CN111961903A - Preparation method of nanoparticle-doped graphene oxide reinforced copper-based composite material - Google Patents
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Abstract
The invention discloses a preparation method of a nanoparticle-doped graphene oxide reinforced copper-based composite material, which comprises the following preparation steps of firstly preparing a graphene oxide dispersion liquid and a nanoparticle powder suspension, and forming nanoparticle-doped reduced graphene oxide composite aerogel after assembly reduction treatment, washing and freeze drying; and then placing the copper powder, copper powder and ethanol into a three-dimensional vibration powder mixer for mechanical mixing treatment, and finally performing spark plasma sintering to obtain the copper-based composite material with the nano particles doped with the reduced graphene oxide. According to the invention, the nano particles and the graphene oxide are assembled and reduced to form the composite aerogel, the composite aerogel and the copper powder are further mixed, and then the nano particle-doped reduced graphene oxide-doped reinforced copper-based composite material is prepared by sintering, so that the problems of poor dispersion of graphene in a copper matrix and poor wettability of graphene and the matrix are effectively solved.
Description
Technical Field
The invention belongs to the technical field of copper-based composite material preparation, and particularly relates to a preparation method of a nanoparticle-doped graphene oxide reinforced copper-based composite material.
Background
The metal copper and the composite material thereof have excellent mechanical and physical properties and are widely applied to the fields of electronics, electricity, aerospace, transportation and the like. Metallic copper has many excellent properties, but also has disadvantages such as low strength. Despite the introduction of a ceramic reinforcing phase (Al) in the copper matrix2O3、SiC、TiC、TiB2Etc.) can improve the mechanical property of the copper-based composite material, but generally the electric conduction and the heat conduction are sacrificed, thereby limiting the wide application of the copper-based composite material. The two-dimensional material graphene is of a hexagonal honeycomb structure, has extremely excellent performances in the aspects of mechanics, electricity, heat and the like, becomes an ideal reinforcing phase of the copper-based composite material, is expected to keep good electric and thermal conductivity of copper, and can improve the strength of the copper-based composite material. However, graphene is very easy to agglomerate and stack due to its large specific surface area and strong van der waals force between sheets, and is difficult to realize uniform dispersion on a metal copper matrix, and the interface bonding between graphene and the metal copper matrix is weak, thereby hindering the development of graphene reinforced copper-based composite materials.
At present, the preparation methods of the graphene reinforced copper-based composite material are more, and mainly comprise a ball milling method, an in-situ generation method, an electrochemical method, a casting method and a cold rolling method. Although the preparation methods improve the performance of the graphene reinforced copper-based composite material to different degrees, the preparation methods also have the problems of complex process, poor graphene dispersibility, poor combination of graphene and a copper two-phase interface and the like. Therefore, the development of a new method for preparing the graphene reinforced copper-based composite material has important engineering significance and practical value.
Disclosure of Invention
The invention aims to provide a preparation method of a nanoparticle-doped graphene oxide reinforced copper-based composite material, which effectively solves the problems of poor dispersion of nanoparticles and graphene in a matrix, poor wettability of the graphene and the matrix and the like, and simultaneously remarkably improves the mechanical property of the graphene reinforced copper-based composite material.
The technical scheme adopted by the invention is that the preparation method of the nanoparticle-doped graphene oxide reinforced copper-based composite material comprises the following specific operation steps:
step 1, weighing graphene oxide and nano-particle powder according to a proportion, respectively adding the graphene oxide and the nano-particle powder into deionized water with corresponding weight, stirring the two mixed solutions at a rotating speed of 400rpm for 30min, and then carrying out ultrasonic treatment for 120min to obtain 0.25-1mg/ml graphene oxide dispersion liquid and 0.5-2mg/ml nano-particle powder suspension liquid;
step 2, stirring the graphene oxide dispersion liquid at the rotating speed of 400rpm, pouring the nanoparticle suspension and the assembled reducing agent in sequence, and stirring for 30min to obtain a mixed solution of the nanoparticles and the graphene oxide;
step 3, carrying out assembly reduction treatment on the mixed solution, cooling the mixed solution to room temperature, and washing the suspended matters for multiple times by using deionized water at 50 ℃ until the washed deionized water is neutral; then, freeze-drying for 24 hours at the temperature of minus 50 ℃ to obtain the nanoparticle-doped reduced graphene oxide composite aerogel;
step 4, putting the composite aerogel, the copper powder and 1.0% ethanol into a three-dimensional vibration powder mixer for two-step powder mixing, so as to crush the graphene composite aerogel and strip the graphene, thereby obtaining mixed powder;
and 5, putting the mixed powder into a graphite die for prepressing, wherein the prepressing pressure is 10MPa, and the pressure maintaining time is 30 s. And then placing the composite material into a discharge plasma sintering furnace, heating to 600-650 ℃, and preserving heat for 5-15min under 30-50MPa to prepare the nano-particle-doped reduced graphene oxide reinforced copper-based composite material.
