Research progress on interlaminar property of carbon nanotube-continuous fiber reinforced resin matrix composites
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摘要: 碳纳米管(Carbon nanotubes，CNTs)具有优异的力学、热学和电磁学性能，重要用途之一是改性传统的连续纤维增强树脂基复合材料，赋予其更佳的机械强度和多功能性。针对连续纤维增强树脂基复合材料，综述了多种引入CNTs的方法，并就CNTs对连续纤维增强树脂基复合材料性能的影响展开评述，重点介绍了CNTs聚集体改性连续纤维增强树脂基复合材料层间性能的最新研究进展，并展望了未来发展方向。Abstract: Carbon nanotubes (CNTs) has excellent mechanical, thermal and electromagnetic properties. One of its important applications is to modify continuous fiber reinforced resin matrix composites to afford them better mecha-nical and multifunctional properties. For continuous fiber reinforced resin matrix composites, several methods of introducing CNTs are summarized. The interlaminar properties of CNTs-continuous fiber reinforced resin matrix composites are revealed. The latest progress on CNT assemblies-continuous fiber reinforced resin matrix compo-sites is introduced in detail and their future development is also discussed.
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图 1 复合材料层间性能改善方法的发展历程
Figure 1. Development of interlaminar property reinforcement of composites
图 2 碳纳米管 (CNTs)改性连续纤维增强树脂基复合材料的方式示意图
Figure 2. Illustration of carbon nanotubes (CNTs) introduced into continuous fiber reinforced resin matrix composites
图 3 垂直排列碳纳米管(VACNTs)阵列转移印刷到预浸料上过程示意图
Figure 3. Illustration of transfer-printing process of vertically-aligned carbon nanotubes (VACNTs) forest to prepreg
图 4 直径20 nm 间距3倍直径的CNTs组成的VACNTs阵列[18-19]
Figure 4. Aligned CNT array structure comprised of millions of 20 nm-diameter CNTs spaced about 3 diameters apart [18-19]
(a) Optical image of CNTs array-wafer specimen (approx. 5×5×0.5 mm); (b) SEM image of the CNTs array (5 billion MWCNTs/cm2, measured density of 0.022-27 g/cm3 and aspect ratio of 25 000 : 1); (c) HRTEM image of CNTs showing a structure of about 10 walls with an outer diameter of 15 nm and an inner diameter of 4-5 nm
表 1 碳纳米管(CNT)聚集体改性连续纤维增强树脂基复合材料的层间剪切强度（ILSS）
Table 1. Interlaminar shear strength (ILSS) of carbon nanotube (CNT) assemblies modified continuous fiber reinforced resin matrix composites
Fiber/
ResinCNT
contentCNTs
morphologyCNTs
assembliesLay-up CNTs integration
methodFabrication method ILSS/MPa
(Increment)Ref. PWCF/
Epoxy13vol% MWCNTs
(10 walls,
douter=15 nm,
dinner=4-5 nm)Array (h=50-500 μm, 5 billion MWCNT/cm2, ρ=0.022-
0.027 g/cm3)NA ①MWCNTs array removed from wafer and bonded to tape; ②MWCNTs array transferred to carbon fabric Press molding 25.6 (0%) [13] T300-PWCF/
Epoxy18vol% MWCNTs
(d=7-10 nm)Array (h=200 μm,
ρ=0.022-0.027 g/cm3, 5 billion MWCNT/cm2, CNT spacing of
10-20 nm)Separate ply:
9 CNTs array layers +
10 prepregs① Sonication method; ② Adhesive tape method; ③ Mechanical twist method Autoclave 45.8 (80%,
Iosipescu-type shear)[14] UD IM7/
977-3NA MWCNTs Array (h=20 μm) 19 CNTs array layers +
20 prepregs (QI)Place hot iron on substrate and dry ice is applied on back of the substrate Vacuum bag 61.5 (50%, SBS) [15] 47.8 (47%,
Iosipescu-type shear)UD IM7-
G/8552NA MWCNTs Forest (h=5-25 μm) Sharing ply:
