CN103602362B - Preparation method of ferrous disulfide-graphene composite nano lubricant - Google Patents

Abstract

The invention discloses a preparation method of a ferrous disulfide-graphene composite nano lubricant. The preparation method is characterized by comprising the following steps: (1), adding matrix graphene, an iron source ferrous chloride and a dispersing agent into water to prepare liquor, regulating pH value to be alkaline, adding a vulcanizing agent thiourea, and uniformly mixing the liquor for future use; and (2), transferring the liquor into a stainless steel reaction kettle, sealing, cooling to the room temperature after carrying out hydrothermal reaction for 16 hours at 140 DEG C-240 DEG C, cleaning products by using deionized water, repeatedly cleaning by using absolute ethyl alcohol, carrying out vacuum drying to obtain black powder, wherein the structure of the black powder is that an FeS2 nanosphere coats on a graphene sheet layer, and dimension is 450 nm-800 nm. According to the preparation method, materials are easily available, price is low, preparation process is simple, parameters are easy to control, production process is safe and environment-friendly, and therefore, the preparation method is especially suitable for large-scale industrial production.

Description

The preparation method of a kind of ferrous disulfide-Graphene composite Nano lubricant

Technical field

The present invention relates to field of nanometer material technology, particularly, is a kind of FeS ₂the preparation method of-Graphene composite Nano lubricant.

Background technology

In recent years, transition-metal sulphides MS ₂(M=Mo, W, Fe, Zn etc.), due to physicochemical property and the novel structure of its uniqueness, get more and more people's extensive concerning and further investigate.These materials are extensively used as lithium ion cell electrode, lubricating oil additive, new catalyst and thermoelectric material etc.As the important a member in transition-metal sulphides, FeS ₂(pyrite) there are very high photoabsorption coefficient (α=6 × 10, visible region ⁵cm ^-1) and suitable band gap width (Eg=0.95eV) optics of its excellence, electrochemistry and magnetic behavior make it have good potential application foreground in fields such as solar energy photoelectric conversion technology, specific function electrode materials and electromagnetic materials in addition.Especially, FeS ₂have laminate structure, respectively with covalent bonds between atom, interlayer combines with more weak Van der Waals force, being used as the slip of lubricating oil additive when being subject to shearing force between easy genetic horizon, thus playing the effect of antifriction.But at present, to its as solid additive at the rare report of the research of tribological field.FeS ₂common preparation method mainly contain electrodip process, heat curing system, chemical vapor transportation method, Laser vaporization, spray pyrolysis, solvent-thermal method etc., all more complicated.

Summary of the invention

The object of the present invention is to provide a kind of preparation method of FeS2-Graphene composite Nano lubricant, raw material be easy to get, cheap, preparation technology is simple, parameter is easily controlled, production process safety and environmental protection, is particularly suitable for large-scale industrial production.

A kind of FeS ₂the preparation method of-Graphene composite Nano lubricant, is characterized in that comprising the steps:

(1) matrix graphite alkene, source of iron iron protochloride, dispersion agent are added to the water obtained solution, adjust ph is alkalescence, adds vulcanizing agent thiocarbamide, is mixed by solution, for subsequent use;

The mol ratio of iron protochloride and thiocarbamide is 2:1-1:3; The mol ratio of Graphene and iron protochloride is 4:1-1:1; The mol ratio 1:4-1:10 of dispersion agent and iron protochloride;

Described dispersion agent is cats product, and as cetyl trimethylammonium bromide, or other materials is as polyvinylpyrrolidone.

(2) solution is moved into stainless steel cauldron, sealing, after 140 DEG C ~ 240 DEG C hydro-thermal reaction 16h, be cooled to room temperature, use washed with de-ionized water product, more repeatedly clean with dehydrated alcohol, obtain black powder after vacuum-drying, structure is FeS ₂nanometer ball is coated on graphene sheet layer, and size is at 450-800nm.

Compared with traditional preparation methods, the present invention adopts water heat transfer FeS ₂, temperature of reaction is lower, preparation process gentle pollution-free, product purity is higher and FeS ₂nano-powder particle size uniformity, good dispersity, add it in base oil rear its of test as lubricating oil additive and there is good frictional behaviour.

