CN117680676A - Preparation method of antioxidant high-conductivity graphene-copper composite powder - Google Patents
Preparation method of antioxidant high-conductivity graphene-copper composite powder Download PDFInfo
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Abstract
The invention provides a preparation method of antioxidant high-conductivity graphene-copper composite powder, belongs to the field of conductive material manufacture, and solves the problems of uneven particle distribution, poor composite material bonding effect and impurity introduction in the traditional preparation process. The preparation method of the invention comprises the following steps: s1, ball milling of copper powder; s2, mixing; s3, drying; s4, heating; s5, cooling. According to the invention, the graphene is coated on the copper powder, so that the oxidation rate of copper is effectively slowed down, and the excellent conductivity of the graphene is improved, and meanwhile, the overall conductivity of the copper powder is improved. According to the invention, by improving the stirring process and optimizing the mixing parameters, the agglomeration phenomenon of copper powder is effectively avoided, and the uniform distribution of copper powder particles is realized. By introducing a proper polymer and optimizing heat treatment parameters, the interface combination between the graphene and the copper powder is enhanced, and the generation of side reaction products is reduced by optimizing reaction conditions.
Description
Technical Field
The invention belongs to the field of conductive material manufacturing, and relates to graphene coated copper powder, in particular to a preparation method of antioxidant high-conductivity graphene-copper composite powder.
Background
Copper is widely used as a conductive material in practical production, but copper is easily oxidized to form a copper oxide layer, so that the conductivity is reduced, and in some applications, particularly in the occasions requiring high stability and long-term use, the oxidation problem limits the use of copper, and in addition, the weight of copper is relatively large, so that the weight becomes a disadvantageous factor in some application scenes requiring light weight.
As the excellent properties of graphene in terms of electrical conductivity, thermal conductivity, mechanical properties and the like are widely recognized, research and application of graphene composite materials gradually become hot spots of research, wherein graphene-coated copper powder is used as an important composite material, and has wide application prospects, for example, in the fields of electrical conductive paint, electronic devices, thermal conductive materials and the like, however, in the current technology, the composite material of graphene and copper powder still has some key problems, so that the performance and stability of the composite material in practical application are restricted, and the main problems are as follows:
non-uniform particle distribution: in the prior art, when preparing the graphene coated copper powder, uniform distribution of copper powder particles is difficult to realize, so that agglomeration phenomenon exists in the composite material, and the overall performance of the material is influenced; a common problem is that good dispersion is not achieved during the mixing process, resulting in agglomeration of the copper powder, which is caused by uneven stirring during the preparation process, improper selection of the dispersing agent or insufficient mixing time, and the like, and it is critical to improve the stirring process, select an appropriate dispersing agent, and optimize the mixing parameters.
The composite material has poor bonding effect: the conventional composite method has certain limitation in enhancing the bonding effect of graphene and copper powder, and especially has insufficient structural integrity and stability under high temperature conditions; conventional compounding methods may suffer from structural imperfections and insufficient stability; for example, the heat treatment process may result in a decrease in the bonding effect between the graphene and copper powder. The improved method comprising introducing a suitable cross-linking agent, optimizing the heat treatment parameters to enhance interfacial bonding is critical to solving this problem.
Impurities may be introduced during the preparation: the existing preparation method often introduces some impurities or residual substances, which affects the purity and performance of the final product; for example, reducing agents, surface modifying agents, or other treating agents used in chemical reduction processes may remain in the composite. How to optimize the reaction conditions to reduce the generation of side reaction products and introduce an effective impurity removal step.
For example, the invention of Chinese patent application number 202111281270.0 discloses a composite material of copper powder coated with graphene and a preparation method thereof, wherein carbon source gas is used as an atomization medium to atomize copper liquid, so that the carbon source gas is catalyzed and decomposed to obtain graphene and is attached to the surface of copper powder formed by atomization; the carbon source gas is a mixed gas of inert gas, hydrogen and organic gas. By selecting a specific atomizing medium, the requirement of graphene growth atmosphere is met, and graphene is also grown on the surface of copper powder in situ while copper powder is formed through atomization by adopting a one-step method, so that the composite material of the graphene coated copper powder is obtained.
Compared with the composite material of the graphene coated copper powder and the preparation method thereof, which have challenges in controlling the uniformity and quality of graphene coating, the preparation method of the composite material is easier to realize in the control and adjustment process by adopting the modes of ball milling, stirring and the like.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a preparation method of antioxidant high-conductivity graphene-copper composite powder.
The aim of the invention can be achieved by the following technical scheme: the preparation method of the antioxidant high-conductivity graphene-copper composite powder comprises the following steps:
s1, ball milling of copper powder: placing the ball milling tank in an environment filled with nitrogen, sequentially adding a ball milling medium, copper powder and a lubricant into the ball milling tank, starting the ball milling machine to perform ball milling operation, and filtering to obtain flaky copper powder after the ball milling operation is finished; ball milling medium according to the weight ratio: copper powder: the lubricant is 20-30:1:0.1-0.2, the particle diameter D50 of the copper powder is 10-30 um, and the copper powder is pure copper; the nitrogen content in the nitrogen environment is more than 90%; the lubricant is at least one of stearic acid and oleic acid.
Stearic acid and oleic acid are used as lubricants, and can effectively reduce the adhesiveness of copper powder in the ball milling process, reduce friction between powder and the inner wall of a ball milling tank, promote the refinement of copper powder, and are also helpful for controlling the surface property of copper powder, improving the quality of a final product, and the copper powder cannot appear in the final product after the subsequent filtering and heating steps.
The ball milling media and copper powder are present in a weight ratio of 20-30:1, which provides a balance between effective grinding and preventing excessive breakage of the copper powder, while ensuring adequate grinding results while avoiding excessive damage to the copper powder.
Copper powder: the lubricant is 1:0.1-0.2, and the ratio is based on optimizing the lubricating effect of the copper powder and avoiding introducing excessive foreign substances, and the excessive lubricant is not easy to remove in the later stage, so that the coating effect and the final conductivity of the copper powder are affected.
Ball milling is an effective physical method for improving the physical properties of the powder, such as particle size and morphology, in which case ball milling may help produce more uniform and fine copper powder particles, which is necessary for the subsequent graphene coating process. The use of high concentrations of nitrogen during the ball milling process was used to create an inert atmosphere to prevent oxidation of the copper powder during the ball milling process. The nitrogen is used as an inert gas, and can effectively isolate oxygen and other gases possibly causing oxidation, so that the purity and the reactivity of the copper powder are protected.
S2, mixing: placing the polymer into absolute ethyl alcohol to form a mixed solution, adding graphene into the mixed solution, and stirring in the graphene adding process at the stirring speed of 200-500rpm for 30-60 minutes; then adding the flaky copper powder and stirring for 50-70 minutes at the stirring speed of 200-500rpm; finally, filtering to obtain initial composite powder; according to the weight ratio, graphene: flake copper powder: the polymer is 0.2-1:1000:100-180; in the mixed solution, the polymer is prepared by the following weight ratio: absolute ethyl alcohol is 1:8-11;
the number of layers of the graphene is 30-200;
the polymer is at least one of polyethylene glycol, polyoxyethylene, polyvinylpyrrolidone and polyvinyl alcohol;
the molecular weight of polyethylene glycol is 5000-20000; the molecular weight of polyoxyethylene is 2000-20000; the molecular weight of polyvinylpyrrolidone is 10000-40000; the molecular weight of the polyvinyl alcohol is 10000-50000.
The number of layers of the graphene is selected to achieve specific physical and chemical properties, when the number of layers is in the range of 30-200, the graphene can maintain unique electrical conductivity, thermal conductivity and mechanical properties, meanwhile, the preparation and treatment are convenient, the smaller number of layers (close to a single layer) leads to higher cost and complex preparation process, the larger number of layers possibly reduces the properties of the graphene, and in the range, the graphene can effectively coat copper powder, so that the properties of the composite material are improved.
The polyethylene glycol is used for helping the graphene to be uniformly dispersed in the copper powder, avoiding agglomeration, improving the adhesiveness between the graphene and the copper powder, enabling the graphene to be better attached to the surface of the copper powder, having a certain stability to the post heat treatment process, and being beneficial to maintaining the structural integrity of the material in the heating stage; the polyoxyethylene can improve the fluidity and the processability of the composite powder; the graphene is uniformly dispersed in the copper powder, so that agglomeration is avoided; the polyvinylpyrrolidone plays a role in the interface of the copper powder and the graphene, reduces the surface tension between the copper powder and the graphene, is favorable for coating the graphene, is favorable for improving the bonding efficiency of the graphene on the surface of the copper powder, and ensures the stability of the coating process; the polyvinyl alcohol can strengthen the adhesion of graphene and copper powder, and is helpful for maintaining the shape and structure of the material at high temperature and reducing the deformation at high temperature.
