Micro/nano multiscale reinforcing strategies toward extreme high-temperature applications: Take carbon/carbon composites and their coatings as the examples

doi:10.1016/j.jmst.2021.03.076

J. Mater. Sci. Technol. ›› 2022, Vol. 96: 31-68.DOI: 10.1016/j.jmst.2021.03.076

• Invited Review • Previous Articles Next Articles

Micro/nano multiscale reinforcing strategies toward extreme high-temperature applications: Take carbon/carbon composites and their coatings as the examples

Qiangang Fu^a^,^*,1(), Pei Zhang^a,1(), Lei Zhuang^a(), Lei Zhou^a(), Jiaping Zhang^a(), Jie Wang^b(), Xianghui Hou^c(), Ralf Riedel^a^,^d(), Hejun Li^a^,^*()

^aState Key Laboratory of Solidification Processing, Shaanxi Key Laboratory of Fiber Reinforced Light Composite Materials, Carbon/Carbon Composites Research Center, Northwestern Polytechnical University, Xi’an 710072, China
^bSchool of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai 200240, China
^cFaculty of Engineering, University of Nottingham, University Park, Nottingham NG7 2RD, United Kingdom
^dInstitut für Materialwissenschaft, Technische Universität Darmstadt, Otto-Berndt-Straße 3, Darmstadt D-64287, Germany

Received:2021-01-24 Revised:2021-03-22 Accepted:2021-03-22 Published:2022-01-10 Online:2022-01-05
Contact: Qiangang Fu,Pei Zhang,Lei Zhuang,Lei Zhou,Jiaping Zhang,Jie Wang,Xianghui Hou,Ralf Riedel,Hejun Li
About author:lihejun@nwpu.edu.cn (H. Li).
ralf.riedel@tu-darmstadt.de (R. Riedel),
Xianghui.Hou@nottingham.ac.uk (X. Hou),
wjie_no1@sjtu.edu.cn (J. Wang),
zhangjiaping@nwpu.edu.cn (J. Zhang),
18710832501@163.com (L. Zhou),
313173104@qq.com (L. Zhuang),
zhangpei89@mail.nwpu.edu.cn (P. Zhang),
*E-mail addresses: fuqiangang@nwpu.edu.cn (Q. Fu),
Qian-gang Fu is the principal professor and the director of Shaanxi Key Laboratory of Fiber Reinforced Light Com- posite Materials, at NWPU, Xi’an. He is mainly engaged in high-temperature oxidation/ablation resistant carbon- based composites, as well as carbon and SiC nanoma- terials for almost 20 years.The main academic achieve- ments includes: the influence rules of the multi-phase in- laid coating structure on the releasing and redistributing of thermal stress in the coating were disclosed, and the oxidation protective property of the coating was made a breakthrough; the strengthening-toughening mechanism of several kinds of SiC nanowires were discovered, and the application of nanowires for anti-oxidation and anti- abrasion coatings was exploited; the synergetic design idea of expand effect from boride oxidation and gradient transition structure was put forward, and the abil- ity for the coating with a wide temperature-range oxidation protection and self- seal anti-ablation was realized. He undertakes more than 10 projects including 6 projects of National Natural Science Foundation of China. He was awarded the first prize of Education Ministry Natural Science, the second prize of State Nature Sci- ence, the first prize of Shaanxi Province Science and Technology and the first prize of Education Ministry Technical Invention. His-doctor thesis was appraised by the National Hundred Excellent Doctor Thesis. He has published 42 patent applications, 2 book chapters, more than 300 papers with over 6831 citations and an H-index of 44 (Scopus). He is a referee of about 20 international scientific journals. He has been invited to give more than 20 Keynote Lectures and Invited Talks in interna- tional conferences and universities, and serve as Session Chair. He also serves in the Editorial Committee of Journal of Materials Science & Technology, Science China Technological Sciences, Journal of Inorganic Materials, Journal of Solid Rocket Technol- ogy, Transactions of Nonferrous Metals Society of China, The Scientific World Journal, Journal of Composites, Materials China , and other journals.
Prof. He-junLi, academician of Chinese Academy of Engi- neering, academician of Asian Pacific Academy of Materi- als, winner of the National Science Fund for Distinguished Young Scholars, director of the innovation group of Na- tional Natural Science Foundation of China, deputy direc- tor of the Science and Technology on Thermostructural Composite Materials Laboratory, has engaged in compos- ite materials area for almost 30 years and mainly focuses on the development of low cost and high performance carbon/carbon composites as well as the technology of oxidation resistant coatings. He has won one second prize of National Natural Science Award, two second prizes of National Technology Invention (ranking the first and the second), one first prize and one second prizes of National Teaching Achievement, six first prizes of provincial and ministerial science and technology, and one Na- tional Defense Innovation Team Award. He has authorized more than 150 invention patents, published more than 600 SCI papers and 3 teaching material or mono- graphs. More than 140 postgraduates were cultivated, among whom more than 30 were promoted to professors or researchers, one student’s paper was awarded as the top 100 national excellent papers, and 8 students were awarded as the provin- cial or first-level academy excellent doctoral dissertation. He has won the hon- orary titles of "Most Beautiful Science and Technology Worker in China", "National Model Teacher", "the 16th China Carbon Outstanding Achievement Award", "Young and Middle-Aged Expert with Outstanding Contributions to Science and Technology Industry of National Defense", etc. He serves as the executive director of Chinese Materials Research Society, member of the materials department of the Science and Technology Committee of the Ministry of Education, member of the expert re- view group of the materials department of the National Natural Science Foundation of China, vice chairman of Society of Materials Research, Composite Materials and Nano Materials in Shaanxi province, review expert of Science and Technology Award in Shaanxi, and vice chairman of the academic committee of Northwestern Poly- technical University. He also serves in the Editorial Committee of Journal of Materi- als Science & Technology, SCIENCE CHINA Materials, Journal of Aeronautics, Carbon Letters, Transactions of Nonferrous Metals Society of China, New Carbon Materials, Rare Metal Materials and Engineering, Materials China, and other journals.First author contact:¹These authors are contributed equally for this work.

