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High thermal conductivity and mechanical properties of nanotube@Cu/Ag@graphite/aluminum composites Xiaopeng Han, Ying Huang, Qiao Gao, Meng YU, and Xuefang Chen Ind. Eng. Chem. Res., Just Accepted Manuscript • DOI: 10.1021/acs.iecr.8b01567 • Publication Date (Web): 17 Jul 2018 Downloaded from http://pubs.acs.org on July 17, 2018

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Industrial & Engineering Chemistry Research

High thermal conductivity and mechanical properties of nanotube@Cu/Ag@graphite/aluminum composites Xiaopeng Han, Ying Huang*, Qiao Gao, Meng Yu, Xuefang Chen Research and Development Institute of Northwestern Polytechnical University in Shenzhen, Shenzhen 518057, PR China MOE Key Laboratory of Material Physics and Chemistry under Extrodinary Conditions, Ministry of Education, School of Science, Northwestern Polytechnical University, Xi'an 710072, PR China

Abstract The weak interfacial bonding and agglomeration of reinforcement are critical challenges for the expected performance and hider extensive application of aluminum matrix composites. In this work, the Cu particles with nanotube, Ag-coated graphite flakes and films, urea and starch were mixed together to fabricate porous performs, which then were infiltrated by vacuum gas pressure infiltration in 720 ℃. Effects of graphite film thickness on microstructure and properties of TC and CTE were investigated. The nanotube@Cu/Ag@graphite/aluminum composites exhibited high TC of 451 W/mK and excellent bending strength(BS) of 74 Mpa, which were approximately increased by 48.8 % and 126 % comparing with the samples without graphite film. Key words: Ag-coating, nanotube, graphite film, thermal conductivity The corresponding author E-mail: [email protected]

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Industrial & Engineering Chemistry Research 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

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1. Introduction More and more application fields including electronic packaging, aviation,

navigation,

automotive,

computer

chip

and

battery

technologies1-5 have placed a wide range of demand due to excellent property of thermal conduction materials6-8,but thermal dissipation is the key technology for the miniaturization and service life of components. The effective method of solving thermal conduction problem is to manufacture materials with excellent thermal conductivity(TC), low density, low coefficient of thermal expansion(CTE), and promising mechanical property, which can transfer thermal out of high temperature equipment. Nowadays, graphite flakes9, nanotube10-11, graphene12-15, carbon fiber16-21 and graphite foams22-23 have great potential to be researched as high thermal conduction materials. Highly oriented graphite flakes and graphite films23-25 have widely applied as reinforcement to synthesis high thermal conduction materials owning to the high in-plane thermal conductivity about 1000W/Mk, low thermal expansion, low density, self-lubricating and tractable. Meanwhile, graphene26-29 or nanotube10-11 can be matched with graphite flakes to reinforce matrix to synthesis high thermal conduction composites. But the excessive interfacial and poor wettability reaction among molten matrix and reinforcement are two pivotal difficulties for the composites with promising functions30. Firstly, the molten aluminum isn’t wetting graphite


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materials due to the contact angle approaching 140°8. Consequently, defects and voids can be formed om the surface of graphite materials, which weaken the TC and bending strength of the Al-based composites. Secondly, the harmful excessive carbide tends to form in high infiltration temperature. The same phenomenons are also appeared in some other graphite reinforcement, such as graphene/Al composites26-28, nanotube/Al composites11, carbon fiber/Al composites19, carbon foam/aluminum composites22, diamond/Al composites31-32 and SiC/Al composites33-34. An innovative method to weak side reactions are to encapsulate metal or inorganic particles, such as Ag35-36, Cu37, Ni24, 38-39, Ti37, W, Gr, Cr40, Si41, SiC42 and so on. The mental coatings have strongly bonding force with matrix, which can effectively eliminate the harmful side effects43-44. Compared with other coatings, Ag-coatings on the graphite materials by chemical plating process have unique uniformity and compactness on the surface of graphite and show better compatibility between the reinforcement and matrix. Meatal-coated graphite materials are applied to fabricate perform as reinforcements, but stenosis passage between graphite flakes make the infiltration pressure become higher. So some workers have concentrated on reinforcing with graphite materials and particles, such as Al2O345, TiC42, B4C34, Si3N4 and so on. Recently, graphite films and nanotube have attracted widely attention



