Scripta Materialia

Ultrahigh Thermal Conductivity of Interface Materials by Good Wettability of Indium and

Diamond
--Manuscript Draft--

Manuscript Number: SMM-20-1571

Article Type: Regular article

Section/Category: Opt in to First Look

Keywords: Low melting point metal; Diamond; Wetting; thermal conductivity

Abstract: The thermal conductivity of Bi-In-Sn/diamond composites was improved by pre-adding

indium particles fabricated using slice technique. Using in situ imaging and particle
dipping experiment, the wetting behavior of diamond microparticle with pure indium,
indium-based and gallium-based liquid metal (LM) was investigated. The diamond
microparticle was well wetted by molten indium and the wettability of diamond particle
with LM can be improved by alloying with indium. Oxide film would hinder the wetting of
LM and diamond. The highest thermal conductivity of the indium-based composites
obtained was up to ~211.12 W m -1 K -1 , which was close to that of aluminum.

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Ultrahigh Thermal Conductivity of Interface Materials by Good

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2 Wettability of Indium and Diamond
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5 Chengzong Zeng, Jun Shen*, Jianbo Zhang
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8 State Key Laboratory of Mechanical Transmission, College of Material Science and Engineering,
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11 Chongqing University, Chongqing, 400044, China.
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The thermal conductivity of Bi-In-Sn/diamond composites was improved by pre-adding indium particles
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16 fabricated using slice technique. Using in situ imaging and particle dipping experiment, the wetting behavior
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19 of diamond microparticle with pure indium, indium-based and gallium-based liquid metal (LM) was
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22 investigated. The diamond microparticle was well wetted by molten indium and the wettability of diamond
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25 particle with LM can be improved by alloying with indium. Oxide film would hinder the wetting of LM and
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28 diamond. The highest thermal conductivity of the indium-based composites obtained was up to ~211.12 W m-
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31 K-1, which was close to that of aluminum.
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34 Keywords: Low melting point metal; Diamond; Wetting; Thermal conductivity
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In the microelectronic industry, more and more attention has been paid to the development of high-
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39 performance thermal solutions due to the increasing integration and continuous miniaturization [1, 2].
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42 According to Arrhenius’s experience rule [3], the failure rate of electronic components will be doubled for
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45 every 10°C increase. Generally, the failure rate of electronic devices caused by excessive temperature was
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48 more than 80% [4]. In practical applications, interface materials are used to fill the microscopic air gaps
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51 between adjacent components to promote the heat transfer of microelectronic devices. Compared with the low
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54 thermal conductivity (1-5 W m-1 K-1 [5]) and high contact thermal resistance (14-100 mm2 K W-1 [6, 7]) of
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59 *
60 Corresponding author: Tel: +86-13883111150; E-mail: shenjun@cqu.edu.cn (J. Shen)
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 polymer-based thermal interface materials (TIMs), low melting point metal (LMPM) present higher thermal
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2 conductivity (10-30 W m-1 K-1 [8]) and lower interfacial thermal resistance (0.25-5 mm2 K W-1 [9]). However,
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5 it is imminently urgent to find LMPMs with higher thermal conductivity to meet the increasing demand of
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8 thermal design [8].
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11 Most researches have indicated that the thermal conductivity of the matrix material can be improved by
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adding high thermal conductivity particles [10-12]. Recent studies have reported successful preparation of
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16 LMPM-based composites containing microparticles of Ag [13, 14], Cu [15], Mg [16], W [17], carbon
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19 nanotubes [18], diamond [19, 20] and so on. According to Wei’s report [19], the reaction rate of LMPM with
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22 most metal materials is very rapid and transform into intermetallic compounds in a very short time. Thus, the
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25 inorganic nonmetal fillers with high thermal conductivity can be a good choice. Dispersions of original
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28 diamond particles in EBiInSn [20] (eutectic field’s alloy Bi32.5In51Sn16.5) and diamond particles coated in a
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31 chromium wetting layer in pure gallium [19] has reportedly achieved three to fourfold increase in thermal
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34 conductivities from that of the base metal (up to 71 W m-1 K-1 and 112 W m-1 K-1, respectively). However,
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the thermal conductivity of LMPM-based composites is still much lower than that of the hot (~150 W m-1 K-
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39 1
