CN112625774A - Graphene-loaded cerium oxide nanoparticle composite material and preparation method thereof - Google Patents
Graphene-loaded cerium oxide nanoparticle composite material and preparation method thereof Download PDFInfo
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- CN112625774A CN112625774A CN202011390755.9A CN202011390755A CN112625774A CN 112625774 A CN112625774 A CN 112625774A CN 202011390755 A CN202011390755 A CN 202011390755A CN 112625774 A CN112625774 A CN 112625774A
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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
- C10M125/02—Carbon; Graphite
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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
- C10M125/10—Metal oxides, hydroxides, carbonates or bicarbonates
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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
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
Abstract
The invention discloses a graphene loaded cerium oxide nanoparticle composite material and a preparation method thereof, wherein the preparation method comprises the following steps: step 1: preparing a graphene oxide dispersion liquid; step 2: preparing a cerous nitrate hexahydrate solution, and adding the cerous nitrate hexahydrate solution into the graphene oxide dispersion liquid; and step 3: adding ammonia water and hydrazine hydrate into the solution obtained in the step (2); and 4, step 4: carrying out hydrothermal reaction on the solution obtained in the step (3), and washing and drying a product after the reaction is finished to obtain the graphene-loaded cerium oxide nanoparticle composite material, wherein the preparation method has strong repeatability, the preparation process is simple and convenient, and the preparation period is short; the prepared graphene-loaded cerium oxide nanoparticle composite material has the advantages that cerium oxide grows on the surface of graphene oxide uniformly and compactly, and the surface roughness of the composite material is improved.
Description
Technical Field
The invention belongs to the field of preparation of nano composite materials, and particularly relates to a graphene-loaded cerium oxide nano particle composite material and a preparation method thereof.
Background
With the continuous development of tribology, the types and the quantities of lubricants and lubricating oil additives are increasing, and the structures which are most widely applied and researched are nano sheets and nano microspheres. The nano microspheres generally comprise sulfide and oxide, and the unique stick-slip effect of the structure endows the materials with good antifriction performance. Sulfide is a lubricating material which is widely researched and applied, but toxicity and pollution of sulfide per se are contrary to green economy and environmental protection advocated today. With the continuous deepening of friction research, the rare earth oxide gradually enters the visual field and practice of people in recent years due to multiple excellent characteristics, and the cerium oxide serving as a microspheric structure is found to have good lubricating and antifriction effects in lubricating oil. Rare earth elements, called "industrial vitamins", have become very important strategic resources in the world today, being able to greatly improve the strength, hardness and toughness of metal alloys. Therefore, the application of rare earth oxide in the field of tribology to research on the frictional wear performance of rare earth oxide has a long-term significance in the aspects of modern industrial development and national improvement of strength.
Although rare earth oxides, particularly cerium oxide, have practical application effects in tribology, the current research shows that pure rare earth oxides have obvious defects in lubricating, friction reducing and wear resisting capabilities and have certain limitations in application range. Therefore, it is necessary and important to develop the excellent performance and application of rare earth oxide materials to improve their respective abilities or develop new rare earth oxide materials for friction and wear reduction. A great deal of research shows that graphene also plays a critical role in the application and material composition of rare earth oxides. Therefore, the graphene/cerium oxide composite material is expected to be widely applied to the field of lubricating additives.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a graphene-loaded cerium oxide nanoparticle composite material and a preparation method thereof, wherein the preparation method has strong repeatability, simple and convenient preparation process and short preparation period; the prepared graphene-loaded cerium oxide nanoparticle composite material has the advantages of uniform appearance and controllable size of cerium oxide nanoparticles, and the roughness of the surface of the composite material is improved.
In order to achieve the above object, the present invention provides a preparation method of a graphene-supported cerium oxide nanoparticle composite material, comprising the steps of:
step 1: adding 0.50-0.70 g of graphene oxide into 40-70 mL of deionized water to obtain a graphene oxide dispersion liquid;
step 2: dissolving 0.5-1 g of cerous nitrate hexahydrate in 20-40 mL of deionized water to obtain a cerous nitrate hexahydrate solution, and adding the cerous nitrate hexahydrate solution into the graphene oxide dispersion liquid obtained in the step 1 to obtain a solution A;
and step 3: adding 1-1.2 mL of ammonia water and 1-1.2 mL of hydrazine hydrate into the solution A to obtain a solution B;
and 4, step 4: and carrying out hydrothermal reaction on the solution B in a reaction kettle at the temperature of 180-250 ℃, and washing and drying a product after the reaction is finished to obtain the graphene loaded cerium oxide nanoparticle composite material.
