CN107686761A - A kind of fast preparation method in situ of Noctiluca scientillans shape graphene bag carborundum microballoon - Google Patents
A kind of fast preparation method in situ of Noctiluca scientillans shape graphene bag carborundum microballoon Download PDFInfo
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 55
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- 241000200174 Noctiluca Species 0.000 title 1
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
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- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/10—Compounds containing silicon
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/04—Detergent property or dispersant property
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- Carbon And Carbon Compounds (AREA)
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Abstract
本发明公开了一种夜光藻状石墨烯包碳化硅微球的原位快速制备方法，步骤如下：将碳化硅颗粒分散在液相介质中，形成一定浓度的悬浮液；将一定能量密度的脉冲激光聚焦后辐照该悬浮液，使碳化硅颗粒在激光辐照的光热和周围液体环境的快速冷却的双重作用下，原位实现碳化硅外延石墨烯的生长、部分多层石墨烯片的剥离以及无规则颗粒的球形化；辐照完后，将悬浮液离心、分离、酸洗，所得沉淀干燥，得到具有高分散性类夜光藻状的石墨烯包覆碳化硅微球。该方法操作简单，常温常压的室温条件下即可完成制备，成本低，产物纯度高，所得石墨烯包碳化硅微球在润滑油中显示出优异的分散稳定性及抗磨减摩性能。
The invention discloses a rapid in-situ preparation method of silicon carbide microspheres coated with luminous algae-like graphene. The steps are as follows: disperse silicon carbide particles in a liquid medium to form a suspension with a certain concentration; After laser focusing, the suspension is irradiated, so that the silicon carbide particles can realize the growth of silicon carbide epitaxial graphene and the formation of some multilayer graphene sheets in situ under the double action of the light heat of laser irradiation and the rapid cooling of the surrounding liquid environment. Exfoliation and spheroidization of random particles; after irradiation, the suspension is centrifuged, separated, pickled, and the resulting precipitate is dried to obtain graphene-coated silicon carbide microspheres with high dispersibility and luminous algae-like shape. The method is simple to operate, can be prepared under room temperature and pressure conditions, has low cost and high product purity, and the obtained graphene-coated silicon carbide microspheres exhibit excellent dispersion stability and anti-wear and anti-friction performance in lubricating oil.
Description
技术领域technical field
本发明涉及一种夜光藻状石墨烯包碳化硅微球的原位快速制备方法，具体涉及一种采用简单液相激光辐照碳化硅粉末原位形成夜光藻状石墨烯包碳化硅微球的方法，属于微纳粉体的制备技术领域。The invention relates to a rapid in-situ preparation method of luminous algae-shaped graphene-coated silicon carbide microspheres, in particular to a method for in-situ formation of luminous algae-shaped graphene-coated silicon carbide microspheres by irradiating silicon carbide powder with a simple liquid phase laser The method belongs to the technical field of preparation of micro-nano powder.
背景技术Background technique
现代工业生产及生活中普遍存在着机械的摩擦与磨损，摩擦与磨损的存在不仅导致大量能量损失，而且损坏零部件表面，严重降低了器械的使用寿命。纳米材料的出现为润滑油添加剂的发展提供了一个新的选择，并引起了人们的广泛关注。二维层状材料，如石墨烯、二硫化钼，在剪切作用下极易发生滑移而具有较低的摩擦系数，其作为润滑油添加剂可以在摩擦副表面形成转移膜，有效地减小磨损；一维球形颗粒，如金刚石、氧化铝、氧化硅，作为润滑油添加剂可以有效地将滑动摩擦变为滚动摩擦，起到微轴承的作用，有效地降低摩擦系数。因此，将片状材料和球形颗粒相结合，充分发挥其协同效应，将同时达到优异的抗磨及减摩性能。Mechanical friction and wear are ubiquitous in modern industrial production and life. The existence of friction and wear not only leads to a large amount of energy loss, but also damages the surface of parts and components, seriously reducing the service life of equipment. The emergence of nanomaterials provides a new option for the development of lubricating oil additives and has attracted widespread attention. Two-dimensional layered materials, such as graphene and molybdenum disulfide, are prone to slip under shear and have a low coefficient of friction. As a lubricant additive, they can form a transfer film on the surface of the friction pair, effectively reducing friction. Wear: One-dimensional spherical particles, such as diamond, alumina, and silicon oxide, as lubricating oil additives can effectively change sliding friction into rolling friction, play the role of micro-bearings, and effectively reduce the friction coefficient. Therefore, combining flake materials and spherical particles and giving full play to their synergistic effects will simultaneously achieve excellent anti-wear and anti-friction properties.
