3D打印连续碳纤维/聚醚酮酮复合材料工艺及其性能调控

周子彦; 范天翔; 张慧颖; 吴杰; 陈烨; 王华平

doi:10.13801/j.cnki.fhclxb.20221215.002

3D打印连续碳纤维/聚醚酮酮复合材料工艺及其性能调控

doi: 10.13801/j.cnki.fhclxb.20221215.002

周子彦^1,,
范天翔¹,
张慧颖¹,
吴杰¹,
陈烨^{1, 2, ,},
王华平¹

1.
东华大学　材料科学与工程学院，纤维材料改性国家重点实验室，上海 201620
2.
东华大学　产业用纺织品教育部工程研究中心，上海 201620

基金项目: 中央高校基本科研业务费专项资金(2232022 G-06)；上海市轻质结构复合材料重点实验室开放课题(2232019 A4-10)

详细信息

通讯作者:
陈烨，博士，教授，博士生导师，研究方向为3D打印及功能、智能化纤维　E-mail: chenye@dhu.edu.cn

中图分类号: TB332
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出版历程
- 收稿日期: 2022-10-20
- 修回日期: 2022-11-21
- 录用日期: 2022-12-02
- 网络出版日期: 2022-12-16
- 刊出日期: 2023-09-15

Process and performance control of 3D printed continuous carbon fiber/poly(ether ketone ketone) composites

1.
State Key Laboratory for Modification of Chemical Fibers and Polymer Materials, College of Materials Science and Engineering, Donghua University, Shanghai 201620, China
2.
Engineering Research Center of Technical Textiles, Ministry of Education, Donghua University, Shanghai 201620, China

Funds: Fundamental Research Funds for the Central Universities (2232022 G-06); Open Project Fund from Shanghai Key Laboratory of Lightweight Structural Composites (2232019 A4-10)

摘要

摘要: 以高热性能热塑性树脂—聚醚酮酮(PEKK)为基体与连续碳纤维(CCF)进行原位浸渍3D打印，制备连续碳纤维/聚醚酮酮复合材料(CCF/PEKK)，并系统研究了3D打印工艺参数中分层厚度、流量比、打印温度及成型方向对复合材料内部结构、基体结晶、表面质量及力学性能等方面的影响。通过扫描电子显微镜观察3D打印CCF/PEKK的微观结构，采用X射线衍射分析复合材料中基体的结晶性能，使用超景深显微镜观察分析3D打印CCF/PEKK的表面形貌，同时对复合材料进行弯曲性能和层间剪切性能测试。结果显示：当分层厚度为0.2 mm、流量比为85%、打印温度为395℃，并使用水平成型方向时，3D打印CCF/PEKK复合材料的综合性能最优，其中弯曲强度达302.0 MPa，层间剪切强度达24.1 MPa。CCF/PEKK的弯曲强度较3D打印纯PEKK提升194%，层间剪切强度较工艺调控前提升113%。表明在未使用任何附加优化手段的情况下，3D打印CCF/PEKK具备制造复杂结构工程零部件的潜力。
- 3D打印 /
- 连续碳纤维 /
- 聚醚酮酮 /
- 弯曲性能 /
- 层间剪切
Abstract: High thermal performance thermoplastic, poly(ether ketone ketone) (PEKK), was used as the matrix for in-situ impregnation 3D printing with continuous carbon fiber (CCF) to prepare continuous carbon fiber/poly(ether ketone ketone) composites (CCF/PEKK). The effects of layer thickness, flow ratio, print temperature and build orientation in 3D printing process parameters on the internal structure, matrix crystallization, surface quality and mechanical properties of the composites were systematically investigated. The microstructure of 3D printed CCF/PEKK was observed by scanning electron microscopy, the crystallization properties of the matrix were analyzed by X-ray diffraction, the surface morphologies of 3D printed CCF/PEKK was observed and analyzed by ultra-deep field microscopy, and the flexural properties and interlaminar shear strength of CCF/PEKK were also tested. The results shows that with the layer thickness of 0.2 mm, the flow ratio of 85%, the printing temperature of 395°C, and the build orientation of flat, the performance of 3D printed CCF/PEKK is optimal, including the flexural strength of 302.0 MPa and the interlaminar shear strength of 24.1 MPa. The flexural strength of CCF/PEKK is improved by 194% compared with 3D printed pure PEKK, and the interlaminar shear strength is improved by 113% after process optimization. It indicates that 3D printed CCF/PEKK has the potential to manufacture complex structural engineering parts without using any additional optimization.
- 3D printing /
- continuous carbon fiber /
- poly(ether ketone ketone) /
- flexural properties /
- interlaminar shear strength

