石墨烯增强铜基复合材料研究进展

陈春姣; 包宏伟; 李燕; 白惠中; 杨朔涵; 马飞

doi:10.13801/j.cnki.fhclxb.20221008.001

石墨烯增强铜基复合材料研究进展

doi: 10.13801/j.cnki.fhclxb.20221008.001

西安交通大学　金属材料强度国家重点实验室，西安 710049

基金项目: 国家重点研发计划资助(2021 YFB3400800)；国家自然科学基金(52271136；51901177)；陕西省自然科学金(2021 JC-06；2019 TD-020)Supported by National Key Research and Development Program (2021 YFB3400800); National Natural Science Foundation of China (52271136; 51901177); Natural Science Foundation of Shaanxi Province (2021 JC-06; 2019 TD-020)

详细信息

通讯作者:
包宏伟，博士，助理教授，硕士生导师，研究方向为材料表界面力学多尺度模拟　E-mail: baohongwei1988@msn.com

马飞，博士，教授，博士生导师，研究方向为先进薄膜与涂层材料　E-mail: mafei@mail.xjtu.edu.cn

中图分类号: TB331
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出版历程
- 收稿日期: 2022-08-01
- 修回日期: 2022-09-06
- 录用日期: 2022-09-20
- 网络出版日期: 2022-10-09
- 刊出日期: 2023-03-15

Research progress of graphene reinforced copper matrix composites

State Key Laboratory for Mechanical Behavior of Materials, Xi’an Jiaotong University, Xi’an 710049, China

摘要

摘要: 铜(Cu)基复合材料具有优异的力学、热学、电学及耐磨和耐腐蚀等性能，广泛应用于各种工业技术领域。石墨烯(Graphene，Gr)具有二维平面结构和优异的综合性能，是金属基复合材料理想的增强相。石墨烯增强铜基复合材料拓展了铜及其合金的应用范围，适当的制备方法可以使其在保持优异导电导热性能的同时拥有更好的力学性能。石墨烯在铜基体中的存在形式主要以还原氧化石墨烯、石墨烯纳米片或与金属氧化物/碳化物纳米颗粒连接，旨在增强两者之间的界面结合。因此，石墨烯在铜基体中的结构完整性及存在形式直接影响了其性能的优劣。本文综述了Cu/Gr复合材料的制备及模拟方法、复合材料的性能评价及力学性能与功能特性的相互影响规律。指明Cu/Gr复合材料的发展关键在于：(1) 分散性与界面结合；(2) 三维石墨烯结构的构建；(3) 界面结合对力学性能与功能特性的影响及两者间的相互协调。
- 铜基复合材料 /
- 石墨烯增强 /
- 界面设计 /
- 高强高导 /
- 研究进展
Abstract: Copper (Cu) matrix composites have excellent mechanical, thermal, electrical, wear and corrosion resistance properties, and are widely used in industrial fields. Graphene (Gr) is an ideal reinforcement phase for metal matrix composites due to its two-dimensional features and excellent physical properties. Gr reinforced Cu have expanded the applications of Cu and its alloys. Appropriate preparation methods can achieve excellent electrical and thermal conductivity while maintaining the excellent mechanical properties. Gr in Cu matrix mainly exist in the form of reduced GO (r-GO), graphene nanosheets or connected with metal oxide/carbide nanoparticles to enhance the interface bonding. Therefore, the structural integrity and the form of graphene in Cu matrix directly affect its performances. In this review paper, the preparation and simulation methods of Cu/Gr composites, the evaluation on the performances and the interaction between mechanical and functional properties are summarized. The key to the development of Cu/Gr composites is suggested: (1) dispersion and interfacial bonding; (2) construction of three-dimensional graphene structures; (3) the effect of interfacial bonding on the mechanical and functional properties.
- copper matrix composites /
- graphene reinforcement /
- interfacial design /
- high-strength and high-conductivity /
- research progress

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图 1 石墨烯增强铜基复合材料主要研究领域的示意图^[14-20]

Figure 1. Main research fields of graphene-reinforced copper matrix composites^[14-20]