for silicon) and the cold terminal (~237 W m-1 K-1 for aluminum, ~401 W m-1 K-1 for copper). Simultaneously,
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42 the wettability of LMPM with diamond particle lacks further research.
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45 In this study, the pure indium particles fabricated by slice technique as a pre-additive compounded with
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48 diamond and EBiInSn. The wetting process of diamond microparticle with molten indium, EBiInSn, and
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51 gallium-based metal was conducted using in situ imaging and particle dipping experimentation. The highest
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54 thermal conductivity of indium-based composites obtained in this work was up to ~211 W m-1 K-1, which was
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57 higher than that of silicon and close to that of aluminum.
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60 Eutectic field’s metal Bi32.5In51Sn16.5 (EBiInSn) particles and indium particles were prepared using slice
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 technique [21] (the purity of the metal is at least 99.995%, Shenyang Jiabei Trading Co., Ltd., China). 30 g
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2 (approx.) metal was added in citric acid solution (0.2 wt% for EBiInSn, 0.1 wt% for indium particles) in
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5 glycerol. The solution prepared in a glass beaker (100 mL) was kept in an oil bath as determined temperature
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8 (120°C for EBiInSn and 220°C for indium) for at least 10 min before slice. The slice rate was 15000 rpm
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11 (using a homogenizer, FSH-2A) and the lasting time was 5 min. Excess citric acid and glycerol were washed
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out with ethanol. Particles were dried in a vacuum oven (BZF-30) and kept in an airtight container. Diamond
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16 particles with MBD8 quality were used in this study (Zhecheng Hongxiang Superhard Material Co., Ltd.,
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19 China). The diamond particles, EBiInSn powder, and indium powder were mechanically mixed and pressed
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22 into tablets with the diameter of 12.5 mm. Then the specimens were sintered (at 180°C for 30 min) in an oven
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25 (LTKC-4-10A) with vacuum condition.
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28 The microstructures and crystallographic structures of the samples were characterized by field emission
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31 scanning electron microscope (FESEM, Zeiss Auriga-39-60) equipped with energy dispersive X-ray
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34 spectrometer (EDS) and X-ray diffraction (XRD, Empryean) with Cu Kα radiation. The melting process and
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the specific heat capacity Cp of the samples were measured using a differential scanning calorimeter (DSC,
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39 TGA/DSC1/1100LF). The density of the specimens  c was measured using the Archimedes principle. The
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42 thermal diffusivity α was measured by a LFA467 MicroFlash (Netzsch) thermal analyzer at room temperature.
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45 Each sample was tested 3~5 times to reduce testing errors of experimental data. The thermal conductivity Kc
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48 was calculated from the equation K c =c C p .
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51 The micrograph of EBiInSn particles was presented in Fig. 1a, highly spherical EBiInSn microparticles
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54 were obtained. Surface of the EBiInSn microparticles was smooth, non-pits and defects were observed.
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57 Diameters of the EBiInSn particles were measured and calculated (Fig. 1b). Whose diameters were
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60 concentrated in 20~30 μm. Depending on the XRD results (Fig. 1c). The EBiInSn particles were mainly
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 composed of Bi, In, Sn and BiIn2 phases, which were consistent with that of bulk EBiInSn [22]. Indium
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2 microparticles were successfully fabricated using slice technique. Quasi-spherical indium powders were
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5 obtained (Fig. 1d). The surface of indium particle was not as smooth as that of EBiInSn particles, which is
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8 chiefly because the lower surface tension of molten indium (~0.556 N m-1 [23]) than that of EBiInSn (~0.58N
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11 m-1 [24]) and the lower Moh’s hardness (1 for indium, 1.8 for tin, and 2.25 for bismuth) of indium [25]. Thus,
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indium particles were too soft to maintain higher and better spherical shape during the slice process of
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16 collisions between particles caused by high-speed shear force. Equivalent diameters of the indium
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19 microparticles were mostly concentrated in 15~20 μm (Fig. 1e). The XRD results indicate that the indium
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22 particles obtained were only the indium without other phases through slice technique (Fig. 1f). Meantime, the
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25 melting point of EBiInSn and indium did not change after slice process (Fig. 1g). Fig. 1h was the schematic
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28 representation of mixing diamond particles, indium particles, and EBiInSn particles in different proportions.