The present invention is also characterized in that,
the nano-particles in the step 1 comprise titanium, vanadium, chromium, zirconium, molybdenum, niobium, nickel, tungsten, aluminum oxide, silicon carbide, titanium diboride, titanium carbide, vanadium carbide, chromium carbide and tungsten carbide, and the size of the nano-particles is 50nm-200 nm. The nano-particles can be a single substance or a plurality of nano-particles.
The mass ratio of the graphene oxide to the nano particles in the step 1 is more than 1: 2.
The chemical components used for assembling the reducing agent in the step 2 are 10% of ascorbic acid, 0.5% of silane coupling agent and 89.5% of deionized water, and the mass ratio of the addition amount of the assembling reducing agent to the graphene oxide is 150-250: 1.
And (3) preserving the assembly reduction treatment in the step 3 for 30-90min in a water bath box at the temperature of 70-90 ℃.
The three-dimensional vibration powder mixing in the step 4 is carried out in two steps: firstly, vibrating for 2-6h at the frequency of 50 Hz; and secondly, vibrating for 6-12h at the frequency of 30 Hz.
And 4, selecting dendritic copper powder with the particle size of 5-74 mu m.
The preparation method of the copper-based composite material with the nano-particles for reducing graphene oxide has the beneficial effects that the nano-particle powder and the graphene oxide form the composite aerogel through an assembly reduction method, and the nano-particles are inserted between the reduction graphene oxide lamella layers, so that the dispersibility of the nano-particles and the graphene is obviously improved. And reducing the graphene oxide in the assembly reduction treatment process, and recovering the conjugated structure of the graphene. The nano-particle doped reduced graphene oxide composite aerogel is subjected to three-dimensional vibration and two-step powder mixing, so that the graphene composite aerogel is stripped and effectively introduced into a copper matrix, the dispersibility of graphene and the wettability between the graphene and the copper matrix are improved due to the introduction of the nano-particle powder, the combination of two-phase interfaces is obviously enhanced, and the copper-based composite material with excellent comprehensive performance, in which the nano-particle doped reduced graphene oxide is obtained.
Drawings
FIG. 1 is a flow chart of the preparation of the nanoparticle-doped reduced graphene oxide reinforced copper-based composite material according to the present invention;
FIG. 2 is an electron scanning photograph of a 100nm titanium-doped reduced graphene oxide composite aerogel according to the present invention;
FIG. 3 is an electron scanning photograph of a 100nm nickel-doped reduced graphene oxide reinforced copper-based composite material.
Fig. 4 is a compression test curve of the doped reduced graphene oxide reinforced copper-based composite material.