PM—Powder metallurgy; HP—Hot press; MLM—Molecular-level mixing; SPS—Spark plasma sintering; CVD—Chemical vapor deposition; ELD—Electroless deposition

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图 2 通过分子水平混合方法制备还原氧化石墨(RGO)/Cu纳米复合材料的工艺示意图：(a) 原始石墨；(b) 采用Hummers方法制备氧化石墨烯(GO)；(c) 铜盐在GO溶液中的分散；(d) 在GO上，Cu离子氧化成Cu氧化物；(e) CuO和GO的还原；(f) 烧结RGO/Cu纳米粉末^[14]

Figure 2. Schematic of fabrication process of reduced graphite oxide (RGO)/Cu nanocomposite: (a) Pristine graphite; (b) Graphene oxide (GO) fabricated by the Hummers method; (c) Dispersion of Cu salt in GO solution; (d) Oxidation from Cu ions to Cu-oxide on the GO; (e) Reduction of Cu-oxide and GO; (f) Sintered RGO/Cu nanocomposite powders^[14]

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图 3 Gr/Cu复合材料制造工艺示意图：(a) 石墨；(b) 铜粉；(c) 带负电荷的GO；(d) 带正电荷的CTAB改性铜粉(CTAB-Cu)；(e) GO-Cu粉末；(f) Gr/Cu复合材料^[24]

Figure 3. Schematic of the fabrication process of Gr/Cu composite: (a) Graphite; (b) Cu powders; (c) GO with the negative charge; (d) CTAB modified Cu powders (CTAB-Cu) with the positive charge; (e) GO-Cu powders; (f) Gr/Cu composite^[24]

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图 4 整体制造过程及Gr网络状形貌示意图：(a) 用蔗糖作为混合前体包覆铜粉；(b) 混合前体经过快速热退火(RTA)过程生长类石墨烯纳米片(GLNs)；(c) 利用热压将GLNs内接成Cu基体中的连续网络结构；(d) 采用热轧法制备全致密三维石墨烯状纳米片网络(3D-GLNN)/Cu复合材料；热压3D-GLNN/Cu复合材料中Cu刻蚀后3D-GLNN的SEM图像 (e) 和TEM图像 (f)；(g) 3D-GLNN的Y型互连区HRTEM图像，其中A层和B层合并为A+B层；(h) 热压3D-GLNN/Cu中3D-GLNN的FIB-3D重建结果快照^[16]

Figure 4. Schematic illustration of overall fabrication processes and Gr microstructure characterizations: (a) Cu powders were firstly coated with sucrose as a hybrid precursor; (b) Hybrid precursor was then subjected to rapid thermal annealing (RTA) process for growing graphene-like nanosheets (GLNs); (c) GLNs were interconnected into a continuous network structure in the Cu matrix by using hot-pressing; (d) Fully-densified 3D graphene-like nanosheet network (3D-GLNN)/Cu bulk composites were fabricated by hot-rolling. SEM image (e) and TEM image (f) of 3D-GLNN after Cu etching in the hot-pressed 3D-GLNN/Cu composites. Scale bar, 5 μm (e); 200 nm (f); (g) HRTEM image of the Y-type interconnection area of 3 D-GLNN, where the layer A and layer B merged into layer A+B. Scale bar, 5 nm; (h) Snapshot of FIB-3D reconstruction results of 3D-GLNN in the h hot-pressed 3D-GLNN/Cu (model size:3.85 × 2.14 × 2.00 μm)^[16]

EtOH—Ethyl alcohol

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图 5 等离子体辅助球磨(PAM)处理制备Gr/Cu复合材料示意图^[17]

Figure 5. Schematic illustration for the fabrication of Gr/Cu composites with plasma assisted milling (PAM) treatment^[17]

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图 6 镀镍石墨烯(NCG)/Cu复合箔制备及表征性能示意图：(a) NCG/Cu的制备；(b) 沉积后衬底的数字照片；(c) 复合箔的截面SEM图像；(d) 应力-应变曲线；(e) 不同浓度NCG复合箔的热导率和热扩散率^[18]

