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NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS ON GREASES AND OILS Recent results Matteo Ferrari EN/STI/TCD Radiation resistant lubricants Meeting • CERN • Oct 22 st , 2019

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Page 1: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

NEUTRON AND GAMMA

IRRADIATION TEST CAMPAIGNS

ON GREASES AND OILS

Recent results

Matteo Ferrari EN/STI/TCD

Radiation resistant lubricants Meeting • CERN • Oct 22st, 2019

Page 2: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

INTRODUCTION

Page 3: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

I n t r o d u c t i o n

HIGH-POWER FACILITIES

CRITICAL APPLICATIONS FOR POLYMERS

• RADIATION DAMAGE

in MIXED FIELDS

• RESIDUAL ACTIVATION

Radiation protection

Maintenance

Waste disposal

1 Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

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I n t r o d u c t i o n

POLYMERS IN FACILITIES UNDER CONSTRUCTION

O-rings

NECESSARY BUT RADIATION-SENSITIVE

2

Lubricants

ESS project

SPES project

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 5: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

I n t r o d u c t i o n

CERN ACCELERATOR COMPLEX

3 Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 6: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

I n t r o d u c t i o n

MAIN CONCERNS

4

BEST PRODUCTS

FOR SPECIFIC

APPLICATIONS

UNDERSTANDING OF

RAD MECHANISMS

Design

Science

PREDICITON

OF REAL-LIFE

DEGRADATION

Maintenance

Prevent failure

FOLLOW-UP ON

USED PRODUCTS

Know-how

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 7: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

I n t r o d u c t i o n

LIMITS OF THE LITERATURE

FEW NEUTRON/MIXED FIELD DATA

5

• Mostly gamma

• Old data, obsolete

products

• Very general tests

• Assumptions

• Lack of understanding

• Lack of thresholds

• More challenging

conditions

‘Equal dose – equal damage’ ?

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 8: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

• Composition

• Temperature

• Atmosphere

• Extreme Pressure

• Compatibility

• Vacuum

• Mechanical features

• Radiation tolerance

• Product availability

• Price

• Producer reliability

I n t r o d u c t i o n

SELECTION OF COMMERCIAL PRODUCTS

6

OFTEN UNKNOWN

NO GENERAL VALIDITY

technic

alrequirem

ents

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 9: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

I n t r o d u c t i o n

TECHNICAL SPECIFICATIONS AT CERN

7 Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

EQUIPMENT

ENVIRONMENT

LUBRICANT

• Equipment ID

• Operation details

• Maintenance

• Existing components/follow up

• Radiation field/rate

• Atmosphere

• Temperature

• Materials

• Consistency/viscosity

• Requirements on composition

• Quantity needed

• Previous products?

By Dominika Senajova

NEW ONGOING STUDY

Page 10: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

I n t r o d u c t i o n

COLLIMATORS LUBRICATION

8 Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

OPERATION CONDITONS

• ~130 collimators - LHC

• 4 roller screws per collimator

• ~10 MGy dose

• limited possible maintenance

A. Bertarelli et al., HL-LHC Collimators and

High Temperature Materials,

HiLumi LHC Goes To Industry Workshop (2015)

CRITICAL

DOSE LEVEL

Page 11: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

I n t r o d u c t i o n

PS DUMP LUBRICATION

9 Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

OPERATION

CONDITONS

• High energy protons

• ±6° rotation

• 250 000 cycles/yr

• 1 MGy dose

CASE STUDIES

• Grease evolution

• Endpoint

• Monitoring

• Failure scenarios

• Maintenance

• Follow up

F-X. Nuiry et al., Designing and prototyping of the

CERN Proton Synchrotron Internal Dump in the

Framework of the LHC Injectors Upgrade Project,

7° High Power Targetry Workshop (2018)

Page 12: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

IRRADIATION AND TESTING

METHODOLOGIES

Page 13: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

I r r a d i a t i o n a n d t e s t i n g m e t h o d o l o g i e s

RADIATION DAMAGE STUDIES: A TIMELINE

10

RDS Radiation Damage Study - polymers

Phd - radiation damage on lubricants

2018 now20162015 2017 2019

case study - MORESCO grease/oil

R2M

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 14: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

