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CN112940825B - Application of silicon phosphide quantum dots as lubricating oil additive, lubricating oil and preparation method and application thereof - Google Patents

Application of silicon phosphide quantum dots as lubricating oil additive, lubricating oil and preparation method and application thereof Download PDF

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CN112940825B
CN112940825B CN202110165316.6A CN202110165316A CN112940825B CN 112940825 B CN112940825 B CN 112940825B CN 202110165316 A CN202110165316 A CN 202110165316A CN 112940825 B CN112940825 B CN 112940825B
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CN112940825A (en
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王道爱
于童童
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Qingdao Center Of Resource Chemistry & New Materials (qingdao Research Development Center Lanzhou Institute Of Chemical Physics Chinese Academy Of Sciences)
Lanzhou Institute of Chemical Physics LICP of CAS
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/26Compounds containing silicon or boron, e.g. silica, sand
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04Mixtures of base-materials and additives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10Compounds containing silicon
    • C10M2201/105Silica
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/02Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/028Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
    • C10M2205/0285Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms used as base material
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2205/00Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
    • C10M2205/16Paraffin waxes; Petrolatum, e.g. slack wax
    • C10M2205/163Paraffin waxes; Petrolatum, e.g. slack wax used as base material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/28Esters
    • C10M2207/2805Esters used as base material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/1033Polyethers, i.e. containing di- or higher polyoxyalkylene groups used as base material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/104Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
    • C10M2209/1045Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only used as base material

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  • Lubricants (AREA)

Abstract

The invention relates to the technical field of lubricating oil additives, in particular to application of silicon phosphide quantum dots as a lubricating oil additive, lubricating oil and a preparation method and application thereof. The invention provides an application of a silicon phosphide quantum dot as a lubricating oil additive. The invention provides lubricating oil which comprises silicon phosphide quantum dots and base oil. The results of the examples show that the lubricating oil provided by the invention has excellent wear-reducing and wear-resisting properties relative to base oil, the friction coefficient is reduced by 18%, and the wear-resisting spot diameter is reduced by 63.5%.

Description

磷化硅量子点作为润滑油添加剂的应用、一种润滑油及其制 备方法和应用Application of silicon phosphide quantum dots as lubricating oil additive, a kind of lubricating oil and its preparation method and application

技术领域technical field

本发明涉及润滑油添加剂技术领域,具体涉及磷化硅量子点作为润滑油添加剂的应用、一种润滑油及其制备方法和应用。The invention relates to the technical field of lubricating oil additives, in particular to the application of silicon phosphide quantum dots as lubricating oil additives, a lubricating oil and a preparation method and application thereof.

背景技术Background technique

随着生产科技的发展,发动机、农机设备以及微机电系统等大力发展,对于润滑油的要求也是越来越高。润滑油是作用于机械摩擦部分的物质,主要用于润滑、冷却和密封。另外,在工业生产中,润滑油还会对摩擦部分起到清洗、防止污染等作用。为了提高润滑油的润滑效果,通常润滑油中会含有润滑添加剂,可以极大的提高润滑油的润滑性能和抗摩擦性能。对于新型润滑添加剂的探索一直以来都是解决优质润滑添加剂问题的重要的措施。With the development of production technology, the vigorous development of engines, agricultural machinery equipment and micro-electromechanical systems, the requirements for lubricating oil are also getting higher and higher. Lubricating oil is a substance that acts on the mechanical friction part, and is mainly used for lubrication, cooling and sealing. In addition, in industrial production, lubricating oil can also clean the friction part and prevent pollution. In order to improve the lubricating effect of the lubricating oil, lubricating additives are usually contained in the lubricating oil, which can greatly improve the lubricating performance and anti-friction performance of the lubricating oil. The exploration of new lubricating additives has always been an important measure to solve the problem of high-quality lubricating additives.

近年来,二维材料因为其层内采用共价键链接,层间采用范德华力链接,既可以作为一种新型的固体润滑剂,又可以作为一种优良的润滑添加剂,成为研究固体润滑与润滑添加剂的热点材料。然而,现有的二维材料仍然存在一定的问题,比如石墨烯的带隙为零、容易团聚,二硫化钼(MoS2)在潮湿的环境中易于发生潮解而失效等问题,从而限制了其应用,因此急需对新型的二维材料作为润滑添加剂方面的应用进行探索。In recent years, two-dimensional materials can be used as a new type of solid lubricant and as an excellent lubricant additive because of the covalent bonds in the layers and the van der Waals force between the layers. Additive hot spot material. However, the existing 2D materials still have certain problems, such as the zero band gap of graphene, easy agglomeration, and the failure of molybdenum disulfide (MoS 2 ) due to deliquescence in a humid environment, which limits its use. Therefore, it is urgent to explore the application of new two-dimensional materials as lubricant additives.

发明内容SUMMARY OF THE INVENTION

有鉴于此,本发明提供了磷化硅量子点作为润滑油添加剂的应用、一种润滑油及其制备方法和应用,本发明提供的润滑油以SiP量子点作为润滑油添加剂,在润滑油中的分散性良好,使润滑油减磨抗磨性能显著提高,摩擦系数平均值为0.064~0.072。In view of this, the present invention provides the application of silicon phosphide quantum dots as lubricating oil additives, a kind of lubricating oil and its preparation method and application. The lubricating oil provided by the present invention uses SiP quantum dots as lubricating oil additives, in lubricating oil The dispersion of the lubricating oil is good, so that the anti-wear and anti-wear performance of the lubricating oil is significantly improved, and the average friction coefficient is 0.064 to 0.072.

为实现上述目的,本发明提供了如下方案:For achieving the above object, the present invention provides the following scheme:

本发明提供了SiP量子点作为润滑油添加剂的应用。The present invention provides the application of SiP quantum dots as lubricating oil additives.

优选的,所述SiP量子点的平均粒径为8~15nm,平均厚度为1~3nm;所述SiP量子点在润滑油中的质量百分数为0.01~0.1%。Preferably, the average particle size of the SiP quantum dots is 8-15 nm, and the average thickness is 1-3 nm; the mass percentage of the SiP quantum dots in the lubricating oil is 0.01-0.1%.

本发明提供了一种润滑油,包括SiP量子点和基础油。The present invention provides a lubricating oil comprising SiP quantum dots and base oil.

优选的,所述SiP量子点的平均粒径为8~15nm,平均厚度为1~3nm;所述SiP量子点在润滑油中的质量百分数为0.01~0.1%。Preferably, the average particle size of the SiP quantum dots is 8-15 nm, and the average thickness is 1-3 nm; the mass percentage of the SiP quantum dots in the lubricating oil is 0.01-0.1%.

优选的,所述基础油为聚乙二醇基础油、聚醚类基础油或合成酯类基础油。Preferably, the base oil is polyethylene glycol base oil, polyether base oil or synthetic ester base oil.