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in heat conversion materials due to their unique thermal diffusion property. They are used to be fillers for graphite/aluminum composites. Al-based materials reinforced with nanotube exhibite anticipative improvement in their thermal diffusion properties10. Besides, graphite materials show unique self-lubricating property when served as reinforcement to matrix for improving the thermal diffusion. More and more researchers have concentrated on adding higher concentration of nanotube to enhance the performance, but excess nanotube results in the side reactions and uniform dispersion. Actually, nanotube is used as reinforcement and the fabrication parameters of the composites are well researched,

so

the

promising

performance

can

be

reasonable

estimated46-48. So nanotube and Cu particles are utilized as reinforcement to manufacture nanotube@Cu/Ag@graphite/aluminum composites, we can improve the dispersion by grinding ways, which is an innovative way to disperse the reinforcement in the matrix. In this study, the composites are reinforced with Cu particles with 1 % nanotube and Ag-coated graphite flakes into aluminum matrix. Finally, we

successfully

fabricated

nanotube@Cu/Ag@graphite/aluminum

composites with anticipant properties by vacuum gas infiltration ways. The contents of nanotube in Al-based composites matrix are characterized at vertical and horizontal directions to investigate the dispersion of graphite materials and Cu particles. Besides, raw materials, the


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Ag-coatings and nanotube@Cu are also characterized. 2. Experimental procedure 2.1. Raw materials The graphite flakes are platelets of 270 µm of average diameter and thickness about 25 µm, purchased from Shandong Graphite Corporation. The vertical and horizontal thermal conductivity values of graphite flakes were analyzed about 1000 W/mK and 38 W/mK, respectively. Cu particles (200 meshes) came from Aladdin, Shanghai. Urea and starch were acquired from PaiNi, China. The AgNO3 powders (purity 99.9 %), were supplied from SINOPHARM, China. Meanwhile, the Al alloy was employed as matrix due to lower melting point comparing with pure aluminum. Multi-walled carbon nanotube about 50 µm were also used as reinforcement, which bought from Molbase. 2.2. Chemical plating process The graphite flakes are etched in alkali solution consisting of NaOH and Na2CO3 under 100 °C to remove impurities from the surface. After being degreased, the graphite flakes are pumped with distilled water and dried under 60 ℃. Then the drying graphite flakes are continuedly sculptured in sulfuric acid for 15 min. After coarsening, the graphite flakes are cleaned with distilled water and baked at 80 ℃ for 10 h. The 5 % AgNO3 solution (AgNO3:graphite flakes 5：100 Wt%) and 80 % NH3·H2O solution are mixed up Ag(NH3)2OH solution. The



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pretreated graphite flakes are dispersed into Ag(NH3)2OH solution, then the 10 % HCHO solution added into mixed solution which can deposit the element sliver on the surface of graphite. Then the Ag-coated graphite materials are collected pumping filtration ways and dried at 80 °C for 12 h. The graphite films are cut into pieces of 52 mm x4 mm and processed in the last way. 2.3. Synthesis of preform Cu particles were mixed with commercial nanotube by milling for 20 min. The Ag-coated graphite flakes, urea, starch and preprocessing Cu particles were mixed in mixer machine under the same rotated direction for 15 min. The mixtures were added into steel mould and processed with intelligent pressure machine. And then compact preform was heated

in

dryer up to 320 ℃ on the base of urea decomposition temperature, the urea was decomposed into NH3 which can form infiltration channels and pores in the preform. 2.4. Infiltration Al alloy was heated at 720 ℃ and the perform was put down into crucible quickly at argon gas pressure of 20 atm. Figure 1 demonstrates the detailed steps of manufacturing the composites.


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Figure 1. The flow diagram for fabricating the Nanotube@Cu/Ag@graphite/Al composites. 2.5. Characterization The microstructures of Nanotube@Cu/Ag@graphite/Al on the fractured surface were analyzed by scanning electron microscope (FE-SEM, Quanta 600FEG). The surface characterization of the synthesized samples was analyzed by using X-ray photoelectron spectroscopy (XPS, Kratos Axis Ultra DLD) with carbon 1s at 284.6 eV as a reference to conduct a charge correction. The thermal diffusivity of Nanotube@Cu/Ag@graphite/Al composites was tested by the lasher flash instrument (LFA447). Archimedes principle was adopted to characterize the density and porosity. XRD patterns were obtained using an X-ray diffractometer (Rigaku D/Max 2500 V/PC) equipped with a Cu Kα



source operating at 36 kV and 200 mA. 3. Results and discussion 3.1. Raw materials and Ag-coatings

