A practical challenge in slicing of low-cost multi-crystalline silicon (mc-Si) wafers by the fixed abrasive diamond wire sawing process is increased wire consumption due to greater wear of the diamond compared to slicing of the more expensive mono-crystalline silicon (mono-Si) wafers. In this paper, we present the results of scribing of mc-Si and mono-Si materials with two conical tip diamond indenters of the same geometry to understand the possible reasons for increased diamond wear in cutting of multi-crystalline silicon. Specifically, the scribing forces and the diamond indenter wear produced in scribing of the two silicon materials are analyzed. The results show that the forces generated in scribing of mc-Si are higher than in scribing of mono-Si. The higher forces in scribing of mc-Si are consistent with the corresponding higher tip radius of curvature (due to wear) of the diamond indenter compared to the tip radius produced in scribing of mono-Si. Scanning electron microscopy and confocal microscopy of the diamond indenters show that wear is primarily due to physical micro-fracture and blunting of the diamond. Raman spectroscopy shows evidence of stress-induced phase transformation of the diamond and the formation of compressive residual stress in the diamond. Plausible physical reasons, including the role of material inhomogeneity in mc-Si, for the wear of diamond during scribing are given.

Crystalline silicon solar cells offer an optimum mix of modularity, distributed grid, and lower capital investment compared to other renewable and clean energy sources.1 However, the cost of energy per kWh from photovoltaic solar cells is still high compared to conventional energy resources. Cost can be reduced by using multi-crystalline silicon (mc-Si) for the silicon wafer substrates, which is cheaper than mono-crystalline silicon (mono-Si).2–4 The reduction in energy conversion efficiency of mc-Si (compared to mono-Si) is offset by the lower substrate cost for many applications.2 However, there are challenges in manufacturing mc-Si wafers by the state-of-the-art fixed abrasive diamond wire sawing (DWS) process.

In recent years, industry has transitioned from conventional loose abrasive slurry sawing (LAS) to fixed abrasive diamond wire sawing (DWS) for slicing silicon wafers because of the higher productivity, lower kerf loss, and reduced environmental impact of the DWS process.5,6 Material removal in DWS occurs via mechanical interaction of the diamond abrasives (∼10 μm in size) bonded to the steel wire by electroplated Ni with the silicon brick.7 While the use of DWS to slice mono-Si wafers is quite widespread in industry, it is not widely used to slice mc-Si wafers. The primary reason for this is the higher consumption of the more expensive diamond wire when slicing mc-Si than in slicing of mono-Si. It has been reported that more new wire has to be continuously fed into the active cutting zone in diamond wire sawing of mc-Si to ensure cutting effectiveness and to prevent wire breakage and resulting loss of productivity.8 This suggests that wear of the diamond wire is greater when cutting mc-Si than when cutting mono-Si. This is likely due to the differences in material properties of mono- and mc-Si. Multi-crystalline silicon is characterized by greater material inhomogeneity compared to the more uniform mono-Si material, and this inhomogeneity is expected to influence the wear behavior of diamond abrasives.3,9–15