Preferably, the graphene oxide in the step 1 is added into deionized water and subjected to ultrasonic dispersion for 2-4 hours.
Preferably, in the step 2, the cerous nitrate hexahydrate is dissolved in deionized water, and the cerous nitrate hexahydrate solution is added into the graphene oxide dispersion liquid, and magnetic stirring is adopted.
Preferably, the volume ratio of the ammonia water to the hydrazine hydrate in the step 3 is 1: 1.
preferably, the ammonia water and the hydrazine hydrate in the step 3 are sequentially added dropwise into the solution A by a pipette.
Preferably, the hydrothermal reaction time in the step 4 is 12-24 h.
Preferably, the hydrothermal reaction in the step 4 is performed in a polytetrafluoroethylene stainless steel reaction kettle.
Preferably, the product obtained in the step 4 is firstly centrifugally washed with deionized water for 1-3 times, and then centrifugally washed with absolute ethyl alcohol for 1-2 times.
Preferably, the product in step 4 is dried at a temperature of 60 ℃ to 80 ℃.
The invention also provides a graphene-loaded cerium oxide nanoparticle composite material prepared by the preparation method.
Compared with the prior art, the preparation method adopts a hydrothermal method to synthesize the graphene-loaded cerium oxide nanoparticle composite material, the experimental process conditions are mild, compared with the traditional lubricating additive, the used raw materials are environment-friendly, safe and nontoxic, and the prepared graphene-loaded cerium oxide nanoparticle composite material is green and pollution-free and is compounded with the current advocated green economy and environmental protection; the preparation method has the advantages of simple process, strong repeatability, low cost, short preparation period, easy realization of large-scale production and wide practical application value and industrial production prospect. In the prepared graphene-loaded cerium oxide nanoparticle composite material, cerium oxide grows uniformly and compactly on the surface of graphene oxide, the size of the cerium oxide nanoparticle is controllable through simple temperature adjustment, the cerium oxide nanoparticle is uniformly and compactly loaded on the surface of the graphene oxide, the roughness of the surface of the composite material is improved, the problem of inertia of the graphene oxide is solved, the friction coefficient of the composite material is improved, the bonding strength between the composite material and a substrate is improved, in addition, the cerium oxide nanoparticle is dispersed more uniformly, the agglomeration problem is avoided, and the application of the composite material in the field of lubricating additives is improved.
Drawings
Fig. 1 is a scanning electron micrograph of graphene oxide;
fig. 2 is a scanning electron microscope image of the graphene-supported cerium oxide nanoparticle composite material prepared according to the embodiment of the present invention;
fig. 3 is a comparative XRD analysis diagram of cerium oxide, graphene oxide, and a graphene-supported cerium oxide nanoparticle composite material prepared according to an example of the present invention.
Detailed Description
The present invention will be further explained with reference to the drawings and specific examples in the specification, and it should be understood that the examples described are only a part of the examples of the present application, and not all examples. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The invention discloses a preparation method of a graphene loaded cerium oxide nanoparticle composite material, which comprises the following steps:
step 1: adding 0.50-0.70 g of graphene oxide into 40-70 mL of deionized water to obtain a graphene oxide dispersion liquid; preferably, adding the graphene oxide into deionized water, and performing ultrasonic dispersion for 2-4 hours;
step 2: dissolving 0.5-1 g of cerous nitrate hexahydrate in 20-40 mL of deionized water to obtain a cerous nitrate hexahydrate solution, and adding the cerous nitrate hexahydrate solution into the graphene oxide dispersion liquid obtained in the step 1 to obtain a solution A; preferably, dissolving the cerous nitrate hexahydrate in deionized water, adding the cerous nitrate hexahydrate solution into the graphene oxide dispersion liquid, and magnetically stirring;
and step 3: adding 1-1.2 mL of ammonia water and 1-1.2 mL of hydrazine hydrate into the solution A to obtain a solution B; preferably, the volume ratio of the used amount of the ammonia water to the used amount of the hydrazine hydrate is 1: 1; ammonia water and hydrazine hydrate are sequentially dripped into the solution A by adopting a pipette drop by drop;
and 4, step 4: and carrying out hydrothermal reaction on the solution B in a reaction kettle at the temperature of 180-250 ℃, and washing and drying a product after the reaction is finished to obtain the graphene loaded cerium oxide nanoparticle composite material. Preferably, the time of the hydrothermal reaction is 12-24 h; the hydrothermal reaction is carried out in a polytetrafluoroethylene stainless steel reaction kettle; and (3) centrifugally washing the product for 1-3 times by using deionized water, centrifugally washing for 1-2 times by using absolute ethyl alcohol, and drying at the temperature of 60-80 ℃.
