Short-term oxidation and residual compression properties of needle-punched carbon/carbon composites

Abstract

Needle-punched carbon/carbon (NP C/C) composite is widely used in rocket-engine nozzles and re-entry vehicles. Recyclable technology expedited the research on repeated oxidation and residual mechaincal properties of thermal-protection materials. In this study, the critical longitudinal compression strengths before and after oxidation are derived based on the Timoshenko beam theory. Three repetitions of short-term oxidation cycles and compression experiments are investigated. The average oxidation rate of this composite was 5∼6% in 10 min and kept linear increase. In-plane and out-of-plane compressive strengths of NP C/C composite diminish quasi-linearly due to oxidation at 1000°C, with their moduli decreasing in a periodically slow-sharp pattern. After three oxidation cycles, the levels of residual in-plane modulus and strength were 55.20% and 56.89%, respectively, while the resudual out-of-plane modulus and strength were 44.65% and 47.23%, respectively. The results showed that the material exhibited the pesudo-plastical behaviour after oxidation, cracks grew along the punched conical structures formed by the punching technology. In-plane and out-of-plane modulus were more sensitive than their strengths after first oxidation cycle.

Keywords

needle-punched carbon/carbon composites repeated oxidation compression properties experimental investigation

Introduction

Fiber reinforced composites are widely used in aerospace engineering, with reuse and recycling research becoming more prominent to achieve low-carbon global targets.^1,2 The reuse and recycling of fiber-reinforced composites³ employ mechanical, thermal and chemical recycling techiques and various studies considered different approaches. Goncalves et al.⁴ demonstrated that the addition of waste fiberglass could be used to modify the brittle behavior and flexural strength of gypsum. Abdou et al.⁵ studied the recycling of polymeric composite from industrial waste for carbon fibers. Chen et al.⁶ studied the effect of reaction conditions on the molecule structure, thermal and mechanical properties of thermoplastic epoxy. Nachtane et al.⁷ studied the relationship between microstructural parameters and the mechanical properties of a recycled thermoplastic composite material. Yao et al.⁸ designed a degradable unsaturated polyester resin and provided a new method for efficient degradation and recycling of fiber-reinforced thermosetting resin composites. Zhang et al.⁹ proposed a 3D printing approach for fully recyclable continuous fiber self-reinforced composites utilizing supercooled polymer melts. Barnett et al.¹⁰ introduced recycled carbon fibers into three matrices (polyphenylene sulfide, acrylonitrile butadiene styrene and structural epoxy), and evaluated their specific energy absorption, crush efficiency and steady-state crush stress. Singh and Bedi¹¹ explored the influence of addition of graphene nanoplatelets on the fatigue performance of glass-fiber-reinforced composites based on recycled polyethylene terephthalate. Esmaeili et al.¹² focused on evaluation of the mechanical and performance characteristics of a new plastic composite sleeper made from recycled polyethylene combined with filler materials. Copenhaver et al.¹³ examined the effects of mechanical recycling on additively manufactured parts from bio-based feedstock.

Carbon/carbon (C/C) composites have an excellent combination of light weight, high strength and thermal protection,^14–18 so they are widly used in the re-entry engineering. The recycle use of C/C composite could reduce the related costs and protect the enviroment. Akbar and Liew¹⁹ investigated the effects of elevated temperatures (up to 900°C) on the reinforcement mechanism of recycled carbon-fiber composites. Hu et al.²⁰ investigated the crack-development behavior in thermally sprayed anti-oxidation coating after short- and long- term oxidation with repeated thermal cycles from 1500°C to room temperature. Research on the multiple oxidation cycles of thermal-protection materials is a newly developed focus as a result of a broader use of the rocket-recovery technology.