目前，用作润滑油添加剂的石墨烯大多采用改性Hummers法制备（Tribologyletters, 2011, 41(1): 209-215），其从水中分离转移至油中及在油中分散稳定非常困难，严重影响了石墨烯作为润滑油添加剂的性能及其工业应用。碳化硅，因其超高硬度，又被称为金刚砂，在高载荷下仍能起到有效地滚动轴承作用，但，因为其超高的熔点及稳定性，目前制备的碳化硅纳米颗粒多存在尖角处或为空心结构（Chemical Communications,2014, 50(9): 1070-1073），会造成摩擦副表面的划伤，未被作为润滑油添加剂进行研究。因此，一种经济、简单、有效的片状石墨烯与光滑球形碳化硅复合材料的制备方法，仍属于技术空白。At present, graphene used as lubricating oil additives is mostly prepared by the modified Hummers method (Tribologyletters, 2011, 41(1): 209-215), and it is very difficult to separate and transfer from water to oil and to disperse and stabilize in oil. It affects the performance of graphene as a lubricating oil additive and its industrial application. Silicon carbide, also known as corundum because of its ultra-high hardness, can still play an effective role in rolling bearings under high loads. However, because of its ultra-high melting point and stability, most of the silicon carbide nanoparticles currently prepared have sharp edges. The corners may be hollow structures (Chemical Communications, 2014, 50(9): 1070-1073), which will cause scratches on the surface of the friction pair, and have not been studied as lubricant additives. Therefore, an economical, simple and effective preparation method of flake graphene and smooth spherical silicon carbide composites is still a technical blank.
发明内容Contents of the invention
为了克服现有技术中存在的不足，本发明提供了一种夜光藻状石墨烯包碳化硅微球的原位快速制备方法，该方法操作简单，流程短，耗时少，能够快速形成类似夜光藻状的石墨烯包碳化硅微球。In order to overcome the deficiencies in the prior art, the present invention provides a rapid in-situ preparation method for luminous algae-like graphene-coated silicon carbide microspheres. Algae-like graphene-coated silicon carbide microspheres.
本发明针对现有化学溶剂法所制备石墨烯在润滑油中分散困难、实心碳化硅球形颗粒制备困难以及两者复合作润滑油添加剂的技术空白，首次提出采用液相激光辐照的方式来制备在油中具有高分散性的夜光藻状石墨烯包覆碳化硅微球。脉冲激光能够在瞬间（纳秒量级）产生超高温超高压的极端非平衡环境，使碳化硅纳米颗粒在激光辐照的光热和周围液体环境的快速冷却的双重作用下，原位实现碳化硅外延石墨烯的生长、部分多层石墨烯片的剥离以及无规则碳化硅颗粒的球形化，在室温室压下即可得到具有高分散性类夜光藻状的石墨烯包覆碳化硅微球。该方法操作简单，反应快速，无需高温高压环境，石墨烯由碳化硅直接分解得到，两者结合牢固，带状石墨烯显著提高了复合颗粒在油中的悬浮分散稳定性，避免了单独制备石墨烯和球形碳化硅颗粒的苛刻复杂工艺、机械混合不均匀、在油中易团聚等不足。In view of the difficulty in dispersing graphene in lubricating oil prepared by the existing chemical solvent method, the difficulty in preparing solid silicon carbide spherical particles, and the technical blank of the combination of the two as lubricating oil additives, the present invention proposes for the first time that the graphene is prepared by liquid-phase laser irradiation. Luminescent algae-like graphene-coated silicon carbide microspheres with high dispersibility in oil. The pulsed laser can generate an extremely non-equilibrium environment of ultra-high temperature and ultra-high pressure in an instant (on the order of nanoseconds), so that silicon carbide nanoparticles can be carbonized in situ under the dual effects of photoheat from laser irradiation and rapid cooling of the surrounding liquid environment. The growth of silicon epitaxial graphene, the peeling off of some multilayer graphene sheets and the spheroidization of random silicon carbide particles can obtain highly dispersed noctiluca-like graphene-coated silicon carbide microspheres at room temperature and pressure . The method is simple to operate, fast in reaction, and does not require a high temperature and high pressure environment. Graphene is directly decomposed from silicon carbide. The harsh and complex process of olefin and spherical silicon carbide particles, uneven mechanical mixing, and easy agglomeration in oil.