Abstract

Abstract:

Carbon fiber reinforced carbon composites (C/Cs), are the most promising high-temperature materials and could be widely applied in aerospace and nucleation fields, owing to their superior performances. However, C/Cs are very susceptible to destructive oxidation and thus fail at elevated temperatures. Though matrix modification and coating technologies with Si-based and ultra-high temperature ceramics (UHTCs) are valid to enhance the oxidation/ablation resistance of C/Cs, it's not sufficient to satisfy the increasing practical applications, due to the inherent brittleness of ceramics, mismatch issues between coatings and C/C substrates, and the fact that carbonaceous matrices are easily prone to high-temperature oxidation. To effectively solve the aforementioned problems, micro/nano multiscale reinforcing strategies have been developed for C/Cs and/or the coatings over the past two decades, to fabricate C/Cs with high strength and excellent high-temperature stability. This review is to systematically summarize the most recent major and important advancements in some micro/nano multiscale strategies, including nanoparticles, nanowires, carbon nanotubes/fibers, whiskers, graphene, ceramic fibers and hybrid micro/nano structures, for C/Cs and/or the coatings, to achieve high-temperature oxidation/ablation-resistant C/Cs. Finally, this review is concluded with an outlook of major unsolved problems, challenges to be met and future research advice for C/Cs with excellent comprehensive mechanical-thermal performance. It's hoped that a better understanding of this review will be of high scientific and industrial interest, since it provides unusual and feasible new ideas to develop potential and practical C/Cs with improved high-temperature mechanical and oxidation/ablation-resistant properties.

Key words: Carbon/carbon composites, Micro/nano multiscale reinforcing strategies, Oxidation, Ablation, Erosion, Hybrid structures

Qiangang Fu, Pei Zhang, Lei Zhuang, Lei Zhou, Jiaping Zhang, Jie Wang, Xianghui Hou, Ralf Riedel, Hejun Li. Micro/nano multiscale reinforcing strategies toward extreme high-temperature applications: Take carbon/carbon composites and their coatings as the examples[J]. J. Mater. Sci. Technol., 2022, 96: 31-68.

Figures/Tables 52

Fig. 1. Hypersonic vehicle, materials properties (a-c) [1] and typical energy accommodation mechanisms (d, e) [3]: (a) Computational fluid-dynamics simulation of Mach 7 hypersonic flight showing surface heat transfer (red, hottest temperature; blue, coolest temperature) and flow-field contours. (b) A photograph of the experimental X-51A Waverider hypersonic aircraft (with expendable booster rocket at the rear) attached to a B-52H mother ship. (c) An Ashby-type map of temperature capability and nominal thermal conductivity of Ni-based superalloys, CMCs, UHTCs and C/C composites (along high-conductivity orientation). Energy accommodation mechanism of (d) ablative thermal protection materials (TPMs) and (e) reusable TPMs.

Fig. 2. Application of C/Cs in some special industrial fields [5].

