CLASS 11 Material Preparation Guide

Class 11: Very Hard Brittle Materials and Cermets

Tungsten carbide microstructure showing typical Class 11 cermet structure

Class 11 groups materials whose defining characteristic is extreme brittleness: they all fail by fracture rather than deformation during preparation, regardless of their actual hardness. The class spans technical glasses (500 HV, amorphous, zero fracture toughness) through cemented carbides and cermets (WC-Co at 1100-1800 HV, TiCN-Ni at 1400-1800 HV) to superabrasives (PCD at 10000+ HV, cBN at 4500 HV). Cemented carbides present the most common challenge: the hard WC grains (1800-2400 HV) sit in a soft cobalt binder (~200 HV), creating severe hardness mismatch that causes binder smearing and carbide pull-out. Superabrasives are harder than almost any polishing abrasive, making material removal extremely slow. Technical glasses have no grain boundaries to arrest crack propagation, so any fracture can run across the entire specimen. Diamond abrasives are mandatory throughout, loads must be minimized, and each material subfamily requires specific preparation adjustments.

Hardness Range
500 HV (technical glasses) to 10000+ HV (polycrystalline diamond); all fail by fracture rather than deformation
Typical Materials
WC-Co Cemented Carbide, TiCN-Ni Cermet, PCD, cBN, Technical Glasses
Preparation Challenge
Fracture Prevention, Binder Smearing, Carbide Retention & Diamond-Only Abrasives

Preparation Characteristics & Challenges

WC-Co cemented carbide microstructure showing carbide grains in cobalt binder

WC-Co cemented carbide, Murakami's etch, 1500X

Despite spanning an enormous hardness range, all Class 11 materials share brittle fracture behavior. Preparation force must be minimized throughout, diamond abrasives are mandatory, and each material subfamily presents distinct challenges from binder smearing in cemented carbides to crack propagation in glasses.

Carbide-Binder Hardness Mismatch

Cemented carbides (WC-Co, TiCN-Ni) combine very hard carbide grains (1800-3200 HV) with a soft metallic binder (cobalt ~200 HV, nickel ~250 HV). The binder grinds and polishes far faster than the carbide, creating relief that leaves carbide grains protruding above the surface. Unsupported carbide edges then chip or pull out during subsequent polishing steps, compounding the damage.

Binder Phase Smearing

The soft cobalt or nickel binder in cemented carbides smears over carbide grain faces during grinding and polishing. This is the single most common preparation artifact in hardmetals: the smeared binder masks the true carbide-binder interface, making grain size measurement and binder mean free path analysis unreliable. Diamond on rigid napless cloths with very light pressure (10-15 N) minimizes smearing.

Carbide & Grain Pull-Out

Excessive grinding force fractures carbide grains free from the binder matrix, leaving voids indistinguishable from real sintering porosity. Once a carbide grain pulls out, the void destabilizes neighboring grains. For pure carbides (WC, TiC) without a binder, entire grains fracture along boundaries. Napped polishing cloths catch grain edges and are the primary cause; napless cloths are mandatory.

Superabrasive Preparation Paradox

Polycrystalline diamond (PCD) and cubic boron nitride (cBN) are harder than almost any abrasive used to prepare them. PCD can only be effectively polished by diamond itself, making material removal rates extremely low. Standard metallographic polishing barely touches these materials. Extended vibratory polishing with fine diamond (1-3 µm) for several hours, or specialized lapping on cast iron plates with diamond paste, is typically required.

Glass Fracture Sensitivity

Technical glasses are amorphous with no grain boundaries to arrest crack propagation. Once a crack initiates during sectioning or grinding, it can run across the entire specimen instantaneously. Extremely slow cutting speeds, gentle clamping with rubber jaws, and starting with finer abrasives (40 µm diamond instead of 75 µm) reduce the risk of catastrophic fracture.

