IND61 METROSION - NPL

IND61 METROSION Metrology to enable high

temperature erosion testing

1

Deliverable Number

3.4.1 Lead Partner PTB

Deliverable Title

Measurement of erodent particles to determine size and size distribution

Contractual Delivery Date

Nov 14 Deliverable type

Data

Actual Delivery Date

Nov 14 Contributors PTB, RSE, BAM

Deliverable Details

In order to measure size and size distribution of erodents, three different methods have been applied and compared. The first was done by RSE by means of a light scattering method (e.g. Malvern FPIA 3000). Such a device analyses a projected 2D-image of the erodents to determine its size. The erodents are oriented (by means of a special flow mechanism) to give its largest area. The calculated size of the erodent is the area-equivalent diameter. RSE analysed the erodents Silica angular, EPRI Alumina, Metrosion Alumina and Fly Ash. The second method was based on an optical measurement, done by NPL. Here a digital image was taken from a set of particles with a microscope. After binarizing the image the area was measured by pixel counting and the area-equivalent diameter calculated. This was done for EPRI Alumina as well as for Metrosion Alumina. The third method was by means of an x-ray computed tomography. To this end the same type of erodents have been embedded in a resin and measured with a Nikon XT H 225 ST, with a voxel edge length of about 3.2 µm. Additionally a sample of Chromia erodents has been measured with a synchrotron CT (BessyII, Berlin, Germany) by BAM. The voxel edge length here was about 0.9 µm. The volume data were then analysed with the program VG Studio Max 2.2.4 (Modul ‘Defect detection’). Since the CT measurement provides volume data, a size determination based on the volume-equivalent diameter has been calculated. In addition a Feret diameter (termed ‘size’) was measured for each erodent and an area-equivalent diameter was calculated. The latter, however, was not always the largest area, but randomly distributed. DTU developed a setup for measuring simultaneously the particle velocity and size, which is based on an LED imaging system. The results are shown in the attached documents.

20 m

m

� Preparation of erodents

Task 3.4: Particle Size, Size Distribution and Sha pe

Ch. Rothleitner, U. Neuschaefer-Rube - METROSION Meeting, Risø, 25-26 Nov, 2014 15

Silicaangular

AluminaEPRI

AluminaMetrosion

Fly Ash

(heat shrink tube and PMMA glue)

20 m

m

� Measured with Nikon XT H 225 ST

� Voxel edge length 3.2 µm

� Data analysis with VG Studio Max (‚Defect detection‘)



Silicaangular

AluminaEPRI

AluminaMetrosion

Fly Ash

Task 3.4: Particle Size, Size Distribution and Sha pe Silica angular

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#particles:


xA=(127.83 ± 1.11) µmxV=(111.94± 0.96) µm

Volume equivalent diameter Area equivalent diameter

Onlyvolumes > 64 voxels

Voxel edgelength 3.2 µm

#particles: 1720

Task 3.4: Particle Size, Size Distribution and Sha peEPRI Alumina

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319

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µmµm


xV=(39.80 ± 0.05) µm xA=(46.10 ± 0.07) µm




14,4

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105,

82

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518

,87

21,8

024

,73

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630

,59

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236

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742

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348

,16

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954

,02

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459

,87

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065

,73

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6

µmµm

#particles: 17619



Metrosion Alumina

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,23

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126,

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15,8

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,98

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086

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xA=(105.96 ± 0.71) µmxV=(85.78 ± 0.52) µm



#particles: 2230



Fly Ash

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µmµm

#particles:



xA=(24.71 ± 0.20) µmxV=(26.27 ± 0.16) µm



#particles: 4684


Chromia• Measured with Synchrotron CT

(BESSY2) by BAM• Voxel edge length 0.876 µm• Defect detection with VG Studio Max• Contains approx. 700 particles


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und …

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Chromia

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xA=(42.64 ± 0.64) µmxV=(38.38 ± 0.55) µm

200 µm Voxel edgelength 0.876 µm

#particles: 697

Silicaangular

EPRI Alumina

Metrosion Alumina

Fly Ash Chromia

µm µm µm µm µm

Volume-equivalentdiameter, x V

Mean / µm 111,94 39,80 85,78 24,71 38,38

Stdev / µm 40,01 5,99 24,46 10,97 14,42

Sterr / µm 0,96 0,05 0,52 0,16 0,55

Area-equivalentdiameter, x A

Mean / µm 127,83 46,10 105,96 26,27 42,64

Stdev / µm 46,21 9,40 33,47 13,88 16,86

Sterr / µm 1,11 0,07 0,71 0,20 0,64



‚SizeX‘ Mean / µm 140,23 52,12 115,70 31,91 48,26

Stdev / µm 52,17 14,99 45,39 17,42 21,10

Sterr / µm 1,26 0,11 0,96 0,25 0,80

RSE Mean / µm 153,53 52,00 122,77 32,31

Stdev / µm

Sterr / µm

Voxel edgelength

3,2 µm 3,2 µm 3,2 µm 3,2 µm 0,9 µm

Erodent Particles – Alumina Optical Size Measurement

Particles are thresholded to obtain binary images of each particle.

The number of pixels in each particle are then counted up and then a centre of mass is calculated and the radius of the circle that encloses the same area as the particle is calculated. calculated.

The perimeter of the particle is then unwrapped and the local curvature is calculated at every point around the entire perimeter.

The curvature plot of all protruding sections is then integrated into a single number and multiplied by the estimated mass of the particle in order to obtain a “Weighted Factor” which is expected to be proportional to its potential to damage a surface when it impinges upon it..

Erodent

Light Scattering MethodX-ray Computed

TomographyOptical Analysis

d(0.1), µm d(0.5), µm d(0.9), µm Particle Size, µmEquivalent

Radius, µm

Equivalent

Diameter, µm

METROSION

Alumina78 123 191 100 73 146

EPRI Alumina 33 52 81 48 28 56

Size and Velocity

2 pulses Δt=1µs in the same frame

FOV size measurement area 3.24 x 2.41 mm

2 pulses Δt=1µs in 2 separate frame

Documents

IND61 METROSION - NPL