Prior work on the wear of diamond wire in slicing of mono-crystalline silicon shows that it is characterized by blunting, brittle fracture, and pull-out of diamond grits from the electroplated nickel coating on the stainless steel wire.7 During initiation of the cutting process, “break-in” of the diamond occurs.16 Limited evidence of graphitization of diamond attributed to the high stresses acting on the diamond wire when slicing mono-Si has been reported.17 Wear of diamond due to tribologically induced phase transformation has been reported.18 Wire dynamics and spooling of the wire can also scratch the electroplated nickel coating, which can be prevented by recently developed wire spooling solutions.19 Based on the wire sawing conditions used, researchers have shown reduction in the diamond density with increase in contact length.20 Studies of single crystal diamond tool wear in machining (turning) of semiconductor grade mono-Si material show that gradual wear of the single crystal diamond tool occurs in ductile mode cutting while micro-chipping of the diamond occurs in brittle mode cutting.21 Wear of diamond during die separation of microelectronics MEMS devices has been also reported.22 The crystallographic orientation of single crystal diamond tools is known to influence the wear of diamond tools, as seen in prior studies of diamond turning,23 and in scratching with diamond tools of specific crystallographic orientations.24 However, the crystal orientations of diamond grits in a fixed abrasive diamond wire are not controlled, especially since the grits are produced by milling of natural or synthetic diamond. Molecular Dynamics (MD) simulations of scratching of a softer material such as silica have shown the wear of diamond to be due to the breaking of C-C bonds,25 which is attributed to mechano-chemical mechanisms of wear. Wear of a diamond AFM tip when sliding on softer silicon has been reported.26 In nanoscale cutting of silicon wafers by diamond turning, XPS analysis of the cut grooves revealed the formation of silicon carbide and diamond-like carbon particles with corresponding scratching and grooving wear of the diamond tool.27 MD simulations of single point diamond turning of silicon also suggested the formation of silicon carbide.28 However, Raman spectroscopy of abrasive grits used in the diamond wire sawing of silicon has not shown any evidence of silicon carbide formation.17 

The existing knowledge of diamond wear in scribing and diamond turning of silicon is not adequate to explain the higher wire consumption in fixed abrasive diamond wire sawing of mc-Si compared to sawing of mono-Si. Hence, an investigation of diamond wire wear in scribing of mc-Si is needed.

This paper analyzes the wear of a diamond indenter in scribing of mc-Si through constant depth of cut scribing experiments. For comparison, scribing experiments on mono-Si material are also analyzed. In Sec. II, the experimental details of the study are presented. This is followed by the results and discussion. The paper concludes with a summary of the key findings.

Mono- and mc-Si blocks (25 mm × 10 mm × 10 mm) with mirror polished (0.054 ± 0.015 μm) parallel and flat surfaces were used as substrates in the diamond scribing experiments. Scribing experiments serve as lab-scale models of the actual diamond wire sawing process, which slices silicon through a mix of ductile and brittle material removal mechanisms.5,29,30 To compare the wear of diamond due to differences in the structure and properties of mono- and mc-Si, we used two 120° included angle diamond tipped conical indenters (J&M Diamond Tools) with nominally identical geometries. The cone angles of the indenters used are representative of the actual abrasives in the fixed abrasive diamond wire.10 

All scribes were 20 mm in length and were made under dry ambient conditions at a constant depth of 10 μm and a scribing speed of 100 mm/min [Fig. 1(a)]. Since the focus of the paper is on understanding the effect of the material (mc-Si versus mono-Si) on diamond wear, the scribing speed was not varied. The silicon blocks were fixed to a flat aluminum baseplate bolted to a three-component piezoelectric force dynamometer (Kistler 9256C), which was mounted on a computer-controlled X-Y-Z motion platform (Aerotech ANT-4V) [Fig. 1(b)]. The force dynamometer detected the initial contact of the scriber tip with the silicon surface, and measured the instantaneous X-Y-Z forces produced during scribing.

We inspected the diamond indenters in a confocal microscope (Olympus LEXT), which was used to measure the radius of curvature of the indenter tip at regular intervals during scribing. The diamond indenters were imaged using a scanning electron microscope (Hitachi 8230 SEM). Each indenter was imaged after scribing distances of 0 mm (new), 140 mm, 200 mm, 260 mm, and 320 mm. Care was taken to ensure that the same face of the indenter was used to generate the entire scribe, and this same face was inspected. Raman spectroscopy was performed on the diamond tips using a Thermo Fischer Raman spectrometer to detect stress-induced phase transformation and graphitization during the scribing process. The excitation wavelength of the laser in the Raman spectrometer was 785 nm with a surface penetration of ∼0.5–0.6 μm, estimated spot size of 1.6 μm, and a spatial resolution of ∼1 μm, which is smaller than the radius of curvature of the diamond tips. An objective of 50× was used to collect data, with scans from 736 to 1790 cm−1. The Raman laser's exposure time was 5 s, with 5 sample exposures used to average the data for each point investigated.