本发明具体技术方案如下：Concrete technical scheme of the present invention is as follows:
一种夜光藻状石墨烯包碳化硅微球的原位快速制备方法，其特征是包括以下步骤：A method for in-situ rapid preparation of silicon carbide microspheres coated with luminous algae-like graphene, characterized in that it comprises the following steps:
（1）将碳化硅粉末超声分散在液相介质中，形成悬浮液；(1) Ultrasonic dispersion of silicon carbide powder in liquid medium to form a suspension;
（2）在室温条件下，用脉冲激光辐照上述悬浮液，使碳化硅纳米颗粒在激光辐照的光热和周围液体环境的快速冷却的双重作用下，实现碳化硅外延石墨烯的生长、部分外层石墨烯片的剥离以及无规则碳化硅颗粒的球形化；(2) At room temperature, irradiate the above suspension with pulsed laser, so that the silicon carbide nanoparticles can grow SiC epitaxial graphene under the double action of the light heat of laser irradiation and the rapid cooling of the surrounding liquid environment. Partial exfoliation of outer graphene sheets and spheroidization of random silicon carbide particles;
（3）辐照完后，将悬浮液离心、分离、酸洗，所得沉淀干燥，得到夜光藻状石墨烯包碳化硅微球。(3) After the irradiation, the suspension was centrifuged, separated, pickled, and the resulting precipitate was dried to obtain luminous algae-like graphene-coated silicon carbide microspheres.
本发明所用的原料为碳化硅粉末，该粉末的粒度需小于1μm，既要保证聚焦后的激光束可以完全辐照整个颗粒，又要使其作为润滑油添加剂可以迅速进入摩擦副之间。原始碳化硅粉末可以为单晶或多晶；形状可为棒状或片状等；其在液相介质中的浓度为0.01-10mg mL-1，保证每个颗粒都可以被激光辐照并完成碳化硅的分解、石墨烯的生成以及无规则碳化硅颗粒的球形化。The raw material used in the present invention is silicon carbide powder, and the particle size of the powder needs to be less than 1 μm. It is necessary to ensure that the focused laser beam can completely irradiate the entire particle, and it must be used as a lubricating oil additive to quickly enter between friction pairs. The original silicon carbide powder can be single crystal or polycrystalline; the shape can be rod or flake, etc.; its concentration in the liquid medium is 0.01-10mg mL -1 , which ensures that each particle can be irradiated by laser and complete carbonization Decomposition of silicon, formation of graphene, and spheroidization of random silicon carbide particles.
本发明方法通过脉冲激光与液相溶剂的共同作用形成石墨烯包碳化硅结构。在选择液相介质时，要保证在整个激光辐照过程中颗粒能够稳定悬浮分散在溶剂中。当以水作为液相介质，激光辐照一段时间后形成的石墨烯包碳化硅颗粒会漂浮在水面上，阻挡了对水面下颗粒的辐照，最终无法保证全部碳化硅颗粒的转化。当选则无水乙醇作为分散介质时，从辐照开始至结束可以完全均匀地分散在液相介质中，故可以的得到均匀的夜光藻状石墨烯包碳化硅微球。The method of the invention forms a graphene-wrapped silicon carbide structure through the combined action of pulsed laser light and a liquid phase solvent. When selecting a liquid medium, it is necessary to ensure that the particles can be stably suspended and dispersed in the solvent during the entire laser irradiation process. When water is used as the liquid medium, the graphene-coated silicon carbide particles formed after laser irradiation for a period of time will float on the water surface, blocking the irradiation of the particles under the water surface, and ultimately cannot guarantee the transformation of all silicon carbide particles. When absolute ethanol is selected as the dispersion medium, it can be completely and uniformly dispersed in the liquid medium from the beginning to the end of the irradiation, so uniform luminescent algae-like graphene-coated silicon carbide microspheres can be obtained.
本发明步骤（2）中，脉冲激光的工作参数如下：波长小于310 nm，频率为2-15 Hz，能量密度为0.4-1.8 J pulse-1 cm-2，辐照时间为1-120 min。在本发明的具体实施方式中，脉冲激光束是采用以下方式形成的：由激光器发出激光束，然后经反光镜和凸透镜聚焦，形成所需光斑大小的脉冲激光束，调整至所需的工作参数，即可辐照悬浮分散液。In step (2) of the present invention, the working parameters of the pulse laser are as follows: the wavelength is less than 310 nm, the frequency is 2-15 Hz, the energy density is 0.4-1.8 J pulse -1 cm -2 , and the irradiation time is 1-120 min. In a specific embodiment of the present invention, the pulsed laser beam is formed in the following manner: the laser beam is emitted by a laser, and then focused by a mirror and a convex lens to form a pulsed laser beam with a required spot size and adjusted to the required working parameters , that is, the suspension dispersion can be irradiated.
