基于皮秒激光7075 Al合金超疏水表面的制备及其工艺优化

孙晓雨; 孙树峰; 王海涛; 王津; 刘世光; 王萍萍

基于皮秒激光7075 Al合金超疏水表面的制备及其工艺优化

孙晓雨^{1, 2,},
孙树峰^{1, 2, ,},
王海涛¹,
王津^{1, 2},
刘世光^{1, 2},
王萍萍^{2, 3}

1.
青岛理工大学　机械与汽车工程学院，青岛 266520
2.
山东省激光绿色高效智能制造工程技术研究中心，青岛 266520
3.
青岛黄海学院　智能制造学院，青岛 266427

基金项目: 国家自然科学基金(51775289)；高等学校学科创新引智计划(D21017)；山东省重点研发计划项目(2019 GGX104097)；青岛西海岸新区2020年度科技源头创新专项资助项目(2020-103)

详细信息

通讯作者:
孙树峰，博士，教授，博士生导师，研究方向为激光精密微纳制造　E-mail: shufeng2001@163.com

中图分类号: TN249
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出版历程
- 收稿日期: 2022-06-08
- 修回日期: 2022-07-04
- 录用日期: 2022-07-19
- 网络出版日期: 2022-08-05
- 刊出日期: 2023-06-15

Preparation and process optimization of superhydrophobic surface on 7075 Al alloy based on picosecond laser

SUN Xiaoyu^{1, 2
,},
SUN Shufeng^{1, 2
, ,},
WANG Haitao¹,
WANG Jin^{1, 2},
LIU Shiguang^{1, 2},
WANG Pingping^{2, 3}

1.
School of Mechanical and Automotive Engineering, Qingdao University of Technology, Qingdao 266520, China
2.
Shandong Research Center of Laser Green and High Efficiency Intelligent Manufacturing Engineering Technology, Qingdao 266520, China
3.
College of Intelligent Manufacturing, Qingdao Huanghai University, Qingdao 266427, China

Funds: National Natural Science Foundation of China (51775289); The 111 project (D21017); Shandong Key R&D Program (2019 GGX104097); Origin Innovation Project of Qingdao West Coast New Area (2020-103)

摘要

摘要: 为在Al合金表面获得稳定的超疏水性能，进一步拓宽Al合金材料在工业领域的应用范围，研究了一种简单、灵活、可靠的超疏水表面制备方法。首先，基于超疏水表面结构特征，采用单因素控制变量法和响应面法对激光加工参数进行了选取和优化。后采用皮秒激光刻蚀和硬脂酸处理相结合的方式获得了(超)疏水表面。通过控制激光扫描间距间接操控表面形貌的方式研究了微纳结构对表面润湿性的影响。利用接触角测量仪、SEM、共聚焦显微镜、FTIR等分析了样品的表面润湿性、形貌及化学成分。结果表明：最佳激光刻蚀参数为：扫描次数2次，扫描速度460 mm/s，频率835 kHz，平均功率21 W；扫描间距为20~80 μm的表面具有超疏水性，扫描间距为100~160 μm的表面具有疏水性。当扫描间距为20、80 μm时，接触角最大为154°，且表面黏附性很低。本文对在金属表面快速获得稳定超疏水性具有指导意义。
- 7075 Al合金 /
- 皮秒激光 /
- 润湿性 /
- 响应面法 /
- 硬脂酸
Abstract: In order to obtain stable superhydrophobic properties on Al alloy surface and further expand the industrial application of Al alloy material, a simple, flexible and reliable preparation method of superhydrophobic surface was studied. Firstly, based on the structural characteristics of superhydrophobic surface, single factor control variable method and response surface method were used to select and optimize the laser machining parameters. The (super) hydrophobic surface was obtained by picosecond laser etching and stearic acid treatment. The influence of micro-nano structure on surface wettability was studied by controlling laser scanning distance to indirectly control surface topography. The surface wettability, morphology and chemical composition of the samples were analyzed by contact angle measuring instrument, SEM, confocal microscope and FTIR. The results show that the optimal laser etching parameters are as follows: number of scanning is 2 times, scanning speed is 460 mm/s, frequency is 835 kHz, average power is 21 W; The surface with scanning interval of 20-80 μm exists superhydrophobicity, and the surface with scanning interval of 100-160 μm exists hydrophobicity. The maximum contact angle is 154° when the scanning interval is 20 μm and 80 μm, and the surface has low adhesion. This paper has guiding significance for obtaining stable superhydrophobicity on metal surface quickly.
- 7075 Al alloy /
- picosecond laser /
- wettability /
- the response surface method /
- stearic acid