The failure mechanism of composite under longitudinal compression is complex and complicated.²¹ Many damages in the failure process are exhibited, for example, shear plastic deformation,^22,23 matrix crack,^24,25 fiber kink band,²⁶ and so on. Lots of experiments and simulations were investigated to explore the mechanism of kink band. Bai and Phoenix developed a new micromechanical model for the compressive failure process in unidirectional composites.²⁷ Narayanan and Schadler²⁸ presented a new mechanism of kink-band formation to explain the experimental observations. Zhang et al.²⁹ conducted theoretical analysis and finite element simulation to analyze kink angle as well as compressive strength of composite. Ferguson et al.³⁰ developed a compressive strength prediction method considering 3D fiber orientation distributions. Wang et al.³¹ proposed a novel inter-fiber failure criterion of composites based on micro-scale failure mechanism, and derived a cross-scale stress formula based on the inclusion theory.

In this paper, a microscale structure of NP C/C composite was analysed with the micro-computed tomography (μ-CT), its repeated short-term oxidation behaviors at 1000°C were investigated experimentally and their morphologies were compared employing the scanning electron microscopy (SEM). In the analysis, the Timoshenko beam theory was used for the fibers, while the matrix was considered as an elastic foundation. The critical compression strengths of composite before and after oxidation were derived, while the residual in-plane and out-of-plane compressive strenghs and moduli of the NP C/C composite after oxidation at 1000°C were surveyed with experiments.

Structure of NP C/C composite

NP C/C composite is a quasi 3D composite material. It is produced by chemical vapor deposition (CVD) or chemical vapor infiltration (CVI) technologies. The preform was layered alternately with orthometric 0° and 90° carbon fiber woven clothes (Figure 1), and the short-cut carbon fiber felts were placed between them. The preform was punched with the specially designed needle plate, the punched parts of short-cut felts forming inverted conical structures to join adjacent layers together in order to increase the mechanical interlaminar performance.

Components and structural morphologyies of NP C/C composites were analized with mirco-computed tomography (μ-CT) technology. The volume fractions of fibers, pyrocarbon matrix and pores were 62.2%, 32.6% and 5.2%, respectively. In the preform, the continuous fibers were deflected in punching areas. Generally, the deflection can extend to the adjacent layers with the same laying angle, even also they were broken in the central area of puncing points. The carried short-cut felts on the needles formed inverted conical structures along the lamination direction, in order to improve the interlaminar properties.

Compression failure citeria

In compression, the failure of 0° layers is caused by localized buckling of fibers,³² with microbuckling and kink-band-formation models being the two main mechanisms.

In an un-oxidized composite, a representative element of a two-dimensional model was established, a long fiber embedded in a homogeneous matrix (Figure 2). The Timoshenko shear-deformation beam theory was employed for the fiber, while the matrix was considered as an elastic foundation. The critical buckling load²⁰ was derived according to the stationarity condition for the total potential energy of the representative element:

P^{f} = \frac{H^{f}}{v^{f}} G_{13}^{c} + {[\frac{(1 - v^{f}) (G^{f} - G^{m})}{(1 - v^{f}) G^{f} + v^{f} G^{m}}]}^{2} \frac{π^{2} D^{f}}{{(\hat{L} L)}^{2}} .

(1)

Here, H^f and H^m are the relative dimensions of the fiber and the matrix in unit thickness, respectively;

G_{13}^{c} = {(\frac{v^{f}}{G^{f}} + \frac{1 - v^{f}}{G^{m}})}^{- 1}

is the effective shear modulus of composite, G^f and G^m are the transverse moduli of the fiber and the matrix, respectively; D^f=E^fI_y is the bending stiffness about the y-axis of the fiber;

v^{f} = \frac{H^{f}}{H^{f} + 2 H^{m}}

is the fiber volume fraction. Superscripts ‘m’, ‘f’ and ‘c’ refer to the matrix, the fiber and the composite, respectively;

\hat{L}

is the normalized effective-length parameter of the Euler beam;

\hat{L} = 1

for a simply supported boundary condition;

\hat{L} = 0.5

for a fixed-fixed boundary condition; L is the fiber length; P is the axial compressive force.

