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石墨烯/铜基复合材料的制备及组织性能
论文作者:童鞋论文网  论文来源:www.txlunwenw.com  发布时间:2019/10/16 9:19:44  

摘要:随着集成电路等电子元器件的特征尺寸逐渐减小,电子元器件的耗散功率密度和发热量越来越大,因此,器件的导热散热已成为需要迫切解决的关键问题。铜及铜基复合材料因其良好的塑韧性和优异的导电导热性能成为电子元器件中导热材料的研究重点。石墨烯具有优异的力学性能和极高的导热性能,石墨烯作为复合材料的第二相,有望提高复合材料的综合性能。本文采用铜作为基体,石墨烯作为第二相,研究石墨烯/铜基(Gr/Cu)复合材料制备及组织性能。

脉冲电沉积法因其设备简单、成本低、效率高和易于向工业生产转化等优点成为金属基石墨烯复合材料的主要制备方法。因此,本文采用脉冲电沉积法制备Gr/Cu复合材料。利用XRD、SEM、TEM和Raman光谱对复合材料的相组成、晶体结构以及组织形貌进行分析;采用纳米压痕技术和万能材料试验机对复合材料的力学性能进行测试;利用激光闪射法和四探针法分别测得复合材料的导热性能和导电性能。探索研究脉冲电沉积参数(电解液pH值、电沉积电压、电沉积温度以及石墨烯浓度)对Gr/Cu复合材料的制备过程、组织与性能的影响,结果如下:

(1)随着电解液pH值由2.5减小至1.0(电压2.0V,温度30℃),电流密度、电沉积速率和沉积层厚度均呈现上升的趋势;Gr/Cu复合材料的抗拉强度由80.0MPa增大到235.9MPa。当电解液pH值为1.0时,Gr/Cu复合材料宏观上均匀平整,晶粒尺寸最小为471nm。

(2)随着电沉积电压由2.0V增加至3.5V(电解液pH值1.0;温度30℃),电流密度、电沉积速率和沉积层厚度均呈现增大的趋势;Gr/Cu复合材料的抗拉强度由235.9MPa降低至205.3MPa。当电沉积电压为2.0V时,Gr/Cu复合材料宏观上均匀平整,晶粒尺寸最小为450nm。

(3)随着电沉积温度由30℃升高至60℃(电解液pH值1.0;电压2.0V),电流密度、电沉积速率和沉积层厚度均呈现上升的趋势;Gr/Cu复合材料的抗拉强度由235.9MPa降低至148.9MPa。当电沉积温度为30℃时,Gr/Cu复合材料宏观上均匀平整,晶粒尺寸最小为380nm。

(4)随着电解液石墨烯浓度由0.04g/L增加到1.6g/L(电解液pH值1.0;电压2.0V;温度30℃),电流密度和电沉积速率均呈现增大的趋势,而沉积层厚度随石墨烯浓度的增加而减小;Gr/Cu复合材料的晶粒尺寸和缺陷密度均呈现先增大后减小的趋势,当石墨烯浓度为0.4g/L时,复合材料的晶粒尺寸与缺陷密度均最大;复合材料的抗拉强度和硬度均呈现先减小后增大的趋势,当石墨烯浓度为0.4g/L时,复合材料的抗拉强度最小,为235.9MPa,硬度最小,为1.44GPa;Gr/Cu复合材料的热导率呈现先增加后降低的趋势,当石墨烯浓度为0.4g/L时,复合材料的热导率最大,为540.145W/m·K,是电沉积纯铜的2.5倍;Gr/Cu复合材料的电阻率随石墨烯浓度的增加而降低,当石墨烯浓度为1.6g/L时,复合材料的电阻率最小,为4.423×10-9Ω·m。

当石墨烯浓度0.4g/L时,制备所得复合材料的抗拉强度为235.9MPa,硬度为1.44GPa,热导率为540.145W/m·K,电阻率为6.711×10-9Ω·m。制备的复合材料以铜晶粒包覆石墨烯片的形式存在,且铜基体中存在大量的孪晶。