Detailed Description
The preparation method of the nanoparticle-doped graphene oxide reinforced copper-based composite material provided by the invention has the flow shown in fig. 1, and comprises the following specific operation steps:
step 1, the weight ratio of the graphene oxide to the nano-particle powder is not less than 1: 2. Taking graphene oxide and nano-particle powder according to different component proportioning amounts, respectively adding the graphene oxide and the nano-particle powder into deionized water with corresponding amounts, respectively stirring the graphene oxide and the nano-particle powder at a rotating speed of 400rpm for 30min, and then carrying out ultrasonic treatment for 120min to respectively obtain 0.25-1mg/ml graphene oxide dispersion liquid and 0.5-2mg/ml nano-particle powder suspension liquid;
step 2, stirring 0.25-1mg/ml graphene oxide dispersion liquid at the rotating speed of 400rpm, firstly pouring 0.5-2mg/ml nanoparticle powder suspension, then pouring an assembly reducing agent (10% ascorbic acid, 0.5% silane coupling agent and 89.5% deionized water), wherein the mass ratio of the addition amount of the assembly reducing agent to the graphene oxide is 150-250:1, and stirring for 30min to obtain a mixed solution of nanoparticles and graphene oxide;
step 3, putting the mixed solution into a constant-temperature water bath tank at 70-90 ℃ for assembly reduction treatment for 30-90min, and after the mixed solution is cooled to room temperature, washing the suspended matters for multiple times by using deionized water at 50 ℃ until the washed deionized water is neutral; then freeze-drying the suspended matter for 24h at-50 ℃ to obtain the nanoparticle reduced graphene oxide composite aerogel;
step 4, putting the composite aerogel, the dendritic copper powder and 1.0% ethanol on a three-dimensional vibration powder mixing machine for two-step powder mixing, wherein the vibration frequency of the first step is 50Hz, and the vibration time is 2-6 h; a second step; vibrating at 30Hz for 6-12h to obtain mixed powder;
and 5, putting the mixed powder into a graphite die for prepressing, wherein the prepressing pressure is 10MPa, and the pressure maintaining time is 30 s. And then placing the composite material into a discharge plasma sintering furnace, heating to 600-650 ℃, and preserving heat for 5-15min under 30-50MPa to prepare the nano-particle-doped reduced graphene oxide reinforced copper-based composite material.
The present invention will be described in detail with reference to specific examples.
Example 1
Step 1, the weight ratio of graphene oxide to nano-particle powder is 2:1, the graphene oxide is 0.02%, and the 50nm molybdenum powder is 0.01%. Weighing 10mg of graphene oxide and 5mg of molybdenum powder according to a ratio, respectively adding the graphene oxide and the molybdenum powder into 20ml of deionized water and 5ml of deionized water, stirring the two mixed solutions at a rotating speed of 400rpm for 30min, and performing ultrasonic treatment for 120min to obtain 0.5mg/ml graphene oxide dispersion liquid and 1mg/ml nano molybdenum powder suspension liquid;
step 2, stirring 0.5mg/ml graphene oxide dispersion liquid at 400rpm, pouring 1mg/ml nano molybdenum powder suspension and 2g of assembly reducing agent in sequence, and stirring for 30min to obtain a mixed solution of nano molybdenum and graphene oxide;
step 3, placing the mixed solution of the nano molybdenum and the graphene oxide in a 90 ℃ constant-temperature water bath box, preserving the heat for 60min, taking out, and washing the suspended matters for 3 times by using 50 ℃ deionized water until the ionized water is neutral; then freeze-drying the suspended matters at-50 ℃ for 24h to obtain the nano molybdenum-doped reduced graphene oxide composite aerogel;
step 4, 49.985g of 5-micron dendritic copper powder is weighed according to the proportion of 99.97%, 1% of ethanol, nano-molybdenum-doped reduced graphene oxide composite aerogel and dendritic copper powder are placed on a three-dimensional vibration powder mixer to be mixed for two steps, the first step is carried out at the vibration frequency of 50Hz for 2 hours; a second step; vibrating at the frequency of 30Hz for 8 hours to obtain mixed powder;
and 5, putting the mixed powder into a graphite die for prepressing, wherein the prepressing pressure is 10MPa, and the pressure maintaining time is 30 s. And then placing the composite material into a discharge plasma sintering furnace, heating to 600 ℃, and preserving heat for 8min under 40MPa to prepare the molybdenum-doped reduced graphene oxide reinforced copper-based composite material. The conductivity and hardness were 93.2% IACS and 80HV, respectively.