Figure 2. Morphologies SEM images of raw materials: (a)Si particles; (b)nanotube; (c)graphite film; (d)graphite flakes; (e)5 % Wt Ag@graphite; (f) 10 % Wt Ag@graphite Figure 2a exhibits micrographs of Cu powders which have uniform size and irregular shapes. It is revealed that the diameter of particles with the size about 74 µm. Figure 2b demonstrates the photograph of nanotube and the length of it approximately 80 µm. Figure 2c shows the smooth surface of graphite film before chemical plating. Figure 2d displays the raw graphite platelets with average diameter of 270 µm. Figure 2e and f exhibits different proportion of 5% Wt and 10% Wt respectively. Compared with Figure 2e, Figure 2f displays the more compact surface ACS Paragon Plus Environment

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morphology of Ag-coated graphite flakes by chemical playing ways, and the results indicates that the thin and uniform coatings on the surface of graphite flakes. Due to high-density of silver, the slight thickness of the coatings must be controlled to ensure the low density of the composites. In general, the existence of coatings implies that the tight combination of elemental Ag and graphite flakes, which can eliminate interface reaction effectively.

Figure 3. Microstructure of Nanotube@Cu/Ag@graphite/Al composites in plane of graphite film: (a) 0.1mm graphite film;(c) 0.3mm graphite film; (e)1mm graphite film; (b,d,f) the corresponding interface bonding images of aluminum and graphite film; (g,h,i) the EDS layered images of d. ACS Paragon Plus Environment


Figure 3a, c and e reveal that the graphite flakes and graphite film are uniformly distributed in the aluminum matrix. The Ag-coated graphite flakes and graphite film can be observed from Figure 3a-f, which show the tightly interface bonding between Ag and graphite flakes and graphite film. It is obvious that no defects can be founded between the aluminum matrix and reinforcement, thus the coatings are sued to eliminate the interfacial reaction. As shown in Figure 3g, Figure 3h and Figure 3i, the clear interface boundaries between C, Al and Ag. What’s more, the Figure 3i display the homogeneous Ag-coatings on the surface of graphite film. In general, it is indicated that nanotube@Cu particles distribute in the matrix uniformly with the increasing of nanotube content. With the increasing of thickness of graphite film, some cracks are observed in the graphite film, it resulting voids in the process of infiltration which lead to high thermal resistance.


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Figure 4. SEM micrographs of section:(a,b) 0.1mm graphite film;(c,d) 0.3mm graphite film;(e,f) 1mm graphite film. The uniform distribution is verified from the images of sections Figure 4.a ， c

and

e

which

is

the

pivotal

step

to

fabricate

Nanotube@Cu/Ag@graphite/Al composites. Due to graphite layers and films along to thermal diffusion direction, which is high efficiency direction to improve thermal performance. The continuous graphite film



transport heat from the composites quickly, which have an advantage of pure graphite flakes. Due to the addition of Cu particles, graphite flakes and film are separated by it which can enhance the mechanical property apparently and provide suitable infiltration-tunnel. With the encapsulation of nanotube, the addition of Cu particles promotes the dispersion of nanotube. Some researchers have found that Cu powders improve the infiltration channel, which can effectively reduce the infiltration temperature and prevent the formation of Al4C3.

Figure 5. XRD analysis of composites with different thickness of graphite film The XRD is characterized to confirm the phase composition of and


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present in Figure 5. Cu9Al4 peaks are observed due to append Cu particles in the various specimen. In the infiltration of the perform, there is no obvious Al4C3 confirmed which can prove the graphite flakes with uniform Ag-coatings and eliminate the side reaction utterly. Due to the Ag-coatings on the in interface of graphite materials, the molten Al only reacts with Ag-coatings and Cu particles. But with thicker of graphite film, some cracks have discovered due to diverse thermal stress between reinforcement and matrix. Furthermore, it can be concluded that only the composites with 0.01 mm graphite film have unique interface binding.

Figure 6. XPS spectra of Nanotube@Cu/Ag@graphite/Al composites: (a) wide scan; (b) Cu region; (c,d,e) the Al 2p region. In order to further investigate the peak of Al4C3, the surface element



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components of Nanotube@Cu/Ag@graphite/Al composites are analyzed by the corresponding X-ray photoelectron spectroscopy and shown in Figure 6. The composites peaks make up Cu, Al, Ag and O elements. There isn’t founded Al peaks in Ag@graphite flakes line comparing with other samples in Figure 6a. With the addition of nanotube, the molten aluminum and nanotube react in the process of infiltration, but the formation of Al4C3 is limited, so the limited carbide doesn’t affect thermal and mechanical performances. Furthermore, some researchers have reported that a few nanosized Al4C3 is important to minimize interfacial thermal resistance and transfer heat quickly. From Figure 6b, the molten aluminum and Cu formed Al9Cu4 under the high infiltration temperature. 3.2.