The polyethylene glycol has a molecular weight of 5000-20000, and exhibits good solubility and adhesion in this molecular weight range, which is useful for dispersion and stabilization of graphene. The polyethylene glycol PEG with higher molecular weight can form longer molecular chains, so that the coating capability on copper powder is enhanced, and meanwhile, the thermal stability and the mechanical strength of the final composite material are improved; the molecular weight of polyoxyethylene is 2000-20000; in the molecular weight range, the polyoxyethylene can effectively reduce friction and aggregation among powder particles, is beneficial to improving the fluidity and dispersibility of copper powder, and meanwhile, the moderate molecular weight is beneficial to keeping the processability of the material and avoiding the excessive viscosity; the molecular weight of polyvinylpyrrolidone is 10000-40000; the polyvinylpyrrolidone with the molecular weight range has good wettability and adhesiveness, is favorable for uniformly dispersing graphene and tightly combining the graphene with copper powder, and is favorable for improving the structural stability and uniformity of the composite material; the molecular weight of the polyvinyl alcohol is 10000 to 50000, and in the molecular weight range, the polyvinyl alcohol shows good film forming property and cohesiveness, which is helpful for forming a stable graphene coating layer on the surface of copper powder, thereby improving the conductivity and corrosion resistance of the material.
The mixed solution of the polymer and the ethanol can adjust the viscosity and rheological property of the whole system, and the proper viscosity is favorable for mixing and dispersing materials in the stirring process, and is also convenient for subsequent processing and forming. The absolute ethyl alcohol is used as a solvent, graphene and copper powder can be effectively dispersed, and the graphene is easy to disperse in the ethanol, so that the graphene is uniformly coated on the surface of the copper powder in the subsequent process, and the absolute ethyl alcohol is selected because the absolute ethyl alcohol has high purity and does not contain moisture, so that the absolute ethyl alcohol is important for maintaining the quality and stability of the graphene. The polymer is favorable for the adhesion of the graphene and the copper powder, ensures that the graphene can be uniformly and stably adhered to the surface of the copper powder, and plays a role in solidification in the stirring and subsequent drying processes, so that the graphene and the copper powder form a firm composite structure.
The stirring is performed during the addition of graphene to ensure that graphene is uniformly dispersed in the mixed solution, so that the graphene can be uniformly covered on copper powder during the subsequent mixing process, and the stirring speed of 200-500rpm is a proper range, because it can ensure enough shearing force to disperse graphene, and can avoid damage to graphene caused by excessive shearing force.
S3, drying: placing the initial composite powder into a vacuum drying oven for drying operation to obtain dry composite powder; the working pressure of the vacuum drying oven is-0.1 Mpa to-0.08 Mpa, and the vacuum drying time is 5-8 hours. The drying process performed has the following key purposes:
1. removing the solvent: the primary purpose is to remove absolute ethanol from the mixed solution, which is a critical step in ensuring the quality and performance of the final product.
2. Enhanced binding: the drying process helps to cure the polymer, thereby enhancing the bond between the graphene and copper powder; this is critical to maintaining uniform distribution and adhesion of graphene on the copper powder surface.
S4, heating: placing the dry composite powder in an environment filled with nitrogen for heating treatment, wherein a sintering furnace is adopted as heating equipment, the flow rate of nitrogen flowing into the sintering furnace is 1-3L/min, and the nitrogen content in the nitrogen environment is more than 90%; the working temperature of the sintering furnace is 400-600 ℃; the temperature rising rate of the sintering furnace is 70-80 ℃/min, and the sintering furnace works for 4-8 minutes. The heating treatment plays the following key roles in the process of preparing the graphene coated copper powder:
1. the structural stability of the material is improved: through heating, the combination of the polymer, graphene and copper powder can be further improved, and the structural stability of the material is enhanced.
2. Improving the dispersibility of graphene: proper heating can help the graphene form a more uniform coating on the copper powder surface, thereby improving its electrical and thermal conductivity.