Figure 6. Schematic diagram of preparation and characterization of nickel plated graphene (NCG)/Cu composite foi: (a) Preparation of NCG/Cu; (b) Digital photograph of the substrate after deposition; (c) Cross-sectional SEM image of the composite foil; (d) Stress-strain curves; (e) Thermal conductivity and thermal diffusivity of the composite foil with different concentrations of NCG^[18]

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图 7 多层Gr/Cu复合材料的模型与拉伸应力-应变曲线：(a) 锯齿状Gr；(b) 扶手椅状Gr；插图(c)~(f)是曲线的特写视图，插图(e)和(f)是屈服点；(g) 含三层Gr的Gr/Cu体系初始模型^[20]

Figure 7. Model and tensile stress-strain curves of Multilayer Gr/Cu composite: (a) Zigzag Gr; (b) Armchair Gr; Insets (c)-(f) are the close-up views of the curves, inserts (e) and (f) are the yield points; (g) Initial model of Gr/Cu system with three Gr layers^[20]

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图 8 Gr/Ni复合材料的原子构型：(a) Gr/Ni复合材料及其嵌入的Gr单元的原子构型(上插图显示弛豫过程中能量随时间的演化)；((b)~(c)) Gr/Ni复合材料的代表性体积单元(RVE)和其嵌入的Gr；(d) Gr-1曲线区域-1上有孔状缺陷；(e) Gr-2在直区域-2上有孔状缺陷^[49]

Figure 8. Atomic configuration of Gr/Ni composites: (a) Atomic configurations of the Gr/Ni composite and its embedded Gr unit (the upper inset shows the energy evolution by time during relaxation); ((b)-(c)) Representative volume element (RVE) of the Gr/Ni composite and its embedded Gr; (d) Gr-1 with hole-like defects on curved region-1; (e) Gr-2 with hole-like defects on straight region-2^[49]

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图 9 复合材料的原子构型：(a) 原始石墨烯(PG)；((b)~(d)) 含1%、10%、50%氢原子的氢功能化石墨烯(1%HFG、10%HFG、50%HFG)；((e)~(h)) 具有1%官能团的甲基、乙基、丙基和丁基功能化石墨烯(1%CH3 FG、1%C2H5 FG、1%C3H7 FG 和1%C4H9 FG)；((i)~(j)) Gr/Cu纳米复合材料的透视图和正面图^[50]

Figure 9. Atomic configurations of composites: (a) Pristine graphene (PG); ((b)-(d)) Hydrogen functionalized graphene (HFG) with 1%, 10%, 50% hydrogen atoms (denoted as 1%HFG, 10%HFG, 50%HFG); ((e)-(h)) Methyl, ethyl, propyl, and butyl functionalized graphene with 1% functional groups (1%CH3 FG,1%C2 H5 FG,1%C3 H7 FG and 1%C4 H9 FG); ((i)-(j)) Perspective view and front view of Gr/Cu nanocomposites^[50]

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图 10 (a) 斑马皮结构和复合微结构；(b) 复合材料的热流模型^[88]

Figure 10. (a) Zebra skin structure and composite microstructure; (b) Heat flow model of the composites^[88]