Accompanying drawing explanation

Fig. 1 is the FeS that the present invention obtains ₂field emission scanning electron microscope (SEM) photo of-Graphene composite Nano lubricant.Fig. 1 is the SEM figure of the product at 180 DEG C in the stainless steel cauldron of tetrafluoroethylene for liner prepared by hydro-thermal reaction 16 hours.Fig. 1 a can find out prepared size uniform, dispersed ball-like structure FeS preferably ₂growth is on graphene sheet layer, and its size is between 450-800nm and particle surface smoother (Fig. 1 b).

Fig. 2 is the FeS that the present invention obtains ₂the XRD spectra of-Graphene composite Nano lubricant.As can be seen from the figure, all peak positions all fit like a glove with standard diffraction figure (JCPDS No.71-2219), and do not have other assorted peaks to occur, illustrate that reaction product is the FeS that purity is higher ₂cubic system, counting lattice lattice constant is 0.5431nm.In figure, each diffraction peak is all strong and sharp-pointed, shows FeS ₂the degree of crystallinity of nano-powder is very good.(amount due to Graphene seldom can only see the Graphene laminate structure of part, and in XRD, the peak value of Graphene cannot detect).

Embodiment

The present invention is further described below by way of embodiment, as known by the technical knowledge, the present invention also describes by other the scheme not departing from the technology of the present invention feature, and the change therefore within the scope of the present invention all or equivalent scope of the invention is all included in the invention.

Embodiment 1:

0.1g Graphene is dissolved in 20ml deionized water for ultrasonic 1h, then the polyvinylpyrrolidone (PVP) of 0.3g and the iron(ic) chloride of 0.2g is added respectively, dripping 5ml concentration is until completely dissolved the NaOH solution of 0.5M, then adds the thiocarbamide of 0.2g, magnetic agitation 30min.Solution is transferred to 180 DEG C of insulation reaction 16h in the band teflon-lined stainless steel cauldron of 50ml.Be cooled to room temperature, centrifuge washing, in vacuum drying oven, 60 DEG C of vacuum-drying 8h, obtain black powder.

Embodiment 2:

Difference from Example 1 is polyvinylpyrrolidone to replace with cetyl trimethylammonium bromide.

Embodiment 3: difference from Example 1 is that the consumption of Graphene is 0.2g, and dispersion agent is cetyl trimethylammonium bromide.

The consumption of the component that embodiment 4 to embodiment 7 adopts and processing parameter as shown in table 1:

Table 1

Frictional behaviour is tested: experimental technique, utilizes ultrasonic generator by dispersion agent span80 and product FeS ₂-Graphene composite Nano lubricant is distributed in base oil (paraffin) uniformly, and the dirty solution oil sample frictional experiment that to be mixed with containing massfraction be 1%-5% carries out frictional experiment (table 2 just lists the friction that mass mark is 5%) on CETR UMT-2 multifunction friction wear testing machine.Adopt ball-disc type contact, rotating speed is 50 ~ 400rpm, and load is 10N ~ 50N, and experimental period is 30min.Testing Stainless Steel Ball model used is 440-C(9Cr18), diameter is 3mm, and hardness is HRC62.

Embodiment 1 to 3 gained FeS ₂the frictional coefficient of-Graphene composite Nano lubricant is as shown in table 2:

Table 2

Claims (1)

1. a preparation method for ferrous disulfide-Graphene composite Nano lubricant, is characterized in that comprising the steps:

(1) matrix graphite alkene, source of iron iron protochloride, dispersion agent are added to the water obtained solution, adjust ph is alkalescence, adds vulcanizing agent thiocarbamide, is mixed by solution, for subsequent use; Described dispersion agent is cetyl trimethylammonium bromide or polyvinylpyrrolidone; The mol ratio of iron protochloride and thiocarbamide is 2:1-1:3; The mol ratio of Graphene and iron protochloride is 4:1-1:1; The mol ratio 1:4-1:10 of dispersion agent and iron protochloride;

(2) solution is moved into stainless steel cauldron, sealing, after 140 DEG C ~ 240 DEG C hydro-thermal reaction 16h, be cooled to room temperature, use washed with de-ionized water product, more repeatedly clean with dehydrated alcohol, obtain black powder after vacuum-drying, structure is FeS ₂nanometer ball is coated on graphene sheet layer, and size is at 450-800nm.