The critical longitudinal compression strength of the composite is solved:

σ_{1}^{c} = v^{f} \frac{P^{f}}{H^{f}} = G_{13}^{c} + \frac{v^{f}}{H^{f}} {[\frac{(1 - v^{f}) (G^{f} - G^{m})}{(1 - v^{f}) G^{f} + v^{f} G^{m}}]}^{2} \frac{π^{2} D^{f}}{{(\hat{L} L)}^{2}} .

(2)

Based on the Timoshenko beam theory, the uniform shear strain of fiber is:

γ_{13}^{f} = \frac{d w^{f}}{d x} - φ^{f} .

(3)

Here, φ is the angular rotation of the planar cross section, w is the vertical displacement of the fiber neutral axis (Figure 2).

The shear stress on the interface can be written as

{\begin{cases} τ_{13}^{f} = τ_{13}^{m} = \frac{G^{f} G^{m}}{(1 - v^{f}) G^{f} + v^{f} G^{m}} \frac{d w^{f}}{d x} = G_{13}^{c} \frac{d w^{f}}{d x} \\ φ^{f} = \frac{(1 - v^{f}) (G^{f} - G^{m})}{(1 - v^{f}) G^{f} + v^{f} G^{m}} \frac{d w^{f}}{d x} \end{cases} .

(4)

It is obvious that the shear stress on the interface depends on the gradient of the vertical displacement along the longitudinal direction.

The misalignment curve of fiber after compression can be assumed to be cosinoidal wave:

w^{f} = A \cos (\frac{π x}{λ_{0}}) .

(5)

Here, A is the transverse amplitude of misalignment corresponding to the mode shape, λ₀ is the initial half-wavelength.

In the process of oxidation, the oxidation rates of interface and matrix were higher than that of fibers, as a result, the fiber was exposed. The oxidized part of the elastic foundation was removed, releasing the initial stress between the fiber and matrix, so the ability of resistance to shear between them was diminished. It meant that the inverse shear stress was applied to the residual fibers. Especially, oxygen diffused through the defects and holes inside the matrix, with the residual fiber between two defects forming a constrained configuration. The critical buckling load was derived with the ‘Euler formula’ as

F^{f} = \frac{π^{2} D^{f}}{{(0.5 l^{f})}^{2}} .

(6)

Here, l^f is the distance between the two fixed ends of the residual fiber after oxidation.

The critical buckling effective stress of the composite is solved:

σ_{b}^{c} = v^{f} \frac{F^{f}}{H_{r}^{f}} = \frac{H^{f} π^{2} D^{f}}{H_{r}^{f} (H^{f} + 2 H^{m}) {(0.5 l^{f})}^{2}} .

(7)

Here,

H_{r}^{f}

is the relative dimensions of the residual fiber after oxidation.

Oxidation behavior of NP C/C composite

NP C/C composite was analyzed with thermogravimetric (TG) analysis (Figure 3) and differential scanning caborimetry (DSC).³³ They were heated from the room temperature to 1000°C in air atmosphere environment, with the rate of 10°C/min. At 829°C and 869°C (Figure 4), the pyrocarbon matrix and the fibers were oxidized, successively. The oxidation process of each component was approximatively linear up to 1000°C.

Repeated short-term oxidation behavior of NP C/C composite was investigated experimentally at constant temperature (1000°C) in Muffle furnace (Figure 5). Six samples were splited into three groups: the first group (#1 and #2) were oxidized for 10 min, the second group (#3 and #4) were oxidized for 20 min and the third group (#5 and #6) were oxidized for 30 min. The mass of each sample was measured every 10 min (Table 1). After 10 min oxidation, the average mass-loss ratio of six samples (#1∼#6) was 5.65%. After 20 min oxidation, the average mass-loss ratio of four samples (#3∼#6) was 11.64%. After 30 min oxidation, the average mass-loss ratio of two samples (#5∼#6) was 18.01%. The evolution of mass-loss ratio with time was almost linear (Figure 6), confirming that they were in the steady-state oxidation regime.

