Monday, 22 November 2010

Rheological studies of dental materials: prosthetic materials and dental cements

Introduction

The handling, working and setting times, adhesion, and stability of dental materials are dependant on their rheological properties. The values of these and their measurement are, in turn, affected by the temperature, humidity, the type of rheometer and the geometry of the measuring device[1]

Rheological parameters commonly in use in dental material science are viscosity, loss and storage modulus, the loss tangent, known as tan delta (tan δ), in shear stress and elastic modulus in elongational flow. Measurements of creep strain and creep recovery are recorded for creep.
The values of these can be modified for any particular material by the particle size distribution, powder:liquid ratio, particle shape, density, volume fraction and the use of additives[2,3]. These latter can be particular (e.g. superplasticisers) or liquid (surfactants). Also involved in these controlling parameters are particle deformability and particle/particle interaction (i.e. attraction or repulsion) [4]

Rheology is defined as the study of the deformation and flow of matter[5]
In rheological terms, materials are either Newtonian, where viscosity is not affected by shear stress, or non-Newtonian, where stress produces shear thinning (pseudoplastic) or shear thickening (dilatant) behaviour[2,5].
The terms psuedoplastic and dilatant, used in earlier studies, may be misleading and are no longer used. Most materials used in dentistry are non-Newtonian. Rheological behaviour is often classified into established models e.g Bingham, Crosse, which can be used to predict future behaviour of the material in differing conditions[1]. These models are used by theoretical rheologists, the building industry, food technologists and pharmaceutical industries[4]. They are used infrequently in dental studies.

Material category

The studies included in this review are of prosthetics materials and also various categories of dental cements. This review does not include endodontic materials, adhesives used in restorative dentistry, fluoride gels, fissure sealants, dental waxes or ceramics. These subjects form the basis of separate reviews.


Viscometer / rheometer type


The geometry and type of the measuring device is of great importance as these will have an effect on the measurement results[1]. The apparatus used in these studies range from two glass plates[6,-9], penetrometer[10-14], reciprocating rheometer[10,15-20,7], oscillating plates[21-44,11], capillary extrusion[6,45-51] , rotational spindle[52,53], ram and piston[14], cone and plate[54-74,24,47,48,27,43], parallel plates[71-73,75-80,17, 35,44], concentric cylinder[ 80,81,50,72], compression rheometer[6,82], cup and bob[81,], displacement rheometer[83-85,30], Instron Universal testing machine[72], creep measurement[83,86] and sinusoidal vibration[87,88]. Some studies use a shark fin method[89, 62], a laser/magnet apparatus[90,91], squeeze film technique[92] and an indenter apparatus[93]. Other methods described are a flow point test[94] , flexural vibration[95] , an amalgam condenser [96],a modified ADA test[97], a Gilmore needle with a Zwick1440 mechanical testing machine [98] and custom made capsule extrusion [99]

Temperature and humidity

The values of rheological measurements are affected by both temperature and humidity. In the prosthetic studies, ambient or working temperature varies from 10ºC to 30ºC. Mouth temperature varies between 32ºC and 37ºC and one early study of compo impression material was tested at temperatures of 45, 50 and 60º C. In most of the studies humidity is not stated but in three studies humidity was controlled at 50% RH [10,55,27] and in one humidity was controlled also at 15%[27].
The dental cements were tested for ambient or working temperatures of 5, 8, 18 (62º F), 22, 23, 25 and 26ºC. Mouth and higher temperatures quoted varied from 29ºC and 60 º C. Again humidity is usually not stated. In four studies [34,37,42,69], humidity was controlled at 50%. Four studies were controlled at 100% humidity [66-68, 86]. One study was controlled between 40 – 60% [96] while another was controlled at 90% [98]


Study design and statistical analysis


Very few studies adhere to the concept of hypothesis testing and in many studies it would appear that the sample size was one or not stated. However sample sizes of between 2 and 10 are reported. Statistical analysis was carried out in 49 of a total of 94 studies reviewed. Of these 43 showed some statistically significant results. However only 20 studies reported use of an experimental control, although some stated that the apparatus had been calibrated before the start of experiment.


