The white, light-grey and dark-grey phases is Si2Al2Ca, the Si-matrix and fcc Al, respec-tively.
(a)BSE-Image of sample 35-65-24-1 taken at 40x. (b)BSE-Image of sample 35-65-24-1 taken at 200x.
Figure 1:BSE-images of sample 35-65-24-1 taken at (a) 40 x and (b) 200x.
(a)BSE-Image of sample 35-65-24-2 taken at 40x. (b)BSE-Image of sample 35-65-24-2 taken at 200x.
Figure 2:BSE-images of sample 35-65-24-2 taken at (a) 40 x and (b) 200x.
Figure 3:BSE-images of sample 35-65-60-1 taken at (a) 40 x and (b) 200x.
(a)BSE-Image of sample 35-65-60-2 taken at 40x. (b)BSE-Image of sample 35-65-60-2 taken at 200x.
Figure 4:BSE-images of sample 35-65-60-2 taken at (a) 40 x and (b) 200x.
Figure 5:BSE-images of sample 35-65-120-1 taken at (a) 40 x and (b) 200x.
(a)BSE-Image of sample 35-65-120-2 taken at 40x. (b)BSE-Image of sample 35-65-120-2 taken at 200x.
Figure 6:BSE-images of sample 35-65-120-2 taken at (a) 40 x and (b) 200x.
Figure 7:BSE-images of sample 35-65-180-1 taken at (a) 40 x and (b) 200x.
(a)BSE-Image of sample 35-65-180-2 taken at 40x. (b)BSE-Image of sample 35-65-180-2 taken at 200x.
Figure 8:BSE-images of sample 35-65-180-2 taken at (a) 40 x and (b) 200x.
Figure 9:BSE-images of sample 35-65-240-1 taken at (a) 40 x and (b) 200x.
(a)BSE-Image of sample 35-65-240-2 taken at 40x. (b)BSE-Image of sample 35-65-240-2 taken at 200x.
Figure 10:BSE-images of sample 35-65-240-2 taken at (a) 40 x and (b) 200x.
The white, light-grey and dark-grey phase is Si2Ca, Si2Al2Ca, and the Si-matrix, respec-tively.
(a)BSE-Image of sample 45-55-24-1 taken at 40x. (b)BSE-Image of sample 45-55-24-1 taken at 200x.
Figure 11:BSE-images of sample 45-55-24-1 taken at (a) 40 x and (b) 200x.
(a)BSE-Image of sample 45-55-24-2 taken at 40x. (b)BSE-Image of sample 45-55-24-2 taken at 200x.
Figure 12:BSE-images of sample 45-55-24-2 taken at (a) 40 x and (b) 200x.
Figure 13:BSE-images of sample 45-55-60-1 taken at (a) 40 x and (b) 200x.
(a)BSE-Image of sample 45-55-120-1 taken at 40x. (b)BSE-Image of sample 45-55-120-1 taken at 200x.
Figure 14:BSE-images of sample 45-55-120-1 taken at (a) 40 x and (b) 200x.
Figure 15:BSE-images of sample 45-55-180-1 taken at (a) 40 x and (b) 200x.
(a)BSE-Image of sample 45-55-240-1 taken at 40x. (b)BSE-Image of sample 45-55-240-1 taken at 200x.
Figure 16:BSE-images of sample 45-55-240-1 taken at (a) 40 x and (b) 200x.
Figure 17:BSE-images of sample 45-55-240-2 taken at (a) 40 x and (b) 200x.
Area fractions of all phases were done with the threshold function in ImageJ. [71] It was assumed that the area fraction was equal to the volume fraction of the phase. The measured area is the white area in the pictures.
C.1 Binary images: Si-metal equilibrated with 35-65 wt% CaO-Al
2O
3slag
The white phase is the Si2Al2Ca phase and the black phase is the Si-matrix.
(a)Binary image of sample 35-65-24-1 analyzed at 40x.
(b)Binary image of sample 35-65-24-2 analyzed at 40x.
Figure 18:Binary images of samples 35-65-24-1 and 35-65-24-2 (1/1 metal/slag ratio).
(a)Binary image of sample 35-65-60-1 analyzed at 40x.
(b)Binary image of sample 35-65-60-2 analyzed at 40x.