3. Removing impurities: in the heating process, some residual solvents and impurities which are not removed by the drying step are removed, the graphene has reducibility, and the graphene can reduce copper oxide into copper in a nitrogen atmosphere.
The heating rate is 70-80 ℃/min, so that the heat stress increase or structural damage of the material caused by the too fast heating is avoided while the efficiency is ensured, and the quality of the final product is ensured. During the heat treatment, the proper nitrogen flow rate is helpful to maintain the inert atmosphere in the furnace, so that the material is prevented from being oxidized at high temperature, the flow rate of 1-3L/min can ensure the sufficient circulation of gas, and meanwhile, the interference of the powder caused by the excessively strong gas flow is avoided.
S5, cooling: and continuously injecting nitrogen in the cooling process until the temperature is reduced to the room temperature, and obtaining the antioxidant high-conductivity graphene-copper composite powder.
In the preparation method of the antioxidant high-conductivity graphene-copper composite powder, in the step S1, the ball milling media are stainless steel balls, the diameter of the ball milling media is 0.6mm-1mm, the working time of the ball mill is 8-15 hours, and the rotating speed of the ball mill is 100-120rpm. Stainless steel balls are selected as ball milling media because they have high hardness, wear resistance, and are not easily reacted with copper powder; the rotational speed range of 100-120rpm not only ensures effective ball milling, but also avoids excessive wear or heat build-up due to excessive rotational speeds.
In the preparation method of the antioxidant high-conductivity graphene-copper composite powder, in the step S2, the stirring operation adopts a mild stirring device, wherein the mild stirring device is specifically one of a double-planetary mixer, a magnetic stirrer and a ribbon mixer. The mild stirring device is chosen to ensure that the structure of the graphene and polymer is not destroyed, while ensuring that they are uniformly distributed on the copper powder surface. Excessive agitation forces may cause structural damage to the material or undesirable polymer breakage.
In the preparation method of the antioxidant high-conductivity graphene-copper composite powder, in the step S3, in the drying operation, a plurality of weight of dried samples are periodically taken and put into a hot air oven to be dried for 30-40 minutes, and the weight change of the dried samples before and after the dried samples is less than 2% to meet the drying requirement; the temperature of the hot air oven is set to be 100-120 ℃.
In the preparation method of the antioxidant high-conductivity graphene-copper composite powder, in the step S4, in the heating operation, a plurality of heated samples with weights are periodically taken, the surface morphology of the samples is observed by using a scanning electron microscope, the graphene is uniformly coated on the surfaces of the samples, and the heating process is finished.
Compared with the prior art, the invention has the following beneficial effects:
improving the conductivity and the oxidation resistance: according to the invention, the graphene is coated on the copper powder, so that the oxidation rate of copper is effectively slowed down, and the excellent conductivity of the graphene is improved, and meanwhile, the overall conductivity of the copper powder is improved.
2. Solves the problem of non-uniform particle distribution: in the process of preparing the antioxidant high-conductivity graphene-copper composite powder, the aggregation phenomenon of copper powder is effectively avoided by improving the stirring process and optimizing the mixing parameters, and the uniform distribution of copper powder particles is realized, so that the overall performance of the composite material is improved, and the consistency and reliability of products are ensured.
3. Reinforcing the structural integrity of the composite material: aiming at the problem of poor bonding effect of graphene and copper powder under high temperature conditions, the invention enhances the interface bonding between the graphene and the copper powder by introducing a proper polymer and optimizing heat treatment parameters, and the improvement not only improves the structural integrity of the material, but also enhances the stability of the material under high temperature conditions.
4. Impurity introduction is reduced, and the product purity is improved: in the preparation process, the invention obviously reduces the generation of side reaction products and reduces the possibility of residual substances by optimizing the reaction conditions and introducing effective impurity removal steps. This improvement not only increases the purity of the final product, but also enhances its properties.
5. Light application prospect: the weight of copper is relatively large, and the possibility of light weight is provided for copper powder by introducing graphene. This would provide significant advantages in applications requiring light weight, such as in certain electronics and conductive paint applications.
In general, the invention has obvious beneficial effects in improving the electric conductivity and oxidation resistance of copper powder, solving the problem of uneven particle distribution, enhancing the structural integrity of composite materials, reducing impurity introduction and light weight application, and the improvement leads the copper powder to have wider application prospect in the fields of electric conduction paint, electronic devices, heat conducting materials and the like.