15 CNTs forest layers +
16 prepregs (QI)①Press wafer facedown on prepreg and cover with protective film; ②Place on hotplate and heat, apply pressure with roller; ③Peel away film and wafer Autoclave 99.6 (6.5%, SBS) [16] IM7-G/
8552NA MWCNTs
(3-7 walls,
d=8 nm)Forest (h=5-65 μm,
ρ=0.0195 g/cm3, ρaerial≈1vol%, CNTs spacing of ≈60 nm)15 CNTs forest layers +
16 prepregs (QI)①Apply pressure with roller; ②Allow forest to wick into adjacent ply NA 104.6 (8.75%, SBS) [17] Woven IM7/
8552NA MWCNTs Forest (h=75 μm) 11 CNTs forest layers +
12 prepregs (QI)NA Autoclave — (2%, SBS) [18] Forest (h=100 μm) — (−6.3%, SBS) UD AS4/
8552NA MWCNTs Forest (h=20 μm) NA ①Flip wafer onto prepreg and placed on hot plate; ②Take prepreg off the plate and apply pressure Autoclave — (0%) [19] Thick HT-
S40/Q-1112NA MWCNTs
(3-5 walls,
douter≈8 nm)Forest (h=20 μm, ρaerial≈1vol%,
109-1010 MWCNTs/cm2)5 CNTs forest layers +
16 prepregs (QI)Attach prepreg to a rolled cylinder, while pressure is applied, across the Si substrate containing CNT forest to transfer CNTs Autoclave 69.8 (0%, SBS) [20] Thin HTS40/
Q-111215 CNTs forest layers +
48 prepregs (QI)80.6 (5%, SBS) UD AS4/
8552NA MWCNTs
(3-7 walls,
douter≈8 nm,
dinner≈5 nm)Forest (h=20 μm, ρaerial≈1vol%, CNTs spacing of ≈60 nm) 15 CNTs forest layers +
16 prepregs (QI)① Si substrate was positioned with CNTs in contact with prepreg; ② Si substrate/ply assembly was placed on hot plate while pressure was applied Autoclave 96.2 (1.2%, SBS) [21] CF/
EpoxyNanofiber is 2wt% resin MWCNTs
(d=10-20 nm, l=5-15 μm)MWCNTs-EP/PSF hybrid nanofiber (MWCNTs-EP was 20wt% PSF) 16 CNTs veil layers +
16 prepregs①CF/Epoxy prepregs were attached
to drum collector; ②MWCNTs-EP/PSF suspension was directly electrospun onto rotating prepregFlat-plate vulcanizer — (11.9%, 3-point bending) [22] UD Hexcel IM2/Epoxy PR2032 0.016wt% MWCNTs (d=
10 nm)Highly aligned CNTs sheet (drawn from 0.3 mm tall VACNTs forests, t≈100 nm, ρ≈0.025 g/m2) Sharing layer: 15 CNTs
sheet-CF fabrics layers①Place CNT sheets on top and
bottom of CF fabrics; ②15 Layers
CNTs-CF fabrics were stacked
togetherRTM — (30%, SBS) [23] E-glass fabric/Epoxy 0.1wt% MWCNTs Aligned CNTs sheet (drawn out horizontally from VACNTs arrays, 100×50×1.5 mm, ρ=0.354 g/m2) Separate ply: 2 CNTs sheet layers + 32 prepregs (S) Transfer CNTs sheet onto prepreg during ply layup Vacuum bag
and hot press44.4 (0, SBS) [24] PWGF/Aero epoxy NA CNTs Stretched, densified sheet
(l=40 mm, w=2 mm, t=1-2 μm)Sharing layer: 11 CNTs sheet layers + 12 prepregs (S) Insert CNTs sheet in-between GF
plies, epoxy was used as adhesiveHot press 42.7 (9.1%, SBS) [25-26] CF/Un-
known resinNA CNTs Buckypaper NA NA Vacuum-bag — (3.3%, SBS) [27] UD GF/
EpoxyNA Commercially MWCNTs (d=5-
12 nm, l=30-
50 nm)Buckypaper (obtain by spray-vacuum filtration) 1 Buckypaper layer +
16 prepregs (S)Buckypaper was located between the mid-plane layers during the hand lay-up process Vacuum bag
and oven— (83.13%, 3-point bending) [28] PEI grafted UD CF/
Epoxy≈6vol% Commercially MWCNTs (d=20-
30 nm, l=10-