优选的,所述SiP量子点的制备方法,包括以下步骤:Preferably, the preparation method of the SiP quantum dots includes the following steps:

将SiP粉体和极性有机溶剂混合后,依次进行超声剥离、搅拌、固液分离和取上清液干燥,得到所述SiP量子点;After mixing the SiP powder and the polar organic solvent, ultrasonic peeling, stirring, solid-liquid separation and drying of the supernatant are sequentially performed to obtain the SiP quantum dots;

所述SiP粉体的平均粒径为1~100μm,平均厚度为500~2000nm;The average particle size of the SiP powder is 1-100 μm, and the average thickness is 500-2000 nm;

所述SiP量子点的平均粒径为8~15nm,平均厚度为1~3nm。The SiP quantum dots have an average particle size of 8-15 nm and an average thickness of 1-3 nm.

优选的,所述极性有机溶剂包括丙酮、无水乙醇、二甲基亚砜、N-甲基吡咯烷酮和二甲基甲酰胺中的一种或多种。Preferably, the polar organic solvent includes one or more of acetone, absolute ethanol, dimethyl sulfoxide, N-methylpyrrolidone and dimethylformamide.

所述超声剥离的功率为1000~1500W,所述超声剥离的频率为20~30kHz,所述超声剥离的时间为2~10h;The power of the ultrasonic peeling is 1000-1500W, the frequency of the ultrasonic peeling is 20-30 kHz, and the time of the ultrasonic peeling is 2-10h;

所述搅拌的速率为500~1000rpm,所述搅拌的时间为2~10h;The stirring speed is 500~1000rpm, and the stirring time is 2~10h;

所述固液分离的方式为离心;所述离心的速率为3000~10000r/min,所述离心的时间为30~100min。The solid-liquid separation method is centrifugation; the centrifugal speed is 3000-10000 r/min, and the centrifugation time is 30-100 min.

本发明提供了上述技术方案所述的润滑油的制备方法,包括以下步骤:The present invention provides the preparation method of the lubricating oil described in the above technical scheme, comprising the following steps:

将SiP量子点和基础油混合,进行超声,得到所述润滑油。The SiP quantum dots and the base oil are mixed and sonicated to obtain the lubricating oil.

优选的,所述超声的功率为1000~1500W,超声的时间为3~10h。Preferably, the power of the ultrasonic is 1000-1500 W, and the ultrasonic time is 3-10 h.

本发明提供了上述技术方案所述润滑油或上述技术方案所述的制备方法得到的润滑油在金属-金属、金属-聚合物、金属-陶瓷等摩擦副中应用。The present invention provides the application of the lubricating oil described in the above technical solution or the lubricating oil obtained by the preparation method described in the above technical solution in friction pairs such as metal-metal, metal-polymer, and metal-ceramic.

本发明相对于现有技术取得了以下技术效果:The present invention has achieved the following technical effects with respect to the prior art:

本发明提供了SiP量子点作为润滑油添加剂的应用,在本发明中,所述SiP量子点具有层状结构,层与层之间存在纳米级的层间距,层内为共价键作用力,层与层之间为范德华力,层间作用力较弱,使SiP量子点层与层之间更易于滑动;而且其结构基元为相互连接的扭曲状的五元环与六元环,呈现面内各向异性,这种环状结构可以消除棱边悬键,使SiP量子点具有优异的稳定性,提高了SiP量子点的抗潮湿性能。以SiP量子点作为润滑油添加剂,实现SiP量子点在润滑油中的良好分散性,得到的润滑油产品减摩抗磨性能优异,且结构稳定,承载能力强。The present invention provides the application of SiP quantum dots as lubricating oil additives. In the present invention, the SiP quantum dots have a layered structure, there is a nano-level interlayer spacing between the layers, and there is covalent bond force in the layers. There is van der Waals force between layers, and the interlayer force is weak, which makes it easier for SiP quantum dot layers to slide between layers; and its structural elements are interconnected twisted five-membered rings and six-membered rings, showing In-plane anisotropy, this ring structure can eliminate edge dangling bonds, make SiP quantum dots have excellent stability, and improve the moisture resistance of SiP quantum dots. Using SiP quantum dots as lubricating oil additives to achieve good dispersion of SiP quantum dots in lubricating oil, the obtained lubricating oil product has excellent anti-friction and anti-wear performance, stable structure and strong bearing capacity.

本发明提供了一种润滑油,包括SiP量子点和基础油,实施例的结果表明,本发明提供的润滑油,摩擦系数平均值为0.064~0.072。The present invention provides a lubricating oil comprising SiP quantum dots and base oil. The results of the examples show that the average friction coefficient of the lubricating oil provided by the present invention is 0.064-0.072.

附图说明Description of drawings

图1为本发明实施例1制备得到的SiP量子点的原子力显微镜图;1 is an atomic force microscope image of the SiP quantum dots prepared in Example 1 of the present invention;

图2为本发明实施例1制备得到的SiP量子点的厚度分布图;2 is a thickness distribution diagram of SiP quantum dots prepared in Example 1 of the present invention;

图3为本发明实施例1制备得到的SiP量子点的粒径统计图;Fig. 3 is the particle size statistics diagram of SiP quantum dots prepared in Example 1 of the present invention;

图4为本发明实施例1制备得到的SiP量子点作为添加剂时所得的润滑油的摩擦系数曲线及磨斑图;4 is a friction coefficient curve and a wear spot diagram of the lubricating oil obtained when the SiP quantum dots prepared in Example 1 of the present invention are used as additives;

图5为本发明实施例2制备得到的SiP量子点作为添加剂时所得的润滑油的摩擦系数曲线及磨斑图;5 is a friction coefficient curve and a wear spot diagram of the lubricating oil obtained when the SiP quantum dots prepared in Example 2 of the present invention are used as additives;

图6为本发明实施例3制备得到的SiP量子点作为添加剂时所得的润滑油的摩擦系数曲线及磨斑图;6 is a friction coefficient curve and a wear spot diagram of the lubricating oil obtained when the SiP quantum dots prepared in Example 3 of the present invention are used as additives;

图7为本发明实施例4制备得到的SiP量子点作为添加剂时所得的润滑油的摩擦系数曲线及磨斑图;7 is a friction coefficient curve and a wear spot diagram of the lubricating oil obtained when the SiP quantum dots prepared in Example 4 of the present invention are used as additives;

图8位本发明实施例5制备得到的SiP量子点作为添加剂时所得的润滑油的摩擦系数曲线及磨斑图;Fig. 8 is the friction coefficient curve and the wear spot diagram of the lubricating oil obtained when the SiP quantum dots prepared in Example 5 of the present invention are used as additives;

图9为本发明实施例6制备得到的SiP量子点作为添加剂时所得的润滑油的摩擦系数曲线及磨斑图;9 is a friction coefficient curve and a wear spot diagram of the lubricating oil obtained when the SiP quantum dots prepared in Example 6 of the present invention are used as additives;

图10为本发明实施例7制备得到的SiP量子点作为添加剂时所得的润滑油的摩擦系数曲线及磨斑图;10 is a friction coefficient curve and a wear spot diagram of the lubricating oil obtained when the SiP quantum dots prepared in Example 7 of the present invention are used as additives;

图11为本发明实施例8制备得到的SiP量子点作为添加剂时所得的润滑油的摩擦系数曲线及磨斑图;11 is a friction coefficient curve and a wear spot diagram of the lubricating oil obtained when the SiP quantum dots prepared in Example 8 of the present invention are used as additives;

图12为基础油PEG-400的摩擦系数曲线及磨斑图。FIG. 12 is the friction coefficient curve and wear scar chart of the base oil PEG-400.