Example 2
Step 1, the weight ratio of graphene oxide to nano-particle powder is 5:1, the graphene oxide is 0.1%, and the 100nm nickel powder is 0.04%. Respectively weighing 25mg of graphene oxide and 10mg of nickel powder according to the proportion, respectively adding the graphene oxide and the nickel powder into 25ml of deionized water and 5ml of deionized water, stirring the two mixed solutions at the rotating speed of 400rpm for 30min, and performing ultrasonic treatment for 120min to obtain 1mg/ml graphene oxide dispersion liquid and 2mg/ml nano nickel powder suspension liquid;
step 2, stirring 1mg/ml graphene oxide dispersion liquid at the rotating speed of 400rpm, pouring 2mg/ml nano nickel powder suspension and 6g of assembly reducing agent in sequence, and stirring for 30min to obtain a mixed solution of nano nickel and graphene oxide;
step 3, placing the mixed solution of the nano nickel and the graphene oxide in a 80 ℃ constant-temperature water bath box, preserving the heat for 90min, taking out, and washing the suspended matters for 5 times by using 50 ℃ deionized water until the deionized water is neutral; then freeze-drying the suspended matters at-50 ℃ for 24h to obtain the nano nickel-doped reduced graphene oxide composite aerogel;
step 4, weighing 24.65g of 5-micron dendritic copper powder according to the proportion of 99.86%, and placing 1% of ethanol, nano-nickel-doped reduced graphene oxide composite aerogel and dendritic copper powder on a three-dimensional vibration powder mixer to perform two-step powder mixing, wherein the first step vibration frequency is 50Hz, and the time is 4 hours; a second step; vibrating at the frequency of 30Hz for 12h to obtain mixed powder;
and 5, putting the mixed powder into a graphite die for prepressing, wherein the prepressing pressure is 10MPa, and the pressure maintaining time is 30 s. And then placing the composite material into a discharge plasma sintering furnace, heating to 650 ℃, and preserving heat for 12min under 45MPa to prepare the nickel-doped reduced graphene oxide reinforced copper-based composite material. The conductivity and hardness were 88.7% IACS and 89HV, respectively.
Example 3
Step 1, the weight ratio of graphene oxide to nano-particle powder is 2.5:1, the graphene oxide is 0.1%, and the 100nm titanium powder is 0.04%. Weighing 30mg of graphene oxide and 12mg of titanium powder according to a ratio, respectively adding the graphene oxide and the titanium powder into 120ml of deionized water and 6ml of deionized water, stirring the two mixed solutions at a rotating speed of 400rpm for 30min, and performing ultrasonic treatment for 120min to obtain 0.25mg/ml graphene oxide dispersion liquid and 2mg/ml nano titanium powder suspension liquid;
step 2, stirring 0.25mg/ml graphene oxide dispersion liquid at the rotating speed of 400rpm, pouring 2mg/ml nano titanium powder suspension and 7.5g of assembly reducing agent in sequence, and stirring for 30min to obtain a mixed solution of nano titanium and graphene oxide;
step 3, placing the mixed solution of the nano titanium and the graphene oxide in a 70 ℃ constant temperature water bath box, preserving the heat for 30min, taking out, and washing the suspended matters for 4 times by using 50 ℃ deionized water until the deionized water is neutral; then freeze-drying the suspended matter for 24h at-50 ℃ to obtain the nano titanium doped reduced graphene oxide composite aerogel;
step 4, weighing 24.58g of 48-micron dendritic copper powder according to the proportion of 99.86%, and placing 1% of ethanol, nano-titanium-doped reduced graphene oxide composite aerogel and dendritic copper powder on a three-dimensional vibration powder mixer to carry out two-step powder mixing, wherein the first step vibration frequency is 50Hz, and the time is 4 hours; a second step; vibrating at the frequency of 30Hz for 12h to obtain mixed powder;
step 5, putting the mixed powder into a graphite die for prepressing, wherein the prepressing pressure is 10MPa, and the pressure maintaining time is 30 s; and then placing the titanium-doped reduced graphene oxide reinforced copper-based composite material into a discharge plasma sintering furnace, heating to 600 ℃, and preserving heat for 12min under 35MPa to obtain the titanium-doped reduced graphene oxide reinforced copper-based composite material. The conductivity and hardness were 83.9% IACS and 78HV, respectively.