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31 Macrograph of the final manufactured specimens was displayed in Fig. 1i.
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34 To study the wettability of diamond microparticles in molten indium and molten EBiInSn, simple in situ
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37 experiments were conducted. Fig. 2a presented the schematic of in situ wetting experiments. The temperature
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39 of the low melting point metal (LMPM) in wetting process was ~30°C higher than that of its melting point,
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42 which was measured by the computer through a data acquisition (UNI-T UT325). The diamond microparticles
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45 of 35/40 mesh were bonded on quartz capillary tubes using silicone glue with heat resistance of 250°C. The
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48 wetting process was recorded using a CCD microscope camera (DM3). Fig. 2b displays the micrograph of
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51 bulk indium with diamond microparticles before and after heating. The diamond particles were pre-attached
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54 to bulk indium. After the bulk indium melted, parts of the diamond particles were “eaten” by molten indium.
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57 This phenomenon could be owing to the diamond wetted by molten indium. Fig. 2c shows the single diamond
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60 microparticle wetting experiment in molten indium. To avoid wetting results of the particle surface affected
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 by the oxide layer of indium, the surface of molten indium was cleaned using a polytetrafluoroethylene scraper
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2 (viewed by a CCD microscope) and the time of single wetting experiment was controlled about 15s. The
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5 diamond microparticle was immersed into the molten indium and then pulled out until the diamond
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8 microparticle and molten indium were completely separated. The diamond particle and molten indium showed
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11 excellent adhesion during the pull-out stage. The wetting process of the single diamond particle with molten
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indium showed that the diamond particle was completely wetted by molten indium and the quartz capillary
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16 tube was also well wetted.
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19 Using the same wetting method, the diamond microparticle was immersed into the molten EBiInSn with
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22 or without oxide present. Fig. 2d was wetting behavior between diamond microparticle and molten EBiInSn
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25 with an oxide layer (prepared by melting EBiInSn placed in air for one hour). The results showed that only a
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28 small part of the diamond microparticle was wetted by molten EBiInSn. However, the majority of the diamond
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31 microparticle were well wetted by clean molten EBiInSn (Fig. 2e). It noted that the oxide film on the molten
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34 EBiInSn would hinder the diamond particle from being wetted. The wetting behavior of gallium and diamond
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was also conducted (Figure S1a, Supporting Information), which showed that the wettability of diamond and
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39 gallium was poor. However, the wetting behavior of gallium and diamond particle can be improved by alloying
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42 with indium (Figure S1b, Supporting Information). This phenomenon is significant for the preparation of
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45 gallium-based low melting point metal composites containing diamond particles.
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48 Fig. 3a illustrates the morphology of EBiInSn-diamond-indium composite (Bi-In-Sn/diamond composite)
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51 before sintering. The EBiInSn particles still kept spherical morphology, while the initial indium particles were
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54 compressed into a flat shape due to their excellent softness (Fig. 3b and c). After sintering, the EBiInSn
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57 particles and indium particles were melted together. The diamond particles were well surrounded by the
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60 indium-based metal (Fig. 3d) owing to good wettability between them. Fig. 3e was the enlarged view of the
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 matrix metal formed by the re-melting of EBiInSn and indium particles. Combined with the microstructure
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2 and its element distribution analysis (Fig. 3f), the Sn element from original EBiInSn had obviously diffused
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5 to the initial indium particles. Fig. 3g presented the fracture surface of the Bi-In-Sn/diamond composite, most
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8 surfaces of diamond particles were well coated with indium-based metal and the diamond microparticles were
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11 effectively connected by the indium-based metal. From the enlarged view (Fig. 3h), the diamond particle was
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obviously and completely wetted by indium-based metal and no obvious gap existed between the diamond
