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Development of new gallium cell s. Euromet Project 732, WP 4. Slovak Institute of Metrology J. Ranostaj ( [email protected] ) S. Ďuriš,. Objective: To develop a new generation of cells at the Gallium fixed point. Workpackage 4 Gallium melting point. Pilot Laboratory: SMU - PowerPoint PPT Presentation
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Development of new Development of new gallium cellgallium cellss
Slovak Institute of MetrologyJ. Ranostaj ([email protected] )
S. Ďuriš,
Euromet Project 732, WP 4Euromet Project 732, WP 4
Objective: To develop a new generation of cells at the Gallium fixed point
Pilot Laboratory: SMU SMUParticipants: FE-LMK, METAS, CMI, FE-LMK, METAS, CMI, Cooperating laboratory: VNIIM VNIIM
Workpackage 4Workpackage 4 Gallium melting pointGallium melting point
ReviewReview of up to date of up to date activitiesactivities
Review of WReview of WPP 4 possibilities 4 possibilities
Collection of information related to gallium Collection of information related to gallium fixed point (literature retrieval)fixed point (literature retrieval)
Realization of cellsRealization of cells selection of supplier and purchase of the galliumselection of supplier and purchase of the gallium chemical analysischemical analysis cell designcell design cleaning procedurecleaning procedure filling procedurefilling procedure manufacturing of the cells – under processmanufacturing of the cells – under process
WORKING STEP (WS) DESCRIPTION SK CH SI CZ
1. Collecction of the information
Participating laboratory will prepare and send to the pilot laboratory all relevant information which concerns the work of this WP (e.g. own literature retrieval, relevant publications, references, …)Pilot laboratory will prepare the list of all collected information.
X
2. Design of the call(s) Participating laboratory will prepare they own design of the Ga cell and enclosure. All prepared designs will be discussed in this WP. There is also the possibility to accept two or more designs and to work simultaneously on several designs.
X
3. Production of the cell
3.1 Procure the Ga Selection of the supplier and buying Ga (investment including). X
3.2 Procure the other materials
Selection of the supplier and buying the other materials (investment including).
X
3.3 Analysis of Ga sample(s)
Providing of chemical / isotopical analyses of the Ga (investment including).
X
3.4 Manufacturing of the cell(s)
Arrangement of the manufacturing of the cell components (investment including).
X
3.5 Filling of the cell Filling of the cell (elaborating of the filling method, corresponding equipment design and realization).
X
4. Testing of the cell Preparation of the “testing protocol” for the study the phase transition, parameters of influence …and / or realization of the measurements according to this protocol
X X X X
Review of Review of WWPP 4 4 posibilities posibilities
CCells realizationells realization
GGalliumallium Supplier: CMK, Ltd. Supplier: CMK, Ltd.
(Slovakia)(Slovakia) Charge No.: 2004057 Charge No.: 2004057 Purity: 7NPurity: 7N Quantity: 1.1 KgQuantity: 1.1 Kg
(2x0.5 Kg, 4x0.025 Kg)(2x0.5 Kg, 4x0.025 Kg) Analyze:Analyze:
– GDMS, CMK, Ltd.GDMS, CMK, Ltd.– GDMS, Shiva GDMS, Shiva
Technologies Europe Technologies Europe (France)(France)
Supplier: CMK, Ltd. Supplier: CMK, Ltd. (Slovakia)(Slovakia)
Charge No.: 2006041Charge No.: 2006041 Purity: 7N – MBE GradePurity: 7N – MBE Grade Quantity: 1.1 KgQuantity: 1.1 Kg
(2x0.5 Kg, 4x0.025 Kg)(2x0.5 Kg, 4x0.025 Kg) Analyze:Analyze:
– GDMS, CMK, Ltd.GDMS, CMK, Ltd.– GDMS, Shiva GDMS, Shiva
Technologies Europe Technologies Europe (France)(France)
CMKShiva tech.
EuropeNRC CMK
Shiva tech.
EuropeNRC CMK
Shiva tech.
EuropeNRC CMK
Shiva tech.
