Thermal Conductivity Measurements of Carbon Fiber Composites and Thermal Interface Materials

Experiments conducted at Purdue University for the CMS Phase II Inner Tracker

Ryan Story, Jack Wheeler, Abraham Matthew Koshy, Sushrut Karmarkar, Andreas Jung, Souvik Das
Purdue University, West Lafayette, IN

Purdue University hosts two home-made instruments for thermal conductivity measurements in steady-state conditions. One measures thermal conductivity through the plane of the material and the other measures conductivity in the plane of the material. This was done to disentangle kxx, kyy and kzz for anisotropic materials like carbon fiber. We do not have a way to measure off-diagonal terms in the thermal conductivity tensor, like kxy, and for isotropic materials and orthogonal layups of unidirectional carbon fiber, we assume them to be zero.

Fig. 1. (a) Image of the Purdue apparatus used to measure through-plane thermal conductivity. (b) Schematic for the through-plane apparatus depicting all major components. It shows 12 thermistors that are used to estimate the heat flux through the sample and the temperature across the sample.
Fig. 2. (a) Image of the Purdue apparatus used to measure in-plane thermal conductivity. (b) Schematic for the through-plane apparatus depicting all major components. It shows 12 thermistors that are used to estimate the heat flux through the sample and the temperature across the sample.

The through-plane conductivity apparatus shown in Fig. 1 has been used to measure thermal conductivities of carbon fiber, thermal greases and thermal adhesives. A typical measurement requires 4 or more samples of the material to eliminate the interface resistance between the flux-meters and the samples. For carbon fiber, each sample has to be a cylindrical disc of 1" diameter. The samples are required to be of maximally varying thicknesses, from 1 mm to 3 mm. For thermal interface materials, such as greases and adhesives, they are applied between 1" diameter sapphire discs to achieve very precise thicknesses between 70 and 200 um.

The in-plane conductivity apparatus shown in Fig. 2 has been used to measure thermal conductivities of carbon fiber. A typical measurement requires 4 or more samples of the material. If we define length to be the direction in which we measure thermal conductivity, we need samples of width = 50.0 mm, thickness = 4.0 mm. For carbon fiber samples where we know thermal conductivity along the length will be O(100) W/mK, we recommend sample lengths in the range from 15 to 60 mm. For samples where we know it will be O(10) W/mK, we recommend sample lengths in the range from 5 to 20 mm. If samples are to be shipped to Purdue, it is of paramount importance to protect the edges from chipping.


Carbon Fiber Composites

K13C2U / EX1515

This is K13C2U fiber from Mitsubishi Chemical Corporation in EX1515 resin from Toray Advanced Composites. It is obtained in pre-preg form. The fiber has k = 600 W/mK, and the resin has k = 0.17 W/mK.

The following are measurements of the material after lamination, assuming infinite thickness. Unidirectional measurements isolate the effective thermal conductivity of a single ply within a laminated bulk. These may be used to inform composite simulations to engineer special layup configurations for optimal thermal properties in desired directions. Cross-ply measurements measure the effective conductivity of the bulk.

Unidirectional Layup


Layup and Curing Direction Theoretical Expectation Measurement at 0 rad Measurement at 1.5 Grad
[0/0/0... ], 4 bar kxx 318 W/mK 335 ± 28 W/mK (INPL11)
kyy 0.53 W/mK 6.6 ± 1.1 W/mK (INPL12)
kzz 0.53 W/mK 1.18 ± 0.15 W/mK (TC5)
[0/0/0... ], 10 bar kzz 1.36 ± 0.08 W/mK (TC20)
[0/0/0... ], 20 bar kzz 2.21 ± 0.31 W/mK (TC16)

Cross-ply Layup

f
Layup and Curing Direction Theoretical Expectation Measurement at 0 rad Measurement after Irradiation
[0/90/0... ], 4 bar kxx, yy 182 ± 14 W/mK (INPL13)
kzz 1.27 ± 0.06 W/mK (TC3) 1.40 ± 0.06 W/mK (TC3_Irradiated to 90 Mrad)
[0/90/0... ], 10 bar kxy 243 ± 17 W/mK (INPL16)
kzz 2.18 ± 0.11 W/mK (TC19) 2.33 ± 0.12 W/mK (TC19_Irradiated to 1.5 Grad)
[0/90/0... ], 20 bar kxy 236 ± 15 W/mK (INPL17)
kzz 2.22 ± 0.15 W/mK (TC18) 2.13 ± 0.20 W/mK (TC18_Irradiated to 1.5 Grad)

With Dopants & Pressure

Dopants, Layup, Curing Direction Theoretical Expectation Measurement at 0 rad Measurement at 1.5 Grad
[0/0/0], 4 bar kzz 0.53 W/mK 1.09 ± 0.15 W/mK (TC5)
1.67% Graphite, [0/0/0], 4 bar kzz 1.40 ± 0.11 W/mK (TC14)
10% Graphite, [0/90/0], 20 bar kzz 2.59 ± 0.12 W/mK (TC15) 2.68 ± 0.10 W/mK (TC15_Irradiated)
10% Diamond Dust (20 um), [0/90/0], 4 bar kzz 1.85 ± 0.06 W/mK (TC22)


K13D2U / EX1515

This is K13D2U fiber from Mitsubishi Chemical Corporation in EX1515 resin from Toray Advanced Composites. It is also obtained in pre-preg form. The fiber has k = 800 W/mK, and the resin has k = 0.17 W/mK. Cured at 4 bar, fiber volume fraction is 51.6%. Cured at 20 bar, it is 74.5%.