30 μm)Buckypaper (obtain by MWCNTs deposition) NA ① Buckypaper is deposited in situ or stacked on PCF; ② Fully impregnated; ③ Bubble elimination; ④ Stacking and hot pressing Hot press 59 (68.6%, SBS test) [29] MT300 CF/603 NA MWCNTs
(3-7 walls, d=6-
10 nm, acid treated)Randomly oriented film
(t=25 μm)1 CNT film layer +
14 prepregs (S)①Resin impregnation into CNT film; ②CF prepreg and CNT film were layered-up to prepare unidirectional composite laminates Autoclave 108 (Slightly decrease) [30] Randomly oriented film
(t=2 μm)13 CNT film layers +
14 prepregs (S)116 (5%) T700S/Epoxy 0.22wt% MWCNTs
(d=10-20 nm)Film
(CNTs bundles, d=50-60 nm)1 CNTs film layer +
12 prepregs (UD)①CNTs aerogel was deposited onto unidirectional CF fabric which was wrapped on a rotating spindle; ②Infused with epoxy resin;
③Stacked ply-by-ply in the same orientationHot-press molding 43.5 (21.51%, SBS) [31] HS CF/
EpoxyNA NA Randomly oriented commercially CNTs sheets (t=18-23 μm) 14 CNTs sheet layers +
16 prepregs (4S)Insert a CNTs sheet at each fiber/epoxy prepreg 0/90 interface, for a total amount of 14 layers Autoclave 70.51 (−2.6%, SBS) [32] Notes: douter—Outer diameter; dinner—Inner diameter; d—Diameter; h—Height; l—Length; t—Thickness; ρ—Density; ρaerial—Aerial density; MWCNTs—Multi-walled CNTs; SBS—Short beam shear; QI—Quasi-isotropic; S—Symmetry; CF—Carbon fiber; PW—Plain weave; UD—Unidirectional; PEI—Polyethylenimine; GF—Glass fiber; RTM—Resin transfer molding; NA—Not available from the cited studies; Separate and sharing ply—Prepreg of samples is individual or whole; EP—Epoxy resin; PCF—PEI funtionalized CF. 
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表 2 CNT聚集体改性连续纤维增强树脂基复合材料的层间断裂韧性
Table 2. Interlaminar fracture toughness of continuous fiber reinforced resin matrix composites modified by CNT assemblies
Fiber/
ResinCNTs
contentCNTs
morphologyCNTs assemblies Lay-up CNTs integration method Fabrication method GIC or GIIC/(J·m−2)
(Increment)Ref. Woven SiCf/
Epoxy2wt% MWCNTs Forest (h=60m) 2 CNTs grown-clothes ①CNTs grown on fiber cloth; ②Infiltrated; ③Stacked to yield a "sandwich" structure Autoclave GIC: 4260 (348%)
GIIC: 140 (54%)[33] IM7/977-3 MWCNTs to
forest is 1vol%CNTs (douter=8 nm) Forest (h=60 m, 150 m,
120 m, MWCNTs
spacing of 80 nm)1 CNTs forest layer +
24 prepregs (S)Prepreg is attached to a rolled cylinder, while pressure is applied, across the Si substrate containing
CNTs forest to transfer CNTsAutoclave GIC: 530 (250%) [34] AS4/8552 GIC: 340 (150%)
GIIC: 1100 (300%)T700/M21 MWCNTs to
forest is 1vol%MWCNTs (7 walls, dr=10 nm) Forest (h=100-200 m) 1 CNTs forest layer +
28 prepregs① Heat and pressure applied to Si substrate; ②Removal of substrate
after cool down period; ③Transplanted CNTs forest infused with resinVacuum bag GIC: 435 (31%)
GIIC: 1155 (161%)[35] T700/
SE84LVNA 1 CNTs forest layer +
14 prepregsGIC: 338 (61%) UD AS4/
8552MWCNTs to
forest is 1vol%MWCNTs (3-
7 walls, dinnerr≈5 nm, douter≈8 nm)Forest (h=(20±5) μm,
109-1010 MWCNTs/cm2, MWCNTs spacing of
80 nm)1 CNTs forest layer +
24 prepregsTransfer CNTs forest onto the tacky surface of the composite prepreg before laminate assembly Autoclave GIC, INIT: 300 (0%)
GIC, PROP: 220 (0%)[36] 1 CNTs forest layer+
30 prepregsGIIC, INIT: 1790 (24%)
GIIC, PROP: 580 (0%)CF/Epoxy Nanofiber is 2wt% resin MWCNTs
(d=10-
20 nm, l=5-15 μm)MWCNTs-EP/PSF hybrid nanofiber (MWCNTs-EP
was 20wt% PSF)16 CNTs veil layers +
16 prepregs①CF/Epoxy prepregs were attached
to drum collector; ②MWCNTs-EP/
PSF suspension was directly electrospun onto rotating prepregFlat-plate vulcanizer GIIC: — (48.4%) [27] G0926 WF/Epoxy vinyl ester 1vol% MWCNTs (3-5 walls, d=3-9 nm, l=1 mm) CNTs veil (t=30 m after infusion,
ρaerial=0.8 g/m2)1 CNTs veil layer+
8 prepregs (S)The interleaves were produced by winding continuous fiber of CNTs directly onto CF fabric wrapped around a cylindrical winder VARTM GIC, PROP: — (60%) [37] Densified CNTs veils GIC, PROP: — (–28.4%) T300 fabric/
E-51NA Carboxyl MWCNTs CNTs-decorated Polycaprolactone (PCL) nanofiber (ρaerial=15 g/m2) 1 CNTs-decorated
PCL layer +
16 prepregs①CNTs/PCL interleaf was placed in the mid-plane of the laminate;
②Hand lay-upHot-press GIC: 670 (68%)
GIIC: 2300 (44%)[38] PWCF/
EpoxyCNTs in interleaf is 0.5 and 1.0vol% Carboxyl MWCNTs (d=20-30 nm, l=10-
30 mm, —COOH content is 1.23wt%)CNTs/PSF nanofibrous paper (CNTs is 5wt% and 10wt% of PSF) 1 CNTs/PSF
nanofibrous paper
layer + 16 prepregs①CNTs/PSF nanofibrous paper is placed in the mid-plane;
②Hand lay-upVacuum bag and hot press GIC: 750 (53%)
GIIC: 1 870 (34%)[39] UD Hexcel IM2/Epoxy PR2032 0.016wt% MWCNTs (d=10 nm) Highly aligned CNTs sheet (drawn from
0.3 mm tall VACNT forests, t≈100 nm, ρ≈0.025 g/m2)Sharing layer:
15 CNTs sheet-CF
fabrics layers①Place CNTs sheets on top and bottom of CF fabrics; ②15 CNTs-CF fabrics layers were stacked together RTM GIC, INIT: — (57%);
GIC, PROP: — (30%)[28] E-glass fabric/
Epoxy0.1wt% MWCNTs Aligned CNTs sheet (drawn out horizontally from VACNTs arrays, 100×50×
1.5 mm, ρ=0.354 g/m2)Separate ply: 2 CNTs sheet layers +
32 prepregs (S)Transfer CNTs sheet onto prepreg during ply layup Vacuum bag and hot press GIC: 273 (46.77%, parallel),
225 (20.97%, perpendicular)
GIIC: 438 (−6.2%, parallel),
547 (17.13%, perpendicular)[29] IM7/8552 NA Single walled- and few walled-CNTs Stretched (121%) directional CNTs sheet (ρaerial=9.8 g/m2) 1 CNTs sheet layer +
32 prepregs (UD)①Pre-infused CNTs/epoxy sheet; ②Interleaving aligned, same direction for CNTs sheets and CF Vacuum hot press GIC: 200 (Decrease)
GIIC: 1101.6 (63%)[40] UD GF/
EpoxyNA Commercially MWCNTs (d=5-12 nm,
l=30-50 nm)Buckypaper (obtain
by spray-vacuum filtration)1 Buckypaper layer +
16 prepregs (S)Buckypaper is located between the
mid-plane layers during hand lay-up processVacuum bag and oven GIC, INIT: ≈800 (174.81%),
GIC, PROP: 2500 (179.97%);
GIIC: ≈1050 (55.12%)[33] PEI grafted UD CF/
Epoxy≈6vol% Commercially MWCNTs (d=20-
30 nm, l=10-30 μm)Buckypaper (obtain by MWCNTs deposition) NA ① Buckypaper is deposited in situ or stacked on PCF; ② Fully impregnated; ③ Bubble elimination; ④ Stacking