EuropeNRC
Li 0.04 0.5 1 Cr 0.3 0.5 0.3 Pd - 1 0.5 Er - 1 -
Be 0.02 0.5 0.8 Mn 0.2 0.5 0.2 Ag 50 50 30 Tm - 1 -
B 0.04 0.5 1 Fe 0.3 0.5 0.5 Cd 8 10 1 Yb - 1 -
C - - - Co 0.1 0.5 0.1 In 0.8 1 0.3 Lu - 1 -
N - - - Ni 0.3 0.5 0.5 Sn 5 1 1 Hf 0.5 1 0.2
O - - - Cu 0.8 0.5 0.5 Sb 1.5 1 0.4 Ta - 500 -
H - - - Zn 1.2 1 1 Te 1.5 1 0.6 W 1 5 0.1
F 5 5 6 Ga Matrix I 0.3 1 0.4 Re - 1 0.2
Na 0.2 1 0.6 Ge 30 30 10 Cs 0.5 1 0.06 Os - 1 0.2
Mg 0.2 0.5 0.7 As 5 1 0.4 Ba 3 1 0.4 Ir - 1 0.3
Al 0.3 0.5 0.4 Se 10 5 5 La 0.5 1 0.3 Pt - 5 0.3
Si 0.4 0.5 0.6 Br 10 1 10 Ce 20 10 10 Au 10 10 5
P 0.5 0.5 0.5 Rb 0.5 1 0.2 Pr - 1 - Hg 5 5 2
S 0.6 1 0.7 Sr 4 1 0.1 Nd - 1 - Tl 0.4 1 0.3
Cl 0.4 1 2 Y 1 1 0.09 Sm - 1 - Pb 0.9 1 1.1
K 6 10 45 Zr 0.2 1 0.1 Eu - 1 - Bi 1.3 1 0.1
Ca 8 5 5 Nb 0.2 1 0.08 Gd - 1 - Th 0.1 0.5 0.04
Sc 0.06 0.5 0.2 Mo 0.8 5 0.5 Tb - 1 - U 0.1 0.5 0.04
Ti 0.08 0.5 0.2 Ru - 1 0.4 Dy - 1 -
V 0.07 0.5 0.1 Rh - 1 0.1 Ho - 1
Detection limits of some GDMS Detection limits of some GDMS analytical laboratories analytical laboratories (ppb wt)(ppb wt)
CMKShiva tech.
EuropeCMK
Shiva tech.Europe
CMKShiva tech.
EuropeCMK
Shiva tech.Europe
Con.Det.limit
Con.Det.limit
Con.Det.limit
Con.Det.limit
Con.Det.limit
Con.Det.limit
Con.Det.limit
Con.Det.liit
Li ND 0.06 ND 0.5 Cr ND 0.1 ND 0.5 Pd - - ND 1 Er - - ND 1
Be ND 0.03 ND 0.5 Mn ND 0.05 ND 0.5 Ag ND 20 ND 50 Tm - - ND 1
B ND 0.05 ND 0.5 Fe 0.3 0.07 ND 0.5 Cd ND 3 ND 10 Yb - - ND 1
C - - - - Co ND 0.03 ND 0.5 In 0.4 0.1 ND 1 Lu - - ND 1
N - - - - Ni ND 0.1 ND 0.5 Sn ND 1.2 ND 1 Hf - - ND 1
O - - - - Cu ND 0.2 ND 0.5 Sb ND 0.3 ND 1 Ta - - ND 500
H - - - - Zn ND 0.4 ND 1 Te ND 0.4 ND 1 W ND 0.1 ND 5
F ND 3 ND 5 Ga Matrix I - - ND 1 Re - - ND 1
Na ND 0.04 ND 1 Ge ND 7 ND 30 Cs - - ND 1 Os - - ND 1
Mg ND 0.04 ND 0.5 As ND 0.5 ND 1 Ba ND 1 ND 1 Ir - - ND 1
Al ND 0.05 ND 0.5 Se ND 5 ND 5 La ND 0.2 ND 1 Pt ND 0.3 ND 5
Si 0.5 0.4 ND 0.5 Br ND 4 ND 5 Ce - - ND 10 Au ND 5 ND 10
P ND 0.1 ND 0.5 Rb - - ND 1 Pr - - ND 1 Hg ND 1 ND 5
S 0.3 0.1 ND 1 Sr - - ND 1 Nd - - ND 1 Tl ND 0.1 ND 1
Cl 2 0.08 ND 1 Y - - ND 1 Sm - - ND 1 Pb ND 0.21 ND 1
K ND 4 ND 10 Zr - - ND 1 Eu - - ND 1 Bi ND 0.5 ND 1
Ca ND 4 ND 5 Nb - - ND 1 Gd - - ND 1 Th ND 0.02 ND 0.5
Sc ND 0.01 ND 0.5 Mo ND 0.1 ND 5 Tb - - ND 1 U ND 0.03 ND 0.5
Ti 0.02 0.01 ND 0.5 Ru - - ND 1 Dy - - ND 1
V ND 0.02 ND 0.5 Rh - - ND 1 Ho - - ND 1
GDMS analysis of Ga 7N GDMS analysis of Ga 7N (ppb wt)(ppb wt)
CMKShiva tech.