具体实施方式Detailed ways

本发明提供了SiP量子点作为润滑油添加剂的应用。The present invention provides the application of SiP quantum dots as lubricating oil additives.

在本发明中,所述SiP量子点的平均粒径优选为8~15nm,进一步优选为9.5~13nm,更优选为12nm;平均厚度优选为1~3nm,进一步优选为1.5~2nm;所述SiP量子点在润滑油中的质量百分数为0.01~0.1%,优选为0.03~0.08%,更优选为0.05~0.06%。In the present invention, the average particle size of the SiP quantum dots is preferably 8-15 nm, more preferably 9.5-13 nm, more preferably 12 nm; the average thickness is preferably 1-3 nm, more preferably 1.5-2 nm; the SiP The mass percentage of the quantum dots in the lubricating oil is 0.01-0.1%, preferably 0.03-0.08%, and more preferably 0.05-0.06%.

本发明提供的所述SiP量子点,具有层状结构,层间作用力较弱;而且具有优异的稳定性以及面内各向异性,以所述SiP量子点作为润滑油添加剂,在润滑油中的具有良好的分散性,得到的润滑油的减磨抗磨性能优异。The SiP quantum dots provided by the present invention have a layered structure, and the interlayer force is weak; and has excellent stability and in-plane anisotropy. The SiP quantum dots are used as lubricating oil additives. It has good dispersibility, and the obtained lubricating oil has excellent anti-wear and anti-wear properties.

本发明还提供了一种润滑油,包括SiP量子点和基础油。The present invention also provides a lubricating oil comprising SiP quantum dots and base oil.

在本发明中,所述SiP量子点在润滑油中的质量百分数优选为0.01~0.1wt%,进一步优选为0.03~0.08%,更优选为0.05~0.06%。In the present invention, the mass percentage of the SiP quantum dots in the lubricating oil is preferably 0.01-0.1 wt%, more preferably 0.03-0.08%, and more preferably 0.05-0.06%.

在本发明中,所述SiP量子点优选通过制备得到;所述IV-V族二维化合物量子点的制备方法,优选包括以下步骤:In the present invention, the SiP quantum dots are preferably obtained by preparation; the preparation method of the IV-V group two-dimensional compound quantum dots preferably includes the following steps:

将SiP粉体和极性有机溶剂混合后,依次进行超声剥离、搅拌、固液分离和取上清液干燥,得到所述SiP量子点;After mixing the SiP powder and the polar organic solvent, ultrasonic peeling, stirring, solid-liquid separation and drying of the supernatant are sequentially performed to obtain the SiP quantum dots;

所述SiP粉体的平均粒径为1~100μm,平均厚度为500~2000nmThe average particle size of the SiP powder is 1-100 μm, and the average thickness is 500-2000 nm

所述SiP量子点的平均粒径为8~15nm,平均厚度为1~3nm。The SiP quantum dots have an average particle size of 8-15 nm and an average thickness of 1-3 nm.

在本发明中,所述SiP粉体的平均粒径优选为1~100μm,进一步优选为40~70μm;平均厚度优选为500~2000nm,进一步优选为800~1500nm,所述SiP量子点的平均粒径优选为8~15nm,进一步优选为9.5~13nm,更优选为12nm;平均厚度优选为1~3nm,进一步优选为1.5~2nm。本发明对所述SiP粉体的来源没有特殊要求,采用市售产品或实验室制备均可。In the present invention, the average particle size of the SiP powder is preferably 1-100 μm, more preferably 40-70 μm; the average thickness is preferably 500-2000 nm, more preferably 800-1500 nm, the average particle size of the SiP quantum dots The diameter is preferably 8 to 15 nm, more preferably 9.5 to 13 nm, and more preferably 12 nm; the average thickness is preferably 1 to 3 nm, further preferably 1.5 to 2 nm. The present invention has no special requirements on the source of the SiP powder, and can use commercially available products or laboratory preparations.

在本发明中,所述SiP粉体优选通过制备得到,所述SiP粉体的制备方法优选包括以下步骤:将SiP单晶进行研磨,得到所述SiP粉体。In the present invention, the SiP powder is preferably obtained by preparation, and the preparation method of the SiP powder preferably includes the following steps: grinding a SiP single crystal to obtain the SiP powder.

在本发明中,所述SiP单晶优选为在5~10mm×1mm×1mm,所述SiP单晶优选依据文献“Controllable seeded flux growth and optoelectronic properties of bulk o-SiP crystals”(Li C,Wang S,Zhang X,et al CrystEngComm)中记载的实验方法制备。在本发明的实施例中,所述SiP单晶的制备方法具体为:将原料按照Si:P:Sn的摩尔比为1:1:5的比例进行配料并充分混合均匀,转移到石英管中,将石英管用分子泵抽真空至5×10-3Pa后,采用氢氧焰进行封结,将石英管置于合成炉中,采用FP23控温表进行控温,控温程序如下:初始温度为室温,升温至723K,并恒温36h,然后经36h升温到973K,再经过48h升温到1423K,随后经500h降温到873K,冷却至室温。将烧结后的样品置于浓盐酸与水比例为1:1的稀盐酸中浸泡,除掉样品中的Sn,采用乙醇清洗并在333K下烘干,得到所述SiP单晶。在本发明中,所述研磨的时间优选为10~30min,所述研磨优选采用玛瑙研钵,手动研磨即可。In the present invention, the SiP single crystal is preferably 5-10 mm×1 mm×1 mm, and the SiP single crystal is preferably based on the literature “Controllable seeded flux growth and optoelectronic properties of bulk o-SiP crystals” (Li C, Wang S , Zhang X, et al CrystEngComm) by the experimental method described in the preparation. In the embodiment of the present invention, the preparation method of the SiP single crystal is as follows: the raw materials are batched according to the molar ratio of Si:P:Sn to 1:1:5, fully mixed, and then transferred to a quartz tube. , after the quartz tube is evacuated to 5×10 -3 Pa with a molecular pump, sealed with a hydrogen-oxygen flame, placed in the synthesis furnace, and the temperature is controlled by an FP23 temperature control table. The temperature control procedure is as follows: Initial temperature At room temperature, the temperature was raised to 723K and kept at a constant temperature for 36h, then heated to 973K after 36h, then heated to 1423K after 48h, then cooled to 873K after 500h, and cooled to room temperature. The sintered sample was soaked in dilute hydrochloric acid with a ratio of concentrated hydrochloric acid to water of 1:1 to remove Sn in the sample, washed with ethanol and dried at 333K to obtain the SiP single crystal. In the present invention, the grinding time is preferably 10-30 min, and the grinding is preferably an agate mortar, which can be manually ground.