HTML全文

图 1 原位浸渍3D打印CCF/PEKK的制备及各工艺参数及示意图

Figure 1. Schematic diagram of process parameters and preparing CCF/PEKK by in-situ impregnation 3D printing

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图 2 PEKK原料的TG曲线 (a) 和DSC曲线 (b)、CCF/PEKK样品光学照片 (c)

Figure 2. TG curve (a) and DSC curve (b) of PEKK, optical photo of CCF/PEKK samples (c)

T_5%—Thermal decomposition temperature; T_g—Glass transition temperature; T_m—Melting temperature

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图 3 不同分层厚度CCF/PEKK截面SEM图像：(a) 0.5 mm；(b) 0.4 mm；(c) 0.3 mm；(d) 0.2 mm

Figure 3. SEM images of CCF/PEKK cross-sections with different layer thickness: (a) 0.5 mm; (b) 0.4 mm; (c) 0.3 mm; (d) 0.2 mm

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图 4 不同分层厚度CCF/PEKK的弯曲性能和纤维含量 (a) 及层间剪切强度(ILSS) (b)

Figure 4. Flexural properties and fiber content (a) and interlaminar shear strength (ILSS) (b) of CCF/PEKK with different layer thickness

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图 5 低流量比 ((a1) F=65%、L=0.2 mm；(a2) F=75%、L=0.3 mm)、中流量比 ((b1) F=75%、L=0.2 mm；(b2) F=85%、L=0.3 mm) 和高流量比((b1) F=85%、L=0.2 mm；(b2) F=95%、L=0.3 mm) CCF/PEKK截面SEM图像对比

Figure 5. SEM images of cross-sections of CCF/PEKK with low flow ratio ((a1) F=65%, L=0.2 mm; (a2) F=75%, L=0.3 mm), middle flow ratio ((b1) F=85%, L=0.2 mm; (b2) F=95%, L=0.3 mm) and high flow ratio ((b1)F=85%, L=0.2 mm; (b2) F=95%, L=0.3 mm)

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图 6 不同流量比CCF/PEKK的弯曲性能 (a) 和ILSS (b)

Figure 6. Flexural properties (a) and ILSS (b) of CCF/PEKK with different flow ratio

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图 7 不同流量比CCF/PEKK表面三维形貌：(a1) L=0.3 mm、F=95%；(a2) L=0.3 mm、F=85%；(a3) L=0.3 mm、F=75%；(b1) L=0.2 mm、F=85%；(b2) L=0.2 mm、F=75%；(b3) L=0.2 mm、F=65%

Figure 7. 3D morphologies of CCF/PEKK surfaces with different flow ratio: (a1) L=0.3 mm, F=95%; (a2) L=0.3 mm, F=85%; (a3) L=0.3 mm, F=75%; (b1) L=0.2 mm, F=85%; (b2) L=0.2 mm, F=75%; (b3) L=0.2 mm, F=65%

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图 8 不同打印温度CCF/PEKK截面SEM图像：((a1)~(a2)) 375℃；((b1)~(b2)) 385℃；((c1)~(c2)) 395℃；((d1)~(d2)) 405℃

Figure 8. SEM images of CCF/PEKK cross-sections with different print temperatures: ((a1)-(a2)) 375°C; ((b1)-(b2)) 385°C; ((c1)-(c2)) 395°C; ((d1)-(d2)) 405°C

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图 9 不同打印温度CCF/PEKK的XRD图谱

Figure 9. XRD patterns of CCF/PEKK with different print temperature

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图 10 不同打印温度下CCF/PEKK的弯曲性能 (a) 和ILSS (b)

Figure 10. Flexural properties (a) and ILSS (b) of CCF/PEKK with different print temperature