Subsurface Fracture Damage

All Class 11 materials develop subsurface microcracks during grinding. In cemented carbides, these cracks follow the carbide-binder interface and are invisible until Murakami's etch reveals them as apparent microstructural features. Each successive preparation step must remove the damage layer from the previous step, typically requiring removal of 2-3x the previous abrasive size in depth.

Cobalt Oxidation Sensitivity

The cobalt binder in WC-Co cemented carbides oxidizes rapidly when exposed to water-based lubricants, producing dark staining identical to the artifact seen in Class 7 WC-Co thermal spray coatings. Oil-based or alcohol-based diamond suspensions must be used throughout all grinding and polishing steps for cobalt-containing materials.

Class 11 Materials

The following materials are classified as Class 11 (Very Hard Brittle Materials). Click on any material to view its detailed preparation procedures.

Preparation Guide

Recommended Preparation Steps

Sectioning

Diamond wafering blades with very slow feed rates and generous coolant. Clamp with rubber or soft jaws to distribute force and avoid point loading, which initiates fracture in brittle materials. For cemented carbides, standard diamond wafering blades work well. For PCD and cBN, use electroplated diamond blades on a precision saw; abrasive blades are completely ineffective against superabrasives. For glasses, the primary risk is crack propagation from the cut face; use the slowest feed rate available and handle with extreme care.

Mounting

Castable epoxy with vacuum impregnation is required. The epoxy fills microcracks from sectioning and stabilizes carbide grain boundaries during grinding. Never use compression mounting: thermal shock from the heating cycle (150-180°C) cracks glasses and can damage carbide-binder interfaces. For WC-Co cemented carbides, vacuum impregnation fills the porous binder network and supports carbide grains at specimen edges. Add alumina filler to the epoxy for edge retention when surface hardness or coating analysis is needed.

Grinding

Diamond grinding discs exclusively: 75, 40, and 15 µm. Apply very light pressure (10-15 N) because these materials fracture rather than deform under excessive load. For cemented carbides (WC-Co, TiCN-Ni), use oil-based lubricants to prevent cobalt or nickel oxidation staining. For glasses, start at 40 µm (not 75 µm) to minimize initial fracture damage. Rigid, flat grinding surfaces are critical. Each step must fully remove the subsurface damage layer from the previous step before proceeding.

Polishing

Polish with 9 µm diamond on a napless cloth, then 3 µm diamond on a napless cloth, then 1 µm diamond on a napless cloth. Final polish with 0.05 µm colloidal silica for 5-15 minutes. Napless cloths are mandatory for cemented carbides to prevent binder smearing. For PCD and cBN, standard polishing has minimal effect; extended vibratory polishing with 1-3 µm diamond for 2-4 hours, or specialized lapping on cast iron plates with diamond paste, is typically required. For glasses, colloidal silica CMP produces excellent results because the chemical component attacks the amorphous surface.

Etching

Cemented carbides: Murakami's reagent (10 g KOH, 10 g K₃Fe(CN)₆, 100 mL water) at room temperature selectively darkens the WC carbide phase while leaving the Co binder bright; swab 5-10 seconds. For eta phase (W₃Co₃C) detection, use Murakami's at elevated temperature (60-80°C). Dilute aqua regia (3:1 HCl:HNO₃, diluted 1:5 with water) selectively attacks the cobalt binder, revealing carbide grain shape and size for image analysis. PCD grain boundaries can sometimes be revealed by plasma etching in a reactive ion etcher. Technical glasses are evaluated entirely as-polished for inclusions, bubbles, and internal stress (under polarized light with crossed polars).

Quality Verification

No carbide pull-out voids or binder smearing over carbide grain faces

Surface flat with minimal relief between carbide grains and binder phase

No subsurface microcracking visible after Murakami's etch (cemented carbides)

No edge chipping at specimen perimeter or mounting interface

Carbide grain boundaries clearly resolved after etching; glass surfaces free of fracture artifacts