A comparison of the average resultant force obtained in each scribe produced in the two materials is presented first, followed by analysis of the observed diamond indenter wear behavior.

The average resultant force for mc-Si and mono-Si is shown as a function of the distance scribed in Fig. 2(a). It can be seen that the average resultant force for mc-Si is almost always higher than for mono-Si. Figure 2(b) shows a box plot of the measured resultant force for the two materials. It can be seen that scatter is larger for mc-Si than for mono-Si, which is indicative of the greater inhomogeneity in material properties of mc-Si due to the presence of grain and twin boundaries, and inclusions.3 While fluctuations in the instantaneous scribing force (not shown here) coincide with some of the grain boundaries crossed by the scribes, the confounding effect of brittle fracture, which results in the removal of chunks of silicon with corresponding steep drops in the scribing force, masks the effect of the grain boundaries. This makes it difficult to distinguish clearly between the force fluctuations due to brittle fracture and those due to grain boundaries. However, prior works on ductile mode scribing9,31 have presented evidence of such correlations. The median force for mc-Si is also higher than for mono-Si for the same scribing conditions. The differences in the average scribing forces are attributed to differences in the material properties of mono- and mc-Si.32 

The surface morphologies of the diamond indenters after scribing mc-Si and mono-Si for the specified distances are shown in Fig. 3. In the following, for convenience, we refer to the indenter used to scribe mc-Si as the “mc-Si tool” and the indenter used to scribe mono-Si as the “mono-Si tool.” It can be seen in Figs. 3(b) and 3(f) that after scribing for 140 mm both mc-Si and mono-Si tools show evidence of wear. The mc-Si tool [Fig. 3(b)] shows clear evidence of blunting of the tip as well as the formation of a trench produced by micro-fracture and located below the tip. The mono-Si tool shows less pronounced tip rounding than the mc-Si tool. Evidence of micro-fracture, while present in the mono-Si tool as well, is more scattered. After 200 mm of scribing, the mc-Si tool surface shows growth of the trench, which now extends from the left to the right of the indenter face [Fig. 3(c)]. The mono-Si tool shows fractured ridges appearing on two sides of the tool as seen in Fig. 3(g). While the increases in tip radii and micro-fracture of the scribing surfaces of the two tools are not that pronounced in going from 200 mm to 260 mm of scribing, they are more evident after 320 mm of scribing (see Fig. 4). Figure 4 also shows the different types of diamond fracture evident in the morphologies of the micro-fractured surfaces of the diamond tools. Two types of micro-morphologies are exhibited by the diamond surfaces—the mc-Si tool shows a typical cleavage fracture with hackly (jagged) fractures and a ridged pattern in the trench, while the fractured surface pattern in the upper part of the mono-Si tool is consistent with the “river pattern” reported by Lawn33 and Hull.34 Both tools showed the hackly fracture pattern on the diamond faces contacting the silicon.

Figure 5 shows the change in radius of curvature of the tips of the mc-Si and mono-Si tools as a function of scribing distance. The error bars plotted represent one standard deviation of ten measurements made with the scriber. It is clear from the trend lines in the figure that while the tip radii increase with scribing distance (wear) for both tools, the rate of wear is higher for the mc-Si tool compared to the mono-Si tool. This further confirms the qualitative observations of tip blunting seen in the SEM images of Fig. 3. The change in the radius of curvature of the indenter tips is due to the cumulative effect of micro-fracture of the diamond tips.