EuropeCMK
Shiva tech.Europe
CMKShiva tech.
EuropeCMK
Shiva tech.Europe
Con.Det.limit
Con.Det.limit
Con.Det.limit
Con.Det.limit
Con.Det.limit
Con.Det.limit
Con.Det.limit
Con.Det.liit
Li ND 0.04 ND 0.5 Cr ND 0.2 ND 0.5 Pd - - ND 1 Er - - ND 1
Be ND 0.02 ND 0.5 Mn ND 0.04 ND 0.5 Ag ND 20 ND 50 Tm - - ND 1
B ND 0.08 ND 0.5 Fe ND0.00.077
ND 0.5 Cd ND 3 ND 10 Yb - - ND 1
C - - - - Co ND 0.02 ND 0.5 In ND 0.3 ND 1 Lu - - ND 1
N - - - - Ni ND 0.1 ND 0.5 Sn ND 1.3 ND 1 Hf ND 0.08 ND 1
O - - - - Cu ND 0.3 ND 0.5 Sb ND 0.4 ND 1 Ta - - ND 500
H - - - - Zn ND 0.4 ND 1 Te ND 0.3 ND 1 W ND 0.2 ND 5
F ND 3 ND 5 Ga Matrix I ND 0.1 ND 1 Re - - ND 1
Na ND 0.03 ND 1 Ge ND 7 ND 30 Cs ND 0.1 ND 1 Os - - ND 1
Mg ND 0.04 ND 0.5 As ND 0.5 ND 1 Ba ND 1 ND 1 Ir ND 0.2 ND 1
Al ND 0.05 ND 0.5 Se ND 5 ND 5 La ND 0.2 ND 1 Pt ND 0.2 ND 5
Si 0.5 0.2 ND 0.5 Br ND 4 ND 5 Ce - - ND 10 Au ND 5 ND 10
P ND 0.1 ND 0.5 Rb ND 0.3 ND 1 Pr - - ND 1 Hg ND 1 ND 5
S 0.2 0.1 ND 1 Sr ND 0.5 ND 1 Nd - - ND 1 Tl ND 0.1 ND 1
Cl 0.7 0.08 ND 1 Y ND 0.5 ND 1 Sm - - ND 1 Pb ND 0.2 ND 1
K ND 3 ND 10 Zr ND 0.3 ND 1 Eu - - ND 1 Bi ND 0.5 ND 1
Ca ND 3 ND 5 Nb ND 0.05 ND 1 Gd - - ND 1 Th ND 0.02 ND 0.5
Sc ND 0.01 ND 0.5 Mo ND 0.1 ND 5 Tb - - ND 1 U ND 0.02 ND 0.5
TiND
0.01
ND 0.5 Ru - - ND 1 Dy - - ND 1
V ND 0.01 ND 0.5 Rh - - ND 1 Ho - - ND 1
GDMS analysis of Ga 7N–MBE Grade GDMS analysis of Ga 7N–MBE Grade (ppb (ppb wt)wt)
Design of the cellDesign of the cellss
Cleaning Cleaning of of the containerthe container and and ffilling of the cellsilling of the cells
Cleaning procedure for teflon crucible and capCleaning procedure for teflon crucible and cap– Washing with detergentWashing with detergent
– Rinsing and ultrasonic washing with distilled waterRinsing and ultrasonic washing with distilled water
– Washing with watered-down aqua regiaWashing with watered-down aqua regia
– Rinsing with vapour of redistilled waterRinsing with vapour of redistilled water
– Heating in argon atmosphereHeating in argon atmosphere
Future activitiesFuture activities
Finalization of prototype cells
Comparison of prototype cells with SMU primary standard gallium point cell (used in CCT-K3 and Euromet No.: 552)
Study of gallium phase transition realized by prototype cells
pressure effect on the temperature of phase transition
effect of different method and effect of thermodynamic conditions of realization
effect of preceding freezing
effect of moisture
...
Comparison of gallium point realization by different NMIs
Thank you for your Thank you for your attentionattention