Figure 19:Binary images of samples 35-65-60-1 and 35-65-60-2 (2.5/1 metal/slag ratio).
Figure 20:Binary images of samples 35-65-120-1 and 35-65-120-2 (5/1 metal/slag ratio).
(a)Binary image of sample 35-65-180-1 analyzed at 40x.
(b)Binary image of sample 35-65-180-2 analyzed at 40x.
Figure 21:Binary images of samples 35-65-180-1 and 35-65-180-2 (7.5/1 metal/slag ratio).
The area fraction on the was only calculated for one parallel for the samples 35-65-240, since sample 35-65-240-2 was imaged both with slag and metal.
slag
The area fraction of the phases in the Si metal equilibrated with 45-55 wt% CaO-Al2O3
slag were calculated by first, calculating the total area of the white and light-grey phase, and then calculating the area fraction for only the white phase. Where the white phase is Si2Ca+Si2Al2Ca and the black phase is the Si-matrix. To find the total area fraction of the light-grey phase, the area of the white phase was subtracted from the area of the light-grey phase + the white phase.
(a)Total area of the white and light-grey phase in sample 45-55-24-1. Analyzed at 40x.
(b)Total area of the white phase in sample 45-55-24-1. Analyzed at 40x.
Figure 23:Binary images of sample 35-65-24-1 (1/1 metal/slag ratio).
Figure 24:Binary images of sample 35-65-24-1 (1/1 metal/slag ratio).
(a)Total area of the white and light-grey phase in sample 45-55-60-1. Analyzed at 40x.
(b)Total area of the white phase in sample 45-55-60-1. Analyzed at 40x.
Figure 25:Binary images of sample 45-55-60-1 (2.5/1 metal/slag ratio).
Figure 26:Binary images of sample 45-55-120-1 (5/1 metal/slag ratio).
(a)Total area of the white and light-grey phase in sample 45-55-180-1. Analyzed at 40x.
(b)Total area of the white phase in sample 45-55-180-1. Analyzed at 40x.
Figure 27:Binary images of sample 45-55-180-1 (7.5/1 metal/slag ratio).
Figure 28:Binary images of sample 45-55-240-1 (10/1 metal/slag ratio).
(a)Total area of the white and light-grey phase in sample 45-55-240-2. Analyzed at 40x.
(b)Total area of the white phase in sample 45-55-240-2. Analyzed at 40x.
Figure 29:Binary images of sample 45-55-240-2 (10/1 metal/slag ratio).
Statistical analysis on the EPMA- and area fractions were performed. A confidence inter-val of 95 % was used, with a student t-distribution. All deviations are based on the average from two replicate splits, and the results were 95 % confidence interval are calculated, the results are written as the averaged values plus/minus the deviation. When assuming a normal distribution of the data, the upper and lower confidence limits (UCL and LCL) can be written as:
Where, X¯n is the average value of between to replicate splits, t is found from the t-distribution table, n is the number of observations, αis the chosen confidence interval (0.05), andSnis the standard deviation between the two averaged values.
D.1 Example Calculation
Here, an example calculation of how the 95 % confidence interval was calculated will be shown here. The parameters are for the Si concentration measured by EPMA in the white, mixed phase (Si2Al2Ca) in the Si metal equilibrated with 35-65 wt% CaO-Al2O3slag for samples 35-65-24-1 and 35-65-24-2. One point was analyzed on three random areas of the same phase for each sample.
Table 5: Parameters for calculating a 95 % confidence interval of the amount of Si in the mixed, white phase (Si2Al2Ca) in the Si metal equilibrated with 35-65 wt% CaO-Al2O3 slag for samples 35-65-24-1 and 35-65-24-2.
Analysis number X
1X ¯
1S
1X
2X ¯
2S
21 37.757 37.792 0.046 39.114 39.267 0.120
2 37.857 39.406
3 37.762 39.282
Since there was two parallels analyzed, n=2. The average between the two parallels are 38.53, while the averaged standard deviation is 0.0967. From the t-distribution table, when
slag is 38.53±0.13.
the metal/slag ratios 1/1 and 10/1 will be presented from each series as much of it looks similar.
E.1 Si metal after equilibration with 35-65 wt% CaO-Al
2O
3Slag
Metal slag ratio of 1/1: