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Rheological study of Pla2num Group Metals aggrega2on in a glass melt DE LA RECHERCHE LINDUSTRIE Norma Maria Pereira Machado Muriel Neyret (CEA Marcoule), Philippe Marchal and Cecile Lemaitre (Universit de Lorraine) September 2019

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SLIDE 1

October 17, 2019

Commissariat à l’énergie atomique et aux énergies alterna=ves

Norma Maria Pereira Machado

DE LA RECHERCHE À L’INDUSTRIE

Commissariat à l’énergie atomique et aux énergies alterna=ves - www.cea.fr

Rheological study of Pla2num Group Metals aggrega2on in a glass melt

September 2019

Norma Maria Pereira Machado Muriel Neyret (CEA Marcoule), Philippe Marchal and Cecile Lemaitre (Université de Lorraine)

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SLIDE 2

October 17, 2019

Commissariat à l’énergie atomique et aux énergies alterna=ves

Norma Maria Pereira Machado

Introduc2on

2

u LDMC – Laboratory for the study and

development of condi2oning matrices, part

  • f the service responsible for vitrifica=on

studies and high temperatures processes

u Responsible for the design, formula2on,

development and characteriza2on of matrices for waste condi2oning

u Installa=ons operate in a non-radioac2ve

environment

CEA Marcoule - LDMC

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SLIDE 3

October 17, 2019

Commissariat à l’énergie atomique et aux énergies alterna=ves

Norma Maria Pereira Machado

Content

3

  • 1. Context
  • 2. Main goals
  • 3. Methodology
  • 4. Perspec2ves
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SLIDE 4

October 17, 2019

Commissariat à l’énergie atomique et aux énergies alterna=ves

Norma Maria Pereira Machado

Context

4

Nuclear Waste Condi2oning

Fission Product

Cold crucible

u A frozen glass layer, called self-crucible, is

formed which creates a thermal and electrical insula2on barrier between the crucible and the melt, preven2ng as well from the corrosive effect of the melt

u Calcina2on u Mel2ng thanks to induced currents in the

crucible (Hot Crucible) or in the glass (Cold Crucible) Hot Crucible

u Induc2on hea2ng oven which transfers its heat to the

glass bath

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SLIDE 5

October 17, 2019

Commissariat à l’énergie atomique et aux énergies alterna=ves

Norma Maria Pereira Machado

Context

5

u High level waste are confined in a borosilicate glass matrix (R7T7)

Nuclear waste in France

Chemical composi2on : borosilicate glass (R7T7 glass)

wt% Min. wt% Max. SiO2 42.4 51.7 Al2O3 3.6 6.6 B2O3 12.4 16.5 Na2O 8.1 11.0 FP* + Act* + NM + ZrO2 4.2 18.5 RuO2 + Pd + Rh 3.0

PGE *FP: Fission Products; Act: ac=nides

u Pla2num metal group (PGM) par2cles are almost

insoluble in the glass leading to modifica2ons in the glass proper2es 10 µm

PGM PARTICLES: Pd-Te beads ( few µm) RuO2 needle shape par2cles(10-20µm)

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SLIDE 6

October 17, 2019

Commissariat à l’énergie atomique et aux énergies alterna=ves

Norma Maria Pereira Machado

Context

6

PGM par2cles influence in the rheological behavior

u The glass with PGM par2cles has a shear-thinning behavior u Low shear:

  • Presence of aggregates
  • Aggregate size and viscosity of glass increases with temperature

and PGM content

u High shear:

  • S=rring destroys aggregates (individual par=cles)
  • Viscosity of glass decreases with temperature and increases with

the content of PGM

Viscosity of a simulated glass containing 4,2%wt of PGM par=cles, for different values

  • f temperature, as a func=on the shear stress
  • C. Hanotin, J. Puig, M. Neyret, P. Marchal, Platinum group metal particles aggregation in nuclear glass

melts under the effect of temperature, Journal of Nuclear Materials 477, 2016

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SLIDE 7

October 17, 2019

Commissariat à l’énergie atomique et aux énergies alterna=ves

Norma Maria Pereira Machado

Context

7

Phenomenological modelling

u Rheological behavior modelling

  • η=f( , T, ​𝝌↓

𝝌↓𝟏 )