在本发明中,所述极性有机溶剂优选包括丙酮、无水乙醇、二甲基亚砜(DMSO)、N-甲基吡咯烷酮(NMP)和二甲基甲酰胺(DMF)中的一种或多种,进一步优选为丙酮、无水乙醇、二甲基亚砜、N-甲基吡咯烷酮或二甲基甲酰胺;当所述极性有机溶剂优选包括丙酮、无水乙醇、二甲基亚砜、N-甲基吡咯烷酮和二甲基甲酰胺中的两种以上时,本发明对上述具体物质的质量配比没有特殊要求,采用任意配比即可。本发明对所述极性有机溶剂的来源没有特殊要求,采用市售产品即可。In the present invention, the polar organic solvent preferably includes one or more of acetone, absolute ethanol, dimethyl sulfoxide (DMSO), N-methylpyrrolidone (NMP) and dimethylformamide (DMF). Various, more preferably acetone, absolute ethanol, dimethyl sulfoxide, N-methylpyrrolidone or dimethylformamide; when the polar organic solvent preferably includes acetone, absolute ethanol, dimethyl sulfoxide , N-methylpyrrolidone and two or more kinds of dimethylformamide, the present invention has no special requirements for the mass ratio of the above-mentioned specific substances, and any ratio can be used. The present invention has no special requirements on the source of the polar organic solvent, and a commercially available product can be used.

在本发明中,所述SiP和极性有机溶剂的质量体积比优选为0.01~0.1g:10~50mL,本发明对所述SiP粉体和极性有机溶剂混合的具体操作过程没有特殊要求。In the present invention, the mass-volume ratio of the SiP and the polar organic solvent is preferably 0.01-0.1 g: 10-50 mL, and the present invention has no special requirements for the specific operation process of mixing the SiP powder and the polar organic solvent.

将所述SiP粉体和极性有机溶剂混合后,本发明还优选包括对混合后得到的分散液进行初步超声,所述初步超声的功率优选为150~300W,更优选为180~250W,最优选为210~245W;所述初步超声的时间优选为1~3h,更优选为1.5~2h。本发明对所述初步超声的设备没有特殊要求,采用本领域技术人员熟知的超声设备即可。在本发明的实施例中,所述初步超声的设备为超声波清洗机。After mixing the SiP powder and the polar organic solvent, the present invention also preferably includes performing preliminary ultrasound on the dispersion obtained after mixing, and the power of the preliminary ultrasound is preferably 150-300W, more preferably 180-250W, most preferably 150-300W. Preferably it is 210-245W; the time of the preliminary ultrasonic is preferably 1-3h, more preferably 1.5-2h. The present invention has no special requirements on the equipment for the preliminary ultrasound, and an ultrasound equipment well-known to those skilled in the art can be used. In the embodiment of the present invention, the equipment for the preliminary ultrasonic wave is an ultrasonic cleaning machine.

本发明通过初步超声,使所述SiP粉体在所述极性有机溶剂中分散的更加均匀。In the present invention, the SiP powder is more uniformly dispersed in the polar organic solvent through preliminary ultrasonic waves.

得到分散液后,本发明将所述分散液进行超声剥离,所述超声剥离的功率优选为1000~1500W,进一步优选为1200~1350W,所述超声剥离的频率优选为20~30kHz,进一步优选为23~28kHz,所述超声剥离的时间优选为2~10h,进一步优选为4~8h。本发明对所述超声剥离的设备没有特殊要求,采用本领域技术人员熟知的超声设备即可,在本发明的实施例中,所述超声剥离的设备为超声波破碎仪。After the dispersion is obtained, the present invention performs ultrasonic peeling of the dispersion, the power of the ultrasonic peeling is preferably 1000-1500W, more preferably 1200-1350W, the frequency of the ultrasonic peeling is preferably 20-30kHz, and more preferably 23-28 kHz, the ultrasonic peeling time is preferably 2-10 h, more preferably 4-8 h. The present invention has no special requirements for the ultrasonic peeling equipment, and an ultrasonic equipment well known to those skilled in the art may be used. In the embodiment of the present invention, the ultrasonic peeling equipment is an ultrasonic disruptor.

在本发明中,所述搅拌的速率优选为500~1000rpm,进一步优选为650~800rpm,所述搅拌的时间优选为2~10h,进一步优选为3.5~7.8h,本发明对所述搅拌的方式没有特殊要求。在本发明的实施例中,所述搅拌的方式优选为磁力搅拌。In the present invention, the stirring speed is preferably 500-1000 rpm, more preferably 650-800 rpm, and the stirring time is preferably 2-10 h, more preferably 3.5-7.8 h. There are no special requirements. In the embodiment of the present invention, the stirring mode is preferably magnetic stirring.

在本发明中,所述固液分离的方式优选为离心;所述离心的速率优选为3000~10000r/min,进一步优选为4500~8900r/min;所述离心的时间优选为30~100min。In the present invention, the solid-liquid separation method is preferably centrifugation; the centrifugal speed is preferably 3000-10000 r/min, more preferably 4500-8900 r/min; the centrifugation time is preferably 30-100 min.

所述固液分离完成后,本发明优选对上清液进行干燥,所述上清液优选为固液分离后液体体积的2/3~4/5,所述干燥的温度优选为80~150℃,干燥的时间优选为2h,所述干燥优选在烘干箱中进行。After the solid-liquid separation is completed, the present invention preferably dries the supernatant liquid, and the supernatant liquid is preferably 2/3-4/5 of the liquid volume after the solid-liquid separation, and the drying temperature is preferably 80-150 °C. ℃, the drying time is preferably 2h, and the drying is preferably carried out in a drying oven.

在本发明中,所述润滑油还包括基础油。在本发明中,所述基础油优选为聚乙二醇基础油、聚醚类基础油或合成酯类基础油,更优选为聚乙二醇基础油、液体石蜡或聚α烯烃(PAO),在本发明的实施例中,所述基础油优选为PEG-400、PEG-800、液体石蜡、聚α烯烃(PAO)。本发明对所述基础油的来源的没有特殊要求,采用市售产品即可。In the present invention, the lubricating oil further includes base oil. In the present invention, the base oil is preferably polyethylene glycol base oil, polyether base oil or synthetic ester base oil, more preferably polyethylene glycol base oil, liquid paraffin or polyalphaolefin (PAO), In the embodiment of the present invention, the base oil is preferably PEG-400, PEG-800, liquid paraffin, polyalphaolefin (PAO). The present invention has no special requirements on the source of the base oil, and a commercially available product can be used.

