.25% of mixeding liquid volume.
Graphene oxide suspension after described dilution and the volume ratio of zirconyl chloride solution are 7:1 ~ 1:2.
Described graphite oxide solution is prepared by Hummers method.
Graphite oxide suspension is very easily peeled off through supersound process, forms the homodisperse graphene oxide suspension only having 1 ~ 2 layer.Due in graphene oxide lamella and lamella marginal distribution a large amount of carboxyl, hydroxyl, epoxy group(ing) isoreactivity functional group, ionization makes graphene oxide with a large amount of negative charges in the solution, very easily with the zirconium base complex generation electrostatic attraction of positively charged, thus be adsorbed on graphene oxide lamella, make its original position nucleating growth on graphene oxide sheet, and oxygenolysis is zirconium oxide nano-particle at high temperature under high pressure.
Observed by transmission electron microscope (TEM) and high-resolution-ration transmission electric-lens (HRTEM) with distribution the pattern of obtained product, its thing phase component is by X-ray powder diffraction (XRD) qualification.
The composite lubricated material of Graphene/zirconia nanopowder disclosed by the invention, the concrete steps applied in rub(bing)test are as follows:
(1) using Graphene/zirconia nanocomposite as lubricating oil additive, with reference to a certain amount of lubricating base oils, take by different mass mark (0.01% ~ 1%), obtain finely dispersed lubricating oil by ultrasonic, and for rub(bing)test;
(2) additive level of concentration optimum in step (1) is filtered out by rub(bing)test;
(3) adopt in (2) optimal concentration selected, carry out different additive contrast rub(bing)test (control sample is respectively: straight lubrication oil, with the addition of graphite lubricating oil, with the addition of zirconic lubricating oil, with the addition of Graphene/zirconic lubricating oil, with the addition of the lubricating oil of Graphene, with the addition of the lubricating oil of zine dialkyldithiophosphates (ZDDP)).
The present invention has following advantage:
(1) the present invention's composite lubricated material of Graphene/zirconia nanopowder that adopted one step hydro thermal method to prepare, have technique simple, can repetitive operation, with short production cycle and be easy to the advantages such as scale operation.
(2) Graphene/zirconia nanocomposite of preparing of the present invention, be made up of the Graphene of nano-lamellar structure and a large amount of nano zirconia particles of Dispersion on surface thereof, wherein the median size of nano zirconia particles is about 5nm, and graphene film only has the thickness of 1 ~ 2 layer.Due to zirconic intercalation, graphene film is made to be not easy to reunite, and zirconium oxide nano-particle is also because the dispersion of Graphene and carrying interaction energy are evenly distributed in graphenic surface, two-way interaction, the dispersiveness of Graphene in lubricating base oils and stability effectively can be improved.
(3) the composite lubricated material of Graphene/zirconia nanopowder prepared of the present invention, make full use of the excellent lubricity of Graphene and high mechanical property feature, simultaneously again in conjunction with Zirconia particles hardness and the feature such as chemical stability is high and tribological property is excellent, obtain the matrix material of excellent combination property, especially significant tribological property.
Accompanying drawing explanation
Fig. 1 is the TEM photo of Graphene/zirconia nanocomposite (embodiment 2) prepared by the present invention, and as can be seen from the figure zirconia particles is evenly distributed on graphene sheet layer, and the product namely obtained is Graphene/zirconia nanocomposite.
Fig. 2 is high-resolution-ration transmission electric-lens (HRTEM) photo of Graphene/zirconia nanocomposite (embodiment 2) prepared by the present invention, and clearly can find out zirconic two-dimensional crystal lattice picture from figure, its spacing is 0.296nm, corresponding to tetragonal ZrO
2(111) crystal face, its average crystal grain is about 5nm.
Fig. 3 is the XRD figure of Graphene/zirconia nanocomposite (embodiment 2) prepared by the present invention, and it is compared discovery with standard card (JCPDSPDFNo.49-1642), does not have other impurity peaks except zirconic peak, the sample purity prepared by explanation is high.
Fig. 4 is the average friction coefficient of bloom in Graphene/zirconia nanocomposite (embodiment 2) of preparing of the present invention and different additive contrast experiment situation, wear volume and wear rate; As can be seen from the table, matrix material significantly can improve the tribological property of pure oil as lubricating oil additive.