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表 1 不同方法制备Gr/Cu复合材料的力学性能

Table 1. Mechanical properties of Gr/Cu composites prepared by different methods

Experimental classification	Processing route	Material	Yield strength/MPa	Maximum strength/MPa	Hardness (HV)	Elogation/%	Ref.
RGO	MLM+SPS MLM+self-assemble+SPS charge adsorption+ thermal reduction+hot-press sintering Oxygen plasma treatment	2.5vol%Gr/Cu Pure Cu 2.5vol%RGO/Cu 2.5vol%CNT-RGO/Cu Pure Cu 0.3wt%RGO+Cu 0.6wt%RGO+Cu 0.9wt%RGO+Cu P-1vol%GNP/Cu 1vol%GNP/Cu	73.9 82.2 107.4 90.8 188 158	284 294 450 601 191.3 206.3 226.7 231.9		7.2 7.5 11.8 14.4 21 12	[14] [66] [67-68]
Gr	Plasma assisted milling treatment vacuum hot-press sintering pulse electrodeposition accumulative roll-compositing wet milling and hot-press sintering nanoporous Cu + rolling + sintering CVD+ball-milling+SPS	Cu Gr/Cu PAM-Gr/Cu Pure Cu Gr/Cu-50 Gr/Cu-80 1.6 g/L-Gr/Cu Gr/Cu 0.6wt%Gr/Cu Cu 800-Gr/Cu Ball-milled Cu Ball-milled Gr@Cu	396 474 505 156 281 65.2 154.3	197 231 260 422 516 549 274 686 290.47 245 354 218.3 254.9	48.6 70.4 78.5	1.66 0.80 0.96 18.7 16.5 49.3 35.2	[17] [43] [70] [27] [71] [72] [73]
Add metal element	Chemically reducing+SPS+Ni electroless deposition engineering design methodology+SPS impregnation reduction+in situ reaction	Cu 0.8vol% GPL/Cu 0.8vol% Ni-GPL/Cu 30 mg/L-NCG/Cu Pure Cu GNPs/Cu GNPs-W/Cu 0.11vol%Mo₂C@ 1.6%GNPs/Cu	68.97 110.16 234.25	172 131 245 338.7 103.50±2.28 171.85±1.53 295.65±1.12 303		6 9 30.2±0.8 10.8±0.3 13.5±0.9	[74] [18] [33] [32]
Notes: GNPs—Graphene nanosheets; GPL—Graphene platelet; NCG—Nickel-plated graphene.

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表 2 不同方法制备Gr/Cu复合材料的导电性能

Table 2. Electric conductivity of Gr/Cu composites prepared by different methods

Experimental classification	Processing route	Material	Electrical conductivity/ %IACS	Ref.
RGO	MLM+self-assemble charge adsorption +thermal reduction+hot-press sintering	2.5vol%RGO/Cu 2.5vol%CNT-RGO/Cu Pure Cu 0.3wt%RGO+Cu 0.6wt%RGO+Cu 0.9wt%RGO+Cu	83 85 99 93 90 85	[66] [67]
Gr	Plasma assisted milling treatment vacuum hot-press sintering SPS HP accumulative roll-compositing wet milling and hot-press sintering	Gr/Cu PAM-Gr/Cu Pure Cu Gr/Cu-50 Gr/Cu-80 Gr/Cu Gr/Cu Gr/Cu 0.6wt%Gr/Cu	71.3 75.5 95.65 94.85 93.2 108.6 98.8 >70 97.5	[17] [43] [15] [27] [71]
Add metal element	impregnation reduction+in situ reaction	0.11vol%Mo₂C@ 1.6%GNPs/Cu	>90	[32]
Note: IACS—International annealed copper standard; CNT—Carbon nanotube.

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表 3 不同方法制备的Gr/Cu复合材料的导热性

Table 3. Thermal conductivity of Gr/Cu composites prepared by different methods

Experimental classification	Processing route	Material	Thermal conductivity/ (W·(m·K)⁻¹)	Ref.
RGO	Sintered charge adsorption + thermal reduction + hot-press sintering pulsed-current co-electro deposition	PTG/Cu-Cu_xO+Cu+0.1wt%PTG UTG+Cu+0.1wt%UTG Pure Cu 0.3wt%RGO+Cu 0.6wt%RGO+Cu 0.9wt%RGO+Cu FGr/Cu	168.5 64.8 375 405 413 364 497	[21] [67] [89]
Gr	Electroless plating method Vacuum hot pressing	5%GNP/Cu 20%GNP/Cu GP/Cu	298.7 221.4 968	[94] [88]
Add metal element	Electroless deposition Vacuum hot pressing+PM	30 mg/L-NCG/Cu B₄C-B@Gr/Cu	431.2 676	[18] [95]
Notes: PTG—Plasma treated graphene; UTG—Untreated graphene; FGr—Functionalization of graphene with conjugated 4-ethynylaniline; GP—Graphene paper.

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