Example 4
Step 1, the weight ratio of graphene oxide to nano-particle powder is 4:1, 0.4% of graphene oxide, 0.05% of 100nm titanium powder and 0.05% of 200nm titanium diboride. Weighing 100mg of graphene oxide, 12.5mg of titanium powder and 12.5mg of titanium diboride according to the mixture ratio; adding graphene oxide into 400ml of deionized water, adding titanium powder and titanium diboride into 50ml of deionized water, respectively stirring the two mixed solutions at the rotating speed of 400rpm for 30min, and then carrying out ultrasonic treatment for 120min to obtain 0.25mg/ml graphene oxide dispersion liquid and 0.5mg/ml nano titanium and titanium diboride powder suspension liquid;
step 2, stirring 0.25mg/ml graphene oxide dispersion liquid at 400rpm, sequentially pouring 0.5mg/ml nano titanium, titanium diboride powder suspension and 15g of assembly reducing agent, and stirring for 30min to obtain a mixed solution of nano titanium, titanium diboride powder and graphene oxide;
step 3, placing the mixed solution of the nano titanium, the titanium diboride powder and the graphene oxide in a constant-temperature water bath cabinet at 85 ℃ for heat preservation for 45min, taking out, and washing the suspended matters for 6 times by using deionized water at 50 ℃ until the deionized water is neutral; then freeze-drying the suspended matter for 24h at-50 ℃ to obtain the reduced graphene oxide composite aerogel doped with nano titanium and titanium diboride powder;
step 4, 24.875g of 20-micron dendritic copper powder is weighed according to the proportion of 99.5%, 1% of ethanol, nano-titanium and titanium diboride powder are doped with reduced graphene oxide composite aerogel together, and the dendritic copper powder is placed on a three-dimensional vibration powder mixer to be mixed for two steps, wherein the first step has the vibration frequency of 50Hz for 5 hours; a second step; vibrating at the frequency of 30Hz for 10h to obtain mixed powder;
and 5, putting the mixed powder into a graphite die for prepressing, wherein the prepressing pressure is 10MPa, and the pressure maintaining time is 30 s. And then placing the copper-based composite material into a discharge plasma sintering furnace, heating to 650 ℃, and preserving heat for 15min under 50MPa to prepare the nano-titanium-doped and titanium diboride reduced graphene oxide reinforced copper-based composite material. The conductivity and hardness were 71.3% IACS and 105HV, respectively.
Example 5
Step 1, the weight ratio of graphene oxide to nano-particle powder is 1:2, the graphene oxide is 0.05%, the 200nm titanium powder is 0.08%, and the 100nm titanium carbide is 0.02%. Respectively weighing 25mg of graphene oxide, 40mg of titanium powder and 10mg of titanium carbide according to the proportion; adding graphene oxide into 50ml of deionized water, putting titanium powder and titanium carbide into 50ml of deionized water, respectively stirring the two mixed solutions at the rotating speed of 400rpm for 30min, and performing ultrasonic treatment for 120min to obtain 0.5mg/ml graphene oxide dispersion liquid and 1mg/ml nano titanium and titanium carbide powder suspension liquid;
step 2, stirring 0.5mg/ml graphene oxide dispersion liquid at 400rpm, pouring 1mg/ml nano titanium, titanium carbide powder suspension and 12.5g of assembly reducing agent in sequence, and stirring for 30min to obtain a mixed solution of nano titanium, titanium carbide powder and graphene oxide;
step 3, placing the mixed solution of the nano titanium, the titanium carbide powder and the graphene oxide in a constant-temperature water bath cabinet at 85 ℃ for heat preservation for 75min, taking out, and washing the suspended matters for 5 times by using deionized water at 50 ℃ until the deionized water is neutral; then freeze-drying the suspended matter for 24h at-50 ℃ to obtain the reduced graphene oxide composite aerogel doped with nano titanium and titanium carbide powder;
step 4, 49.925g of 74-micron dendritic copper powder is weighed according to the proportion of 99.85%, 1% of ethanol, nano-titanium and titanium carbide powder are doped with reduced graphene oxide composite aerogel, and the dendritic copper powder is placed on a three-dimensional vibration powder mixer to be mixed for two steps, wherein the first step has the vibration frequency of 50Hz for 3 hours; a second step; vibrating at the frequency of 30Hz for 12h to obtain mixed powder;
and 5, putting the mixed powder into a graphite die for prepressing, wherein the prepressing pressure is 10MPa, and the pressure maintaining time is 30 s. And then placing the composite material into a discharge plasma sintering furnace, heating to 620 ℃, and preserving heat for 15min under 40MPa to prepare the nano titanium and titanium carbide doped reduced graphene oxide reinforced copper-based composite material. The conductivity and hardness were 93.8% IACS and 79HV, respectively.