优选的，步骤（2）中，脉冲激光的波长为193 nm、248 nm、308 nm。Preferably, in step (2), the wavelength of the pulse laser is 193 nm, 248 nm, 308 nm.
优选的，步骤（2）中，脉冲激光的能量密度为0.8-1.2 J pulse-1 cm-2。Preferably, in step (2), the energy density of the pulsed laser is 0.8-1.2 J pulse -1 cm -2 .
优选的，步骤（2）中，脉冲激光辐照5-30 min即可得到较好的产品。Preferably, in step (2), better products can be obtained by irradiating the pulsed laser for 5-30 min.
进一步，为了使辐照更均匀，悬浮分散液在搅拌下进行脉冲激光辐照，搅拌速度大于200 r min-1。Further, in order to make the irradiation more uniform, the suspension dispersion is irradiated with pulsed laser while stirring, and the stirring speed is greater than 200 r min -1 .
进一步，为了除去碳化硅分解得到的硅颗粒，需将离心后的沉淀进行酸洗，所用酸液为混合酸溶液，包括5-10 wt%氢氟酸和5-10 wt%双氧水。Further, in order to remove the silicon particles obtained by the decomposition of silicon carbide, the precipitate after centrifugation needs to be pickled, and the acid solution used is a mixed acid solution, including 5-10 wt% hydrofluoric acid and 5-10 wt% hydrogen peroxide.
本发明上述方法可以得到夜光藻状的石墨烯包碳化硅微球，该核壳结构利用漂浮带状的石墨烯提高了复合颗粒在油中的分散稳定性，同时充分发挥了二维层状材料和球状颗粒作为润滑油添加剂的优势，表现出优异的抗磨和减摩性能，添加量在0.06 wt%左右。The above method of the present invention can obtain luminous algae-like graphene-coated silicon carbide microspheres. The core-shell structure utilizes floating strip-shaped graphene to improve the dispersion stability of composite particles in oil, and at the same time fully utilizes the two-dimensional layered material. And the advantages of spherical particles as lubricating oil additives, showing excellent anti-wear and anti-friction performance, the addition amount is about 0.06 wt%.
本发明将碳化硅粉末分散在无水乙醇中，形成悬浮液，经反光镜和凸透镜聚焦后的激光束直接辐照该悬浮液，使溶剂中的碳化硅粉末瞬间（纳秒量级）获得高能量被烧蚀并被溶液迅速（纳秒量级）冷却，从而实现夜光藻状石墨烯包碳化硅微球的制备。In the present invention, the silicon carbide powder is dispersed in absolute ethanol to form a suspension, and the laser beam focused by a mirror and a convex lens is directly irradiated to the suspension, so that the silicon carbide powder in the solvent is instantly (on the order of nanoseconds) obtained high The energy is ablated and rapidly (on the order of nanoseconds) cooled by the solution, thereby realizing the preparation of luminous algae-like graphene-coated silicon carbide microspheres.
与现有技术相比，本发明的有益效果为：本制备方法新颖、产物纯度高无杂质污染，所得石墨烯包碳化硅微球在摩擦过程中具有优异的减摩和抗磨性能。Compared with the prior art, the beneficial effects of the present invention are: the preparation method is novel, the product has high purity and no impurity pollution, and the obtained graphene-coated silicon carbide microspheres have excellent anti-friction and anti-wear properties in the friction process.