We used Raman spectroscopy to investigate possible graphitization and any change in the internal stress state of the diamond tools due to scribing. The Raman spectra for both tools before scribing (Fig. 6) showed the T2g peak of diamond centered at 1332 cm−1. This peak is related to the T2g symmetric vibration of the sp3 carbon bond.35 The Raman measurements were repeated at several points on each indenter face prior to scribing and no evidence of graphite was found in the two tools. Therefore, any peak shift observed after scribing can be attributed to the effect of the scribing process.

After scribing for 320 mm, the diamond peak in the Raman spectra exhibited shifts from the 1332 cm−1 peak of diamond17 to peaks at 1334.4 cm−1 for the mc-Si tool and 1334 cm−1 for the mono-Si tool. The classic D band peak for graphitic carbon is typically observed around 1350 cm−1 depending on the laser power used.36,37 The D band in disordered carbon systems is known to be produced by defects in graphite, whereas the G band (around 1580 cm−1) in graphitic materials is due to the E2g Raman active mode for sp2 hybridized carbon.38 The D band spectra can be influenced by the surrounding zone of the diamond phase, which is at 1332 cm−1. Any shift in the Raman spectra can be attributed to the formation of nano-crystalline graphite phase,39 which can form under high stress, as suggested by Yang et al.17 Moreover, the peak shift could also be attributed to residual stress introduced in the diamond by the scribing process.40,41 For phase transformation to occur, a combination of hydrostatic stress and shear stress is required.40 Prior research shows that a shear stress of 95 GPa is required for graphitization to occur.42 Evidently, our experiments did not produce such high shear stresses. However, as suggested by Yang et al.,17 in actual diamond wire sawing, repeated interactions of the abrasive with the silicon can create a cumulative effect, giving rise to sufficiently high shear stresses that can cause graphitization.

The Raman spectra for both mc-Si and mono-Si tools showed a positive shift in the diamond T2g peak, which implies compressive residual stresses generated by the scribing process.43 To quantify the residual stress in the diamond tools, we used Hemley's model44 given by the following equation, which is valid for non-hydrostatic conditions, where vd is the peak location (cm−1) and P is the pressure in GPa:

vd=1332.6+1.294P0.0062P2.

Using the above model, we obtained the residual stress to be 1.087 GPa for mono-Si and 1.400 GPa for mc-Si. We use another model adapted from Gogotsi et al.40 for calculating the residual stress from the maximum shift of the diamond band (13 cm−1), which corresponds to a compressive residual stress of 8 GPa (1.625 cm−1/GPa). This model yielded residual stresses of 1.18 GPa and 1.47 GPa for mono-Si and mc-Si, respectively. The positive shift was found to occur each time the spectra were collected (6 measurements for each diamond indenter). The residual stresses signify that under combined loading of hydrostatic and shear stresses (during scribing) the diamond indenters undergo phase transformation, which gives rise to the residual stress. Figure 2 shows the resultant scribing force detected by the piezoelectric force dynamometer attached to the silicon block. Since equal and opposite forces act on the indenter, the scribing force, which is a result of the interaction of the indenter surface with silicon, is responsible for deforming the diamond, which gives rise to the compressive residual stress.