Fig. 3. Lab-scale high-temperature oxidation (a) and ablation (b) [16] tests, and erosion test in wind tunnel (simulate the real service environment) (c) (corresponding testing installation diagram was shown in (d)) [11] for C/Cs.

Fig. 4. The schematic showing (a) the protection approaches ((1) Modification of carbon/carbon matrix and (2) High-temperature protective coatings)) and (b) the application of promising micro/nano multiscale reinforcing strategies for C/Cs applied for extreme high-temperature environments, where the red arrows refer to reinforce C/Cs and the black ones refer to toughen coatings.

Fig. 5. Schematic of the typical preparation of SiCWs toughened multiphase and multilayer coatings [59].

Fig. 6. SEM micrographs showing the SiCWs toughened multiphase and multilayer coatings (take SiCWs-HfB2-SiC-Si/SiC coatings as an example): (a) cross-section; (b,c) SiCWs bridging features on the fracture surface; (d) SiCWs pull-out and debonding features on the fracture surface [59].

Table 1 Summary of isothermal oxidation testing data of SiC whiskers (SiCWs) toughened coatings.

Coating materials	Toughening materials	Fabrication methods	Time (h)	Temperature (K)	Mass loss (%)	Refs.
SiC	-	slurry+PC	48	1773	5	[49]
	5 wt.% SiCWs		48	1773	2.8
	10 wt.%SiCWs		48	1773	1.5
	15 wt.% SiCWs		48	1773	2.5
	20 wt.% SiCWs		48	1773	5.5
MoSi₂-SiC-Si	-		200	1773	2.31	[52]
MoSi₂-SiC-Si	10 wt.% SiCWs		200	1773	0.33	[52]
SiC—CrSi₂	15 wt.% SiCWs		50	1673	0.74	[53]
SiC—CrSi₂	15 wt.% SiCWs		50	1773	0.67	[53]
SiC—CrSi₂	-		50	1773	2.43	[54]
SiC—CrSi₂	15 wt.% SiCWs		50	1773	0.66	[54]
MoSi₂-SiC	SiCWs	slurry	2.67	1773	0.08	[56]
TMS/MS	SiCWs/SiCWs	slurry	2.67	1773	0.02	[56]
HfB₂-SiC-Si/SiC	SiCWs	PC+CVD+slurry	468	1773	0.88	[58]
HfB₂-SiC-Si/SiC	-	PC+slurry	468	1773	4.86	[58]
MoSi₂/SiC	Y₂Si₂O₇W	PC+HEPD	100	1773	0.73	[63]
MoSi₂/SiC	1 wt% Al₂O₃W	PC+SAPS	76	1773	0.17	[66]

Table 2 Summary of thermal shock testing data of SiC whiskers (SiCWs) toughened coatings.

Coating materials	Toughening materials	Fabrication methods	Cycle	Temperature (K)	Mass loss (%)	Refs.
SiC	-	slurry+PC	30	1773	4.05	[49]
	5 wt.% SiCWs		30	1773	3.09
	10 wt.% SiCWs		30	1773	2.19
	15 wt.% SiCWs		30	1773	2.85
	20 wt.% SiCWs		30	1773	3.72
SiC—CrSi₂	-		20	1773	8.36	[54]
	5 wt.% SiCWs		20	1773	7.58
	10 wt.% SiCWs		20	1773	7.06
	15 wt.% SiCWs		20	1773	6.70
	20 wt.% SiCWs		20	1773	9.58
HfB₂-SiC-Si/SiC	SiCWs	PC+CVD+slurry	50	1773	4.48	[58]
HfB₂-SiC-Si/SiC	-	PC+slurry	50	1773	19.46	[58]
silicate glass/SiC	mullite whiskers	PC+MSHD	100	1573	2.21	[64]
mullite/SiC	mullite whiskers	PC+MSHD	100	1573	1.87 × 10^-3 g cm^-2	[65]

Table 3 Summary of isothermal oxidation testing data of nanopaticle (NPs) toughened coatings.

Coating materials	Toughening materials	Fabrication methods	Oxidation test			Refs.
Coating materials	Toughening materials	Fabrication methods	Time (h)	Temperature (K)	Mass loss (%)	Refs.
SiC	-	slurry+PC	30	1773	0.27	[70]
SiC	SiCNPs		215	1773	0.27	[70]
SiC	-		70	1873	4.52	[71]
	10 wt.% ZrO₂NPs ticle_nannanostructured		70	1873	1.05
	10 wt.% ZrO₂NPs ticle_nannanostructured		100	1873	1.75
SiC	SiCNPs	PC+hydrothermal electrophoretic deposition	202	1773	0.79	[72]
SiC	SiCNPs		64	1873	1.3	[72]
MoSi₂/SiC	SiCNPs		260	1773	~1.06	[74]
MoSi₂/SiC	SiCNPs		80	1873	~1.26	[74]

Table 4 Summary of thermal shock test data of nanoparticles (NPs) toughened coatings.