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图 1 气液界面受力分析示意图

Figure 1. Schematic diagram of force analysis on gas-liquid interface

P_d—Total downward force; P_u—Total upward force

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图 2 皮秒激光微加工系统示意图

Figure 2. Schematic diagram of the picosecond laser micro-machining system

M_1,M₂—Reflecting mirror; F—Focal length; θ—Angle; d—Scan spacing; CCD—Camera system

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图 3 7075 Al合金基体上未处理表面 (a)、激光和硬脂酸处理表面 (b) 的接触角

Figure 3. Contact angle of untreated surface (a), laser and stearic acid treated surface (b) on 7075 Al alloy substrate

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图 4 激光和硬脂酸处理后7075 Al合金表面粗糙度与激光扫描间距之间的关系图

Figure 4. Relationship between surface roughness of 7075 Al alloy and laser scanning spacing after laser and stearic acid treatment

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图 5 激光和硬脂酸处理后7075 Al合金表面接触角与激光扫描间距的关系图

Figure 5. Relationship between surface contact angle of 7075 Al alloy and laser scanning spacing after laser and stearic acid treatment

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图 6 水滴(5 μL)与7075 Al合金表面接触过程图像

Figure 6. Image of water droplets (5 μL) in contact with 7075 Al alloy surface

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图 7 不同扫描间距7075 Al合金表面的扫描电镜图及局部放大图

Figure 7. SEM and partial enlargement images of 7075 Al alloy surface at different scanning intervals

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图 8 不同扫描间距7075 Al合金表面的三维形貌图 ((a), (b)) 和平均轮廓图 ((c), (d))

Figure 8. 3D morphologies ((a), (b)) and average contour ((c), (d)) of 7075 Al alloy surface with different scan spacing

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图 9 7075 Al合金表面的自组装单分子膜

Figure 9. Self-assembled monolayer on 7075 Al alloy surface

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图 10 改性前后7075 Al合金表面的FTIR图谱

Figure 10. FTIR spectra of 7075 Al alloy surface before and after modification

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图 11 7075 Al合金表面接触角与磨损周期之间的关系图

Figure 11. Relationship between surface contact angle of 7075 Al alloy and abrasion cycles

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表 1 7075 Al合金成分表

Table 1. Chemical composition of 7075 Al alloy

Element	Si	Fe	Cu	Mn	Mg	Cr	Zn	Ti	Al
Mass fraction/wt%	≤0.4	≤0.5	1.2-2.0	≤0.3	2.1-2.9	0.18-0.28	5.1-6.1	≤0.2	Bal

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表 2 单因素控制变量法试验方案

Table 2. Test scheme of single factor control variable method

	A/n	B/(mm·s⁻¹)	C/μm	D/kHz	E/W
1	1-8	500	4	500	21
2	4	200-900	4	500	21
3	4	500	0-14	500	21
4	4	500	4	200-900	21
5	4	500	4	500	9-30
Notes: A—Number of scanning; B—Scanning speed; C—Feed distance; D—Laser frequency; E—Average power.