在本发明中,所述SiP量子点在润滑油中的质量百分数为0.01~0.1%,优选为0.03~0.08%,更优选为0.05~0.06%。In the present invention, the mass percentage of the SiP quantum dots in the lubricating oil is 0.01-0.1%, preferably 0.03-0.08%, more preferably 0.05-0.06%.

本发明提供了上述技术方案所述的润滑油的制备方法,包括以下步骤:The present invention provides the preparation method of the lubricating oil described in the above technical scheme, comprising the following steps:

将SiP量子点和基础油混合,进行超声,得到所述润滑油。The SiP quantum dots and the base oil are mixed and sonicated to obtain the lubricating oil.

本发明对所述混合的具体操作过程没有特殊要求。The present invention has no special requirements on the specific operation process of the mixing.

在本发明中,所述超声的功率优选为1000~1500W,进一步优选为1150~1350W;所述超声的时间优选为3~10h,进一步优选为4.5~8.5h。In the present invention, the power of the ultrasonic wave is preferably 1000-1500W, more preferably 1150-1350W; the ultrasonic time is preferably 3-10h, more preferably 4.5-8.5h.

本发明提供了上述技术方案所述润滑油或上述技术方案所述的制备方法得到的润滑油在金属-金属、金属-聚合物、金属-陶瓷等摩擦副中应用。The present invention provides the application of the lubricating oil described in the above technical solution or the lubricating oil obtained by the preparation method described in the above technical solution in friction pairs such as metal-metal, metal-polymer, and metal-ceramic.

为了更好地理解本发明,下面结合实施例进一步阐明本发明的内容,但本发明的内容不仅仅局限于下面的实施例。In order to better understand the present invention, the content of the present invention is further illustrated below in conjunction with the embodiments, but the content of the present invention is not limited to the following embodiments.

实施例1Example 1

将原料按照Si:P:Sn的摩尔比为1:1:5的比例进行配料并充分混合均匀,转移到石英管中,将石英管用分子泵抽真空至5×10-3Pa后,采用氢氧焰进行封结,将石英管置于合成炉中,采用FP23控温表进行控温,控温程序如下:初始温度为室温,升温至723K,并恒温36h,然后经36h升温到973K,再经过48h升温到1423K,随后经500h降温到873K,冷却至室温。将烧结后的样品置于浓盐酸与水比例为1:1的稀盐酸中浸泡,除掉样品中的Sn,采用乙醇清洗并在333K下烘干,得到所述SiP单晶。在本发明中,所述研磨的时间优选为10~30min,所述研磨优选采用玛瑙研钵,手动研磨即可。The raw materials were prepared according to the molar ratio of Si:P:Sn to 1:1:5, mixed well, and then transferred to a quartz tube. After the quartz tube was evacuated to 5×10 -3 Pa with a molecular pump, hydrogen The oxygen flame is sealed, the quartz tube is placed in the synthesis furnace, and the FP23 temperature control table is used to control the temperature. The temperature control program is as follows: the initial temperature is room temperature, the temperature is raised to 723K, and the temperature is kept constant for 36h, then the temperature is raised to 973K after 36h, and then It was heated to 1423K after 48h, then cooled to 873K after 500h, and cooled to room temperature. The sintered sample was soaked in dilute hydrochloric acid with a ratio of concentrated hydrochloric acid to water of 1:1 to remove Sn in the sample, washed with ethanol and dried at 333K to obtain the SiP single crystal. In the present invention, the grinding time is preferably 10-30 min, and the grinding is preferably an agate mortar, which can be manually ground.

将SiP单晶采用玛瑙研钵研磨10min,得到SiP粉末(粒径为50μm,厚度为500nm),然后将SiP粉末和丙酮混合(两者的质量体积比为0.1g:50mL),先采用200W的超声波清洗机,进行初步的超声分散,处理时间为1h,然后采用功率为1000W,频率为20kHz的超声波破碎仪对SiP粉末进行液相超声剥离,超声剥离时间为2h;获得SiP的丙酮分散液;The SiP single crystal was ground with an agate mortar for 10 minutes to obtain SiP powder (particle size was 50 μm, thickness was 500 nm), and then the SiP powder was mixed with acetone (the mass-volume ratio of the two was 0.1 g: 50 mL). Ultrasonic cleaning machine, for preliminary ultrasonic dispersion, the treatment time is 1h, and then the SiP powder is subjected to liquid-phase ultrasonic peeling with a power of 1000W and a frequency of 20kHz, and the ultrasonic peeling time is 2h; SiP acetone dispersion is obtained;

将获得的SiP的丙酮分散液转移到烧杯中,进行磁力搅拌2h,搅拌的速率为500rpm,最后以3000r/min的离心速度进行离心60min,取固液分离后液体体积的2/3作为上清液,将取得的上清液进行干燥(干燥温度为80℃,干燥时间为2h),得到SiP量子点;Transfer the obtained SiP acetone dispersion into a beaker, conduct magnetic stirring for 2 hours, and stir at a rate of 500 rpm. Finally, centrifuge at a centrifugal speed of 3000 r/min for 60 minutes, and take 2/3 of the liquid volume after solid-liquid separation as the supernatant. The obtained supernatant was dried (the drying temperature was 80 °C, and the drying time was 2 h) to obtain SiP quantum dots;

将SiP量子点和PEG-400基础油混合,采用1200W超声波破碎仪超声3h,得到含有SiP量子点质量分数为0.03%的润滑油。The SiP quantum dots and the PEG-400 base oil were mixed, and the 1200W ultrasonic breaker was used to ultrasonicate for 3 hours to obtain a lubricating oil containing SiP quantum dots with a mass fraction of 0.03%.

图1为本实施例制备得到的SiP量子点的原子力显微镜图,从图1中可以得出本实施例制备得到的SiP量子点呈现分散状态,粒径均匀;FIG. 1 is an atomic force microscope image of the SiP quantum dots prepared in the present embodiment, and it can be concluded from FIG. 1 that the SiP quantum dots prepared in the present embodiment are in a dispersed state and have a uniform particle size;

图2为本实施例制备得到的SiP量子点的厚度分布图,其中纵坐标为SiP量子点的厚度尺寸,横坐标为若干SiP量子点横向排布的尺寸,从图2中可以得出本实施例制备得到的SiP量子点的厚度小于3nm;图3为本实施例制备得到的SiP量子点的平均粒径统计图,粒径的平均尺寸在12.4nm。Fig. 2 is a thickness distribution diagram of the SiP quantum dots prepared in the present embodiment, wherein the ordinate is the thickness size of the SiP quantum dots, and the abscissa is the size of the lateral arrangement of several SiP quantum dots. The thickness of the SiP quantum dots prepared in this example is less than 3 nm; FIG. 3 is a statistical graph of the average particle size of the SiP quantum dots prepared in this example, and the average size of the particle size is 12.4 nm.