Coating materials	Toughening materials	Fabrication methods	Temperature (K)	Cycles	Mass loss (%)	Refs.
SiC	SiCNPs	slurry+PC	1773	40	1.52	[70]
SiC	10 wt.% ZrO₂NPs ticle_nannanostructured	slurry+PC	1873	8	No spalling and cracking	[71]
SiC	SiCNPs	PC+hydrothermal electrophoretic deposition	1773	16		[73]
MoSi₂/SiC	SiCNPs	PC+hydrothermal electrophoretic deposition	1773	16		[74]

Fig. 7. SEM morphologies of as-deposited (a,b) conventional ZrC coatings and (c,d) ZrC nanostructured coatings [75].

Fig. 8. SEM (a,b) and TEM (c,d) images of CNTs directly grown on C/C [89].

Fig. 9. Mass losses of some C/C (a) and C/C-ZrC-SiC (b and c) samples with different coatings during thermal cycling [91,92].

Fig. 10. Summary of isothermal oxidation (1473 K/2 h) testing data of CNTs toughened coatings (type a [88] and type b [89]), where PyC5, 10, 15 represent that the PyC deposition time was 5, 10 and 15 min, respectively.

Fig. 11. Micrographs of SiCNWs and coatings: (a) SiCNWs obtained by CVD, (b) surface of coatings prepared by PC and (c) cross-section of coatings obtained by the CVD-PC two-step technique [134].

Fig. 12. SEM morphologies: (a) SiC-Si internal coatings on C/Cs; (b) as-synthesized ultra-long SiCNWs on the SiC-Si internal coatings (inset refers to SEM image of SiCNWs directly peeled from the coatings, with a scale bar of 1 μm); (c) high-magnification of the part area in (b); (d) surface and (e) cross-section of the ultra-long SiCNWs reinforced SiC-Si coatings: and representative features on the fracture surface of the coatings like nanowires pullout (f), pullout of the reticulate SiCNWs architecture (g) and nanowires bridging (h); as well as (i) cross-section of the coated C/C samples with ultra-long SiCNWs after isothermal oxidation test and (j) magnified partial area of the void as well as (k) magnified partial area of the crack in (i) [146].

Fig. 13. SEM morphologies: (a) surface of the porous layer with the bamboo-shaped SiCNWs on C/Cs (inset of figure refers to cross-section image, with a scale bar of 100 μm); (b) high-magnification of the part area in (a); (c) radial cracks in the pure HfC coatings generated during the indentation testing; (d) radial cracks in the ultrafine bamboo-shaped SiCNWs-reinforced HfC coatings generated during the indentation testing, (e) high-magnification of (d) indicates the presence of the crack deflection mechanism (f) corresponding to the schematic illustration image; (g) fracture surface of the ultrafine bamboo-shaped SiCNWs-reinforced HfC coatings indicates the presence of the unique mechanical interlocking mechanism (h) corresponding to the schematic illustration image [149].

Fig. 14. (a) SEM morphology of the porous SiC nanoribbons layer on C/Cs; (b) high-magnification image of (a) [152].

Fig. 15. (a) SEM fracture surface morphology of the interfacial area between the coatings and C/C substrate; (b) and (c) schematic description of the anchoring mechanism of in-situ grown SiC nanoribbons on the interfacial area between the coatings and C/C substrate [152].

Table 5 Comparison of isothermal oxidation properties of SiC nanowires (SiCNWs) toughened coatings.