Table 1.

Mass loss of samples in cyclic oxdation.

		10 minutes		20 minutes		30 minutes
Sample NO.	Initial mass ratio/%	Residual mass ratio/%	Mass loss ratio/%	Residual mass ratio/%	Mass loss ratio/%	Residual mass ratio/%	Mass loss ratio/%
#1	100	95.58	4.42	-	-	-	-
#2	100	94.01	5.99	-	-	-	-
#3	100	95.43	4.57	89.35	10.65	-	-
#4	100	92.41	7.59	87.59	12.41	-	-
#5	100	94.11	5.89	88.99	11.01	81.59	18.40
#6	100	94.5	5.50	87.50	12.50	82.38	17.62
Average	100	94.34	5.65	88.36	11.64	81.99	18.01

The microscale morphologies of un-oxidized and oxidized (sample #6) NP C/C composite were analysed with the SEM. Before oxidation, the deposited pyrocarbon particles surrounded and bonded the preforms (Figure 7(a)), then they formed the interface and the matrix. The pyrocarbon matrix supported the fibers and provided an adhesive layer to carry the load.

In the process of oxidation, due to desorption and diffusion of oxygen through pores, the deposited pyrocarbon particles were oxidized first. Due to the small space inside of the fiber bundle, pyrocarbon particles deposited as smooth layer (SL) morphology. Rough layer (RL) and isotropic morphologies were formed between the fiber bundles, so the matrix between them and the interfaces inside them were oxidized more quickly. The oxidized fibers demonstrated the shape of bamboo shoots (Figure 7(b)). In order to screen the elements of the NP C/C composite, the energy spectrum was analyzed (Figure 8). The results indicated that some calcium and silicon were in the pyrocarbon matrix.

Residual compression behavior

The in-plane and out-of-plane compression tests on samples were preformed before and after oxidation were investigated. The dimensions of the samples were 15 mm × 15 mm × 15 mm. The loading velocity was controled at 0.5 mm/min. The test results and stress-strain curves were recorded as shown in Figures 9–11.

In-plane compression

Before oxidation, brittle failure appeared under the uniaxial in-plane compressive load. A 35° penetrating crack was found inside the pyrocarbon matrix (Figure 9); it means that the shear stress resulted in the matrix failure. A small number of fibers was broken.

After the exposure, the pyrocarbon matrix and the fiber bundles were oxidized from outside into inside. Because the oxidation velocity of matrix was higher,³⁴ the fiber bundles of the outside were exposed as shown in Figure 10. Due to the different oxidation histories, the in-plane compressive strength and the modulus were affected to different degrees. With the increase in the oxidation time, the ultimate strain of this composite was enhanced (Figure 11) and the material after oxidation exhibited the pesudo-plastical behaviour. The oxidized pyrocarbon matrix could not support the residual bundle and provided the space for deformation of the bundle. Actually, the residual porous pyrocarbon matrix and the bundles carried the compressive load. The increase of porosity due to oxidation was the cause of increased strain.

The magnitudes of the in-plane compressive modulus and strength of the NP C/C composite after oxidation were compared with those before oxidation (Figure 11). When the specimens were oxidized repeatedly for three times, the respective mass loss ratios were 5.99%, 12.41% and 17.62% after subsequent cycles. The corresponding levels of the residual modulus were 90.23%, 65.82% and 55.20%, while those of the residual strength were 84.64%, 68.17% and 56.89% (Table 2).

Table 2.

In-plane compressive properties.