实施例2Example 2

将SiP单晶采用玛瑙研钵研磨15min,得到SiP粉末(粒径为50μm,厚度为2000nm),然后将SiP粉末和NMP混合(两者的质量体积比为0.01g:10mL),先采用200W的超声波清洗机,进行初步的超声分散,处理时间为1h,然后采用功率为1200W,频率为50kHz的超声波破碎仪对SiP粉末进行液相超声剥离,超声剥离时间为3h;获得SiP的NMP分散液;The SiP single crystal was ground in an agate mortar for 15 minutes to obtain SiP powder (50 μm in particle size and 2000 nm in thickness), and then the SiP powder and NMP were mixed (the mass-to-volume ratio of the two was 0.01 g: 10 mL). Ultrasonic cleaning machine, carry out preliminary ultrasonic dispersion, the treatment time is 1h, and then the SiP powder is subjected to liquid-phase ultrasonic peeling with a power of 1200W and a frequency of 50kHz, and the ultrasonic peeling time is 3h; The NMP dispersion of SiP is obtained;

将获得的SiP的NMP分散液转移到烧杯中,进行磁力搅拌3h,搅拌的速率为600rpm,最后以3000r/min的离心速度进行离心60min,取固液分离后液体体积的2/3作为上清液,将取得的上清液进行干燥(干燥的温度为100℃,干燥的时间为2h),得到SiP量子点;Transfer the obtained SiP NMP dispersion into a beaker, conduct magnetic stirring for 3 hours, and stir at a rate of 600 rpm. Finally, centrifuge at a centrifugal speed of 3000 r/min for 60 min, and take 2/3 of the liquid volume after solid-liquid separation as the supernatant. The obtained supernatant is dried (the drying temperature is 100 °C, and the drying time is 2 h) to obtain SiP quantum dots;

将SiP量子点和PEG-400基础油混合,采用1500W超声波破碎仪超声3h,得到含有SiP量子点质量分数为0.05%的润滑油。The SiP quantum dots and the PEG-400 base oil were mixed, and the 1500W ultrasonic breaker was used to ultrasonicate for 3 hours to obtain a lubricating oil containing SiP quantum dots with a mass fraction of 0.05%.

实施例3Example 3

将SiP单晶采用玛瑙研钵研磨20min,得到SiP粉末(粒径为50μm,厚度为800nm),然后将SiP粉末和DMF混合(两者的质量体积比为0.05g:50mL),先采用250W的超声波清洗机,进行初步的超声分散,处理时间为3h,然后采用功率为1300W,频率为40kHz的超声波破碎仪对SiP粉末进行液相超声剥离,超声剥离时间为2h;获得SiP的DMF分散液;The SiP single crystal was ground with an agate mortar for 20 min to obtain SiP powder (particle size was 50 μm, thickness was 800 nm), and then the SiP powder and DMF were mixed (the mass-volume ratio of the two was 0.05 g: 50 mL), and a 250 W Ultrasonic cleaning machine, carry out preliminary ultrasonic dispersion, the treatment time is 3h, and then the SiP powder is subjected to liquid-phase ultrasonic peeling with a power of 1300W and a frequency of 40kHz, and the ultrasonic peeling time is 2h; The DMF dispersion of SiP is obtained;

将获得的SiP的DMF分散液转移到烧杯中,进行磁力搅拌5h,搅拌的速率为800rpm,最后以5000r/min的离心速度进行离心60min,取固液分离后液体体积的2/3作为上清液,将取得的上清液进行干燥(干燥的温度为120℃,干燥的时间为2h),得到SiP量子点;Transfer the obtained DMF dispersion of SiP into a beaker, conduct magnetic stirring for 5h, the stirring speed is 800rpm, and finally centrifuge at a centrifugal speed of 5000r/min for 60min, and take 2/3 of the liquid volume after solid-liquid separation as the supernatant The obtained supernatant is dried (the drying temperature is 120 °C, and the drying time is 2 h) to obtain SiP quantum dots;

将SiP量子点和PEG-400基础油混合,采用1500W超声波破碎仪超声3h,得到含有SiP量子点质量分数为0.03%的润滑油。The SiP quantum dots and PEG-400 base oil were mixed, and the 1500W ultrasonic breaker was used to ultrasonicate for 3 hours to obtain a lubricating oil containing SiP quantum dots with a mass fraction of 0.03%.

实施例4Example 4

将SiP单晶采用玛瑙研钵研磨20min,得到SiP粉末(粒径为50μm,厚度为1500nm),然后将SiP粉末和DMSO混合,先采用300W的超声波清洗机,进行初步的超声分散,处理时间为3h,然后采用功率为1500W,频率为40kHz的超声波破碎仪对SiP粉末进行液相超声剥离,超声剥离时间为5h;获得SiP的DMSO分散液;The SiP single crystal was ground with an agate mortar for 20 minutes to obtain SiP powder (particle size was 50 μm, thickness was 1500 nm), and then the SiP powder was mixed with DMSO, and a 300W ultrasonic cleaner was used for preliminary ultrasonic dispersion. The treatment time was 3h, and then use an ultrasonic breaker with a power of 1500W and a frequency of 40kHz to carry out liquid-phase ultrasonic peeling of the SiP powder, and the ultrasonic peeling time is 5h; the DMSO dispersion of SiP is obtained;

将获得的SiP的DMSO分散液转移到烧杯中,进行磁力搅拌5h,搅拌的速率为800rpm,最后以6000r/min的离心速度进行离心60min,取固液分离后液体体积的2/3作为上清液,将取得的上清液进行干燥(干燥的温度为120℃,干燥的时间为2h),得到SiP量子点;Transfer the obtained SiP DMSO dispersion into a beaker, conduct magnetic stirring for 5h, the stirring speed is 800rpm, and finally centrifuge at a centrifugal speed of 6000r/min for 60min, and take 2/3 of the liquid volume after solid-liquid separation as the supernatant The obtained supernatant is dried (the drying temperature is 120 °C, and the drying time is 2 h) to obtain SiP quantum dots;

将SiP量子点和PEG-400基础油混合,采用1500W超声波破碎仪超声3h,得到含有SiP量子点质量分数为0.07%的润滑油。The SiP quantum dots and the PEG-400 base oil were mixed, and sonicated by a 1500W ultrasonic disruptor for 3 hours to obtain a lubricating oil containing SiP quantum dots with a mass fraction of 0.07%.