The invention is described below with reference to specific examples:
example 1:
1. preparing a graphene oxide dispersion liquid: weighing 0.50g of graphene oxide, adding the graphene oxide into a beaker containing 40mL of deionized water, and performing ultrasonic dispersion for 2 hours to obtain a graphene oxide dispersion liquid;
2. weighing 0.54g of cerous nitrate hexahydrate, dissolving into 20mL of deionized water, slowly pouring the solution into the graphene oxide dispersion liquid prepared in the step 1, and continuously stirring;
3. respectively measuring 1mL of ammonia water and 1mL of hydrazine hydrate solution, sequentially dropwise adding the ammonia water and the 1mL of hydrazine hydrate solution into the mixed solution obtained in the step (2) by using a pipette, and continuously stirring for 5 min; then transferring the mixture into a 100mL polytetrafluoroethylene stainless steel reaction kettle, and placing the reaction kettle in an oven at 200 ℃ for reaction for 24 hours; and (3) washing a product obtained by the reaction with a centrifugal washing agent, and then drying at 60 ℃ to finally obtain a gray graphene/cerium oxide composite material.
Example 2:
1. preparing a graphene oxide dispersion liquid: weighing 0.60g of graphene oxide, adding the graphene oxide into a beaker containing 40mL of deionized water, and performing ultrasonic dispersion for 3 hours to obtain a graphene oxide dispersion liquid;
2. weighing 0.54g of cerous nitrate hexahydrate, dissolving into 20mL of deionized water, slowly pouring the solution into the graphene oxide dispersion liquid prepared in the step 1, and continuously stirring;
3. respectively measuring 1mL of ammonia water and 1mL of hydrazine hydrate solution, sequentially dropwise adding the ammonia water and the 1mL of hydrazine hydrate solution into the mixed solution obtained in the step 2 by using a pipette, and continuously stirring for 6 min; then transferring the mixture into a 100mL polytetrafluoroethylene stainless steel reaction kettle, and placing the reaction kettle in an oven at 210 ℃ for reaction for 24 hours; and (3) drying a product obtained by the reaction at 60 ℃ by using a centrifugal washing agent to finally obtain a gray graphene/cerium oxide composite material.
Example 3:
1. preparing a graphene oxide dispersion liquid: weighing 0.70g of graphene oxide, adding the graphene oxide into a beaker containing 40mL of deionized water, and performing ultrasonic dispersion for 2.5 hours to obtain a graphene oxide dispersion liquid;
2. weighing 0.54g of cerous nitrate hexahydrate, dissolving into 20mL of deionized water, slowly pouring the solution into the graphene oxide dispersion liquid prepared in the step 1, and continuously stirring;
3. respectively measuring 1mL of ammonia water and 1mL of hydrazine hydrate solution, sequentially dropwise adding the ammonia water and the 1mL of hydrazine hydrate solution into the mixed solution obtained in the step 2 by using a pipette, and continuously stirring for 4 min; then transferring the mixture into a 100mL polytetrafluoroethylene stainless steel reaction kettle, placing the reaction kettle in an oven at 220 ℃ and reacting for 24 hours; and (3) washing a product obtained by the reaction with a centrifugal washing agent, and then drying at 60 ℃ for 5h to finally obtain the gray graphene/cerium oxide composite material.
Example 4:
1. preparing a graphene oxide dispersion liquid: weighing 0.50g of graphene oxide, adding the graphene oxide into a beaker containing 50mL of deionized water, and performing ultrasonic dispersion for 2 hours to obtain a graphene oxide dispersion liquid;
2. weighing 0.5g of cerous nitrate hexahydrate, dissolving into 20mL of deionized water, slowly pouring the solution into the graphene oxide dispersion liquid prepared in the step 1, and continuously stirring;
3. respectively measuring 1mL of ammonia water and 1mL of hydrazine hydrate solution, sequentially dropwise adding the ammonia water and the 1mL of hydrazine hydrate solution into the mixed solution obtained in the step 2 by using a pipette, and continuously stirring for 5 min; then transferring the mixture into a 100mL polytetrafluoroethylene stainless steel reaction kettle, and placing the reaction kettle in an oven at 180 ℃ for reaction for 12 hours; and (3) washing a product obtained by the reaction with a centrifugal washing agent, and then drying at 60 ℃ for 6h to finally obtain a gray graphene/cerium oxide composite material.
Example 5:
1. preparing a graphene oxide dispersion liquid: weighing 0.6g of graphene oxide, adding the graphene oxide into a beaker containing 60mL of deionized water, and performing ultrasonic dispersion for 3 hours to obtain a graphene oxide dispersion liquid;
2. weighing 0.7g of cerous nitrate hexahydrate, dissolving into 30mL of deionized water, slowly pouring the solution into the graphene oxide dispersion liquid prepared in the step 1, and continuously stirring;
3. respectively measuring 1.1mL of ammonia water and 1.1mL of hydrazine hydrate solution, sequentially dropwise adding the ammonia water and the hydrazine hydrate solution into the mixed solution obtained in the step 2 by using a pipette, and continuously stirring for 8 min; then transferring the mixture into a 100mL polytetrafluoroethylene stainless steel reaction kettle, placing the reaction kettle in an oven at 220 ℃ and reacting for 18 h; and (3) washing a product obtained by the reaction with a centrifugal washing agent, and then drying at 70 ℃ for 4h to finally obtain a gray graphene/cerium oxide composite material.
Example 6:
1. preparing a graphene oxide dispersion liquid: weighing 0.7g of graphene oxide, adding the graphene oxide into a beaker containing 70mL of deionized water, and performing ultrasonic dispersion for 4 hours to obtain a graphene oxide dispersion liquid;
2. weighing 1.0g of cerous nitrate hexahydrate, dissolving into 40mL of deionized water, slowly pouring the solution into the graphene oxide dispersion liquid prepared in the step 1, and continuously stirring;
3. respectively measuring 1.2mL of ammonia water and 1.2mL of hydrazine hydrate solution, sequentially dropwise adding the ammonia water and the hydrazine hydrate solution into the mixed solution obtained in the step 2 by using a pipette, and continuously stirring for 10 min; then transferring the mixture into a 100mL polytetrafluoroethylene stainless steel reaction kettle, placing the reaction kettle in an oven at 250 ℃ and reacting for 24 hours; and (3) washing a product obtained by the reaction with a centrifugal washing agent, and then drying at 80 ℃ for 3h to finally obtain a gray graphene/cerium oxide composite material.
Example 7:
1. preparing a graphene oxide dispersion liquid: weighing 0.55g of graphene oxide, adding the graphene oxide into a beaker containing 45mL of deionized water, and performing ultrasonic dispersion for 2.5 hours to obtain a graphene oxide dispersion liquid;
2. weighing 0.7g of cerous nitrate hexahydrate, dissolving into 25mL of deionized water, slowly pouring the solution into the graphene oxide dispersion liquid prepared in the step 1, and continuously stirring;
3. respectively measuring 1.15mL of ammonia water and 1.05mL of hydrazine hydrate solution, sequentially dropwise adding the ammonia water and the hydrazine hydrate solution into the mixed solution obtained in the step 2 by using a pipette, and continuously stirring for 15 min; then transferring the mixture into a 100mL polytetrafluoroethylene stainless steel reaction kettle, and placing the reaction kettle in an oven at 190 ℃ for reaction for 22 h; and (3) washing a product obtained by the reaction with a centrifugal washing agent, and then drying at 75 ℃ for 4h to finally obtain a gray graphene/cerium oxide composite material.
Example 8:
1. preparing a graphene oxide dispersion liquid: weighing 0.65g of graphene oxide, adding the graphene oxide into a beaker containing 65mL of deionized water, and performing ultrasonic dispersion for 4 hours to obtain a graphene oxide dispersion liquid;
2. weighing 0.8g of cerous nitrate hexahydrate, dissolving into 35mL of deionized water, slowly pouring the solution into the graphene oxide dispersion liquid prepared in the step 1, and continuously stirring;
3. respectively measuring 1.05mL of ammonia water and 1.2mL of hydrazine hydrate solution, sequentially dropwise adding the ammonia water and the hydrazine hydrate solution into the mixed solution obtained in the step 2 by using a pipette, and continuously stirring for 14 min; then transferring the mixture into a 100mL polytetrafluoroethylene stainless steel reaction kettle, placing the reaction kettle in a 240 ℃ oven, and reacting for 23 h; and (3) washing a product obtained by the reaction with a centrifugal washing agent, and then drying at 78 ℃ for 4h to finally obtain a gray graphene/cerium oxide composite material.