	Mass loss ratio/%	Modulus/GPa	Strength/MPa	Residual modulus ratio/%	Residual strength ratio/%
Initial	0	4.71	207.03	100.00	100.00
#2	5.99	4.25	175.24	90.23	84.64
#4	12.41	3.1	141.14	65.82	68.17
#6	17.62	2.6	117.77	55.20	56.89

Out-of-plane compression

Under the out-of-plane compressive load before oxidation, perforating cracks initiated at 45° and extended, with the inverted conical structures formed by the punching technology influencing their extension path: cracks grew along the punched conical structures (Figure 12). The intralaminar continous fibers broke due to the shear stress.

When the NP C/C composite was oxidized for 10 miniutes, the inclined crack appeared (Figure 13(a)), demonstrating that the residual pyrocarbon matrix could bear the shear stress and broke the bundles. When this composite was oxidized twice (20 miniutes in total) and thrice (30 miniutes), no cracks were visible (Figure 13(b) and 13(c)).

The out-of-plane compressive modulus and strength of NP C/C composite after oxidation were compared with those before oxidation (Figure 14). After one, two and three successive cycles, the corresponding levels of the residual modulus were 87.20%, 55.08% and 44.65%, respectively, while the residual strength was 90.39%, 68.53% and 47.23%, respectively (Table 3).

Table 3.

Out-of-plane compressive properties.

	Mass loss ratio/%	Modulus/GPa	Strength/MPa	Residual modulus ratio/%	Residual strength ratio/%
Initial	0	7.19	282.23	100	100
#1	4.42	6.27	255.1	87.20	90.39
#3	10.65	3.96	193.42	55.08	68.53
#5	18.41	3.21	133.31	44.65	47.23

In-plane and out-of-plane compressive strengths of the NP C/C composite reduced quasi-linearly due to oxidation at 1000°C, while their modulus was decreased nonlinearly (Figure 15). The extent of reduction of mechanical properties of the oxidized 0° layer in orthometric laminates was more severe. When the mass loss ratio was less than 6%, the moduli decreased gently, with the first layer (90° layer) in the process of oxidation. When the second layer (0° layer) began oxidation, the compressive moduli declined more sharply than strength. After the mass loss ratio exceeded 12%, they decrease slowed again because the 90° layer started oxidation. The in-plane and out-of-plane compressive moduli were in a periodically slow-sharp decrease. The residual in-plane and out-of-plane compressive strength of composite mainly depended on the strengths of the weaker phase (pyrocarbon matrix), so the influence from oxidation of 0° and 90° layers was little different for compressive strengths that declined quasi-linearly with the mass loss due to oxidation.

The curves of residual levels of mechanical parameters versus the mass-loss ratio were fitted (Figure 15), with the fitting equations given as follows:

{\begin{cases} λ_{E_{i n}} (c) = 55.20 + \frac{44.80}{1 + {(c / 8.75)}^{3}} (%) \\ λ_{σ_{i n}} (c) = 98.8 - 2.42 c (%) \\ λ_{E_{o u t}} (c) = 44.65 + \frac{55.35}{1 + {(c / 8.42)}^{3}} (%) \\ λ_{σ_{o u t}} (c) = 103.11 - 3.11 c (%) \end{cases} .

(8)

Here, $λ_{E_{i n}}$ and $λ_{E_{o u t}}$ are the residual levels (in percent) of in-plane and out-of-plane modulus, respectively; $λ_{σ_{i n}}$ and $λ_{σ_{o u t}}$ are the residual levels of the in-plane and out-of-plane strengths, respectively; c is the mass-loss ratio of the composite. It showed that when the mass-loss ratio reached 34%, the residual level of the out-of-plane strength was close to zero, and that of the one of in-plane strength was only 16.5%.

Before oxidation, micro-buckling of fibers was a common failure mechanism under axial compression (Figure 16(a)), while the bonding between the pyrocarbon matrix and the fibers kept relatively well. After oxidation, residual fibers lost the support from the matrix due to oxidation, so the micro-bending deformation of fibers appeared under compression, with residual fibers broken due to buckling under lower stress (Figure 16(b)).