Embodiment
Embodiment 1: the preparation method of the composite lubricated material of a kind of Graphene/zirconia nanopowder
Raw material adopts graphite oxide solution, eight water zirconium oxychlorides, ultrapure water and hydrazine hydrate, its preparation process is specially: first by obtained graphite oxide solution ultrasonic disperse 2h, obtaining and only have the graphene oxide suspension of 1 ~ 2 layer thickness, is then 2.33mg/mL by its concentration dilution; Compound concentration is the zirconyl chloride solution of 10mM simultaneously, subsequently above-mentioned graphene oxide suspension and zirconyl chloride solution are respectively measured 30mL, mixing and stirring, and supersound process 30 minutes, then the hydrazine hydrate of 1mL is added to this mixing solutions, at the Water Under thermal response 18h of 180 DEG C, the black solid thing ultrapure water obtained to be washed, lyophilize process, finally obtain Graphene/zirconia nanocomposite.
Embodiment 2: the preparation method of a kind of Graphene/zirconia nanopowder lubricant
Raw material adopts graphite oxide solution, eight water zirconium oxychlorides, ultrapure water and hydrazine hydrate, its preparation process is specially: first by obtained graphite oxide solution ultrasonic disperse 2h, obtaining and only have the graphene oxide suspension of 1 ~ 2 layer thickness, is then 2.33mg/mL by its concentration dilution; Compound concentration is the zirconyl chloride solution of 10mM simultaneously, measure the above-mentioned graphene oxide suspension of 40mL and the above-mentioned zirconyl chloride solution of 20mL subsequently, and by the two mixing and stirring, supersound process 30 minutes, then the hydrazine hydrate of 1mL is added to this mixing solutions, at the Water Under thermal response 18h of 180 DEG C, the black solid thing ultrapure water obtained to be washed, lyophilize process, finally obtain Graphene/zirconia nanocomposite.
Embodiment 3: the preparation method of a kind of Graphene/zirconia nanopowder lubricant
Raw material adopts graphite oxide solution, eight water zirconium oxychlorides, ultrapure water and hydrazine hydrate, its preparation process is specially: first by obtained graphite oxide solution ultrasonic disperse 2h, obtaining and only have the graphene oxide suspension of 1 ~ 2 layer thickness, is then 2.33mg/mL by its concentration dilution; Compound concentration is the zirconyl chloride solution of 10mM simultaneously; Measure the above-mentioned graphene oxide suspension of 45mL and the above-mentioned zirconyl chloride solution of 15mL subsequently, and by the two mixing and stirring, supersound process 30 minutes, then the hydrazine hydrate of 1mL is added to this mixing solutions, at the Water Under thermal response 18h of 180 DEG C, the black solid thing ultrapure water obtained is washed, lyophilize process, finally obtain Graphene/zirconia nanocomposite.
Claims (5)
1. a preparation method for the composite lubricated material of Graphene/zirconia nanopowder, is characterized in that concrete steps are as follows:
1) by graphite oxide solution supersound process 1 ~ 2h, be uniformly dispersed and only had the graphene oxide suspension of 1 ~ 2 layer thickness, then being diluted with ultrapure water;
2) eight water zirconium oxychlorides are dissolved in ultrapure water prepare zirconyl chloride solution;
3) by the graphene oxide suspension after dilution and zirconyl chloride solution mixing, stir, and supersound process 10 ~ 30 minutes;
4) in the mixed solution of step 3), add hydrazine hydrate, react under hydrothermal conditions, wherein temperature of reaction is 150 ~ 220 DEG C, and the reaction times is 18 ~ 24h;
5) reacted black solid product ultrapure water is cleaned, and lyophilize 6 ~ 12h, obtain zirconium oxide nano-particle at the composite lubricated material of the homodisperse Graphene/zirconia nanopowder of graphenic surface.
2. the method for claim 1, is characterized in that the concentration of the graphene oxide suspension after the dilution of described step 1) is 2.0 ~ 2.8mg/mL.
3. the method for claim 1, is characterized in that the concentration of described zirconyl chloride solution is 10 ~ 25mM.
4. the method for claim 1, is characterized in that the volume of hydrazine hydrate used accounts for 0.15 ~ 0.25% of mixeding liquid volume.
5. the method for claim 1, is characterized in that the volume ratio of the graphene oxide suspension after described dilution and zirconyl chloride solution is 7:1 ~ 1:2.
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