Fig. 1 is an SEM image of graphene oxide, and it can be seen that graphene oxide exhibits a typical two-dimensional lamellar morphology, and van der waals force bonds between layers and easily slides when subjected to tangential force, thereby reducing the coefficient of friction.
Scanning a graphene/cerium oxide composite material prepared by the method disclosed by the invention through an SEM (scanning electron microscope), referring to fig. 2, cerium oxide nanoparticles are uniformly and compactly loaded on the surface of graphene oxide in fig. 2, so that the surface roughness is improved, the problem of inertia of the graphene oxide is solved, the combination between the composite material and a matrix is improved, and in addition, the problem of agglomeration is avoided due to the fact that the composite material is dispersed more uniformly.
Comparing the XRD analysis of the cerium oxide, the graphene oxide and the graphene/cerium oxide nanocomposite prepared by the present invention, referring to fig. 3, it can be seen that the XRD peaks of the graphene/cerium oxide nanocomposite prepared by the present invention can correspond to the peaks of CeO one by one, and simultaneously the (001) and (002) crystal planes of the graphene oxide disappear, indicating that the graphene oxide has been reduced to reduced graphene oxide, and the cerium oxide has successfully grown on the surface of the reduced graphene oxide.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of a graphene-loaded cerium oxide nanoparticle composite material is characterized by comprising the following steps:
step 1: adding 0.50-0.70 g of graphene oxide into 40-70 mL of deionized water to obtain a graphene oxide dispersion liquid;
step 2: dissolving 0.5-1 g of cerous nitrate hexahydrate in 20-40 mL of deionized water to obtain a cerous nitrate hexahydrate solution, and adding the cerous nitrate hexahydrate solution into the graphene oxide dispersion liquid obtained in the step 1 to obtain a solution A;
and step 3: adding 1-1.2 mL of ammonia water and 1-1.2 mL of hydrazine hydrate into the solution A to obtain a solution B;
and 4, step 4: and carrying out hydrothermal reaction on the solution B in a reaction kettle at the temperature of 180-250 ℃, and washing and drying a product after the reaction is finished to obtain the graphene loaded cerium oxide nanoparticle composite material.
2. The preparation method of the graphene-supported cerium oxide nanoparticle composite material according to claim 1, wherein the graphene oxide is added into deionized water in the step 1 and subjected to ultrasonic dispersion for 2-4 hours.
3. The method for preparing the graphene-supported cerium oxide nanoparticle composite material according to claim 1, wherein in the step 2, the cerium nitrate hexahydrate is dissolved in deionized water, and the cerium nitrate hexahydrate solution is added to the graphene oxide dispersion liquid, and magnetic stirring is adopted.
4. The method for preparing the graphene-supported cerium oxide nanoparticle composite material according to claim 1, wherein the volume ratio of the ammonia water to the hydrazine hydrate in the step 3 is 1: 1.
5. the preparation method of the graphene-supported cerium oxide nanoparticle composite material according to claim 1 or 4, wherein the ammonia water and the hydrazine hydrate in the step 3 are sequentially added dropwise into the solution A by a pipette.
6. The preparation method of the graphene-supported cerium oxide nanoparticle composite material according to claim 1, wherein the hydrothermal reaction time in the step 4 is 12-24 hours.
7. The preparation method of the graphene-supported cerium oxide nanoparticle composite material according to claim 1 or 6, wherein the hydrothermal reaction in the step 4 is performed in a polytetrafluoroethylene stainless steel reaction kettle.
8. The method for preparing the graphene-supported cerium oxide nanoparticle composite material according to claim 1 or 6, wherein the product obtained in the step 4 is first centrifugally washed with deionized water for 1-3 times, and then centrifugally washed with absolute ethyl alcohol for 1-2 times.
9. The method for preparing the graphene-supported cerium oxide nanoparticle composite material according to claim 1 or 6, wherein the product obtained in the step 4 is dried at a temperature of 60-80 ℃.
10. A graphene-supported cerium oxide nanoparticle composite material, characterized by being prepared by the method for preparing the graphene-supported cerium oxide nanoparticle composite material according to any one of claims 1 to 9.
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