After in-plane compression, cracks generated between the layers and extended along the interface, with conical structures formed with punched fibers blockading the extension of cracks to some degree (Figure 17). The fracture position (highlighted with red in Figure 17) occurred at the tips of conical structures and in spaces between the fiber bundles.

In order to analyze the effect of repeated oxidation on the degradation of mechanical properties, a non-dimensional degradation rate (κ) was defined as follows:

κ = \frac{1 - λ}{c} .

(9)

Here, λ is the residual levels (in percent) of mechanical property aforementioned, c is the mass-loss ratio of the composite.

The dagradation rates of in-plane and out-of-plane moduli and strengths were listed in Tables 4 and 5, respectively. Their column charts were drew in Figures 18 and 19. The results indicated that degradation rates of mechanical properties were gentle after first oxidaiton cycle, they declined severely after twice and thrice oxidation cycle. In-plane and out-of-plane modulus are more sensitive than their strengths after first oxidation cycle, because pyrocarbon interface and matrix were oxidized firstly. So it is important to take some protective measures to prevent further oxidation before and after first service.

Table 4.

Degradation rate of in-plane properties.

	c/%	$λ_{E_{i n}}$ /%	$λ_{σ_{i n}}$ /%	( $1 - λ_{E_{i n}}$ )/%	( $1 - λ_{σ_{i n}}$ )/%	$κ_{E_{i n}}$	$κ_{σ_{i n}}$
#2	5.99	90.23	84.64	9.77	15.36	1.63	2.56
#4	12.41	65.82	68.17	34.18	31.83	2.75	2.56
#6	17.62	55.20	56.89	44.80	43.11	2.54	2.45

Table 5.

Degradation rate of out-of-plane properties.

	c/%	$λ_{E_{o u t}}$ /%	$λ_{σ_{o u t}}$ /%	( $1 - λ_{E_{o u t}}$ )/%	( $1 - λ_{σ_{o u t}}$ )/%	$κ_{E_{o u t}}$	$κ_{σ_{o u t}}$
#1	4.42	87.20	90.39	12.80	9.61	2.89	2.17
#3	10.65	55.08	68.53	44.92	31.47	4.22	2.95
#5	18.41	44.65	47.23	55.35	52.77	3.01	2.87

Conclusions

Oxidation and mechanical behaviours of the NP C/C composite at extremely high temperature affects the inservice safety of equipments. The approach, employing on the Timoshenko beam theory for fibers, with the matrix considered as an elastic foundation allowed the assessment of critical compression strengths of the composite before and after oxidation. The mass loss and compressive mechanical properties of the material were investigated experimentally after repeated oxidation. Before oxidation, brittle failure appeared under the uniaxial in-plane compressive load. A 35° penetrating crack was found inside the pyrocarbon matrix. Under the out-of-plane compressive load, perforating cracks initiated at 45° and extended. After three oxidation cycles, the levels of residual in-plane modulus and strength were 55.20% and 56.89%, respectively, while the resudual out-of-plane modulus and strength were 44.65% and 47.23%, respectively. The results showed that the material exhibited the pesudo-plastical behaviour after oxidation, cracks grew along the punched conical structures formed by the punching technology. In-plane and out-of-plane modulus were more sensitive than their strengths after first oxidation cycle. It is important to take some protective measures to prevent further oxidation after first service to reuse.

Footnotes

Declaration of Conflicting Interests

The author(s) declared no potential conflicts of interest with respect to the research, authorship, and/or publication of this article.

Funding

The author(s) disclosed receipt of the following financial support for the research, authorship, and/or publication of this article: This work was partially supported by National Natural Science Foundation of China (Grant No.12102152); State Key Laboratory of Mechanics and Control of Mechanical Structures (Nanjing University of Aeronautics and Astronautics, Grant No. MCMS-E-0221Y02).

ORCID iD

Meng Han

Data Availability Statement

The datasets generated and analyzed during the current study are available from the corresponding author on reasonable request.*

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