Coating materials	Toughening materials	Fabrication methods	Oxidation test			Refs.
Coating materials	Toughening materials	Fabrication methods	Time (h)	Temperature (K)	Mass loss (%)	Refs.
MoSi₂-SiC	-	PC	110	1773	4.53	[133]
MoSi₂-SiC	SiCNWs	CVD+PC	110	1773	1.78	[133]
SiC-MoSi₂—CrSi₂	-	PC	155	1773	1.06	[134]
SiC-MoSi₂—CrSi₂	SiCNWs	CVD+PC	155	1773	0.64	[134]
SiC	-	CVD+PC	20	1773	7	[136]
SiC	SiCNWs	CVD+PC	44	1773	2.68	[136]
SiC	SiCNWs	CVD	420	1673	0.48	[137]
MoSi₂-WSi₂-SiC-Si	-	CVD+PC	24	1773	14.08	[139]
MoSi₂-WSi₂-SiC-Si	SiCNWs	CVD+PC	82	1773	3.24	[139]
CrSi₂-SiC-Si/SiC	-	PC+PC	76	1773	4.27	[140]
CrSi₂-SiC-Si/SiC	SiCNWs	PC+CVD+PC	316	1773	1.24	[140]
SiC-ZrB₂-ZrC/ SiC-Si	-	PC+PC	210.5	1773	4.49	[144]
SiC-ZrB₂-ZrC/ SiC-Si	SiCNWs	PC+EPD+PC	210.5	1773	0.27	[144]
mullite/SiC	-	PC+PADD	160	1773	3.7	[145]
mullite/SiC	SiCNWs	PC+HEPD+PADD	235	1773	3.57	[145]
SiC-Si/SC-Si	-	PC+PC	22	1773	3.74	[146]
SiC-Si/SC-Si	Ultra-long SiCNWs	PC+CVD+PC	150	1773	0.44	[146]
SiC	Bamboo-shaped SiCNWs	CVD+PC	72	1773	0.5	[150]
Si-Cr/SiC-Si	Bamboo-shaped SiCNWs	PC+HT+PC	185	1773	-0.79	[151]

Table 6 Summary of thermal shock testing data of SiC nanowires (SiCNWs) toughened coatings.

Coating material	Toughening materials	Fabrication methods	Cycle	Temperature (K)	Mass loss (%)	Refs.
SiC-Si	-	CVD+HPRS	30	1773	4.14	[102]
SiC-Si	SiCNW	CVD+HPRS	30	1773	2.41	[102]
SiC-MoSi₂—CrSi₂	-	PC	30	1773	6.92	[134]
SiC-MoSi₂—CrSi₂	SiCNW	CVD+PC	30	1773	3.42	[134]
SiC	-	CVD+PC	20	1773	4.15	[135]
SiC	SiCNW	CVD+PC	20	1773	1.25	[135]
SiC	-	CVD	15	1773	7.075	[138]
	SiCNW	CVD	15	1773	4.29
	SiCNW	OPT+CVD	15	1773	2.225
MoSi₂-WSi₂-SiC-Si	-	CVD+PC	30	1773	4.83	[139]
MoSi₂-WSi₂-SiC-Si	SiCNW	CVD+PC	30	1773	2.08	[139]
SiC-ZrB₂-ZrC/SiC-Si	-	PC+PC	30	1773	11.13	[144]
	SiCNW	PC+CVD+PC	30	1773	2.28
	SiCNW	PC+EPD+PC	30	1773	0.52
Mullite/SiC	-	PC+PADD	40	1773	4.39	[145]
Mullite/SiC	SiCNW	PC+HEPD+PADD	50	1773	0.03	[145]

Fig. 16. SEM morphologies: as-prepared SiC nanowires (SiCNWs) (a); SiCNWs wrapped by PyC layers (SiCNW@PyC) with the thickness of 1.5 μm before (b) and after (c) heated at 2373 K and SiCNW@PyC with the thickness of 1 μm heated at 2373 K (d); as well as pure SiCNWs after heat treatment at 2073 K (e), 2173 K (f), 2273 K (g), and 2373 K (h) The bottom-left corner insets are the corresponding X-ray diffraction (XRD) pattern and the top-right corner insets are the high magnification [160].

Fig. 17. Transmission electron microscopy (TEM) image of the SiCNW@PyC structures showing the location of the nanowires (a), high-resolution TEM (FRTEM) image of the SiCNW/PyC interface (area A) (b) and TEM images of SiCNWs wrapped by PyC layers with the thickness of 1 μm heated at 2373 K. The insets are the corresponding selected-area electron-diffraction (SAED) pattern [160].

Fig. 18. Schematic of preparing SAPS-ZrB2-ZrC coatings with SiCNW@PyC core-shell networks on C/C-ZrB2-ZrC-SiC substrates (a), and SEM/TEM images of SiCNW@PyC core-shell structures (b) [162].

Fig. 19. Schematic illustration of preparing HfC nanowires (HfCNWs)-toughened coatings on SiC—C/Cs [176].

