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Diamond Composites J Mater Sci (2018) 53:15514–15529 CompositesCOMPOSITES Microstructural characterization and quantitative analysis of the interfacial carbides in Al(Si)/diamond composites Christian Edtmaier1,* , Jakob Segl1 , Erwin Rosenberg1 , Gerhard Liedl2 , Robert Pospichal2 , and Andreas Steiger-Thirsfeld3 1 Institute of Chemical Technologies and Analytics, TU Wien, Getreidemarkt 9/164, 1060 Vienna, Austria 2 Institute of Production Engineering and Laser Technology, TU Wien, Vienna, Austria 3 USTEM - University Service Centre for Transmission Electron Microscopy, TU Wien, Vienna, Austria Received: 27 April 2018 ABSTRACT Accepted: 23 July 2018 The existence of interfacial carbides is a well-known phenomenon in Al/dia- Published online: mond composites, although quantitative analyses are not described so far. The 30 July 2018 control of the formation of interfacial carbides while processing Al(Si)/diamond composites is of vital interest as a degradation of thermophysical properties Ó The Author(s) 2018 appears upon excessive formation. Analytical quantification was performed by GC–MS measurements of gaseous species released upon dissolving the matrix and interfacial reaction products in aqueous NaOH solutions and the CH4/N2 ratio of the evolving reaction gases can be used for quantification. Although the formation of interfacial carbides is significantly suppressed by adding Si to Al, also a decline in composite thermal conductivity is observed in particular with increasing contact time between the liquid metal and the diamond particles during gas pressure infiltration. Furthermore, surface termination of diamond particles positively affects composite thermal conductivity as oxygenated dia- mond surfaces will result in an increase in composite thermal conductivity compared to hydrogenated ones. In order to understand the mechanisms responsible for all impacts on the thermal conductivity and thermal conduc- tance behaviour, the metal/diamond interface was electrochemical etched and characterized by SEM. Selected specimens were also cut by an ultrashort pulsed laser system to characterize interfacial layers at the virgin cross section in the reactive system Al/diamond. Address correspondence to E-mail: [email protected] https://doi.org/10.1007/s10853-018-2734-1 J Mater Sci (2018) 53:15514–15529 15515 Introduction squeeze casting, a decrease in composite thermal conductivity is observed [6, 8]. Monolithic materials cover a wide range of combi- In order to monitor the formation of Al4C3 during nations of coefficient of thermal expansion (CTE) and infiltration, a method first employed by Simancik thermal conductivity (TC); however, the required et al. [9] for the quantification of Al4C3 by mass- combination of highest thermal conductivity and spectrometric coupled gas chromatography tech- lowest CTE is virtually not occupied. The most nique (GC–MS) can be applied. This routine is based promising class of materials to reach thermal con- on the simple context, that Al4C3 releases CH4 upon ductivity beyond that of copper or silver are metal dissolving in aqueous media (Eq. 1). By measuring matrix composites (MMCs) containing diamonds. the CH4 amount in relation to the amount of N2, used Although these materials have received some interest as an internal standard, the Al4C3 content can be since the early 1990s, most are still at scientific level, determined through prior calibration. only very few companies commercialized such Al4C3 þ 12 H2O þ 4NaOH 4 NaAlðÞ OH 4 þ 3CH4 " products. ð1Þ Unfortunately, the diamond/metal contacts have a finite interface thermal conductance (ITC, or TBC, One less exploited aspect concerns the role of sur- thermal boundary conductance). Even if perfect face termination of diamond surfaces by oxygenation mechanical bonding is achieved at the interface, or hydrogenation on the Kapitza resistance and intrinsic interface thermal resistance (ITR) arises due subsequently on the thermophysical properties of to the scattering of phonons and electrons when diamond MMCs [10–14]. From a scientific perspec- travelling between materials with different elasticity tive, it is essential to understand how this interface and dielectric constants. The presence of limited heat has to be designed in order to minimize the Kapitza flow across interfaces resulted in a high quantity of resistance and to improve ITC. So far, the role of scientific investigations to improve bonding between surface termination of diamond surfaces on ITC was matrix and inclusion phases and therefore heat mainly shown on ‘‘clean-model’’ systems, i.e. well- transfer across the interface that may give access to defined plain and large synthetic diamond mono- an overall improved thermal conductivity of the crystal surfaces with sputtered layers of Al and other composites. metals creating a carbide-forming interlayer. The ITC Most of the work to improve ITC concerns the is then calculated by means of TDTR time-domain introduction of carbide-forming elements to form thermoreflectance experimental setup [10, 11, 15]. In stronger chemical and physical bonds at the interface [14] the positive influence