In conjunction with the embodiment, fig. 2 is a scanning electron micrograph of the 100nm titanium-doped graphene oxide composite aerogel, in which nanoparticles are uniformly dispersed on the surface of the reduced graphene oxide. FIG. 3 shows a 100nm nickel-doped graphene oxide reinforced copper-based composite material, in which graphene is uniformly dispersed and is in a three-dimensional network structure in a copper matrix. FIG. 4 is a graph showing the compression performance curves of pure copper, example 2 and example 3, wherein the yield strength of the pure copper is 118MPa, the yield strength of the copper-based composite material prepared in example 2 is 302MPa, and the yield strength is 184MPa higher than that of the pure copper. The yield strength of the copper-based composite material prepared in example 3 is 340MPa, which is increased by 222MPa compared with pure copper.
Claims (7)
1. The preparation method of the nanoparticle-doped graphene oxide reinforced copper-based composite material is characterized by comprising the following specific operation steps of:
step 1, weighing graphene oxide and nano-particle powder, respectively adding the graphene oxide and the nano-particle powder into deionized water, respectively stirring the two mixed solutions at a rotating speed of 400rpm for 30min, and then carrying out ultrasonic treatment for 120min to obtain 0.25-1mg/ml graphene oxide dispersion liquid and 0.5-2mg/ml nano-particle powder suspension liquid;
step 2, sequentially pouring the nanoparticle suspension and an assembly reducing agent into the graphene oxide dispersion liquid, stirring at 400rpm during the adding process, and then continuing to stir at 400rpm for 30min after the adding is finished, so as to finally obtain a mixed solution of the nanoparticles and the graphene oxide;
and 3, carrying out assembly reduction treatment on the mixed solution: after the mixed solution is cooled to room temperature, washing the suspended matters for multiple times by using deionized water at 50 ℃ until the washed deionized water is neutral; then, freeze-drying for 24 hours at the temperature of minus 50 ℃ to obtain the nanoparticle-doped reduced graphene oxide composite aerogel;
step 4, putting the composite aerogel, the copper powder and 1.0% acetone into a three-dimensional vibration powder mixing machine for two-step powder mixing, wherein in the first step, the vibration frequency is 50Hz, and the vibration time is 2-6 h; secondly, vibrating for 6-12 hours at the frequency of 30Hz to obtain mixed powder;
and 5, putting the mixed powder into a graphite die for prepressing, wherein the prepressing pressure is 10MPa, and the pressure maintaining time is 30 s. And then placing the composite material into a plasma electric spark sintering furnace, heating to 600-650 ℃, and preserving heat for 5-15min under 30-50MPa to prepare the nanoparticle-doped reduced graphene oxide reinforced copper-based composite material.
2. The method for preparing the nanoparticle-doped graphene oxide reinforced copper-based composite material according to claim 1, wherein the nanoparticles comprise titanium, vanadium, chromium, zirconium, molybdenum, niobium, nickel, tungsten, aluminum oxide, silicon carbide, titanium diboride, titanium carbide, vanadium carbide, chromium carbide and tungsten carbide, the size of the nanopowder of the nanoparticles is 50nm-200nm, and the nanoparticles can be a single substance or multiple nanoparticles.
3. The method for preparing the copper-based composite material doped with the reduced graphene oxide nanoparticles as claimed in claim 1, wherein the mass ratio of the graphene oxide to the nanoparticles in the step 1 is greater than 1: 2.
4. The method for preparing the nanoparticle-doped graphene oxide reinforced copper-based composite material according to claim 1, wherein the assembly reducing agent in the step 2 comprises 10% by mass of ascorbic acid, 0.5% by mass of silane coupling agent and 89.5% by mass of deionized water.
5. The method as claimed in claim 1, wherein the mass ratio of the addition amount of the assembly reducing agent to the graphene oxide in step 2 is 150-250: 1.
6. The method for preparing the nanoparticle-doped graphene oxide reinforced copper-based composite material according to claim 1, wherein the assembly reduction treatment in the step 3 is heat preservation in a thermostatic water bath at 70-90 ℃ for 30-90 min.