Fig. 20. Surface SEM morphology (a) (scale bar in the inset figure is 100 nm); XRD pattern (b) of the synthesized HfCNW porous layer on SiC-coated C/C samples; TEM image of a single HfCNW (c) (inset is the EDX pattern of the HfCNWs); SAED (selected area electron diffraction) pattern (d) and HRTEM (high resolution transmission electronmicroscopy) image (e) recorded from the square area in (c) [176].

Fig. 21. SEM morphologies of the synthesized SiC/HfC coatings (a,b) and those with HfCNWs (c,d), as well as cross-section SEM morphologies of SiC/HfC coated samples (e,g,i) and those with HfCNWs (g,h,j) in central ablation region after the cyclic ablation [177].

Table 7 Summary of isothermal oxidation test data of HfC nanowires (HfCNWs) toughened coatings.

Coating materials	Fabrication methods	Oxidation test					Refs.
		Without HfCNWs		With HfCNWs		Mass loss reduced by (%)
		Condition	Mass loss (%)	Condition	Mass loss (%)	Mass loss reduced by (%)
SiC	CVD+ PC	1773 K/20 h	12.54	1773 K/76 h	3.80	-	[173]
TaSi₂-TaC-SiC-Si	CVD+ PC	1773 K/77 h	6.43	1773 K/100 h	1.38	-	[174]
TaSi₂-TaC-SiC-Si/SiC	PC+CVD+ PC	1773 K/151 h	3.34	1773 K/340 h	1.77	-	[175]
Si-Mo-Cr/SiC	PC+CVD+ PC	1773 K/270 h	1.18	1773 K/270 h	0.19	83.9	[176]

Table 8 Summary of thermal shock test data of HfC nanowires (HfCNWs) toughened coatings.

Coating materials	Fabrication methods	Thermal shock test from 1773 K to room temperature for 30 time			Refs.
		Without HfCNWs	With HfCNWs	Mass loss reduced by (%)
		Mass loss (%)	Mass loss (%)	Mass loss reduced by (%)
TaSi₂-TaC-SiC-Si	CVD+ PC	4.37	3.18	27.23	[174]
TaSi₂-TaC-SiC-Si/SiC	PC+CVD+ PC	2.73	0.96	64.84	[175]
Si-Mo-Cr/SiC	PC+CVD+ PC	3.56	2.36	33.71	[176]

Fig. 22. Schematic diagram of SiC/HfC coated samples in central ablation region during cyclic ablation tests: (a)-(c) without HfCNWs; (d)-(f) with HfCNWs [177].

Table 9 Ablation testing data of nanomaterials toughened coatings.

Coating materials	Toughening materials	Fabrication methods	Ablation conditions	Time (s)	Mass ablation rate (mg/s)	Linear ablation rate (μm/s)	Refs.
ZrC	-	LPCVD	Oxyacetylene, flame ~3300 K, 4200 kW/m², O₂:0.4 MPa-0.42 L/s, C₂H₂:0.95 MPa-0.31 L/s	100	0.19	0.73	[75]
	ZrCNPs	LPCVD		100	0.11	0.36
SiC	-	PIP	Oxyacetylene, O₂/C₂H₂ (gas flow) =2:1	600	2.6	6.2	[76]
	9.09 wt.% SiCNPs			600	2.1	5.1
	16.67 wt.% SiCNPs			600	1.3	4.1
	23.68 wt.% SiCNPs			600	1.6	4.6
HfC	SiCNWs	CVD+CVD	Oxyacetylene, surface 2573 K, O₂:0.4 MPa-0.244 L/s, C₂H₂:0.095 MPa-0.167 L/s	60	0.19	-2.7	[153]
	-	CVD		60	0.34	-6.3
Si-Mo-Cr	SiCNWs	BT+CVD+PC	Oxyacetylene, surface 1873 K, O₂:0.4 MPa-0.88 m³/h, C₂H₂:0.095 MPa-0.65 m³/h	30 × 5s	15.31 mg cm^-2	-	[154]
	-	BT+PC		30 × 5s	28.56 mg cm^-2	-
SiC/HfC	HfCNWs	PC+LPCVD+SAPS	Oxyacetylene, 2400 kW/m², O₂:0.4 MPa-0.244 L/s, C₂H₂:0.095 MPa-0.167 L/s	3 × 60s	0.444	-0.767	[177]
	-	PC+SAPS		3 × 60s	1.341	-0.333
HfC	HfCNWs (CCVD for 1 h)	CCVD+CVD		120	1.21	1.48	[172]
	-	CVD		120	0.41	-1.53
SiC/ZrB₂-SiC	HfCNWs	PC+LPCVD+SAPS		90	-0.12	-	[178]
	-	PC+SAPS		90	0.20	-

Fig. 23. SEM morphologies of carbon fibres after grafting SCNTs (spreading grafting CNTs) (a,c and the inset of c) and RCNTs (radial grafting CNTs) (b,d and the inset of d) [196].