Drawings
Fig. 1 is a SEM scanning electron microscope image of pure copper powder.
Fig. 2 is a diagram of copper flake powder after ball milling in an exemplary embodiment.
Fig. 3 is a graph of graphene coated copper powder in a specific embodiment.
Detailed Description
The following are specific embodiments of the present invention and the technical solutions of the present invention will be further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
Specific examples:
as shown in fig. 2 and 3, the preparation method of the antioxidant high-conductivity graphene-copper composite powder comprises the following steps:
s1, ball milling of copper powder: placing the ball milling tank in an environment filled with nitrogen, sequentially adding a ball milling medium, copper powder and a lubricant into the ball milling tank, starting the ball milling machine, performing ball milling operation, and filtering after the ball milling operation is finished to obtain flaky copper powder; ball milling medium according to the weight ratio: copper powder: the lubricant is 25:1:0.2, and the nitrogen content in the nitrogen environment is more than 90%; the lubricant is stearic acid.
S2, mixing: placing the polymer into absolute ethyl alcohol to form a mixed solution, adding graphene into the mixed solution, and stirring in the graphene adding process at the stirring speed of 200-500rpm for 60 minutes; then adding the flaky copper powder and stirring for 60 minutes at the stirring speed of 200-500rpm; finally, filtering to obtain initial composite powder; according to the weight ratio, graphene: flake copper powder: the polymer is 01:1000:150; in the mixed solution, the polymer is prepared by the following weight ratio: absolute ethyl alcohol is 1:9;
s3, drying: placing the initial composite powder into a vacuum drying oven for drying operation to obtain dry composite powder; the pressure of the vacuum drying oven is-0.09 Mpa, and the drying time is 6 hours;
s4, heating: placing the dry composite powder in an environment filled with nitrogen for heating treatment, wherein a sintering furnace is adopted as heating equipment, the flow rate of nitrogen flowing into the sintering furnace is 1.5L/min, and the nitrogen content in the nitrogen environment is more than 90%; the working temperature of the sintering furnace is 500 ℃; the temperature rising rate of the sintering furnace is 75 ℃/min, and the working time of the sintering furnace is 5 minutes;
s5, cooling: and continuously injecting nitrogen in the cooling process until the temperature is reduced to the room temperature, and obtaining the antioxidant high-conductivity graphene-copper composite powder.
In step S1, the ball milling medium is stainless steel ball, the diameter of the ball milling medium is 0.8mm, the working time of the ball mill is 13 hours, and the rotating speed of the ball mill is 110rpm.
In step S2, a mild stirring device is used for the stirring operation, and the mild stirring device is a double-planetary mixer.
In the step S3, in the drying operation, a plurality of weight of dried samples are put into a hot air oven for drying for 30-40 minutes, the weight change of the dried samples before and after the drying is less than 1.5%, and the temperature of the hot air oven is set to 120 ℃.
Performance test: taking pure copper powder shown in fig. 1 and the antioxidant high-conductivity graphene-copper composite powder prepared in the specific embodiment, respectively putting the pure copper powder and the antioxidant high-conductivity graphene-copper composite powder into a die to form a cuboid with the length of 100mm, the width of 10mm and the height of 5mm, measuring the resistance of the farthest two ends of the cuboid, recording the original resistance, respectively putting the cuboid into a double-85 ageing oven to perform ageing test for 72 hours, measuring the resistance of the farthest two ends of the cuboid by using the method, and recording the resistance, wherein the result is shown in the table:
list one
Through the analysis of the table, the following conclusions are drawn:
the oxidation resistance is improved: the resistivity change rate of the pure copper powder after aging is 6.57%, and the resistivity change rate of the antioxidant high-conductivity graphene-copper composite powder is only 2.56%. This shows that the graphene coating significantly slows down the oxidation rate of copper, thereby improving the stability of the material in a high-temperature and high-humidity environment, and the conductivity is reduced due to the easy oxidation of copper, which is particularly important.
Conductivity properties are improved: the initial resistance of the oxidation-resistant high-conductivity graphene-copper composite powder before aging is 195mΩ, compared with 213mΩ of pure copper powder, the oxidation-resistant high-conductivity graphene-copper composite powder has better conductivity, and the excellent conductivity of graphene is beneficial to improving the overall conductivity of copper powder.