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16 and the matrix metal. It indicated that the diamond particles can be well wetted by pre-adding indium and the
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19 effective heat conduction path for diamond particles can be formed.
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22 Priorly, the thermal conductivity of Bi-In-Sn/diamond composites influenced by the pre-adding indium
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25 particles volume fraction was analyzed (Fig. 4a). The volume fraction of diamond particles was set at 30%
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28 and the rest was EBiInSn except for pre-adding indium particles. The thermal conductivity of the composites
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31 increased from ~43.19 W m-1 K-1 to 55.15 W m-1 K-1 as the volume fraction of pre-adding indium particles
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34 increased from 0% to 30%. Next, the thermal conductivity of the composites affected by the volume fraction
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of diamond particles was measured. On the one hand, the volume fraction of EBiInSn was at the rate of 50%
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39 and the rest was pre-adding indium particles. The thermal conductivity of the composites increased with the
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42 diamond particles volume fraction as the diamond content was no more than 30% (Fig. 4b). When the diamond
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45 volume fraction was 40%, the thermal conductivity of the composites was no significant increase. This may
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48 be attributable to the fact that the ratio of diamond to pre-adding indium was in relative equilibrium. On the
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51 other hand, the pre-adding indium volume fraction was fixed at 30% and the rest was EBiInSn. The thermal
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54 conductivity of the composites increased from ~31.84 W m-1 K-1 to ~105.84 W m-1 K-1 as the volume fraction
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57 of the diamond increased from 10% to 50% (Fig. 4c). Further, the thermal conductivity of indium-based metal
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60 composites containing diamond particles influenced by the dimension of the diamond was analyzed. The
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 thermal conductivity of the composites increased with the size of diamond particles (Fig. 4d). The highest
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2 thermal conductivity achieved in this work was indium/diamond composite, which was ~211.12 W m-1 K-1.
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5 Fig. 4e was the DSC curves of the composites varied with the ratio of original EBiInSn and pre-adding indium.
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8 Two obvious melting stages were observed. The initial melting temperature of the composites was close to the
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11 melting point of EBiInSn (~60°C) and the complete melting temperature was delayed with the increase of pre-
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adding indium volume fraction. The effect of aging on the DSC curve of the composites was small (Fig. 4f).
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16 Compared with the melting point of uniform alloying of Bi, In, and Sn (Fig. 4g), the melting point of pre-
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19 adding indium into EBiInSn was much lower. This is mainly because the pre-adding indium and original
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22 EBiInSn were difficult to form a homogeneous alloy at a lower temperature with the obstacles of diamond
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25 particles. Namely this material can be melted at a relatively low temperature.
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28 A simplified 2D model with the size of 500 μm×500 μm was built to predict the thermal conductivity of
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31 the composites. Before simulation, some assumptions were made: 1. The pre-adding indium particles were
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34 circular and the diamond particles were orthohexagnal, 2. The gap between pre-adding indium and diamond
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was filled with EBiInSn, 3. The mutual diffusion of EBiInSn and pre-adding indium was ignored. The
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39 temperature of the bottom wall and the top wall was set at 57oC and 20oC. The left and the right were set as
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42 insulation walls. The thermal conductivity Kc of this model can be calculated using the equation
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K c  qavg D Thot  Tcold  , where qavg is the average surface heat flux, D is the distance between the cold end
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48 and the hot end, Thot and Tcold were the temperature of the hot end and the cold end, respectively. Fig. 5a
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51 presents the heat flux density with vectors in the composites varied with the volume fraction of diamond
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54 particles. It states that the heat flux mainly passed through the diamond particles and the pre-adding indium
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57 particles nearing the diamond. The heat flux density was increased with the increase of diamond volume
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60 fraction, which was directly proportional to the thermal conductivity calculated by the model. Compared with
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 the results without pre-adding indium particles (Fig. 5a iii), the heat flux density of the model with pre-adding
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2 indium was significantly improved (Fig. 5a iV). The changing trend of experimental results and simulation