Several mechanisms have been hypothesized for diamond wear, with the predominant wear mechanism depending on the cutting conditions. As seen in prior research on ultraprecision diamond turning,21,23,27 diamond (groove) wear can occur (1) due to mechanical abrasion from hard particles such as inclusions in the multi-crystalline silicon material, (2) due to adhesion at the high pressure micro-scale contact between silicon and diamond, and (3) due to diffusion of carbon from the diamond to silicon based on mechano-chemical effects. Mechanisms of mechanical (non-thermal) wear of abrasive bonded grinding wheels include (1) attritious wear (wear flat development),45 (2) micro-fracture, (3) macro-fracture, and (4) pull-out and loss of abrasives.46,47 Our scribing results suggest that wear of the diamond abrasive is primarily by mechanical abrasion resulting in micro-fracture of the diamond. In our experiments, the high localized stresses in the micro-scale contact region cause micro-fracture and chipping of the diamond. Our micro-fracture patterns are similar to those reported by Lawn et al. and Hull et al.,33,34 and more recently in work on diamond scratching of tantalum-tungsten (Ta12W) high hardness (3 GPa) alloy.24 For multi-crystalline silicon, the scribing forces are higher due to the grain/twin boundaries and inhomogeneity in the local material properties in comparison to mono-crystalline silicon. Comparing the hardness of silicon [9–12 GPa (Refs. 48 and 49)] to the hardness of silicon carbide [20–30 GPa (Ref. 50)] and silicon nitride [20–35 GPa (Ref. 51)] multi-crystalline silicon with carbide and nitride impurities is expected to produce higher cutting forces in DWS, as confirmed by our scribing results. Assuming a similar area of contact of the indenters used to scribe mono- and mc-Si, diamond wire sawing of mc-Si is expected to be characterized by higher applied stress, which can cause phase transformation and greater wear of the diamond abrasives.

Zong et al.'s XPS measurements on the mono-Si surface produced by ductile mode machining in diamond turning showed evidence of silicon carbide (SiC),27 which was explained by the diffusion of carbon atoms from diamond to silicon. This experimental observation was also predicted by MD simulations, which yielded sp3-sp2 disorder of diamond.28 However, our XPS measurements did not find any evidence of SiC in either the silicon grooves or on the surface of the diamond indenters, which agrees with the results of prior work.17 There are two possible reasons for lack of SiC formation in our tests. First, unlike in diamond turning, our scratches are characterized by brittle fracture, which hinders the carbon diffusion mechanism responsible for SiC formation.27 Second, the tool-workpiece contact length in diamond turning is much larger (∼kilometers), and is therefore difficult to replicate in our scratching tests.

The increase in forces in the single grit scribing experiments on mc-Si can be translated to diamond wire sawing, where the increased forces can delaminate or pull-out the diamond grits. Grit loss would lead to the sawing forces being distributed on even fewer grits in the cutting zone in the kerf, leading to even more increased force on grit, and the silicon, thus increased wear of the diamond wire, or worse causing wire breakage and stalling production. Increased force per grit would also lead to deeper micro-cracks in the sawn wafers,7 which can lower the manufacturing yield of wafers. The wear rate of diamond when cutting multi-crystalline silicon by diamond wire sawing can be reduced by engineering the silicon ingot to lower its impurity and inclusion content and by reducing the number of grain/twin boundaries. This would also improve the electrical properties of the mc-Si solar cells produced using the sliced substrates. Future work will consider these aspects.

The paper investigated the wear of diamond in scribing of multi-crystalline silicon with the aim of understanding the underlying reasons for increased wire consumption in diamond wire sawing of multi-crystalline silicon wafers. The results were compared with those obtained in scribing of mono-Si material. The scribing results showed that the scribing forces for mc-Si are higher than for mono-Si, reflecting the influence of localized defects in mc-Si such as grain and twin boundaries, and inclusions. Results showed micro-fracture of the contacting face of the diamond tips and a higher rate of increase in the radius of curvature of the diamond tip when scribing mc-Si. Although no evidence of graphitization of the diamond indenters was found, the residual stress detected in the diamond indenters suggests that some phase transformation took place.

The authors acknowledge the support of the National Science Foundation (CMMI Grant No. #1538293) and the Saint-Gobain Northboro Research and Development Center. Parts of the work reported in the paper were performed at the Georgia Tech Institute for Electronics and Nanotechnology (IEN), a member of the National Nanotechnology Coordinated Infrastructure, which is supported by the National Science Foundation (Grant No. ECCS-1542174). The first author acknowledges helpful discussions on material characterization with Rebhadevi Monikandan, Eric Woods, Todd Walters, David Tavakoli, and Walter Henderson of the Georgia Tech IEN Materials Characterization Facility (MCF).

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