Fig. 24. Schematic of the structure (Left) and fracture morphology (Middle), as well as flexural stress-strain curves (Right) of C/C, C/C—Cu and C/C—Cu-CNTs [198].

Fig. 25. (a) Illustration of the ablation setups; (b) the variation of surface temperature with ablation time during the ablation process; (c) simulated velocity filed of the ablation process by Ansys Fluent; (d) effect of the velocity field on the surface morphology of C/Cs [199].

Fig. 26. Ablation behaviors of C/Cs versus EPD time (min): (a) ablated surface morphology; (b) linear and mass ablation rates and (c) height map for the ablated samples, where the surface of the original sample was marked as 0; (d) brief illustration of the ablation process cross section [199].

Fig. 27. Literature summary of the common matrix modification measures for decreasing the mass (a) and (b) linear ablation rates of C/Cs at a lower density, successively cited from [[200], [201], [202], [203], [204], [205], [206], [207], [208], [209], [210], [211], [212], [213]] and [199], where the data are average values.

Fig. 28. Carbon-bonded carbon fibers composites (CBCFCs) with in-situ grown SiCNWs: (a) schematic illustration for the fabrication of CBCFCs with in-situ grown SiCNWs; (b) the SiCNWs bridging between the PyC matrix and the carbon fibers at the fracture surface of CBCFCs; (c) the stress-strain curves for flexural tests [214].

Fig. 29. Schematic diagram of carbon fiber cloth laminated perform introduced with SiCNWs (a); SEM morphologies of carbon fiber cloth before (b) and after (c) electrophoretically depositing (EPD) SiCNWs and the corresponding cross-section image (d) [216].

Fig. 30. SEM morphologies of C/Cs and SiCNWs-C/Cs after oxidation [216].

Fig. 31. SEM micrographs show different roles of SiCNW networks in the formation of the network reinforced film after ablation for 240 s: (a) interlocking effect among molten sheets, (b) network bridging and bonding, (c) crack deflection and bridging, (d) pinning effect [217].

Fig. 32. Schematic diagrams of preparation process of SiCNW@PyC—C/C-ZrC-SiC (A) [36] and HfCNWs-C/C (B) [37] composites.

Fig. 33. TEM images of GO-grafted CF (a) and (b), and TEM images of CNTs grown on GO-grafted CFs (c) and (d) [225].

Fig. 34. (a) Photo of carbon fiber (CF)/high-silica fiber (HSF) preform, (b) Schematic diagram of the 0/90 lay-up structure, and (c) Integral structure photo of CF-HSF/C-SiC composite [227].

Fig. 35. Geometry of the hybrid thermal protection material (TPM) (a) macrograph of the test samples with dimensions of 120 × 120 × 30 mm3, which were attached to an aluminum alloy plate filled in a copper water-cooled basement, where the dimensions of the coated-C/Cs (Upper) were 20 × 120 × 10 mm3, and the dimensions of the mullite fiber (MF) tiles (Lower) were 20 × 120 × 20 mm3; (b) schematic of the test samples in plasmatron, where the basement enabled the test models to be moved into or out of the flow via mechanical control, and an angle of 15° was selected between the torch tube and the sample; (c) typical screenshot for the video recording of sample in plasma flow [229].

Table 10. Summary of isothermal oxidation testing data of micro/nano multiscale strategies reinforced C/Cs.

Matrix materials	Toughening materials	Fabrication methods	Oxidation test			Refs.
Matrix materials	Toughening materials	Fabrication methods	Time (min)	Temperature (K)	Mass loss (%)	Refs.
C/C	-	CVI	200	873	19.2	[226]
	SiCNWs	EPD+CVI	200	873	8.6
	-	CVI	40	1073	89.5
	SiCNWs	EPD+CVI	40	1073	69.7
C/C	-	CVI	180	873	2.04	[195]
	CNTs	CCVD+CVI	180	873	0.85
	-	CVI	180	1173	78.27
	CNTs	CCVD+CVI	180	1173	69.24
C/C	-	CVI	500	843	41.1	196]
	SCNTs	CCVD+CVI	500	843	29.8
	RCNTs	CCVD+CVI	500	843	16.1
C/C	-	CVI	10	973	0.6	197]
	CNF	CCVD+CVI	10	973	0.2
	-	CVI	10	1173	3.7
	CNF	CCVD+CVI	10	1173	3.2

Table 11. Ablation testing data of micro/nano multiscale strategies reinforced C/Cs.