实施例5Example 5

将SiP单晶采用玛瑙研钵研磨20min,得到SiP粉末(粒径为50μm,厚度为1000nm),然后将SiP粉末和无水乙醇混合(两者的质量体积比为0.1g:50mL),先采用220W的超声波清洗机,进行初步的超声分散,处理时间为3h,然后采用功率为1100W,频率为40kHz的超声波破碎仪对SiP粉末进行液相超声剥离,超声剥离时间为5h;获得SiP的无水乙醇分散液;The SiP single crystal was ground in an agate mortar for 20 min to obtain SiP powder (50 μm in particle size and 1000 nm in thickness), and then the SiP powder was mixed with absolute ethanol (the mass-volume ratio of the two was 0.1 g: 50 mL), and the A 220W ultrasonic cleaning machine was used for preliminary ultrasonic dispersion, and the treatment time was 3h. Then, the SiP powder was subjected to liquid-phase ultrasonic peeling with a power of 1100W and a frequency of 40kHz. The ultrasonic peeling time was 5h; the anhydrous SiP was obtained. Ethanol dispersion;

将获得的SiP的无水乙醇分散液转移到烧杯中,进行磁力搅拌5h,搅拌的速率为800rpm,最后以7000r/min的离心速度进行离心60min,取固液分离后液体体积的2/3作为上清液,将取得的上清液进行干燥(干燥的温度为120℃,干燥的时间为2h),得到SiP量子点;Transfer the obtained SiP anhydrous ethanol dispersion into a beaker, conduct magnetic stirring for 5h, the stirring speed is 800rpm, and finally centrifuge at a centrifugal speed of 7000r/min for 60min, take 2/3 of the liquid volume after solid-liquid separation as The supernatant is dried (the drying temperature is 120° C., and the drying time is 2 h) to obtain SiP quantum dots;

将SiP量子点和PEG-400基础油混合,采用1400W超声波破碎仪超声3h,得到含有SiP量子点质量分数为0.06%的润滑油。The SiP quantum dots and the PEG-400 base oil were mixed, and sonicated by a 1400W ultrasonic disruptor for 3 hours to obtain a lubricating oil containing SiP quantum dots with a mass fraction of 0.06%.

实施例6Example 6

将SiP单晶采用玛瑙研钵研磨30min,得到SiP粉末(粒径为80μm,厚度为1800nm),然后将SiP粉末和丙酮混合(两者的质量体积比为0.05g:25mL),先采用250W的超声波清洗机,进行初步的超声分散,处理时间为1h,然后采用功率为1600W,频率为20kHz的超声波破碎仪对SiP粉末进行液相超声剥离,超声剥离时间为2h;获得SiP的丙酮分散液;The SiP single crystal was ground in an agate mortar for 30 min to obtain SiP powder (particle size was 80 μm, thickness was 1800 nm), and then the SiP powder was mixed with acetone (the mass-volume ratio of the two was 0.05 g: 25 mL). Ultrasonic cleaning machine, for preliminary ultrasonic dispersion, the treatment time is 1h, and then the SiP powder is subjected to liquid-phase ultrasonic peeling with a power of 1600W and a frequency of 20kHz, and the ultrasonic peeling time is 2h; SiP acetone dispersion is obtained;

将获得的SiP的丙酮分散液转移到烧杯中,进行磁力搅拌7h,搅拌的速率为500rpm,最后以3000r/min的离心速度进行离心60min,取固液分离后液体体积的2/3作为上清液,将取得的上清液进行干燥(干燥的温度为80℃,干燥的时间为2h),得到SiP量子点;Transfer the obtained SiP acetone dispersion into a beaker, conduct magnetic stirring for 7 hours, and stir at a rate of 500 rpm. Finally, centrifuge at a centrifugal speed of 3000 r/min for 60 minutes, and take 2/3 of the liquid volume after solid-liquid separation as the supernatant. The obtained supernatant is dried (the drying temperature is 80 °C, and the drying time is 2 h) to obtain SiP quantum dots;

将SiP量子点和PEG-400基础油混合,采用1700W超声波破碎仪超声3h,得到含有SiP量子点质量分数为0.02%的润滑油。The SiP quantum dots and the PEG-400 base oil were mixed, and the 1700W ultrasonic breaker was used to ultrasonicate for 3 hours to obtain a lubricating oil containing SiP quantum dots with a mass fraction of 0.02%.

实施例7Example 7

将SiP单晶采用玛瑙研钵研磨30min,得到SiP粉末(粒径为50μm,厚度为1500nm),然后将SiP粉末和NMP混合(两者的质量体积比为0.1g:50mL),先采用270W的超声波清洗机,进行初步的超声分散,处理时间为6h,然后采用功率为1700W,频率为20kHz的超声波破碎仪对SiP粉末进行液相超声剥离,超声剥离时间为3h;获得SiP的NMP分散液;The SiP single crystal was ground with an agate mortar for 30 min to obtain SiP powder (particle size was 50 μm, thickness was 1500 nm), and then SiP powder and NMP were mixed (the mass-volume ratio of the two was 0.1 g: 50 mL), and a 270 W Ultrasonic cleaning machine, for preliminary ultrasonic dispersion, the treatment time is 6h, and then the SiP powder is subjected to liquid-phase ultrasonic peeling with a power of 1700W and a frequency of 20kHz, and the ultrasonic peeling time is 3h; SiP NMP dispersion is obtained;

将获得的SiP的NMP分散液转移到烧杯中,进行磁力搅拌5h,搅拌的速率为800rpm,最后以8000r/min的离心速度进行离心60min,取固液分离后液体体积的2/3作为上清液,将取得的上清液进行干燥(干燥的温度为80℃,干燥的时间为2h),得到SiP量子点;Transfer the obtained NMP dispersion of SiP into a beaker, conduct magnetic stirring for 5h, the stirring speed is 800rpm, and finally centrifuge at a centrifugal speed of 8000r/min for 60min, and take 2/3 of the liquid volume after solid-liquid separation as the supernatant The obtained supernatant is dried (the drying temperature is 80 °C, and the drying time is 2 h) to obtain SiP quantum dots;

将SiP量子点和PEG-400基础油混合,采用1500W超声波破碎仪超声3h,得到含有SiP量子点质量分数为0.09%的润滑油。The SiP quantum dots and the PEG-400 base oil were mixed, and the 1500W ultrasonic breaker was used to sonicate for 3 hours to obtain a lubricating oil containing SiP quantum dots with a mass fraction of 0.09%.

