1. Analysis of impregnation process
José Luis Rudeiros Fernández (TE-MSC-LMF)*
Olivier Housiaux (TE-MSC-LMF)
Jerome Axensalva (TE-MSC-LMF)
Dariusz Pulikowski (TE-MSC-LMF)
Frédéric Savary (TE-MSC-LMF)

2. Compilation and comparison of impregnation parameters
Contents
Compilation and comparison of impregnation parameters
Analysis of epoxy resin
Next steps
J. L. Rudeiros Fernández et al.

3. 1. Compilation and comparison of impregnation parameters
CR1
CR2
CR3
CR4
CR5
CR6
CR7
GE01
GE02
GE03
GE04
GE05
GE06
GE07
GE08
GE09
GE10
GE11
Fibres
Different batches but same types on all coils
Impregnation date
No information
10/03/2017
06/04/2017
06/06/2017
24/07/2017
25/06/2018
15/08/2018
09/10/2018
30/10/2018
26/11/2018
17/12/2018
29/01/2019
14/02/2019
Resin batch
NOT IMPREGNATED DUE TO CRITICAL NCR
o Part A : ; o Part B : ; o Part C :
Machine
Elytt
CERN
Heating system
Number of N2 drying cycle 5
Pressure of the mixer after 1h degazing
0.44mbar
Pression in the coil before injection
0.5mbar
0.5
Preparation of the resin
10h50
Before 10h
Beginning of the injection
12h50
11h08
9h20
Resin arrival in upper tank
13h45
12h
10h09
Soaking No
yes
Yes
Pressure of the upper tank before thermal cycle
2bar
Pressure of the mixer before thermal cycle
2.8bar
Thermal cycle
link
Number of cold test cycles
1 (first proto) + 2 (hybrid)
1 (first proto)
0 (under installation in HCLMBHB001-CR000002)
2 (hybrid)
J. L. Rudeiros Fernández et al.

4. 1. Compilation and comparison of impregnation parameters
MQXFBC
101
102
103
104
105
107
108
109
201
202
203
Fibres
Different batches but all type same types on all coils
Impregnation date
24/04/2017
01/08/2017
01/09/2017
21/03/2018
31/05/2018
06/07/2018
29/08/2018
04/10/2018
15/01/2019
06/02/2019
Resin batch
Machine
Elytt
CERN
Heating system
Number of N2 drying cycle
Pressure of the mixer after 1h degazing
Pression in the coil before injection
Preparation of the resin
Beginning of the injection
12h15
Resin arrival in upper tank
13h55
Soaking No
Yes (2h43)
Yes
Pressure of the upper tank before thermal cycle
Pressure of the mixer before thermal cycle
Thermal cycle
link
No info
Number of cold test cycles
J. L. Rudeiros Fernández et al.

5. 2. Analysis of epoxy resin
Introduction
The state of cure, 𝐶, is related to the extent of conversion, and can be estimated a posteriori by measuring the glass transition temperature, 𝑇 𝑔 , of the epoxy resin.
The 𝑇 𝑔 can be defined as the temperature at which a transition between a glassy state and a rubbery state occurs, as a result of the activation of long-range translational motion of the polymer chains.
The 𝑇 𝑔 can be measured by different techniques, including DSC and DMA. The DSC method relies on an observable step change in the specific heat capacity, during the phase transition.
𝐶= 𝑇 𝑔 − 𝑇 𝑔0 𝑇 𝑔∞ − 𝑇 𝑔0
DSC measurements carried out by D. Ternova and B. Teissandier following ASTM E1356
J. L. Rudeiros Fernández et al.

6. 2. Analysis of epoxy resin
Summary of results
DSC measurements carried out by D. Ternova and B. Teissandier following ASTM E1356
J. L. Rudeiros Fernández et al.

7. 2. Analysis of epoxy resin
What is the impact of a variation of 𝑇 𝑔 ? – Initial literature review
Swier, S., Assche, G. Van & Mele, B. Van, Reaction Kinetics Modeling and Thermal Properties of Epoxy – Amines as Measured by Modulated-Temperature. J. Appl .Polym. Sci., 91(5), pp.2798–2813.
Varley, R.J. et al., Toughening of a trifunctional epoxy system. II. Thermal characterization of epoxy/amine cure. Journal of Applied Polymer Science, 60(12), pp.2251–2263.
J. L. Rudeiros Fernández et al.

8. 2. Analysis of epoxy resin
What is the impact of a variation of 𝑇 𝑔 ? – Initial literature review
Detwiler, Andrew T., and Alan J. Lesser. "Aspects of network formation in glassy thermosets." Journal of Applied Polymer Science 117, no. 2 (2010):
Cantwell W.J., Kausch H.H. (1993) Fracture behaviour of epoxy resins. In: Ellis B. (eds) Chemistry and Technology of Epoxy Resins. Springer, Dordrecht
J. L. Rudeiros Fernández et al.

9. 2. Analysis of epoxy resin
What about particles and residues?
EDMS :
Residues produced during reaction
EDMS :
Rodgers, Reneé M., Hassan Mahfuz, Vijaya K. Rangari, Nathaniel Chisholm, and Shaik Jeelani. "Infusion of SiC nanoparticles into SC‐15 epoxy: an investigation of thermal and mechanical response." Macromolecular Materials and Engineering 290, no. 5 (2005):
Mica degradation
J. L. Rudeiros Fernández et al.

10. 3. Next steps
Proposal
Analysis of resin samples from all previous impregnated coils available. Specially relevant to analyse long coils along their lengths.
Study of non-uniformity of 𝑇 𝑔 along coil’s length and potential correlation with mould temperature variation.
Analysis of potential differences between coils, including significant variation between MQXFB and 11T coils (e.g. presence of mica residues, temperature, pressure, soaking time vs. pot life).
Further analysis of resin:
Mass loss vs. temperature (TGA study).
Comparison of DMA and DSC 𝑇 𝑔 measurements.
Analysis of CTD-101K curing process (stoichiometric mix) through DSC, impact of curing cycle parameters (i.e. time and temperature), and presence of pyrolysis/oxidation residues from impregnation (e.g. degraded mica).
Evaluation of potential test to characterise fracture behaviour (e.g. crack growth due to samples subjected to cryogenic temperatures, Charpy impact test at 4.2 K).
Establishment of correlation between 𝑇 𝑔 and stiffness for the CTD101K system.
Definition of acceptable 𝑇 𝑔 range for the coil.
J. L. Rudeiros Fernández et al.

11. Thanks!
J. L. Rudeiros Fernández