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DryLyte® Technology is an effective surface finish technique, which follows the same traditional electrolytic cell principle, but uses an electrolytic solid non-conductive medium rather than a liquid one. For the last 10 years, this technology has been attracting a lot of attention compared to conventional ones due to the selective smoothing of the surface technique, interacting only with the roughness peaks and not with the valleys, etc. In this book’s chapter, for 3D-printed cemented carbides (WC-Co) polished with DryLyte® Technology, it is shown the correlation between the microstructure and the surface integrity, in terms of mechanical properties, at submicrometric length scale. Also, a particular case study is presented of 3D-printed WC-Co as a function of the testing temperature, ranging from room temperature up to service-like working conditions. Finally, the mechanical properties are correlated as function of the chemical nature and/or crystallographic phase.
*Address all correspondence to: jj.roa@gpainnova.com
1. Introduction
The tribological and mechanical behavior of a tool under service-like working conditions depends not only on intrinsic properties of the constitutive phases but also on the material surface and subsurface properties—such as topography and residual stress state. During the last 10 years, extensive research has been dedicated to investigating the relation between chemistry, microstructure, and the resulting mechanical properties [1, 2, 3]. In addition to those bulk-related features, surface characteristics are also crucial in determining the functional response of a given material. Commonly, materials used for structural components are shaped into final dimensions and geometry changed as the material goes through different surface modification processes as mechanical working operations, material removal methods, heat treatment, and other finishing practices.
In this regard, surface alterations and/or modifications become critical in controlling the properties and performance of final products, particularly if service conditions involve contact loading (e.g., wear, impact, fatigue, etc.) and/or environmental (e.g., corrosion, oxidation, etc.) interaction.
In the case of manufacturing stages involving material removal (e.g., grinding, lapping, etc.), a complex surface interaction exists between the tool and workpiece. In this sense, the temperature near the surface increases which could produce microstructural changes, including oxidation and also possible local melting at the surface level. Furthermore, plastic deformation, tearing, and fracture also occur. For all the aforementioned information, mechanical and thermal changes at the surface level take place along thermal stages which may induce relevant residual stresses [4].
The existence of a pronounced influence of manufacturing methods on mechanical properties and service performance, as a result of the type of surface produced, is well-establish. Within this framework, the concept of surface integrity in terms of roughness has been introduced as a key parameter. In this sense, the surface integrity, which contained not only the geometry consideration, including surface roughness and accuracy, but also other microstructural aspects at the surface and/or subsurface level.
Within this framework, this topic demands synergic interdisciplinary expertise in different fields: materials science, machining and shaping technology, as well as surface integrity in terms of mechanical properties [5, 6].
Ceramic/metallic materials and in particular the WC-Co cemented carbides (also known as hardmetals), are the key materials for tooling industry. These materials present an excellent combination of properties (e.g., hardness, strength, fracture toughness, wear, and abrasion resistance) [7, 8, 9, 10, 11, 12]. Hardmetal tools are produced through a powder metallurgical (PM) route, where mixed WC and Co powders are sintered at high temperatures to consolidate the composite material [4, 13]. WC-Co grades are classified according to their Co content and WC grain size. The proportion of WC phase is generally between 70 and 97% of the total weight of the composite and its grain size averages between 0.4 and 10 μm. This range of cemented carbides can be subdivided into its major application area as described below [14, 15]:
Nano, ultrafine, and submicron grades, with a metallic Co binder content in the range of 3–10 wt.% and WC grain size below 1 μm. WC-Co grades are widely used in a wide range of wear part applications as well as cutting tools designed, where the resulting tool needs high strength, wear resistance and sharp cutting edges are essential under service-like working conditions.
Fine and medium grades, with a metallic Co binder ranging between 6 and 30 wt. % and WC grain size ranging between 1 and 3 μm. WC-Co material is used mainly in wear parts and cutting tools is employed in applications where strength and shock resistance is required.