  • Main parameters: Shear rate, Temperature, PGM content

Viscosity of simulated glass containing different PGM content at 1200°C, as a func=on the shear rate

γ

  • C. Hanotin, J. Puig, M. Neyret, P. Marchal, Platinum group metal particles aggregation in nuclear glass

melts under the effect of temperature, Journal of Nuclear Materials 477, 2016

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SLIDE 8

October 17, 2019

Commissariat à l’énergie atomique et aux énergies alterna=ves

Norma Maria Pereira Machado

Context

8

Aggrega2on Criteria

u Aggrega2on of PGM par2cles highlighted by rheological

measurements for the following criteria:

Viscosity of a simulated glass containing different PGM content at 1200°C, as a func=on the shear rate

| PAGE 8

Viscosity of a simulated glass containing different PGM content as a func=on of temperature

  • C. Hanotin, J. Puig, M. Neyret, P. Marchal, Platinum group metal particles aggregation in

nuclear glass melts under the effect of temperature, Journal of Nuclear Materials 477, 2016

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SLIDE 9

October 17, 2019

Commissariat à l’énergie atomique et aux énergies alterna=ves

Norma Maria Pereira Machado

Main Goals

9

u Op2mize the model’s parameters u Extend the domain of the proposed model u Analyze the impact of the composi2on of the

glass

  • 1. Consolida2on of the rheological model

u Establish the aggrega2on kine2cs of the PGM

par=cles

u Propose a model es2ma2ng the size of the

aggregates

  • 2. Proposi2on of a PGM par2cles aggrega2on model

u Calculate and measure sedimenta2on rates as a func=on of aggregate size and other influen=al parameters

  • 3. Establish a rela2on with sedimenta2on
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SLIDE 10

October 17, 2019

Commissariat à l’énergie atomique et aux énergies alterna=ves

Norma Maria Pereira Machado

Methodology

10

u Improve the rheological measurement protocol

  • Iden=fy the equipment’s limits
  • Characterize the measurement reproducibility

u Viscosity analyses as func2on of 2me

  • PGM content impact
  • Temperature impact

u Modeling integra2ng 2me

  • Support on simula=on of thixotropic fluids (GEMICO)

u Tes2ng of new parameters thermo-hydraulic simula2on studies of the glass bath

Consolida2on of the rheological model



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SLIDE 11

October 17, 2019

Commissariat à l’énergie atomique et aux énergies alterna=ves

Norma Maria Pereira Machado

Methodology

11

  • A. Glass Approch (high temperature)

u Development of an experimental protocol u Experimental tests with glass u Mathema2cal model

  • B. Model suspension Approch (lower temperature)

u Rheological tests on model suspensions → iden2fy a representa2ve suspension u Different characteriza2on tests for concentra2on analyses at lower temperatures

  • RMN +Rheo (LEMTA)
  • Laser 3D (Ins=tute de Physique de Nice)
  • Ultrasounds (CEA)

Proposi2on of a PGM par2cles aggrega2on model

‚

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SLIDE 12

October 17, 2019

Commissariat à l’énergie atomique et aux énergies alterna=ves

Norma Maria Pereira Machado

Methodology

12

u Development of an experimental protocol u Experimental tests with glass u Mathema2cal model

Establish a rela2on with sedimenta2on

ƒ

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SLIDE 13

October 17, 2019

Commissariat à l’énergie atomique et aux énergies alterna=ves

Norma Maria Pereira Machado

Perspec2ves

13

Goals

  • 1. Rheological Model

2.Aggrega2on model

  • 3. Sedimenta2on Link

Approach A Approach B

Iden2fy Model suspension Measurement protocol consolida2on Measurement protocol consolida2on Tests using PGM glass Modelling Tests using PGM glass Tests using PGM glass Measurement protocol consolida2on Modelling Modelling Modelling Simula2on Experimental Tests

2019 2020 2021

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SLIDE 14

October 17, 2019

Commissariat à l’énergie atomique et aux énergies alterna=ves

Norma Maria Pereira Machado

Commissariat à l’énergie atomique et aux énergies alterna=ves - www.cea.fr

Thank you for the aden2on

Financial support:

September 2019

norma.pereiramachado@cea.fr