Thermal

properties

of

Nanotube@Cu/Ag@graphite/Al

composites In order to assess the effect of Cu particles and nanotube addition on TC, the following equations are used40, 49: λ=α×Cp×ρ

（1）

where α is the thermal diffusivity, λ is the thermal conductivity, Cp specific heat capacity and ρ is the density. The specific heat capacity of Nanotube@Cu/Ag@graphite/Al composites is predicted by the linear rule of composites including every part (graphite materials, Cu particles, nanotube, and Al alloy). Table 1 displays the property of the composites. Table1.The properties of the nanotube@Cu/Ag@graphite/aluminum


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composites Graphite film(mm)

nanotube

Cp

(Wt%)

Density

TCa

Bending

(g/m3)

(W/mK)

strength(Mpa)

0.1

1

0.740

2.4134

451.07

34.89

0.3

1

0.688

2.3807

324.87

50.42

1

1

0.797

2.3302

209.46

73.05

0.688

2.4233

266.16

32.88

0

1

a In-plane of graphite flakes 3.3 . TC of the composites

Figure 7.

The TC of the composites with different graphite film



thickness. The TC of the Al-based composites decreases with excess nanotube due to superfluous carbides according to the previous study. And the 1 % content of nanotube to matrix has been ensured optimum proportion. With the increase of graphite film, the TC of the composites decreases gradually as shown in Figure 7. When the 0.1mm graphite films added into the matrix, the specimen has highest thermal conductivity at 451.07 W/mK. Based on the microstructures of Nanotube@Cu/Ag@graphite/Al composites, the infiltration channel is formed uniformly due to Cu powders encapsulated with nanotube. Furthermore, the agglomeration of reinforcements can be solved effectively by grinding ways. With the increasing of graphite film thickness, the thermal property of the composites decreases gradually due to voids and cracks in the matrix in Figure 3f, so the 0.1mm graphite film have an excellent improvement on the thermal property. 3.4. CTE of the composites


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Figure 8. The data for CTE of the composites It is revealed that the CTE and the relative changes of length in the composites changed gradually with diverse temperature in Figure 8. What’s more, the CTE rise rapidly within 100 °C. Compared with various thickness of graphite film, the CTE of the composites with 0.1 mm and 0.3 mm graphite film remain unchanged during high temperature. But the CTE improved gradually when addition of 0.1 mm graphite film. By this way, the CTE of the composites can be controlled in promising range. 3.5. BS property of the composites



Figure 9. The bending strength of different specimens with different thickness of graphite film Figure 9 shows the BS of the composites as a comparison of different thickness of graphite film. The addition of 1 mm graphite film to the matrix increase the BS of the composites for about two times. Due to the thickness of 1mm graphite film, it can effectively decrease the interface reaction of molten aluminum comparing with graphite layers and improve the mechanical property. Thus, the in-plane TC is promoted gradually due to the introduction of 0.1 mm graphite film uniformly. But the mechanical performance enhanced owning to the thicker of graphite film gradually. What’s more, Ag-coatings are successfully improved the bonding force of graphite


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flakes, graphite film and Al matrix.

4. Conclusion This work provides an innovative method, taking advantages of chemical plating mental coatings and encapsulating nanomaterials, for manufacturing aluminum matrix composites reinforced graphite film, Cu particles, nanotube and graphite flakes. Ag-coatings are successfully encapsulated on the surface of graphite layers and graphite film by chemical plating process to eliminate the formation of carbide between molten aluminum and graphite effectively. The porous perform are manufactured

by

the

decomposition

of

urea

under

chemical

decomposition temperature, which can be infiltrated at lower pressure and temperature by vacuum gas pressure infiltration process. The composites with 0.1 mm graphite film have promising in-plane TC of 451 W/mK and stable CTE in high temperature application environment. What’s more, the bending strength of the composites have been enhanced to approximately 73Mpa.

Acknowledgements This work was financially supported by the Research and Development Institute of Northwestern Polytechnical University in Shenzhen, and the fundamental Research Funds for the Central Universities (No. JCJY20170306153232969).

Reference



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