（1）本发明只需要一步即可实现：石墨烯的原位外延生长、部分石墨烯层的剥离以及无规则碳化硅颗粒的球形化，得到具有夜光藻状的石墨烯包碳化硅微球，操作简单，制备成本低；(1) The present invention only needs one step to realize: the in-situ epitaxial growth of graphene, the peeling off of part of the graphene layer, and the spheroidization of random silicon carbide particles to obtain graphene-coated silicon carbide microspheres with noctilucent algae shape, Simple operation and low preparation cost;
（2）本发明可以适用于不同原始形貌和不同晶型的碳化硅粉末，如块状、棒状等不同形貌，单晶和多晶等不同晶型，原料选择范围广；(2) The present invention can be applied to silicon carbide powders with different original shapes and different crystal forms, such as different shapes such as block and rod, different crystal forms such as single crystal and polycrystalline, and a wide range of raw material selection;
（3）本发明制备过程只需要激光辐照分散在无水乙醇中的碳化硅粉末，不需要其他的氧化还原气氛、反应试剂和复杂实验装置，条件易控，工艺简单，成本低，解决了现有石墨烯制备及碳化硅球形化过程复杂和难以应用于润滑油添加剂的难题；(3) The preparation process of the present invention only needs to irradiate the silicon carbide powder dispersed in absolute ethanol with laser light, and does not require other redox atmospheres, reaction reagents and complicated experimental devices. The conditions are easy to control, the process is simple, and the cost is low. The existing graphene preparation and silicon carbide spheroidization process is complex and difficult to apply to lubricating oil additives;
（4）本发明方法得到的产物纯度高，无杂质污染，该石墨烯包碳化硅微球表面有漂浮带状的石墨烯，如同海洋生物夜光藻，能稳定分散在液体中，用作润滑油添加剂时能够快速吸附到摩擦副表面，同时球形颗粒可以有效地将滑动摩擦变为滚动摩擦，从而达到减摩和抗磨的双重优异性能。(4) The product obtained by the method of the present invention has high purity and no impurity pollution. The surface of the graphene-coated silicon carbide microspheres has graphene in a floating ribbon shape, which can be stably dispersed in liquids and used as lubricating oil, just like marine organisms nocturnal algae Additives can quickly adsorb to the surface of the friction pair, and at the same time, spherical particles can effectively change sliding friction into rolling friction, so as to achieve the double excellent performance of friction reduction and anti-wear.
附图说明Description of drawings
图1是无规则碳化硅粉末原料的透射电子显微镜图；Fig. 1 is the transmission electron microscope picture of random silicon carbide powder raw material;
图2是脉冲激光辐照后形成的夜光藻状石墨烯包碳化硅微球的扫描电子显微镜图；Figure 2 is a scanning electron micrograph of the noctilucent algae-like graphene-coated silicon carbide microspheres formed after pulsed laser irradiation;
图3是脉冲激光辐照后形成的夜光藻状石墨烯包碳化硅微球的透射电子显微镜图；Figure 3 is a transmission electron micrograph of the noctilucent algae-like graphene-coated silicon carbide microspheres formed after pulsed laser irradiation;
图4为脉冲激光辐照后形成的夜光藻状石墨烯包碳化硅微球的拉曼谱图；Fig. 4 is the Raman spectrum of the noctilucent algae-like graphene-coated silicon carbide microspheres formed after pulsed laser irradiation;
图5为对比例1所得产品的扫描电子显微镜图。Figure 5 is a scanning electron micrograph of the product obtained in Comparative Example 1.
具体实施方式detailed description
下面对本发明的实施例作详细说明，下述实施例是在本发明技术为前提下进行实施的，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。The embodiments of the present invention are described in detail below. The following embodiments are implemented on the premise of the technology of the present invention, and detailed implementation methods and specific operating procedures are provided, but the protection scope of the present invention is not limited to the following Example.
实施例1Example 1
（1）称取500 mg纳米碳化硅粉末（纯度99.9%，粒径小于0.04-0.2 μm）于烧杯中，加入50mL无水乙醇，超声分散，直至烧杯底部无任何沉淀，形成均匀悬浮液；(1) Weigh 500 mg of nano-silicon carbide powder (purity 99.9%, particle size less than 0.04-0.2 μm) into a beaker, add 50 mL of absolute ethanol, and ultrasonically disperse until there is no precipitation at the bottom of the beaker to form a uniform suspension;
（2）将通过反光镜和凸透镜聚焦后的氩氟激光束（193 nm）辐照上述步骤（1）制得的悬浮液，激光能量密度为0.8 J pulse-1 cm-1, 频率为2 Hz，辐照时间为20 min。激光束辐照过程中，磁力搅拌机以300 r min-1转速不断搅拌悬浮液；(2) The suspension prepared in the above step (1) was irradiated with the argon-fluorine laser beam (193 nm) focused by a mirror and a convex lens, with a laser energy density of 0.8 J pulse -1 cm -1 and a frequency of 2 Hz , and the irradiation time was 20 min. During the laser beam irradiation process, the magnetic stirrer kept stirring the suspension at a speed of 300 r min -1 ;
（3）辐照完后，离心悬浮液，然后用混合酸液（5 wt%氢氟酸和5 wt%双氧水）和去离子水各洗涤三次，干燥粉末，得到产品。(3) After irradiation, the suspension was centrifuged, then washed three times with a mixed acid solution (5 wt% hydrofluoric acid and 5 wt% hydrogen peroxide) and deionized water, and dried to obtain the product.