Medium coarse, coarse, and extra coarse grades, with a metallic Co binder content ranging between 6 and 15 wt.% and a WC grain size above 3 μm. WC-Co grades are employed in oil and gas, and mining applications in which resistance to high impact and abrasive wear is required.
However, during the last decade 10 years, the Additive Manufacturing (AM) routes are gaining more importance in this field. However, due to the complex shapes as well as closed cavities, conventional post-processing routes do not give out the desired quality in terms of surface finish.
2. Surface modification techniques on WC-Co grades
In the production of conventional WC-Co components, it is occasionally necessary to carry out a number of shaping operations before final sintering. Green compacts can then be produced in simple shapes, such as rectangular and round blanks, by means of conventional methods, such as turning, drilling, and grinding.
After sintering, the corresponding blank has achieved its fully density and final mechanical properties, and it is ready to be dispatched. In this regard, most blanks need to be further post-processed in order to get the desired shape, size, flatness, and surface finish by using the traditional post-processing routes on WC-Co grades; being the most common techniques: diamond wheel grinding, diamond lapping, and grinding and electrical discharge machining (EDM) [16]. All these traditional post-processing technologies will be briefly described in Section 2.1.
During the post-processing process, two aspects need to be taken into account: (a) the functionality of the machined workpiece and (b) the economic efficiency. According to different applications, the functionality of the workpiece after the post-processing process can be divided into different groups as follows [17]:
Mechanical functions, defined as the capability of carrying mechanical loads; even monotonically and/or cyclically.
Thermal functions, considering the heat resistance and/or conductivity as a function of the testing temperature.
Tribological functions, defined as the surface interaction with other media
Flow functions, which consider the influence on the flow of fluids.
Each of the aforementioned steps in a manufacturing chain influences the workpiece properties, which directly link to its functionality. Along this chapter of the book, we will focus attention to changes induced at the surface level changing the resulting roughness. In particular, the traditional post-processing techniques will be briefly explained (see Section 2.1) and in particular compared with a disruptive dry-electropolished technology (see Section 2.2) focusing the attention to these technologies on WC-Co AM specimens.
2.1 Traditional polishing techniques
The main requirements which lead to use post-processing routes on WC-Co cemented carbides are:
to reduce superficial roughness
to keep geometry and preserve the specimen tolerances
to polish complex shapes
to reduce the polishing times.
The most widely employed post-processing techniques on WC-Co cemented carbides are:
Diamond wheel grinding contains abrasive compounds for grinding and abrasive machining operation. The wheels generally are made with composite material. This consists of coarse-particle aggregate pressed and bonded together by a cementing matrix to form a solid, circular shape. Grinding wheels are consumables, although the life span can vary widely depending on the use case, from less than a day to man years. Mainly, the abrasive aggregate is selected primarily according to the hardness of the material being cured.
Lapping also known as mechanical lapping, is widely applied in diamond polishing for its simple process, low cost, and high efficiency [18]. This technique consists on a machining process in which two surfaces are rubbed together with an abrasive between them, by hand movement or using a machine. This technique often follows other subtractive processes with more aggressive material removal as a first step, such as milling and/or grinding. Lapping can take two forms: (a) traditionally often called grinding, which involves rubbing a brittle material, producing a microscopic conchoidal fractures as the abrasive rolls about between the two surfaces and removes material from both and (b) involves a softer material such as pitch or a ceramic for the lap, which is charged with the abrasive. The lap is then used for finishing of WC-Co cutting tools, have proven to be economical for this typology of materials.
Grinding is virtually unchallenged for machining of materials which, due to their extreme hardness or brittleness, cannot be efficiently shaped by other methods. In the particular case of study, machining is almost exclusively dependent on this process [19, 20]. This post-processing technique is a representative abrasive process in which a grinding wheel is used. These wheels are composed of two materials—tiny abrasive particles called grains and a softer bonding agent to hold the countless grits together in a solid mass. During this process, each protruding abrasive grain interacts with the workpiece surface and a local stress field upon each contact point causes irreversible material deformation in the form of dislocation, cracks, and voids [21].
