The differential volume change method was devised by the authors. As well known, as-quenched alloys have many vacancies which affect ageing rate. Many researches have been published to clarify the effects of these vacancies, but most of the researches were conducted by means of indirect measuring methods; for example, by an electrical resistance method, etc. Moreover, analyses were not accomplished by small angle X-ray reflection, because atomic number 13 of Al is situated at between numbers of Mg and Si, which are 12 and 14, respectively. In this study, the authors newly devised a direct method capable of measuring volume change due to the variation in number of vacancies.
The volume change was measured by the variation in buoyancy of aluminum alloy specimen immersed in special corrosion-resisting solution. For this purpose, the micro-balance of 1/100mg in accuracy (see Fig. 1) was employed. The balance was set in the room at 20°C for prevening the effects of air convection on either of two pans.
The special corrosion-resisting solution (1ppm of Na
2SiO
3 in pure water) was employed. Although the rate of corrosion was extremely low, aluminum specimens were generally corroded in pure water or city water. The corrosion was ascertained by gas bubbles adhered to the surface of specimen after immersed for 1/2 or 1hr. However, they were not the original adhesion of air before immersion. Against all endeavors to inhibit the corrosion of quenched specimen mentioned above, a very trace of corrosion would not possibly be avoided even under the formation of barrier layer. As a countermeasure, the differential measurement was devised. A quenched piece and an annealed one, having same compositions and same dimension (65×45×3mm), were prepared.
The former piece was for use for ageing test and the latter was for balancing weight.
The change of weight corresponding to the variation in buoyancy due to volume change of the quenched specimen under the above conditions was continuouly measured for 500hr. or more. (A wire of the same composition as that of the quenched specimen was employed for hanging both the specimen and the balancing weight in the solution. The vessel, holding the immersing solution, was placed in a larger vessel of holding water for preventing the temperature change of the solution).
Test results: The differential volume change of Al-1.4% Mg
2Si due to ageing at 20°C is shown in Fig. 3. (For comparison, Fig. 2 and 4 show disappearing of quenched-in vacancies of 99.999% pure aluminum after being quenched from 500°C and of Al-1.4% Mg
2Si after artificially aged at 150°C for 20hr. However, no expansions are observed at initial period of ageing).
In Fig. 6, which shows the analysis of ageing conditions of Al-1.4%Mg
2Si at 20°C, ABCD represents the observed differential volume change due to ageing at 20°C immediately after quenched, and OE represents the supposed vacancy sink line drawn in parallel to the region of BC (that is, the observed curve corresponding to disappearing of vacancies).
OFG, which is obtained by the superposition of ABCD and OE, may show the volume change solely due to clustering of the quenched alloy. OFG is nearly parallel to OHI which shows the observed hardness change due to the ageing.
Proceeding of ageing can be expressed by curves of OFG and OHI, which are in parallel each other, and by volume change (represented by OFG) solely due to clustering.
It is most noticeable that the rapid rate of clustering was in advance of the rate of vacancy disappearing at the initial period of clustering.
In other words, clustering rate is slightly greater than the rate of vacancy disappearing. However, the both rates were equal before the lapse of a long period and the vacancy disappearing at 20°C continues for a long time.
In contrast to the ageing at 20°C, volume expansion due to ageing at
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