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图 11 打印温度为395℃并采用85%流量比时CCF/PEKK弯曲性能 (a) 和层间剪切强度 (b) 随分层厚度的变化；打印温度为395℃并采用0.2 mm分层厚度时CCF/PEKK弯曲性能 (c) 和层间剪切强度 (d) 随流量比的变化

Figure 11. Flexural properties (a) and interlaminar shear strength (b) of CCF/PEKK preparing at 395℃ and flow ratio of 85% with different layer thickness; Flexural properties (c) and interlaminar shear strength (d) of CCF/PEKK preparing at 395℃ and layer thickness of 0.2 mm with different flow ratio

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图 12 不同成型方向PEKK及CCF/PEKK的弯曲性能 (a) 和CCF/PEKK的层间剪切强度 (b)

Figure 12. Flexural properties (a) and interlaminar shear strength (b) of PEKK and CCF/PEKK with different build orientation

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图 13 不同成型方向CCF/PEKK的三维模型图 (a)、样品光学照片和载荷施加示意图 (b) 及弯曲断裂处水平方向 (c) 和垂直方向 (d) 的光学显微镜照片

Figure 13. 3D model of CCF/PEKK with different build orientation (a), optical photo of samples and load application schematic (b), optical microscope photo at flexural fracture position on flat (c), on-edge (d)

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表 1 3D打印制备连续碳纤维/聚醚酮酮复合材料(CCF/PEKK)工艺参数设定

Table 1. Process parameters setting of 3D printed continuous carbon fiber/poly(ether ketone ketone) composites (CCF/PEKK)

Process parameters	Set value	Other values of paraments
Layer thickness L/mm	0.5, 0.4, 0.3, 0.2	F=85%, T=375℃, B=Flat
Flow ratio F/%	65, 75, 85, 95	L=0.2/0.3 mm, T=375℃, B=Flat
Print temperature T/℃	375, 385, 395, 405	L=0.2 mm, F=85%, B=Flat
Build orientation B	Flat, on-edge	L=0.2 mm, F=85%, T=395℃

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表 2 不同分层厚度下CCF/PEKK样品的总层数、基体挤出速度(E_r)、挤出量(E_a)及纤维含量(W_f)

Table 2. Number of layers, matrix extrusion rate (E_r), extrusion amount (E_a) and fiber content (W_f) of CCF/PEKK with different layer thickness

L/mm	Number of layer	E_r/(mg∙min⁻¹)	E_a/mg	W_f/wt%
0.5	4	48.1	400.5	14.3
0.4	5	37.3	403.8	17.1
0.3	7	32.2	393.1	20.0
0.2	10	23.0	383.2	25.8

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表 3 不同流量比CCF/PEKK的E_r和E_a

Table 3. E_r and E_a of CCF/PEKK with different flow ratios

F/%	L/mm	E_r/(mg∙min⁻¹)	E_a/mg
65	0.2	17.9	297.7
75	0.2	20.7	345.5
75	0.3	27.5	335.7
85	0.2	23.0	383.3
85	0.3	32.2	393.1
95	0.3	34.2	416.9

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表 4 不同打印温度CCF/PEKK的结晶性能

Table 4. Crystallization properties of CCF/PEKK with different print temperature

	375℃	385℃	395℃	405℃
X_s/nm	8.8	9.7	10.8	13.4
X_c/%	6.0	7.5	8.7	10.0
Notes: X_s—Grain size of PEKK matrix in CCF/PEKK; X_c—XRD crystallinity of PEKK matrix in CCF/PEKK.

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表 5 本文与3D打印短切碳纤维(CF)/PEEK和常规工艺制备CCF/PEKK力学性能及纤维含量的比较

Table 5. Comparison of mechanical properties and fiber content between 3D printed short carbon fiber CF/PEEK and CCF/PEKK composites of common processes and this work

Fabrication method	Flexural strength/MPa	ILSS/MPa	Fiber content/wt%	Ref.
Hot press molding with CCF/PEKK prepreg	687.6	78.2	65.0	[43]
Vacuum molding with dry PEKK powder and CCF	849.0	59.0	60.0	[44]
Vacuum molding with CCF/PEKK prepreg	—	30.9	66.0	[45]
3D printed short CF/PEEK	147.2	—	15.0	[20]
3D printed CCF/PEKK	302.0	24.1	25.8	This work

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