EDM is a post-processing technique, which is increasingly used on WC-Co suppliers. This is a thermal process where a workpiece electrode is shaped through the action of a succession of discrete electrical discharges which local erode (melt or vaporize) the material surface. Mainly, this technology is used for close tolerances [10].
Mainly, the most common post-processing technology to process the workpieces of WC-Co is the grinding (Figure 1a) and EDM process (Figure 1b), as shown in the SEM micrographs presented on Figure 1.
Figure 1.
Scanning electron microscopy (SEM) micrographs of the microstructural quality for WC-Co post-processed by (a) grinding and (b) EDM technologies.
After that, it is necessary to reduce the surface roughness induced by these techniques by using chemo-mechanical process and/or chemical polishing process until the WC-Co cemented carbides workpieces present a precise dimension and shape that fulfill requirements in real applications [22, 23, 24, 25]. However, the media used to reduce the surface roughness induced by the ground and chemo-mechanical polishing process can induce localized leaching at the metallic Co binder as shown in Figure 2a. As reported in Refs. [26, 27, 28], when the pH media is below 7, the media induces a galvanic couple, where the ceramic reinforcement particles (WC) act as the cathode while the metallic Co binder as an anode. Thus, the potential difference between both parts generates a microgalvanic couples that induce a corrosion effect generating a difference in height between both constitutive phases of around 100 nm as shown in Figure 2b. This difference in height may produce a reduction of the workpiece under service-like working conditions.
Figure 2.
Scanning electron microscopy (SEM) micrographs of the microstructural quality for the WC-Co chemo-mechanical polished. (a) Surface micrograph and (b) focused ion beam (FIB)—cross section showing the leaching induced (painted in red in the SEM micrograph) between both constitutive phases.
From all the aforementioned information, the conventional post-processing techniques present some drawbacks for the WC-Co workpieces when these have been superficially treated by a ground and/or EDM process. Furthermore, these drawbacks are more evident when the geometry of the specimens’ have complex shapes. In this sense, the AM specimens cannot be post-processed using conventional techniques as these technologies do not lead to the final workpiece:
(1) keep the geometry and preserve the tolerances and
(2) be able to polish complex shapes in a short polishing time.
For all the aforementioned information, recently the DryLyte® Technology increases their applicability in the market.
2.2 DryLyte® technology
This technology was developed to overcome the limitations of classic polishing technologies (e.g., mechanical process, chemo-mechanical process, electropolishing, etc.). In this sense, DryLyte® (contraction of the words dry- and electrolyte) Technology is based on a dry-electrolyte and dry-suspension electrolyte made up of an ionic exchange resin.
In this sense, the structural characteristics, together with the functional group’s nature and degree of the resin, has an important effect on its exchange-ion behavior. Morphologically, they can be classified as macroreticular or gel-type resins and macroreticular or macroporous resins:
Macroporous resins have stable macropores in the dry state and to fabricate them, a minimum of around 10% cross-link degree is required. Their appearance is opaque. The beads have a porous multi-channeled structure which provides them with a high effective surface area. Nonetheless, they are more fragile than gel-type resins as reported in [29].
Gel-type resins are a three-dimensional (3D) swollen structure with a solvent evenly dispersed through it. When the solvent is removed, the gel shrinks and its porosity is not appreciable in the dry state. This type of resins presents heterogeneous micropores (ranging between 0.7 and 2 nm) and a cross-link degree between 4 and 10%. Visually, they have a translucid aspect [30].
The electrolyte presents a multi-modal particle size distribution (see Figure 3a) with an interconnected porous microstructure (see Figure 3b) and is chemically constituted of PolyStyrene DiVinylBenzene (PS-DVB). In this sense, the electrolyte particles are arranged in such a way that they make electrical contact with the negative pole of the power supply (cathode) and with the metal part to be polished (anode), generating a close circuit as schematically depicted in Figure 3b.
Figure 3.
(a) SEM micrograph of the PS-DVB electrolyte showing a multi-modal particle size distribution; (b) SEM magnification micrograph showing the internal porosity; and (c) schematic representation of how the electricity passes through the PS-DVB particles during the dry-electropolishing process.
From all the aforementioned information, unlike traditional polishing systems, DryLyte® Technology achieves a uniform surface finish, avoiding surface marks patterns such as those generated by machining, and it is able to process complex geometries without generating micro-scratches on the surfaces, preserving the edges of complex geometries as the one produced by AM routes. Furthermore, this technology leads to polish close cavities by using internal cathodes. This is the main advantage to employ this technology to polish AM specimens in comparison with the traditional post-processing routes.
As it does not generate any polishing and/or surface modification texture (e.g., grinding patterns, etc.), this technology improves surface integrity in terms of mechanical properties (e.g., fatigue and wear) and chemical properties (e.g., corrosion resistance, aging, etc.). In this sense, along the entire chapter, this technology will be applied to ceramic/metal samples and in particular, to WC-Co cemented carbides produced by AM routes.
AM technologies process has emerged as an alternative to traditional manufacturing process that can fabricate very complicated geometries with high efficiency and reduce post-processing [31, 32, 33, 34, 35, 36, 37].
AM technology is increasingly considered as a key manufacturing technology of tomorrow’s society due to the fact, it makes possible the production of complex near-set shaped parts which are not feasible with conventional technologies (e.g., PM and/or subtractive). With this bottom-up approach, material is added layer-by-layer where necessary and the complex shape obtained. This technology offers several advantages, like:
greater design freedom compared to conventional routes.
the possibility of creating close cavities and/or channels to reduce the density and optimize the cooling process, respectively.
the possibility of saving on raw material consumption.
to reduce the production time.
no need of using customized tools.
From all these advantages, AM technology is being employed in many industries, like biomedical [38] and electronic [39] ones, as well as within scientific fields, such as mechanical devices [40, 41], periodic microstructures [42], and ceramics [43]. In this regard, the increasing interest in this technology is driven by its ability to produce custom devices, its simplicity and speed.
During the last 10 years, the AM of WC-Co has been the subject of several research efforts, and it is still in an early stage of development. AM technologies offer attractive advantages in terms of producing WC-Co hardmetal cutting tools with complex geometries, such as U-shaped or helical cooling channels inside. These internal, contour-adapted cooling channels allow higher cutting speeds and, consequently, a remarkable increase in the productivity of the machining process. The main AM technologies suitable for metal are selective laser melting (SLM), selective electron beam melting (SEBM), laser powder deposition, binder jet AM (BJAM), and wire arc AM (WAAM) [44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54]. So far, AM technologies have been successfully applied to stainless steels [55, 56, 57, 58, 59], Ni alloys [60, 61], Ti alloys [62, 63], refractory metals [64, 65], Al alloys [66, 67], etc.
For WC-Co, it remains very challenging to use AM due to its very high melting temperature. SLM and BJAM are the most attempted AM processes for manufacturing WC-Co hardmetals. Besides, a few studies on SEBM [46], 3D gel-printing (3DGP) [68], and fused filament fabrication (FFF) [69] of WC-Co hardmetal samples were deeply investigated.
The AM techniques used for fabrication of WC-Co hardmetals and the main research groups working on WC-Co AM were summarized in Tables 1 and 2.
AM process
Other names
Advantages
Disadvantages
SLM
Laser powder bed fusion, L-PBF
(1) High dimensional accuracy (2) High geometric freedom (3) Less performing steps (4) High hardness
(1) High residual stress (2) Uneven microstructure (3) Carbon loss (4) Evaporation of metallic Co binder
SEBM
Electron beam powder bed fusion, E-PBF
(1) High dimensional accuracy (2) High geometric freedom (3) Less performing steps (4) High hardness (5) High scan speed
(1) High residual stress (2) Uneven microstructure (3) Expensive equipment (4) Needs vacuum to avoid the oxidation of the metallic Co binder
Institute for Materials Applications in Mechanical Engineering RWTH Aachen University/Germany
2023
Table 2.
