CERAMIC MATERIALS
QUALITY CONTROL

In general, during the elaboration, powder forming, processing operations and/or various mechanical, thermal and chemical treatments, the properties and structures of ceramic products are influenced. All these influences lead to metallographic quality controls such as: examinations of porosities, dimensioning, tearing, structures and microstructures, searches for heterogeneities, search for and examination of inclusions and/or impurities, hardness tests, grain size controls, etc.

Obtaining an inspection surface requires a succession of operations, each as important as the next, regardless of the material. These steps are in the following order:

• The removal of the product to be examined (if necessary), called “CUTTING”.
• Standardisation of the geometry of the sample taken (if necessary), called “MOUNTING”.
• Improvement of the surface condition of this sample, called “POLISHING”.
• Characterisation of the sample: microscopic observation (optical or electronic).

=> Each of these steps must be carried out rigorously, otherwise the following steps will not be possible.

The purpose of cutting is to remove a precise section of a product, in order to obtain a suitable surface for inspection, without altering the physico-chemical properties of the ceramic product. In other words, it is essential to avoid heating or any deformation of the metal that could lead to degradation of the material. Cutting is a fundamental step which conditions the further preparation and inspection of parts.

PRESI’s wide range of medium and large capacity cutting and micro-cutting machines can be adapted to any need with regard to cutting precision, sizing or quantity of products to be cut:

All cutting machines are used with a lubricating/cooling liquid composed of a mixture of water and anti-rust additive in order to obtain a clean cut without overheating. The additive also protects the sample and the machine from corrosion.

=> The choice of the cut-off wheel type has to be adequate, in order to avoid cutting failure, or excessive cut-off wheel wear or even breakage. The hardness of the workpiece determines the wheel selection.

Samples can be difficult to handle due to their complex shape, fragility or small size. Mounting makes them easier to handle by standardising their geometry and dimensions.

Achieving good-quality mounting is essential to protect fragile materials and also to achieve good preparation results for polishing and future analysis.
Before mounting, the specimen should be deburred with coarse abrasive paper, for example, to remove any cutting burrs. Cleaning with ethanol (in an ultrasonic tank for even greater efficiency) is also possible. This allows the resin to adhere as well as possible to the sample and thus limits shrinkage (space between the resin and the sample).

If shrinkage persists, it can lead to problems during polishing. Abrasive grains may become lodged in this space and then be released at a later stage, thus creating a risk of pollution for the sample and the polishing surface. In this case, cleaning with an ultrasonic cleaner between each step is recommended.

As ceramic materials are fragile, the hot mounting process is not possible because the pressures exerted are too high and could therefore damage the samples. In such cases, the cold mounting process is to be preferred. Some complex geometries also require cold mounting to allow the resin to impregnate the specimen as well as possible. This type of mounting is also preferred if a large number of parts are to be mounted in series.

The cold process can be used with:

Cold resins do not always provide a flat mounting “back” because of the meniscus of the liquid resin. Before any polishing operation, a brief step using abrasive paper will remove this menis- cus. The important thing is to ensure that this operation renders the two sides of the mounting parallel.

To meet user needs, PRESI offers a full range of cold mounting moulds.
The cold process has different mounting moulds with diameters from 20-50mm. These are divided into several types: optimised moulds called “KM2.0”, rubber, Teflon or polyethylene moulds. Cold mounting is also more flexible, hence the existence of rectangular moulds for more specific needs.

The last and crucial phase in the sample preparation process is polishing. The principle is simple, each step uses a finer abrasive than the previous one. The aim is to obtain a flat surface and to eliminate scratches and residual defects that would hinder the performance of metallographic control examinations such as microscopic analysis, hardness tests, microstructure or dimensional inspections.

PRESI offers a wide range of manual and automatic polishing machines, with a wide choice of accessories, to cover all needs, from pre-polishing to super-finishing and polishing of single or series samples.

The MINITECH range of manual polishers incorporates the most advanced technologies. User-friendly, reliable and robust, they provide a simple answer to all needs.

The MECATECH range of automatic polishers allows both manual and automatic polishing. With its advanced technologies, motor power from 750-1500 W, all the PRESI experience is concentrated in this very complete range. Whatever the sample number or size, MECATECH guarantees optimal polishing.

All the polishing ranges below are given for automatic sample preparation (for manual polishing: do not take into account the parameters at the top). They are the most commonly used and are given for information and advice.

All the first steps of each range are called “levelling” and consist of removing material quickly to level the surface of the sample (and resin). Those given below are standard and can therefore be modified as required.

Applied pressures vary according to sample size, but in general the following applies: 1daN per 10mm mounting diameter for the pre-polishing steps (ex: Ø40mm = 4 daN) then reduce force by 0.5daN at each polishing step with an abrasive suspension.

Polishing range N°2 includes supports and suspensions that offer an alternative to those used in Polishing range N°1.

All the polishing ranges listed above are standard and versatile ranges that can be modified according to the subtleties of the samples. (Cf Lab’Notes of the material concerned).
Moreover, they are not necessarily to be carried out in their entirety; observations will define needs (except for titanium samples for which all the steps of the range must be performed).

At the end of this preparation phase, the polished samples can be directly observed without metallographic etching. Otherwise, metallographic etching allows differences in relief and/or colour to be made between the different components and so allows them to be observed. It is mainly used on metals (see Lab’Notes on the material concerned).

All micrographs presented were produced using PRESI VIEW software: