Search

The gel point is the lowest solids content at which a fibre suspension forms a continuously connected network and is related to the fibre aspect ratio. In this paper we firstly investigated the conditions required to accurately measure a gel point using sedimentation. We found that very heavily treated cellulose nanofibres can produce anomalous sedimentation data, due to the electrostatic repulsion from fibre surface charges dominating the gravity driven sedimentation. Screening the anionic surface charges by adding high levels of Na+ or Ca2+ ions reduced the electrostatic interactions between the fibres and allowed them to settle normally. Gel point measurement was then used to probe the development of nanofibre quality with increasing energy input for three different feedstocks: eucalypt kraft pulp, commercial microfibrillated cellulose and de-lignified, bleached spinifex pulp. By combining the data of the aspect ratio and average diameter, determined from SEM and TEM, we were able to compare the differences in feedstock processability. The aspect ratio of all three feedstocks increased with increasing homogenisation energy, showing that the fibre delamination dominated over fibre shortening. The slope of the aspect ratio versus energy consumption showed the ease of processing of each sample. The spinifex fibres had the fastest rate of aspect ratio increase and therefore were the most processable. Gel point is an excellent tool to track quality development of nanocellulose through processing and to compare the potential of different feedstocks for nanocellulose production.

Cellulose nanofibre aspect ratio controls the properties of sheets made from nanofibres and processing conditions, but aspect ratio is very difficult to measure. In this paper, aspect ratio was estimated from the gel point of a cellulose nanofibre suspension, the solids concentration at which the transition from a dilute to a semi-dilute suspension occurs. Four batches of cellulose nanofibres were tested. Two were produced from softwood fibres using ball milling. Commercially produced microfibrillated cellulose material was also used, both in as supplied form and after removal of the larger fibres by filtering. The average diameter measured from SEM images of fibres ranged from 33 to 73 nm. One sample was too heavily treated and an average dimension could not be measured. The gel-point was measured both from the height of a layer of cellulose nanofibres sedimented from a dilute suspension or from the lowest solids concentration at which a yield stress could be measured using a vane rheometer. The two methods were closely in agreement for all samples. Aspect ratio was then calculated using either the effective medium (EMT) or crowding number (CN) theories. Aspect ratio calculated with an assumed fibre density of 1,500 kg/m3, using the CN theory ranged from 155 to 60. Use of the EMT theory reduced the calculated aspect ratio by between 11 and 23 %. Reducing the assumed density in suspension from 1,500 to 1,166 kg/m3 reduced the calculated aspect ratio by 12–14 %. The heavily treated sample had by far the lowest aspect ratio.