As the characterization size of electroniccomponents such as integrated circuits is gradually reduced, the powerdissipation and heat generation of electronic components are becoming largerand larger. Therefore, heat dissipation of devices has become a key issue thatneeds to be urgently solved. Copper and its matrix composites have become afocus research on thermal conductive materials in electronic components due totheir good plastic toughness, excellent electrical and thermal conductivity.Graphene has excellent mechanical properties and extremely high thermalconductivity. Graphene, as the second phase, is expected to improve theperformance of the composites. In this paper, copper was used as the matrix andgraphene as the second phase to study the preparation, microstructure andproperties of graphene/copper matrix (Gr/Cu) composites.

Pulse electrodeposition was the main methodto prepare metal matrix graphene composites because of its simple process, lowcost, high efficiency and easy conversion to industrial production. Therefore,pulse electrodeposition was used to fabricate Gr/Cu composites. X-raydiffraction (XRD), scanning electron microscopy (SEM), and transmissionelectron microscopy (TEM) were used to analyse the phase compositions of Gr/Cucomposites, the crystalline structure and the microstructure characterization.The mechanical properties of Gr/Cu composites were tested by universal testingmachine and nanoindentation method. The thermal conductivity and electricalconductivity of Gr/Cu composites were measured by laser flashing and four-probemethods. The effects of pulse electrodeposition parameters (electrolyte pH, electrodeposition voltage, electrolyte temperature and grapheneconcentration) were performed on the preparation process, microstructure andproperties of Gr/Cu composites.

(1) As the pH of the electrolyte decreasedfrom 2.5 to 1.0 (voltage 2.0V, temperature 30 °C), the current density,electrodeposition rate and thickness of the composites showed an increasingtrend. The tensile strength of Gr/Cu composites increased from 80.0 MPa to235.9 MPa. When the pH value of the electrolyte was 1.0, the Gr/Cu compositeswas uniformly flattened macroscopically, and the smallest grain size was 471nm.

(2) As the electrodeposition voltageincreased from 2.0V to 3.5V (electrolyte pH 1.0, temperature 30°C), the currentdensity, electrodeposition rate and thickness of the composites showed anincreasing trend. The tensile strength of Gr/Cu composites was reduced from235.9 MPa to 205.3 MPa. When the electrodeposition voltage was 2.0V, the Gr/Cucomposites was uniformly flattened macroscopically, and the smallest grain sizewas 450nm.

(3) As the electrodeposition temperatureincreased from 30°C to 60°C (electrolyte pH 1.0, voltage 2.0V), the currentdensity, electrodeposition rate and thickness of the composites showed anincreasing trend. The tensile strength of Gr/Cu composites was reduced from235.9 MPa to 148.9 MPa. When the electrodeposition temperature was 30°C, theGr/Cu composites was uniformly flattened macroscopically, and the smallestgrain size was 380nm.

(4) As the graphene concentrationsincreased from 0.04g/L to 1.6g/L (electrolyte pH value 1.0, voltage 2.0V,temperature 30°C), the current density and electrodeposition rate showed anincreasing trend. The thickness of Gr/Cu composites decreased with the increaseof graphene concentrations. The grain size and defect density of Gr/Cucomposites increased first and then decreased. When the graphene concentrationwas 0.4g/L, composites had the largest grain size and highest defect density.The tensile strength and hardness of composites decreased first and thenincreased. When the graphene concentration was 0.4g/L, the smallest tensilestrength of composites was 235.9MPa, and the lowest hardness was 1.44GPa. Thethermal conductivity of the composites increased first and then decreased. Whenthe graphene concentration was 0.4g/L, t

关键词:Gr/Cu复合材料;脉冲电沉积法;纳米压痕;热导率;电阻率

Gr/Cu composites;pulseelectrodeposition;nanoindentation;thermal conductivity;resistivity

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