Main findings of each material type


Impression materials

Rheometers quoted as suitable for measuring impression materials are reciprocating, capillary extrusion, oscillating, extrusion from disposable syringes and micro-fourier squeeze film. It is stated that the ideal setting property of an impression material is a long working time followed by a sharp set at mouth temperature. It has been found that the viscosity during setting is highly dependant on the temperature. Manufacturers’ working times have been rendered inaccurate by some of these studies and clinically relevant shear rates for syringe extrusion have been suggested. It is generally considered that tan delta is a suitable measure for setting characteristics of dental impression materials.

Acrylics and resins

Increased viscosity and therefore reduced doughing time is produced by increase in small particles and aesthetic fibres. Shear thickening and thixotropy have been demonstrated and light cured resins have higher viscosity than rubber based materials. Viscosity increases with time, temperature and rotational speed of the apparatus. There may be an induction time before a certain increase in viscosity is reached and this increase is an exponential function of time.


Soft linings/tissue conditioners


Significant difference in rheology of these materials has been found. Gelation can be controlled by presence of ethyl alcohol and polymer molecular weight. Particle size and molar volume also have effect. High values of tan delta and storage modulus improve masticatory function and in a study on dietary effects, corn oil and heptane produced a rapid reduced compliance.

Adhesives

The viscosity of denture adhesives is in the order of 1000000 poise and is affected by the rate of dilution of saliva.


Dental cements


Unset dental composites exhibit a yield stress and on setting are pseudoplastic (i.e. exhibit shear thinning behaviour) and shear dependant (i.e. non-Newtonian). However one study found that composites were dilatant (i.e. shear thickening) while setting. Polymerization rate of composites depends on constituent particle size. There is much discrepancy in the flow of different brands of composites and this affects their handling properties. As would be expected, flowable composites have greater flow but less mechanical strength and are unsuitable for stress bearing areas. Increased filler content increases viscosity and reduces creep strain.
Glass ionomers show power law behaviour and their viscosity may be associated with polymer cross-linking. Mixing glass ionomer orthodontic cements on a chilled slab increases their working time with no effect on the sharpness of set at mouth temperature. The effect of +-tartaric acid varies with concentration: at medium concentration it prolongs working time and sharpens set. Flow properties can be manipulated by cement formulation but also by the geometry of capsule design.
The viscosity of luting cements is shear rate dependant and dual cure setting greatly reduces the working time. The variation in yield stress of temporary pastes has an effect on their handling properties.
Viscosity of cements is affected more by temperature and geometry than shear rate. It is also affected by particle size distribution. Reduced viscosity and increased strength can be achieved by interparticle fillers.

Discussion

This review demonstrates that there has been extensive rheological studies of prosthetic materials and dental cements but there has been great variation in the aim of the studies, the geometry of the apparatus used and the experimental temperatures. With a few notable exceptions, the importance of humidity has not be known or considered. In some cases, this may be because it was felt that within the confined space of certain devices, humidity was not an important factor. The measurement of relative humidity as a percentage of the total humidity possible is however dependant on barometric pressure and height above sea level.
The actual measurement of humidity would be more accurate although the use of the term absolute humidity is no longer recommended.

Study design

For an experiment to be reproducible, the duration of these rheological tests should be stated, as this could vary across a particular range of shear and might give different results. In some studies, different shear rates are used for different materials, which means that the results for the different materials cannot be accurately compared.
Sometimes more than one rheometer or experimental geometry has been used because of the wide range of viscosity of the experimental materials or lengthy setting times. Most modern stress controlled rheometers have a very wide range, so this should no longer a problem. The amount of material required for each test varies from one device to another and can be a factor in choice of rheometer.
Some studies tested different materials at different temperatures, again rendering the results not accurately comparable.
In many of the studies, not all of the results of the reported experiments have been given, only some being quoted as representative. This leads to incompleteness of the data and reduced measurement quality.

Rheological studies are laboratory based and not clinical. In many of these studies, a clinical application or explanation is suggested. There is often a tendency for this to be subjective and not proven.

Table 3 Rheological studies of dental materials 1966-2008


Conclusion


Rheology is a very useful tool for the study of dental materials and has given much information about the intrinsic nature of materials, their properties and behaviour. Many of these excellent studies could be improved by reducing the number of variables, ensuring an adequate sample size followed by suitable statistical analysis and completeness of data reporting.


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