图1是步骤（1）中原始碳化硅粉末的透射电子显微镜图，从图中可以看出，原料中碳化硅的形貌多样、杂乱无规则。图2是辐照后所得产品的扫描电子显微镜图，从图中可以看出，产品形貌单一，为球形，其粒径为0.1-0.2 μm。图3是辐照后所得产品的透射电镜图，从图中可以看出碳化硅微球被石墨烯包覆，且部分石墨烯剥离形成漂浮带状结构，如同海洋生物夜光藻，故在液体中显示出较大悬浮力，进而能够稳定地分散在润滑油中。Figure 1 is a transmission electron microscope image of the original silicon carbide powder in step (1). It can be seen from the figure that the morphology of silicon carbide in the raw material is various and disorderly. Figure 2 is a scanning electron microscope image of the product obtained after irradiation. It can be seen from the figure that the product has a single appearance and is spherical, and its particle size is 0.1-0.2 μm. Figure 3 is a transmission electron microscope image of the product obtained after irradiation. It can be seen from the figure that the silicon carbide microspheres are coated with graphene, and part of the graphene is peeled off to form a floating ribbon structure, just like marine organisms nocturnal algae, so in the liquid It shows a large suspension force and can be stably dispersed in lubricating oil.
图4是辐照后所得石墨烯包碳化硅颗粒的拉曼图谱，从图中三个特征峰（D、G和2D）可以证明外延石墨烯的成功制备。Figure 4 is the Raman spectrum of graphene-coated silicon carbide particles obtained after irradiation. The three characteristic peaks (D, G and 2D) in the figure can prove the successful preparation of epitaxial graphene.
实施例2Example 2
（1）称取250 mg超细碳化硅粉末（纯度99%，粒径0.5-0.7 μm）于烧杯中，加入50 mL无水乙醇，超声分散，直至烧杯底部无任何沉淀，形成均匀悬浮液；(1) Weigh 250 mg of ultrafine silicon carbide powder (purity 99%, particle size 0.5-0.7 μm) into a beaker, add 50 mL of absolute ethanol, and ultrasonically disperse until there is no precipitation at the bottom of the beaker to form a uniform suspension;
（2）将通过反光镜和凸透镜聚焦后的氪氟激光束（248 nm）辐照上述步骤（1）制得的悬浮液，激光能量密度为1.0 J pulse-1 cm-1, 频率为10 Hz，辐照时间为10 min。激光束辐照过程中，用磁力搅拌机以700 r min-1转速不断搅拌悬浮液；(2) The suspension prepared in the above step (1) was irradiated with the krypton-fluorine laser beam (248 nm) focused by the mirror and the convex lens, the laser energy density was 1.0 J pulse -1 cm -1 , and the frequency was 10 Hz , and the irradiation time was 10 min. During laser beam irradiation, the suspension was continuously stirred with a magnetic stirrer at a speed of 700 rpm;
（3）辐照完后，离心悬浮液，然后用混合酸液（10 wt%氢氟酸和10 wt%双氧水）和去离子水各洗涤三次，干燥粉末，得到产品。所得产品形貌与实施例1类似，粒径为0.3-0.5μm。(3) After irradiation, the suspension was centrifuged, then washed three times with a mixed acid solution (10 wt% hydrofluoric acid and 10 wt% hydrogen peroxide) and deionized water, and dried to obtain the product. The appearance of the obtained product is similar to that of Example 1, and the particle size is 0.3-0.5 μm.
实施例3Example 3
（1）称取5 mg纳米碳化硅粉末（纯度99.9%，粒径小于0.04-0.2 μm）于烧杯中，加入50mL无水乙醇，超声分散，直至烧杯底部无任何沉淀，形成均匀悬浮液；(1) Weigh 5 mg of nano-silicon carbide powder (purity 99.9%, particle size less than 0.04-0.2 μm) into a beaker, add 50 mL of absolute ethanol, and ultrasonically disperse until there is no precipitation at the bottom of the beaker to form a uniform suspension;
（2）将通过反光镜和凸透镜聚焦后的氙氯激光束（308 nm）辐照上述步骤（1）制得的悬浮液，激光能量密度为1.2 J pulse-1 cm-1, 频率为15 Hz，辐照时间为5 min。激光束辐照过程中，用磁力搅拌机以1000 r min-1转速不断搅拌悬浮液；(2) The suspension prepared in the above step (1) was irradiated with the xenon-chlorine laser beam (308 nm) focused by the mirror and the convex lens, the laser energy density was 1.2 J pulse -1 cm -1 , and the frequency was 15 Hz , and the irradiation time was 5 min. During the laser beam irradiation process, the suspension was continuously stirred with a magnetic stirrer at a speed of 1000 r min -1 ;
（3）辐照完后，离心悬浮液，然后用混合酸液（5 wt%氢氟酸和10 wt%双氧水）和去离子水各洗涤三次，干燥粉末，得到产品。所得产品形貌与实施例1类似，粒径为0.1-0.2μm。(3) After irradiation, the suspension was centrifuged, washed three times with mixed acid solution (5 wt% hydrofluoric acid and 10 wt% hydrogen peroxide) and deionized water, and dried to obtain the product. The appearance of the obtained product is similar to that of Example 1, and the particle size is 0.1-0.2 μm.
实施例4Example 4
（1）称取100 mg纳米碳化硅粉末（纯度99.9%，粒径小于0.04-0.2 μm）于烧杯中，加入50mL无水乙醇，超声分散，直至烧杯底部无任何沉淀，形成均匀悬浮液；(1) Weigh 100 mg of nano-silicon carbide powder (purity 99.9%, particle size less than 0.04-0.2 μm) into a beaker, add 50 mL of absolute ethanol, and ultrasonically disperse until there is no precipitation at the bottom of the beaker to form a uniform suspension;
（2）将通过反光镜和凸透镜聚焦后的氪氟激光束（248 nm）辐照上述步骤（1）制得的悬浮液，激光能量密度为0.9 J pulse-1 cm-1, 频率为8 Hz，辐照时间为30 min。激光束辐照过程中，用磁力搅拌机以1200 r min-1转速不断搅拌悬浮液；(2) The suspension prepared in the above step (1) was irradiated with the krypton-fluorine laser beam (248 nm) focused by the mirror and the convex lens, the laser energy density was 0.9 J pulse -1 cm -1 , and the frequency was 8 Hz , and the irradiation time was 30 min. During the laser beam irradiation process, the suspension was continuously stirred with a magnetic stirrer at a speed of 1200 r min -1 ;
（3）辐照完后，离心悬浮液，然后用混合酸液（10 wt%氢氟酸和5 wt%双氧水）和去离子水各洗涤三次，干燥粉末，得到产品。所得产品形貌与实施例1类似，粒径为0.1-0.2μm。(3) After irradiation, the suspension was centrifuged, then washed three times with a mixed acid solution (10 wt% hydrofluoric acid and 5 wt% hydrogen peroxide) and deionized water, and dried to obtain the product. The appearance of the obtained product is similar to that of Example 1, and the particle size is 0.1-0.2 μm.
对比例1Comparative example 1
采用实施例1的方法制备石墨烯包碳化硅微球，不同的是：所采用碳化硅颗粒的直径为0.4-3 μm。辐照结束后，离心、分离、酸洗、干燥，得到产品。所得产品经扫描电镜测试显示颗粒形貌多样，大颗粒仍为存在尖角的多边形，难以球形化，只有粒径小于1 μm的颗粒转化为球形，如图5所示，这些无规则颗粒作为润滑油添加剂极易划伤摩擦副表面。The method of Example 1 was used to prepare graphene-coated silicon carbide microspheres, except that the diameter of the silicon carbide particles used was 0.4-3 μm. After the irradiation, centrifuge, separate, pickle and dry to obtain the product. The scanning electron microscope test of the obtained product shows that the particles have various shapes. The large particles are still polygons with sharp corners, which are difficult to spheroidize. Only the particles with a particle size of less than 1 μm are transformed into spherical shapes. As shown in Figure 5, these irregular particles are used as lubricants. Oil additives can easily scratch the surface of the friction pair.
对比例2Comparative example 2
采用实施例2的方法制备石墨烯包碳化硅微球，不同的是：激光能量密度为0.2 Jpulse-1 cm-1。辐照结束后，离心、分离、酸洗，得到产品。所得产品经扫描电镜测试显示碳化硅颗粒形貌基本未变化，仍为多边形，说明激光能量太低，不足以将高熔点的碳化硅颗粒熔融成球。Graphene-coated silicon carbide microspheres were prepared by the method of Example 2, except that the laser energy density was 0.2 Jpulse −1 cm −1 . After the irradiation, centrifuge, separate and pickle to obtain the product. The scanning electron microscope test of the obtained product shows that the shape of the silicon carbide particles is basically unchanged, and is still polygonal, indicating that the laser energy is too low to melt the silicon carbide particles with a high melting point into balls.
