Analysis of impregnation process

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Presentation transcript:

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) 29-05-2019

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.

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 7389-006 7389-053 7405-043 NOT IMPREGNATED DUE TO CRITICAL NCR o Part A : 7405-043 ; o Part B : 7389-053 ; o Part C : 7405-043. 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.

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 7389-006 7389-053 7405-043 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.

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.

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.

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, 2003. 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., 1996. 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.

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): 1021-1034. 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.

2. Analysis of epoxy resin What about particles and residues? EDMS : 1706562 Residues produced during reaction EDMS : 1829040 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): 423-429. Mica degradation J. L. Rudeiros Fernández et al.

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.

Thanks! J. L. Rudeiros Fernández