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5 results was basically consistent (Fig. 5b). However, the difference between experimental results and
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8 simulation results became larger as the diamond volume fraction higher than 40%, which could be due to the
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11 gap occurred between diamond and matrix metal. Fig. 5c shows the comparison of thermal conductivity of
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interface materials obtained in this work with that of other relative researches. It indicates that the thermal
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16 conductivity of the materials in this study was in a better level and the highest thermal conductivity achieved
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19 was ~211.12 W m-1 K-1, which was close to that of aluminum (~224 W m-1 K-1 [27]).
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22 In summary, quasi-spherical indium particles and spherical EBiInSn particles were successfully
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25 manufactured by slice technique. Wetting behavior of diamond microparticle with indium, EBiInSn, and
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28 gallium-based metal was studied using in situ imaging and particle dipping experiment. The results presented
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31 that the diamond microparticle was well wetted by molten indium and the wettability of diamond particle with
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34 LMPM can be improved by alloying with indium. The wettability between diamond microparticle and LMPM
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would be affected by oxide film of LMPM. The thermal conductivity of indium-based composites containing
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39 diamond particles varied with the volume fraction of pre-adding indium, the diamond volume fraction, and
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42 the dimension of diamond particles. It had little effect on the initial melting temperature of EBiInSn by pre-
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45 adding indium particles and the complete melting temperature of the composite was relatively low. Namely
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48 this material can be operated at a relatively low temperature. The highest thermal conductivity of the indium-
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51 based composites obtained in this work was up to ~211.12 W m-1 K-1, which was close to that of aluminum.
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54 Acknowledgement
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57 This research is supported by a Fundamental Research Funds for the Central Universities of China (Grant
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60 No. 2018CDGFCL0003).
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 Figures
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Fig. 1. SEM images of (a) EBiInSn particles and (d) indium particles; size distribution of (b) EBiInSn particles
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33 and (e) indium particles; X-ray diffractogram of (c) EBiInSn particles and (f) indium particles; (g) DSC cures
34 of EBiInSn and indium (both bulk metal and corresponding particles) as measured at a ramping rate of 5°C
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36 min-1; (h) schematic diagram of diamond, indium and EBiInSn mixtures (not to scale); (i) macrograph of the
37 mixtures.
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19 Fig. 2. (a) The schematic of in-situ wetting experimental platform (not to scale); (b) micrograph of diamond
20 particles with indium before and after heating; (c) wetting behavior of diamond microparticle with molten
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22 indium; (d) immersion of diamond microparticle into EBiInSn with oxide attachment (digital microscope
23 view); (e) immersion of diamond microparticle into clean molten EBiInSn.
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22 Fig. 3. SEM images of (a) EBiInSn-diamond-indium composite before sintering and (b) the enlarged view
23 with (c) EDS image; SEM images of (d) EBiInSn-diamond-indium composite after sintering and (e) the
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25 enlarged view with (f) EDS mapping; (g) the fracture surface of the composite and (h) an enlarged view.
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29 Fig. 4. The thermal conductivities of Bi-In-Sn/diamond composites varied with (a) initial indium particles
30 volume fraction (the diamond was fixed at 30 vol%) and diamond volume fraction: (b) the initial EBiInSn
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was fixed at 50 vol%, (c) the initial indium was fixed at 30%; (d) measured thermal conductivities along with
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33 particle size of diamond at different initial mixing ratios; DSC curves of the Bi-In-Sn/diamond composites:
34 (e) at different initial ratios of EBiInSn and indium particles, (f) influenced after aging; (g) liquidus projection
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36 of the ternary system Bi-In-Sn [26].
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29 Fig. 5. Thermal flux in Bi-In-Sn/diamond composites varied with the volume fraction of diamond particles;
30 (b) comparison between experimental and simulation results; (c) comparison of thermal conductivity with
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Manuscript (word or pdf w/ figures) Click here to view linked References

1 Conflict of interest
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3 The authors declare that they have no conflict of interest.
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Supplementary Material

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Supplementary Material
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