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Atomic layer deposition of ZnO/Al2O3/ZrO2 nanolaminates for improved thermal and wear resistance in carbon-carbon composites
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Image of FIG. 1.
FIG. 1.

(Color online) Structure of ALD trilayer ZnO/Al2O3/ZrO2 nanolaminates (not to scale).

Image of FIG. 2.
FIG. 2.

(Color online) X-ray tomography images in (a) 3D and (b) 2D (x-y plane slice) of ALD ZrO2 infiltrated graphite foam. (c) Cross-sectional TEM image of ALD ZrO2 infiltrated CCC that shows surface and subsurface ZrO2 infiltration, and higher magnification images taken inside subsurface pores of (d) interface between amorphous carbon and ZrO2 and (e) two ZrO2 grains. Images (d) and (e) were taken from the dashed and solid boxes shown in (c), respectively. The dotted arrows in (c) refer to the subsurface ZrO2 coating that has not reached the targeted ∼300 nm thickness. The e-beam Pt is a protective layer used during FIB-milling to prevent damage to layers.

Image of FIG. 3.
FIG. 3.

(Color online) Cross-sectional TEM image of four trilayer ZnO/Al2O3/ZrO2 nanolaminates infiltrated into CCC displaying the ALD capability to conformally and uniformally coat subsurface pores. The red rectangle shows the four trilayer sequence grown on the CCC with the brighter white ∼5 nm thick Al2O3 layer serving as a useful marker to distinguish the trilayers. The dashed line represents the surface of the sample where the protective Pt was deposited.

Image of FIG. 4.
FIG. 4.

(Color online) Cross-sectional SEM (top row) and corresponding EDS elemental maps (bottom row) of ∼300 nm thick ALD ZrO2 coated CCC under exposure times of (a) 1 s (deposition #1) and (b) 2 s (deposition #2).

Image of FIG. 5.
FIG. 5.

(Color online) XRD of ALD (a) ZnO layer and bilayer of ZnO/Al2O3, (b) ZrO2 (deposition #2), and (c) ZnO/Al2O3/ZrO2 nanolaminate (deposition #3) coated CCC.

Image of FIG. 6.
FIG. 6.

(Color online) (a) Cross-sectional TEM micrograph of ALD ZrO2 (deposition #2) coated CCC. (b) HRTEM image that shows a-C, crystalline (0002) graphite and (101) ZrO2 lattice planes with corresponding FFT pattern shown in inset, and (c) inverse FFT pattern of (0002) graphite (spot 1), and (d) inverse FFT pattern of (101) tetragonal ZrO2 (spot 2).

Image of FIG. 7.
FIG. 7.

(Color online) Cross-sectional TEM images on the top surface of (a) one trilayer (deposition #3), (b) two trilayers (deposition #4), and (c) four trilayers (deposition #5) ALD ∼220 nm thick ZnO/Al2O3/ZrO2 nanolaminates infiltrated into CCC. See Table III for ALD processing conditions.

Image of FIG. 8.
FIG. 8.

(Color online) FFT pattern taken from the ZnO layer in Fig. 7(a). The beam direction is [].

Image of FIG. 9.
FIG. 9.

(Color online) Typical friction coefficient traces of uncoated CCC, ALD ZrO2 (deposition #2) coated CCC, one trilayer (deposition #3), and four trilayers (deposition #5) ZnO/Al2O3/ZrO2 nanolaminate coated CCC. The initial mean Hertzian contact stress is 0.9 GPa (normal load = 2.45 N). The arrows point to steady-state friction coefficient (μss) values.

Image of FIG. 10.
FIG. 10.

(a) (Color online) Cross-section TEM image inside the wear track of ALD ZrO2 (deposition #2) coated CCC that shows formation of a mechanically mixed layer (MML) inside the wear contact after 200 m of sliding. S.D. = sliding direction. (b) Optical microscopy image of the corresponding transfer film adhered to the steel ball after sliding on the ALD ZrO2 coated CCC wear track.

Image of FIG. 11.
FIG. 11.

(Color online) Optical microscopy images of the transfer films on 440C steel balls (top row) and corresponding wear tracks (bottom row) for (a) uncoated CCC and (b) ALD ZnO/Al2O3/ZrO2 nanolaminate coated CCC (deposition #3) after 200 m of sliding. The other images have the same scale bar as in (a).

Image of FIG. 12.
FIG. 12.

(Color online) (a) SEM image of the ALD ZnO/Al2O3/ZrO2 nanolaminate wear track taken from the box location in Fig. 11(b). The rectangular bar is e-beam evaporated Pt deposited in the SEM to protect the surface during FIB-milling. Cross-sectional HRTEM images (b), (c) inside the wear track showing MML and undeformed trilayer, (d) MML and fractured trilayer taken from the box location in (c), and (e) plastically deformed ZnO (0002) orientated grain taken from the box location in (d). The arrows point to a high density of sliding (slip)-induced basal stacking faults. (f) FFT pattern taken from the ZnO grain showing streaking of the {0002} diffraction spots (denoted by circles) indicative of basal stacking faults. Additional nonstreaked diffraction spots are not labeled, and some are from other overlapping ZnO grains. The beam direction is [].


Generic image for table

Physical, mechanical, electrical and thermal properties of CCC and graphite foam.

Generic image for table

ALD deposition recipes to deposit ∼300 nm thick ZrO2 films.

Generic image for table

ALD deposition recipes to deposit overall ∼220 nm thick one, two, and four trilayer(s) of ZnO/Al2O3/ZrO2 nanolaminates. Numbers of cycles for two and four trilayers are half and quarter of cycles for one trilayer, respectively.


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752b84549af89a08dbdd7fdb8b9568b5 journal.articlezxybnytfddd
Scitation: Atomic layer deposition of ZnO/Al2O3/ZrO2 nanolaminates for improved thermal and wear resistance in carbon-carbon composites