Matrix materials	Toughening materials	Fabrication methods	Abl ation conditions	Time (s)	Mass ablation rate (mg/s)	Linear ablation rate (μm/s)	Refs.
C/C-ZrB₂-ZrC-SiC	SiCNWs	CVI+PIP	Plasma flame, surface ~2573 K	240	0.173	0.063	[217]
C/C-ZrC-SiC	SiCNWs	CLVD	Oxyacetylene, surface 2573 K	90	1.39 ± 0.27	1.72 ± 0.20	[36]
	SiCNW@PyC		Oxyacetylene, surface 2573 K	90	0.47 ± 0.19	0.73 ± 0.14
	SiCNWs		Oxyacetylene, surface 3273 K	90	4.57 ± 0.29	3.74 ± 0.22
	SiCNW@PyC		Oxyacetylene, surface 3273 K	90	1.99 ± 0.21	1.59 ± 0.12
C/C	-	ICVI	Oxyacetylene, surface 2573 K	20	6.8	29.7	[37]
	HfCNWs	PIP+ICVI	Oxyacetylene, surface 2573 K	20	3.2	7.5
C/C	-	CVI+PIP	H₂(7.6 L/min)-O₂(4.6 L/min) flame, surface ~3073 K	750	8.14	5.29	[228]
	SiCF	CVI+PIP	H₂(7.6 L/min)-O₂(4.6 L/min) flame, surface ~3073 K	750	2.16	1.88

Fig. 36. SEM morphologies of the C/Cs with co-deposition of SiCNWs and CNTs by EPD for 120 s: (a) Cross-section morphology; (b) Surface morphology; (c) Magnification of (b) [233].

Fig. 37. SEM morphologies after oxidation of the SiC coated C/Cs without (a) and with (b) the co-deposition of SiCNWs and CNTs; (c) Magnification of (b); (d) XRD pattern of the coated C/Cs after oxidation [233].

Table 12. Summary of isothermal oxidation testing data of hybrid micro/nano multiscale routes reinforced coatings.

Coating materials	Toughening materials	Fabrication methods	Oxidation test			Refs.
Coating materials	Toughening materials	Fabrication methods	Time (h)	Temperature (K)	Mass loss (%)	Refs.
SiC	-	-	10	1373	15	[230]
SiC	CNTs-SiCWs	-	10	1373	0.7	[230]
SiC	-	CVR	1	1673	1.72	[232]
SiC/SiC	HMNR	CVR+CVD	400	1673	1.67	[232]
SiC	-	PC	45	1773 K	~1.35	[233]
	SiCNWs-CNTs	EPCD+PC	45	1773 K	-0.03052
	SiCNWs-CNTs	EPCD+PC	100	1773 K	1.08

Table 13. Summary of thermal shock test data of hybrid micro/nano multiscale routes reinforced coatings.

Coating materials	Toughening materials	Fabrication methods	Temperature (K)	Cycles	Mass loss (%)	Refs.
SiC	SiCNWs	-	1773	25	2.75	[231]
SiC	CNS-SiCNWs	-	1773	25	2.38	[231]
SiC/SiC	HMNR	CVR+CVD	1673	34	1.67	[232]

Fig. 38. Fracture behavior of SiCNWs-reinforced CBCFCs. (a) SEM surface image of the composite at low magnification. (b) SEM image of the composite at a high magnification (insert shows high magnification of SiCNWs). (c) SiCNWs pull-out of the silicon oxycarbide (SiOC) ceramics. (d) SiCNWs bridging the carbon fibers and SiOC ceramics. (e) SEM image of carbon fibers pull-out of SiOC ceramics. (f) SEM image of the tensile fracture of carbon fibers and SiCNWs [234].

Fig. 39. Microstructure of different preforms: Distribution of SiCNWs on each direction (a) and single bundle (b) of carbon fiber cloth via electrophoretic deposition (EPD) with the magnified view (c). Microstructure of SiCNWs decorated with carbon nanosheet (CNSs) on carbon fibers (d) and the inset. EDS pattern of SiCNWs decorated with carbon nanosheet, elemental distribution of carbon (e) and silicon (f). Raman spectra of different carbon fibers preforms (g) [235].

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Micro/nano multiscale reinforcing strategies toward extreme high-temperature applications: Take carbon/carbon composites and their coatings as the examples

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