State of the art of the AM techniques used for printing WC-Co hardmetals.
3.2 Can the DryLyte® technology act as a post-processing technique for the AM specimens?
However, laser-based AM technologies for manufacturing WC-Co hardmetals have encountered several issues as thermally induced cracks, heterogeneous microstructures, and embrittlement due to the formation of undesirable phases [71, 126]. On the other hand, sinter-based AM technologies offer the highest potential to process complex WC-Co parts with properties similar to commercial grades [127]. For these techniques, at this point in time limitations are found in regard to layer deposition quality, part size, and batch size. Recently, solved on granules 3D-Printing (SG-3DP) has been successfully used to process fully dense WC-Co complex parts. In this chapter, the feasibility to polish SG-3DP by means of the DryLyte® Technology with lower Co content is explored. This technique consists in spreading powder-binder granules produced by a spry-drier technique (see Figure 4a) which were deposited layer-by-layer. Figure 4b shows the WC-Co granules microstructure where low Co content is clearly visible. As it is shown in Figure 4c by using the SG-3DP technology a drill bit head was printed with a thickness layer of around 74 μm as determined by using the Confocal Scanning Laser Microscopy, CSLM (see Figure 4d). As it is clearly evidenced in the SEM and CLSM micrographs, the sintered drill bit produced by the AM technology, presents a complex shape with high roughness values. To reduce the roughness of this complex specimen is not possible using conventional post-processing technology as the AM specimen will not preserve the desired geometry. In this sense, by using the DryLyte® Technology, it is possible to reduce considerably the superficial average roughness (Sa) until reaching a value of around 20 nm as shown in Figure 4e. This Sa reduction implies a roughness reduction of around 33% of the initial roughness.
Figure 4.
(a) Low SEM micrograph of the WC-Co sintered granules; (b) high-magnification SEM micrograph showing the internal part of the sintered WC-Co granules where it is evident the low amount of metallic Co content; (c) 3DP WC-Co drill bit head; (d) confocal laser scanning microscopy (CLSM) 3D reconstruction of the AM WC-Co drill bit investigated [40]; and (e) SEM micrograph after being polished by using the DryLyte® Technology [128].
After using the post-processing technologies, it is possible to superficially change the mechanical integrity in terms of hardness and elastic modulus. In this sense, preliminary results highlight that the surface mechanical integrity for the WC-Co specimens polished with DryLyte® Technology remains constant [128, 129] and equals as the once reported in the literature after being polished using conventional post-processing techniques [2]. Then, by using the DryLyte® technology leads to polish complex shapes processing from the AM routes keeping constant the mechanical surface integrity at the superficial level.
The conventional post-processing techniques do not lead to homogeneously polish the AM specimens due to the fact these techniques do not keep constant the geometry, preserve tolerances, etc.
DryLyte® Technology presents several advantages compared with the conventional post-processing techniques as it allows to homogeneously polish complex specimens. Keeping constant the surface integrity in terms of mechanical properties under service-like working conditions.
The authors are grateful to HILTI AG (Schaan, Liechtenstein) to provide us with the different samples investigated here. Furthermore, the authors are also grateful to Zeppelin 3D methodology company (especially to Javier Ledesma and María Gil) and the Centro de Fabricacción Avanzada Aeronáutica (especially to Guillermo González) to conduct the 3D measurements by using the InfiniteFocus G5 plus from Bruker Alicona. Finally, G.R. acknowledges the Ministerio de Ciencia e Innovación for the industrial PhD (Grant number: DIN2021-011846).
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Written By
Guiomar Riu Perdrix and Joan Josep Roa Rovira
Submitted: 01 December 2022Reviewed: 30 January 2023Published: 04 March 2023
Open access peer-reviewed chapter