The stability and durability of the material are increased: from the results of the aging test, the oxidation-resistant high-conductivity graphene-copper composite powder has low change rate of resistance in the aging process, which indicates that the material has better stability and durability, and is very important for application scenes such as electronic devices, conductive coatings and the like which are used for a long time.
The specific embodiments described herein are offered by way of example only to illustrate the spirit of the invention. Those skilled in the art may make various modifications or additions to the described embodiments or substitutions thereof without departing from the spirit of the invention or exceeding the scope of the invention as defined in the accompanying claims.
Claims (5)
1. The preparation method of the antioxidant high-conductivity graphene-copper composite powder is characterized by comprising the following steps of:
s1, ball milling of copper powder: placing the ball milling tank in an environment filled with nitrogen, sequentially adding a ball milling medium, copper powder and a lubricant into the ball milling tank, starting the ball milling machine to perform ball milling operation, and filtering to obtain flaky copper powder after the ball milling operation is finished; ball milling medium according to the weight ratio: copper powder: the lubricant is 20-30:1:0.1-0.2, the particle diameter D50 of the copper powder is 10-30 um, and the copper powder is pure copper; the nitrogen content in the nitrogen environment is more than 90%; the lubricant is at least one of stearic acid and oleic acid;
s2, mixing: placing the polymer into absolute ethyl alcohol to form a mixed solution, adding graphene into the mixed solution, and stirring in the graphene adding process at the stirring speed of 200-500rpm for 30-60 minutes; then adding the flaky copper powder and stirring for 50-70 minutes at the stirring speed of 200-500rpm; finally, filtering to obtain initial composite powder; in the mixing process, according to the weight ratio, graphene: flake copper powder: the polymer is 0.2-1:1000:100-180; in the mixed solution, the polymer is prepared by the following weight ratio: absolute ethyl alcohol is 1:8-11;
the number of layers of the graphene is 30-200;
the polymer is at least one of polyethylene glycol, polyoxyethylene, polyvinylpyrrolidone and polyvinyl alcohol;
the molecular weight of polyethylene glycol is 5000-20000; the molecular weight of polyoxyethylene is 2000-20000; the molecular weight of polyvinylpyrrolidone is 10000-40000; the molecular weight of the polyvinyl alcohol is 10000-50000;
s3, drying: placing the initial composite powder into a vacuum drying oven for drying operation to obtain dry composite powder; the working pressure of the vacuum drying oven is-0.1 Mpa to-0.08 Mpa, and the vacuum drying time is 5-8 hours;
s4, heating: placing the dry composite powder in an environment filled with nitrogen for heating treatment, wherein a sintering furnace is adopted as heating equipment, the flow rate of nitrogen flowing into the sintering furnace is 1-3L/min, and the nitrogen content in the nitrogen environment is more than 90%; the working temperature of the sintering furnace is 400-600 ℃; the temperature rising rate of the sintering furnace is 70-80 ℃/min, and the working time of the sintering furnace is 4-8 minutes;
s5, cooling: and continuously injecting nitrogen in the cooling process until the temperature is reduced to the room temperature, and obtaining the antioxidant high-conductivity graphene-copper composite powder.
2. The method for preparing the antioxidant highly conductive graphene-copper composite powder according to claim 1, wherein in the step S1, the ball milling media are stainless steel balls, the diameter of the ball milling media is 0.6mm-1mm, the working time of the ball mill is 8-15 hours, and the rotating speed of the ball mill is 100-120rpm.
3. The method for preparing the antioxidant highly conductive graphene-copper composite powder according to claim 1, wherein in the step S2, a mild stirring device is adopted for the stirring operation, and the mild stirring device is specifically one of a double planetary mixer, a magnetic stirrer and a ribbon mixer.
4. The method for preparing the antioxidant highly conductive graphene-copper composite powder according to claim 1, wherein in the step S3, in the drying operation, a plurality of weight of dried samples are periodically taken and put into a hot air oven for drying for 30-40 minutes, and the weight change of the dried samples before and after the drying is less than 2% to meet the drying requirement; the temperature of the hot air oven is set to be 100-120 ℃.
5. The method for preparing the antioxidant highly conductive graphene-copper composite powder according to claim 1, wherein in step S4, a plurality of heated samples are taken in the heating operation, the surface morphology of the samples is observed by using a scanning electron microscope, the surface of the samples is uniformly coated with graphene, and the heating process is finished.
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