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表 3 因素水平表

Table 3. Factor levels table

Factors	Factor levels
Factors	Low value (−1)	Median value (0)	High value (1)
A/n	2	3	4
B/(mm·s⁻¹)	400	500	600
C/μm	0	4	8
D/kHz	700	800	900
E/W	21	24	27

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表 4 正交试验方案及结果

Table 4. Scheme and results of orthogonal test

Experimental group	A/n	B/mm·s⁻¹	C/μm	D/kHz	E/W	L/μm	D/μm
1	3	500	0	700	24	107.38	6.23
2	3	500	4	800	24	102.17	5.65
3	3	600	8	800	24	101.31	5.99
4	4	500	8	800	24	97.88	7.51
5	4	400	4	800	24	107.45	8.33
6	3	500	4	800	24	103.03	7.54
7	3	400	0	800	24	104.16	7.85
8	3	500	0	800	27	104.07	7.74
9	2	500	4	800	21	96.58	5.29
10	3	500	4	700	21	106.31	7.55
11	3	500	4	900	27	97.40	7.06
12	3	500	0	800	21	99.28	6.55
13	3	500	8	800	27	104.04	7.48
14	3	600	4	800	27	101.45	6.45
15	3	400	8	800	24	100.73	6.80
16	3	500	4	800	24	103.92	7.29
17	3	400	4	800	27	99.11	7.54
18	3	600	4	900	24	102.23	6.58
19	4	500	4	800	21	105.66	7.54
20	3	500	4	900	21	95.65	6.60
21	3	500	4	800	24	99.02	6.89
22	3	500	8	700	24	104.06	7.25
23	4	500	0	800	24	101.41	8.49
24	3	400	4	700	24	106.74	8.11
25	2	500	4	900	24	94.54	5.62
26	2	500	8	800	24	97.24	5.71
27	4	600	4	800	24	103.49	7.51
28	2	500	4	700	24	106.90	6.16
29	4	500	4	800	27	102.23	7.89
30	3	500	4	700	27	105.72	6.88
31	3	500	8	800	21	100.14	6.25
32	3	500	4	800	24	96.10	6.64
33	3	600	0	800	24	99.16	6.03
34	3	600	4	700	24	103.16	6.59
35	3	500	4	800	24	99.92	6.36
36	4	500	4	700	24	109.18	8.16
37	3	400	4	800	21	100.14	6.82
38	3	600	4	800	21	99.54	6.19
39	3	400	4	900	24	98.52	6.83
40	2	500	4	800	27	96.62	4.38
41	2	600	4	800	24	94.09	4.83
42	3	500	0	900	24	96.22	6.60
43	3	500	8	900	24	94.53	5.60
44	2	500	0	800	24	95.60	5.21
45	2	400	4	800	24	96.82	5.52
46	4	500	4	900	24	98.64	8.28
Notes: L—Width; D—Depth.

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表 5 微槽宽度和深度二次多项式模型的方差分析(ANOVA)

Table 5. Analysis of variance (ANOVA) of quadratic polynomial model for the depth and width of the microgroove

	Source	Sum of squares	d_f	Mean square	F-value	P-value
Width	Model 1	539.03	20	26.95	3.85	0.0009	Significant
	Residual	175.07	25	7.00
	Lack of fit	132.56	20	6.63	0.7796	0.6898	Not significant
	Pure error	42.51	5	8.50
	Cor total	714.10	45	—
Depth	Model 2	36.48	20	1.82	7.06	<0.0001	Significant
	Residual	6.46	25	0.2584
	Lack of fit	4.15	20	0.2075	0.4493	0.9082	Not significant
	Pure error	2.31	5	0.4618
	Cor total	42.94	45	—

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表 6 试验与预测结果对比表

Table 6. Comparison table of experimental and predicted results

No.	Width/μm		Relative error rate/%	Depth/μm		Relative error rate/%
No.	The test results	Predictive value	Relative error rate/%	The test results	Predictive value	Relative error rate/%
1	93.85	93.39	0.49	5.30	5.39	1.67
2	96.26		3.07	5.15		4.45
3	92.43		1.03	5.12		5.00

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