实施例8Example 8

将SiP单晶采用玛瑙研钵研磨20min,得到SiP粉末(粒径为50μm,厚度为500nm),然后将SiP粉末和NMF混合(两者的质量体积比为0.1g:50mL),先采用250W的超声波清洗机,进行初步的超声分散,处理时间为3h,然后采用功率为1300W,频率为20kHz的超声波破碎仪对SiP粉末进行液相超声剥离,超声剥离时间为2h;获得SiP的NMF分散液;The SiP single crystal was ground in an agate mortar for 20 min to obtain SiP powder (50 μm in particle size and 500 nm in thickness), and then the SiP powder and NMF were mixed (the mass-to-volume ratio of the two was 0.1 g: 50 mL). Ultrasonic cleaning machine for preliminary ultrasonic dispersion, the treatment time is 3h, and then the SiP powder is subjected to liquid-phase ultrasonic peeling with a power of 1300W and a frequency of 20kHz, and the ultrasonic peeling time is 2h; SiP NMF dispersion is obtained;

将获得的SiP的NMF分散液转移到烧杯中,进行磁力搅拌5h,搅拌的速率为800rpm,最后以5000r/min的离心速度进行离心60min,取固液分离后液体体积的2/3作为上清液,将取得的上清液进行干燥(干燥的温度为80℃,干燥的时间为2h),得到SiP量子点;Transfer the obtained SiP NMF dispersion into a beaker, conduct magnetic stirring for 5 hours, and stir at a rate of 800 rpm. Finally, centrifuge at a centrifugal speed of 5000 r/min for 60 min, and take 2/3 of the liquid volume after solid-liquid separation as the supernatant. The obtained supernatant is dried (the drying temperature is 80 °C, and the drying time is 2 h) to obtain SiP quantum dots;

将SiP量子点和PEG-400基础油混合,采用1500W超声波破碎仪超声3h,得到含有SiP量子点质量分数为0.03%的润滑油。The SiP quantum dots and PEG-400 base oil were mixed, and the 1500W ultrasonic breaker was used to ultrasonicate for 3 hours to obtain a lubricating oil containing SiP quantum dots with a mass fraction of 0.03%.

测试例1Test Example 1

对实施例1~8制备得到的润滑油和PEG-400基础油进行摩擦磨损测试,测试方法为:采用四球摩擦试验机,测试的时间为30min,载荷为200kgf,所用的球为不锈钢球,直径为12.7mm。测试得到的摩擦系数及磨斑如图4~12(其中图4~11依次为实施例1~8所述的润滑油的摩擦系数及磨斑图,图12为PEG-400基础油的摩擦系数及磨斑图),具体的摩擦系数和磨斑尺寸如表1所示。从表1和图4~12的结果可以得出,实施例1~8制备得到的润滑油与PEG-400基础油相比,减磨抗磨性能优异,摩擦系数平均值为0.064~0.072,磨斑尺寸明显变小。The lubricating oil and PEG-400 base oil prepared in Examples 1 to 8 were subjected to friction and wear test. The test method was as follows: a four-ball friction tester was used, the test time was 30 min, and the load was 200 kgf. is 12.7mm. The friction coefficient and wear scar obtained from the test are shown in Figures 4 to 12 (wherein Figures 4 to 11 are the friction coefficient and wear scar diagram of the lubricating oils described in Examples 1 to 8 in turn, and Figure 12 is the friction coefficient of the PEG-400 base oil. and wear scar diagram), the specific friction coefficient and wear scar size are shown in Table 1. From the results in Table 1 and Figures 4 to 12, it can be concluded that compared with the PEG-400 base oil, the lubricating oils prepared in Examples 1 to 8 have excellent anti-wear and anti-wear properties, the average friction coefficient is 0.064 to 0.072, and the friction coefficient is 0.064 to 0.072. The spot size was significantly smaller.

表1PEG-400和实施例1~8制备得到的润滑油摩擦磨损测试数据Friction and wear test data of lubricating oil prepared by table 1PEG-400 and Examples 1-8

Figure BDA0002937588360000101
Figure BDA0002937588360000101

Figure BDA0002937588360000111
Figure BDA0002937588360000111

本发明中应用了具体个例对本发明的原理及实施方式进行了阐述,以上实施例的说明只是用于帮助理解本发明的方法及其核心思想;同时,对于本领域的一般技术人员,依据本发明的思想,在具体实施方式及应用范围上均会有改变之处。综上所述,本说明书内容不应理解为对本发明的限制。In the present invention, specific examples are used to illustrate the principles and implementations of the present invention, and the descriptions of the above embodiments are only used to help understand the method and the core idea of the present invention; There will be changes in the specific implementation manner and application scope of the idea of the invention. In conclusion, the contents of this specification should not be construed as limiting the present invention.

Claims (8)

  1. The application of the SiP quantum dots as the lubricating oil additive is characterized in that the average particle size of the SiP quantum dots is 8-15 nm, and the average thickness of the SiP quantum dots is 1-3 nm; the mass percentage of the SiP quantum dots in the lubricating oil is 0.01-0.1%.
  2. 2. A lubricating oil, comprising SiP quantum dots and a base oil; the average particle size of the SiP quantum dots is 8-15 nm, and the average thickness of the SiP quantum dots is 1-3 nm; the mass percentage of the SiP quantum dots in the lubricating oil is 0.01-0.1%.
  3. 3. The lubricating oil of claim 2, wherein the base oil is a polyethylene glycol base oil, a polyether base oil, or a synthetic ester base oil.
  4. 4. The lubricating oil of claim 2, wherein the preparation method of the SiP quantum dots comprises the following steps:
    mixing SiP powder and a polar organic solvent, and then sequentially carrying out ultrasonic stripping, stirring, solid-liquid separation and supernatant fluid drying to obtain the SiP quantum dots;
    the average particle size of the SiP powder is 1-100 mu m, and the average thickness of the SiP powder is 500-2000 nm;
    the average particle size of the SiP quantum dots is 8-15 nm, and the average thickness of the SiP quantum dots is 1-3 nm.
  5. 5. The lubricating oil of claim 4, wherein the polar organic solvent comprises one or more of acetone, absolute ethanol, dimethyl sulfoxide, N-methylpyrrolidone, and dimethylformamide;
    the power of ultrasonic stripping is 1000-1500W, the frequency of ultrasonic stripping is 20-30 kHz, and the time of ultrasonic stripping is 2-10 h;
    the stirring speed is 500-1000 rpm, and the stirring time is 2-10 hours;
    the solid-liquid separation mode is centrifugation; the centrifugation speed is 3000-10000 r/min, and the centrifugation time is 30-100 min.
  6. 6. A method for preparing the lubricating oil according to any one of claims 2 to 5, characterized by comprising the steps of:
    and mixing the SiP quantum dots with base oil, and performing ultrasonic treatment to obtain the lubricating oil.
  7. 7. The preparation method of claim 6, wherein the power of the ultrasound is 1000-1500W, and the time of the ultrasound is 3-10 h.
  8. 8. The lubricating oil according to any one of claims 2 to 5 or the lubricating oil obtained by the preparation method according to claim 6 or 7 is used in friction pairs such as metal-metal, metal-polymer, metal-ceramic and the like.
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