为了验证所得产品的减摩性能，进行以下实验。In order to verify the antifriction performance of the obtained product, the following experiments were carried out.
1、将上述各实施例和对比例制得产品分别添加到石蜡基础油中，进行摩擦性能测试，添加量均为基础油质量的0.06 wt% ；1, the above-mentioned each embodiment and comparative example are added to the paraffin base oil respectively, carry out the friction performance test, the addition is 0.06 wt% of the base oil quality;
2、摩擦性能测试方法：四球摩擦磨损实验，同时，以纯石蜡油为空白对照；2. Friction performance test method: four-ball friction and wear test, at the same time, pure paraffin oil is used as a blank control;
3、结果。各实施例和对比例产品的摩擦性测试结果，见下表1。3. Results. The friction test results of the products of each embodiment and comparative examples are shown in Table 1 below.
表1Table 1
由此可以看出，本发明方法制得的夜光藻状石墨烯包碳化硅微球在减摩和抗磨性能上有了很好的提升，明显高于对比例产品。原料的粒度和浓度、激光辐照的参数等条件对产品性能有较大影响。It can be seen from this that the noctilucent algae-like graphene-coated silicon carbide microspheres prepared by the method of the present invention have a good improvement in friction reduction and anti-wear properties, which are obviously higher than those of the comparative product. The particle size and concentration of raw materials, the parameters of laser irradiation and other conditions have a great impact on product performance.
Claims (6)
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Cited By (6)
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| CN108400311A (en) * | 2018-03-21 | 2018-08-14 | 济南大学 | A kind of cotton-shaped carbon silicon combination electrode material of N doping and its in-situ preparation method |
| CN108405871A (en) * | 2018-04-13 | 2018-08-17 | 济南大学 | It is a kind of that the method for sub-micron metal ball particle and its application in lubricating oil are prepared based on laser ablation method |
| CN110229709A (en) * | 2019-06-28 | 2019-09-13 | 中国人民解放军空军勤务学院 | SiC adulterates the preparation and application of onion shape graphitization carbon ball nanocomposite |
| CN110257128A (en) * | 2019-06-28 | 2019-09-20 | 中国人民解放军空军勤务学院 | Nitrogen-doped graphene/silicon carbide microsphere nano composite material, preparation and application |
| CN112408363A (en) * | 2020-12-01 | 2021-02-26 | 齐鲁工业大学 | In-situ preparation method of carbon nano tube |
| CN116496825A (en) * | 2023-04-24 | 2023-07-28 | 济南银河路桥试验检测有限公司 | Antiwear antifriction lubricating oil additive and modified lubricating oil using additive |
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| CN108400311A (en) * | 2018-03-21 | 2018-08-14 | 济南大学 | A kind of cotton-shaped carbon silicon combination electrode material of N doping and its in-situ preparation method |
| CN108400311B (en) * | 2018-03-21 | 2020-04-14 | 济南大学 | Nitrogen-doped flocculent carbon-silicon composite electrode material and in-situ preparation method thereof |
| CN108405871A (en) * | 2018-04-13 | 2018-08-17 | 济南大学 | It is a kind of that the method for sub-micron metal ball particle and its application in lubricating oil are prepared based on laser ablation method |
| CN110229709A (en) * | 2019-06-28 | 2019-09-13 | 中国人民解放军空军勤务学院 | SiC adulterates the preparation and application of onion shape graphitization carbon ball nanocomposite |
| CN110257128A (en) * | 2019-06-28 | 2019-09-20 | 中国人民解放军空军勤务学院 | Nitrogen-doped graphene/silicon carbide microsphere nano composite material, preparation and application |
| CN110229709B (en) * | 2019-06-28 | 2022-01-28 | 中国人民解放军空军勤务学院 | Preparation and application of SiC-doped onion-shaped graphitized carbon sphere nano composite material |
| CN112408363A (en) * | 2020-12-01 | 2021-02-26 | 齐鲁工业大学 | In-situ preparation method of carbon nano tube |
| CN116496825A (en) * | 2023-04-24 | 2023-07-28 | 济南银河路桥试验检测有限公司 | Antiwear antifriction lubricating oil additive and modified lubricating oil using additive |
| CN116496825B (en) * | 2023-04-24 | 2025-02-07 | 济南银河路桥试验检测有限公司 | Anti-wear and friction-reducing lubricating oil additive and modified lubricating oil using the additive |
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