of oxygenation on ITC was [1–6], which is especially of importance for matrix for the first time shown to be true in the low (4 K) to systems like copper and silver, which are both known ambient temperature range for a Ag3Si/diamond not to wet and bond to carbon allotropes. In case of system, fabricated under typical ‘‘messier’’ lab-scale aluminium as matrix metal, the formation of carbides conditions of gas pressure infiltration using synthetic like Al4C3 is well documented [7]. However, exces- diamond particles. Note, that different terminations sive formation of Al4C3 is undesirable, as it has low of diamond surfaces can be created by acid and thermal conductivity and readily corrodes in moist plasma treatments, respectively, and can result in the air to form aluminas, such as Al(OH)3. It is further- formation of different proportions of COOH, C–O, 2 3 more commonly accepted that Al4C3 formation can C=O, C sp and C sp bonding types depending on be controlled by alloying Al with Si because of the applied chemicals and processes [10, 16, 17]. competitive formation of SiC and by the limitation of In the present work the influence of the contact solubility of carbon in liquid aluminium which time (i.e. the time between the liquid and the dia- results in reduced capability to form Al4C3 at given monds during the gas pressure infiltration process) temperatures, respectively [6]. It is furthermore on the thermal conductivity, the amount of Al4C3 notable that a minimum concentration of Al4C3 at the formed and the interfacial structure of the resulting interface is essential to enhance thermal transport, as MMCs are studied. Furthermore, the influence of the at very low concentration or even total absence of addition of Si as an alloying element on the afore- carbides, i.e. caused by rapid consolidation like mentioned characteristics will be observed. As men- tioned above, the aspect of surface termination of 15516 J Mater Sci (2018) 53:15514–15529 diamond surfaces by oxygenation or hydrogenation diamonds) and the infiltrated bodies were furnace is of interest for understanding thermal transport at cooled under pressurized condition within less than the interface, thus, it is of interest to study its impact 20 min to room temperature. After cool down, com- on Al4C3 formation in dependence of process posite pieces were dismantled from the die. This fast parameters like contact time and amount of Si in Al. cooling process guarantees a rather precise determi- nation of the contact time, however, it may also cause the system to be not in thermal equilibrium, for Experimental procedure which reason composites were subsequently annealed at 573 K for 1 h in Argon atmosphere. The Diamond/metal composites were produced by liquid diamond volume fraction was determined by den- metal infiltration of Al, Al0.5Si, Al1Si and Al3Si sitometry to be 64 ± 1 vol.- pct for all MMCs. This is matrix materials into a tapped and vibrated powder in good agreement with the relative densities of up to bed of synthetic diamond grit of mesh sizes 70/80. 99.5 pct., indicating that the composite samples were The synthetic diamonds were of the SDB1125 type fully infiltrated and contained little, if any, porosity. from E6 and purchased by ServSix GmbH, Karlstein, Thermal conductivity measurements were per- Germany. The Al–Si matrix alloys were inductively formed in a steady-state heat flow equipment close to melted and cast using 3N8 Al and 4N Si base ele- ambient temperature. The thermal conductivity was ments. The different Si concentrations in Al were determined by the temperature gradients in the serial properly selected due to the fact, that Al0.5Si repre- arrangement of the sample and a reference. The sent an alloy of very low solubility of Si in the a-Al, gradient is established by a heating and a cooling thus Si may be dissolved in the lattice or will form circuit anchored between one side of the serial fine precipitates while cooling to ambient. Whereas in arrangement of the sample and the other side of the the Al1Si and Al3Si system, Si is formed—in different reference. Sample size is a rod of 8 mm diameter and weight fractions—by the eutectic reaction during an overall length of about 33 mm. The temperature solidification. evolution along the sample length L is controlled by Furthermore, the diamond particles were surface means of Pt100 sensors. Experimental errors origi- treated to create H- and O-termination, respectively. nating from the determination of the geometrical To create H-termination on the diamond surfaces, the cross sections and active length of the given sample as-received diamond powders were placed in a fur- geometry may cause systematic errors. As a conse- nace at 1123 K in H gas atmosphere for 60 min. 2 quence, the composite thermal conductivity jc can O-termination was realized by immersing diamonds become uncertain. Based on simultaneous measure- in hot sulphuric acid for a period of 5 min, subse- ments of the thermal and the electrical conductivity quently rinsed with de-ionized water and 2-propanol of the matrix alloy alone, and taking into account and finally dried at 383 K.
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