I r r a d i a t i o n a n d t e s t i n g m e t h o d o l o g i e s

ELASTOMERIC O-RINGS

PIE

• A. Zenoni et al., Radiation resistance of elastomeric O-rings in mixed neutron and

gamma fields: Testing methodology and experimental results, Review of Scientific

Instruments 88, 113304 (2017) https://doi.org/10.1063/1.5011035

• M. Ferrari et al., Degradation of EPDM and FPM elastomers irradiated at very high

dose rates in mixed gamma and neutron fields, Polymer Engineering and Science

(2019) https://doi.org/10.1002/pen.25249

11

> >

IRRADIATION

FACILITY

SAMPLES

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

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6 Matteo Ferrari TCD Extended Section Meeting CERN - 1 Oct 201912 Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 16: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

I r r a d i a t i o n a n d t e s t i n g m e t h o d o l o g i e s

A REAL APPLICATION FOR AN EPDM O-RING

GATE VALVE - SPES facility

SAFE USABILITY AREA

13

Battini, D. et al, Experimental testing and numerical

simulations for life prediction of gate valve O-rings

exposed to mixed neutron and gamma fields,

Materials and Design vol. 156, 514-527 (2018)

https://doi.org/10.1016/j.matdes.2018.07.020

CONDITIONS

• Dynamic operation

• 0.7 MGy neutrons + gamma

• Vacuum

• About 85°C

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 17: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

I r r a d i a t i o n a n d t e s t i n g m e t h o d o l o g i e s

LUBRICANTS

PIE

M.Ferrari et al., Experimental study of consistency degradation of different

greases in mixed neutron and gamma radiation,

Heliyon, Vol 5 Issue 9 e02489 (2019)

https://doi.org/10.1016/j.heliyon.2019.e02489

14

IRRADIATION

FACILITY

> >

SAMPLES

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 18: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

I r r a d i a t i o n a n d t e s t i n g m e t h o d o l o g i e s

IRRADIATION CAMPAIGNS

243 hours

83 samples

5 years

15

• O-RINGS

4 products

• O-RINGS

real application study

• O-RINGS

Dose rate effect

• GREASES

9 products

• LUBRICANT

1 oil

2 experiments:

+ proton irr. at IRRAD

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 19: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

Lateral

In-core

MIXED RAD FIELDS

HIGH FLEXIBILITYMonte Carlo simulation

MCNPX reactor model

I r r a d i a t i o n a n d t e s t i n g m e t h o d o l o g i e s

NEUTRON AND GAMMA REACTOR FACILITIES

16 Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 20: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

Matteo Ferrari RAD 2018 Ohrid

TRIGA Mark II

RESEARCH REACTOR

Pavia, Italy

17 Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

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I r r a d i a t i o n a n d t e s t i n g m e t h o d o l o g i e s

DOSIMETRY CALCULATIONS

18

COMPLEX

DOSIMETRY

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

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RADIATION STUDY ON GREASES

Page 23: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

619 Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

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G r e a s e s

GREASE CONSISTENCY

‘Grease is an exceptionally complex product incorporating a high

degree of technology in chemistry, physics, rheology, tribology

and the environmental sciences.’

MULTI-PHASE:

• Oil

• Thickener

• Additives

CONSISTENCY:

ASTM D217-02

Semi-fluid

20

R. M. Mortier et al., Chemistry and Technology of Lubricants, 3rd edn., Springer (2010).

Page 25: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

G r e a s e s

CONSISTENCY TEST: GRIZZLYGREASE No.1

0.15 MGy

RADIATION-INDUCED

FLUIDIZATION

0.45 MGy

21 Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 26: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

DRIPPING

GREASE

22

Page 27: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

G r e a s e s

CONSISTENCY TEST: PETAMO GHY 133 N

COLOR CHANGE BUT STABLE

0 MGy

0.40 MGy

23 Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 28: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