7. The method for preparing the nanoparticle-doped graphene oxide reinforced copper-based composite material according to claim 1, wherein the copper powder in the step 4 is dendritic copper powder with a particle size of 5-74 μm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112391549A (en) * | 2020-12-07 | 2021-02-23 | 西安稀有金属材料研究院有限公司 | Preparation method of reduced graphene oxide and aluminum oxide co-reinforced copper-based composite material |
| CN113061768A (en) * | 2021-03-22 | 2021-07-02 | 中南大学 | Preparation method of dispersion-strengthened copper-based composite material |
| CN113737038A (en) * | 2021-07-29 | 2021-12-03 | 暨南大学 | High-toughness Ti-rich nanoparticle reinforced CuAl-based composite material and preparation method and application thereof |
| CN114855020A (en) * | 2022-05-18 | 2022-08-05 | 深圳市明鑫工业材料有限公司 | Preparation process of oxygen-free copper-based high-strength composite material |
| CN115852199A (en) * | 2022-11-30 | 2023-03-28 | 河南科技大学 | Composite material with electric contact function and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105583408A (en) * | 2015-12-22 | 2016-05-18 | 浙江理工大学 | Preparation method and application of Cu nanowire-reduced graphene oxide three-dimensional porous film |
| CN105695788A (en) * | 2016-04-08 | 2016-06-22 | 上海和伍复合材料有限公司 | Graphene strengthening nickel base composite material and preparing method thereof |
| CN108624775A (en) * | 2018-04-20 | 2018-10-09 | 西安理工大学 | A kind of the graphene enhancing Cu-base composites and preparation method of supported copper |
| CN109266890A (en) * | 2018-09-14 | 2019-01-25 | 西安理工大学 | A method of preparing modified graphene enhancing Cu-base composites |
| CN110639516A (en) * | 2019-10-16 | 2020-01-03 | 浙江大学台州研究院 | Graphene-loaded multi-metal nanowire aerogel composite material and preparation method thereof |
-
2020
- 2020-08-19 CN CN202010835873.XA patent/CN111961903B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105583408A (en) * | 2015-12-22 | 2016-05-18 | 浙江理工大学 | Preparation method and application of Cu nanowire-reduced graphene oxide three-dimensional porous film |
| CN105695788A (en) * | 2016-04-08 | 2016-06-22 | 上海和伍复合材料有限公司 | Graphene strengthening nickel base composite material and preparing method thereof |
| CN108624775A (en) * | 2018-04-20 | 2018-10-09 | 西安理工大学 | A kind of the graphene enhancing Cu-base composites and preparation method of supported copper |
| CN109266890A (en) * | 2018-09-14 | 2019-01-25 | 西安理工大学 | A method of preparing modified graphene enhancing Cu-base composites |
| CN110639516A (en) * | 2019-10-16 | 2020-01-03 | 浙江大学台州研究院 | Graphene-loaded multi-metal nanowire aerogel composite material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| HUI ZHANG等: "Performance Analysis of Silver-Based Graphene Nanocomposite Bulk Materials Obtained by Spark Plasma Sintering", 《THE MINERALS, METALS & MATERIALS SOCIETY》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112391549A (en) * | 2020-12-07 | 2021-02-23 | 西安稀有金属材料研究院有限公司 | Preparation method of reduced graphene oxide and aluminum oxide co-reinforced copper-based composite material |
| CN113061768A (en) * | 2021-03-22 | 2021-07-02 | 中南大学 | Preparation method of dispersion-strengthened copper-based composite material |
| CN113061768B (en) * | 2021-03-22 | 2023-08-25 | 中南大学 | Preparation method of dispersion strengthening copper-based composite material |
| CN113737038A (en) * | 2021-07-29 | 2021-12-03 | 暨南大学 | High-toughness Ti-rich nanoparticle reinforced CuAl-based composite material and preparation method and application thereof |
| CN114855020A (en) * | 2022-05-18 | 2022-08-05 | 深圳市明鑫工业材料有限公司 | Preparation process of oxygen-free copper-based high-strength composite material |
| CN115852199A (en) * | 2022-11-30 | 2023-03-28 | 河南科技大学 | Composite material with electric contact function and preparation method thereof |
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