and hot pressingHot press GIIC: 650 (44.4%) [34] T700 CF/Epoxy NA Commercially MWCNTs (d=8-15 nm, l=5-15 mm) Crosslinked buckypaper (t=18-23 mm,
d=280 mm)1 Buckypaper +
16 prepregs (UD)Buckypaper is directly incorporated into the middle interface of laminates Autoclave GIC: 660 (74%)
GIIC: 2330 (82%)[41] Bi-direction-
al E-glass woven fabric/EpoxyNA MWCNTs Plasma-treated buckypaper (d=70 mm, t=50-75 μm) 1 Buckypaper +
14 prepregs①Attach plasma-treated buckypaper to roller and applied to impregnated GF surface; ②Wet hand lay-up Heat + press GIC: 560 (16%)
GIIC: 1796 (23%)[42] U3160/3266 NA MWCNTs (d=50-
100 nm, l=100-500 μm)CNTs film
(t=30-40 μm)23 CNTs films +
24 prepregs (UD)①CNTs film is laid between CF fabrics; ②Fully impregnated; ③Bubble elimination RTM GIC: 314.8 (0%)
GIIC: 2869 (120%)[43] UD HMC/ SE84LV NA Amino-MWCNTs
(6 walls, d=10 nm,
l=300 m)CNTs webs (10 layers, ρaerial=0.2 g/m2,
w=60 mm)10 CNTs web layers +
12 HMC/SE84LV prepregs (S)①CNTs forests grow; ②CNTs are directly drawn and wound onto Al frames;③Amino functionalization;
④ CNTs webs are laid down perpendicular to fiberHeat under constant vacuum GIC, CNTs: 467 (−9%)
GIC, EDA-CNTs: 580 (13%)
GIC, DAD-CNTs: 428 (−16%)[44] NTPT 402 NA MWCNTs (6 walls, d=10 nm, l=300 m) CNTs webs (10 layers, ρaerial=0.2 g/m2,
70×70 mm2)10 CNTs web layers +
6 NTPT 402 prepregs +
12 SE84LV prepregs (S)①CNTs forests grow; ②CNTs are directly drawn and wound onto Al frames to produce 70×70 mm2 webs; ③CNTs webs were laid down perpendicular to fiber Autoclave GIC, INIT: 140 (−44%);
GIC, PROP: 140 (−68%)[45] TeXtreme/SE84LV 10 CNTs web layers +
2 TeXtreme prepregs +
12 SE84LV prepregs (S)GIC, INIT: 160 (−11%)
GIC, PROP: 250 (0%)T300 fabrics/
EpoxyNA MWCNTs (d=10 nm, l=1 mm) CNTs film (CNTs deposition, ρaerial=0.58-12.48 g/m2) 1 CNTs film +
14 prepregs (UD)①CNTs film is laid between CF fabrics; ②Bubble elimination of epoxy;
③Fully impregnatedVARTM GIC, Quasi-static: 626 (100%)
GIC, Dynamic: 1380 (140%)[46] T300 fabrics/
EpoxyNA NA CNTs belt (100 mm×
5 mm×10 μm, ρaerial=
4.68 g/m2)CNTs belt layers +
12 prepregs (UD)①CNTs belts cut from CNTs film; ②Pre-impregnated CNTs belts; ③CNTs belts stitch UD CF fabrics; ④Impregnated VARTM GIC, VIS: 420.05 (95.2%)
GIC, PROP: 574.57 (62.5%)
GIIC: 1238.56 (94.3%)[47] Notes: EP—Epoxy resin; PSF—Polysulfone; CF—Carbon fiber; VARTM—Vacuum assisted resin transfer molding; GC—Critical energy release rate; HMC/SE84LV—High modulus carbon fibre/toughened epoxy resin prepreg; EDA—Ethylenediamine; DAD—1, 10-Diaminodecane; INIT—Initial; PROP—Propagation; PVA—Polyvinyl alcohol.
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表 3 不同高度VACNTs 阵列-碳纤维增强环氧树脂复合材料的力学性能[14]
Table 3. Mechanical properties of VACNTs array-carbon fiber/epoxy composite samples with VACNTs array of different heights [14]
VACNTs height/µm VACNTs content/
vol%ILSS/
MPaTensile strength/MPa 0 0 25.4 189.4 100 16 25.6 204.2 200 18 45.8 155.9 300 15 41 96.6 500 31 32.3 108.6 1000 33 32.2 NA Note: ILSS—Interlaminar shear strength.
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