G r e a s e s

DIFFERENT BEHAVIOURS AT HIGH DOSES

24

Peta

mo

GH

Y 133N

RG

-42R-1

NON IRR 1 MGy 5 MGy 10 MGy

SOFTENING VS HARDENING

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 29: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

G r e a s e s

USABILITY ENDPOINTS FOR GREASES (1)

FLUID

Structural

endpoint

25

SEVERE MATERIAL MODIFICATION

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 30: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

G r e a s e s

USABILITY ENDPOINTS FOR GREASES (2)

STABLE

CONSIST.

CLASS

Functional

endpoint

DOSE THRESHOLDS FOR USERS

26

<10%

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

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RP-42R OIL: A CASE STUDY

Page 32: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

ESS project

Lund, Sweden

MORESCO

Kobe, Japan

UniBs DIMI

Brescia, Italy

R P- 4 2 R o i l : a c a s e s t u d y

A RESEARCH COLLABORATION

27 Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 33: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

R P- 4 2 R o i l : a c a s e s t u d y

OIL CHARACTERIZATION

PERFORMED TESTS:

• Kinetic viscosity

• Total acid number

• NMR spectra

• GPC gel permeation

• GC gas chromatography

• FT-IR spectroscopy

GC

Kinetic viscosity

28

Acid

number

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 34: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

R P- 4 2 R o i l : a c a s e s t u d y

MORESCO RP-42R: VISCOSITY

29

0.7

8 M

Gy

1.5

5 M

Gy

7.7

8 M

Gy

NO

N IR

R

REMARKABLE

MODIFICATIONS

RP-42R-1 grease: stable

+350%

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 35: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

30 Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 36: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

R P- 4 2 R o i l : a c a s e s t u d y

GEL PERMEATION FRACTION ANALYSIS

31

RAD-INDUCED

POLYMERIZATION

Molecular chains >2500

0% nonIRR

20% at 8 MGy

DO

SE

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 37: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

R P- 4 2 R o i l : a c a s e s t u d y

NMR ANALYSIS

32

CHEMICALLY STABLE

DO

SE

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 38: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

ONGOING STUDIES

Page 39: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

O n g o i n g s t u d i e s

GAMMA VS MIXED FIELD: VISCOSITY

33

DIFFERENT EFFECT AT EQUAL DOSE

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

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O n g o i n g s t u d i e s

OIL EXTRACTED FROM THE GREASE

34

BULK OIL vs OIL IN GREASE:

DIFFERENT EFFECTS

Kinetic Viscosity

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 41: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

CONCLUSIONS AND

FURTHER DEVELOPMENTS

Page 42: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

C o n c l u s i o n s

TAKE HOME MESSAGE

• Large sensitivity range: 0.1 MGy -10 MGy

• Irradiation and testing methodologies

• Dose thresholds are not universal

• Scarce knowledge of radiation damage mechanisms

• Ingredients and final product: different resistance

• Prediction of damage in real application: a challenge

EXPERIMENTAL TEST OF PRODUCTS:

MANDATORY FOR FACILITIES

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

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C o n c l u s i o n s

FURTHER RESEARCH TOPICS

• Different rad fields

• Dose rate effect

• Oxygen effect

• Grease/bulk oil/extracted oil

• Radiation mechanisms: thickener vs oil

• Thresholds determination

• Specific case studies

• New products

TO BE INVESTIGATED

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019

Page 44: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

THANK YOU FOR YOUR ATTENTION!

Special thanks to Hayashi San

(MORESCO)

R2M

Radiation to Materials

[email protected]

[email protected]

Page 45: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …
Page 46: NEUTRON AND GAMMA IRRADIATION TEST CAMPAIGNS …

G r e a s e s

THRESHOLDS OF RADIATION DAMAGE: GREASES

27

M.Ferrari et al., Heliyon, Vol 5 Issue 9 e02489 (2019)

Matteo Ferrari Radiation resistant lubricants Meeting CERN – 22 Nov 2019