Unidirectional Layup

Layup and Curing Direction Theoretical Expectation Measurement at 0 rad
[0/0/0... ], 4 bar kxx 410 W/mK 376 ± 31 W/mK (INPL9)
kyy 7.5 ± 4.4 W/mK (INPL10)
kzz 1.44 ± 0.24 W/mK (TC6)
[0/0/0... ], 7 bar kxx 437 ± 26 W/mK (INPL25)
kyy (INPL26)
kzz 1.39 ± 0.10 (TC29)
[0/0/0... ], 10 bar kzz
[0/0/0... ], 20 bar kzz 2.79 ± 0.46 W/mK (TC17)

Cross-ply Layup

Layup and Curing Direction Theoretical Expectation Measurement at 0 rad Measurement at 1.5 Grad
[0/90/0... ], 4 bar kxx, yy 210 ± 7 W/mK (INPL24)
kzz 1.36 ± 0.04 W/mK (TC21) 1.41 ± 0.05 W/mK (TC21_Irradiated)
[0/90/0... ], 7 bar kxx, yy 239 ± 9 W/mK (INPL23)
kzz 1.5 ± 0.1 W/mK (TC28)
[0/90/0... ], 10 bar kzz
[0/90/0... ], 20 bar kzz 4.0 ± 0.6 W/mK (TC8)

With Dopants & Pressure

Dopants, Layup, Curing Direction Theoretical Expectation Measurement at 0 rad Measurement at 1.5 Grad
10% Graphite, [0/90/0], 7 bar kzz 2.17 ± 0.10 W/mK (TC23)
1.77 ± 0.13 W/mK (TC27)
2.50 ± 0.17 W/mK (TC23 Irradiated to 1.5 Grad)
kxx, kyy 182 ± 7 W/mK (INPL21)
206 ± 7 W/mK (INPL22)
158 ± 8 W/mK (INPL21 Irradiated to 1.5 Grad)


Thermal Interface Materials

Moresco + Diamonds

This will be our TIM between the modules and carbon fiber Dee. Moresco RG-42R-1 is a low viscosity polyphenyl ether that is used as a grease. It is radiation resistant up to 1.1 Grad. We dope it with lapidiary diamond dust of 20 um average diameter at varying concentrations and measure the thermal conductivity of the resulting mixtures.

Diamond 20 um Concentration by Weight Measurement at 0 rad Measurement at 1.5 Grad
0% 0.20 ± 0.02 W/mK (SAND18)
33% 0.33 ± 0.03 W/mK (SAND19)
70% 0.90 ± 0.08 W/mK (SAND23) Sample irradiated: 1.03 ± 0.09 W/mK (SAND23_Irradiated),
Material irradiated: 0.88 ± 0.07 W/mK (SAND31)

Loctite EA9396 + Diamonds

This will be our TIM adhesive between the cooling pipe and carbon foam. Loctite EA9396 is a two-part mixture that when cured does not compromise structural integrity up to 1.1 Grad. We dope it with lapidiary diamond dust of 20 um average diameter at varying concentrations and measure the thermal conductivity of the resulting mixtures.

Diamond 20 um Concentration by Weight Measurement at 0 rad Measurement at 1.5 Grad
0% 0.34 ± 0.02 W/mK (SAND27)
30% 0.44 ± 0.02 W/mK (SAND28)
50% 0.74 ± 0.02 W/mK (SAND30)
70% 1.28 ± 0.06 W/mK (SAND29) 1.14 ± 0.09 W/mK (SAND29_Irradiated)

Araldite 2011 + Diamonds

This is a secondary candidate for the TIM adhesive between the cooling pipe and carbon foam. Araldite 2011 is a two-part mixture that rapidly cures within 1 hour when cured and does not compromise structural integrity up to 1.1 Grad. We dope Version 3 of Araldite 2011 with lapidiary diamond dust of 20 um average diameter at varying concentrations and measure the thermal conductivity of the resulting mixtures.

Diamond 20 um Concentration by Weight Measurement
0% 0.25 ± 0.01 W/mK (SAND24)
30% 0.33 ± 0.01 W/mK (SAND25)
50% 0.53 ± 0.03 W/mK (SAND26)


Carbon Foam

This is the carbon foam used in the Dee.
Material Details Manufacturer Datasheet Measurement
Allcomp / Lockheed Martin, K9 densified, graphitized, Hi-K carbon foam. 130 PPI. SN 6, 10th Lot. (January, 2018) 21.59 W/mK 39 ± 7 W/mK