阅读说明：本技术 一种基于正交实验的低粘附性超疏水表面制作方法 (Low-adhesion super-hydrophobic surface manufacturing method based on orthogonal experiment ) 是由 庞继红 管翔云 杨焕 周鸿勇 曹宇 张祥雷 于 2021-05-24 设计创作，主要内容包括：本发明公开了一种基于正交实验的低粘附性超疏水表面制作方法,包括以下步骤：步骤S1、确定加工材料的影响因子,影响因子有四个且分别为速度、间距、加工次数和功率；步骤S2、确定四个影响因子下的不同水平,在每个影响因子下各有三个水平；步骤S3、基于各影响因子和水平确定L9(3～(4))的正交表并进行实验；步骤S4、利用极差分析法对实验结果进行分析,并确立最优方案；步骤S5、检验最优方案是否满足低粘附性超疏水的要求。实施本发明,能有效减少实验次数、时间和精力,并得到符号要求的低粘附性超疏水表面。(The invention discloses a method for manufacturing a low-adhesion super-hydrophobic surface based on an orthogonal experiment, which comprises the following steps of: step S1, determining four influence factors of the processing material, wherein the four influence factors are respectively speed, space, processing times and power; step S2, determining different levels under four influence factors, wherein each influence factor has three levels; step S3, determining L9 (3) based on each influence factor and level 4 ) And performing experiments; step S4, analyzing the experimental result by utilizing a range analysis method, and establishing an optimal scheme; and step S5, checking whether the optimal scheme meets the requirement of low-adhesion super-hydrophobicity. By implementing the method, the experiment times, time and energy can be effectively reduced, and the low-adhesion super-hydrophobic surface with the symbol requirement can be obtained.)

1. A method for manufacturing a low-adhesion super-hydrophobic surface based on an orthogonal experiment is characterized by comprising the following steps:

step S1, determining four influence factors of the processing material, wherein the four influence factors are respectively speed, space, processing times and power;

step S2, determining different levels under four influence factors, wherein each influence factor has three levels;

step S3, determining L9 (3) based on each influence factor and level⁴) And performing experiments;

step S4, analyzing the experimental result by utilizing a range analysis method, and establishing an optimal scheme;

and step S5, checking whether the optimal scheme meets the requirement of low-adhesion super-hydrophobicity.

2. The method for manufacturing a low-adhesion superhydrophobic surface based on orthogonal experiments as claimed in claim 1, wherein the step S3 specifically comprises:

step S31, power,The four factors of speed, spacing and processing times are sequentially marked as A, B, C, D, three levels are sequentially marked as 1, 2 and 3, and L9 (3) is established⁴) The orthogonal table of (2);

step S32, convert the contents in the orthogonal table into each influence factor and its level representation.

3. The method for manufacturing a low-adhesion superhydrophobic surface based on an orthogonal experiment as claimed in claim 1, wherein the step S4 specifically comprises:

step S41, based on the orthogonal table in the step S3, measuring by using a contact angle measuring instrument and a rolling angle measuring instrument to obtain an experimental result;

step S42, performing analysis and comparison by a range analysis method:

(1) determining the sizes of contact angles and rolling angles of the same influence factor at different levels;

(2) analyzing range, and determining range values of all the influence factors;

(3) determining an optimal scheme, namely determining the primary and secondary sequence of each influence factor according to the range value of each influence factor; and for the multi-index, determining an optimal scheme according to the weight ratio.

Technical Field

The invention relates to the technical field of metal surface treatment, in particular to a method for manufacturing a low-adhesion super-hydrophobic surface based on an orthogonal experiment.

Background

The low-adhesion super-hydrophobicity of the surface of the material refers to the phenomenon that the apparent contact angle of a water drop on the surface is more than or equal to 150 degrees, and the rolling angle is less than or equal to 10 degrees, so that the material has excellent self-cleaning property, corrosion resistance, fluid drag reduction and waterproof performance, and has wide application prospects in industrial production and daily life.

The existing super-hydrophobic surface is roughly manufactured by the following steps: the method comprises the steps of scanning a 304 stainless steel sheet cleaned by plasma water under different process parameters by using laser to obtain micro-nano structures with different shapes and sizes, modifying the surface of the stainless steel by using a sodium stearate ethanol solution to reduce the surface energy, and finally air-drying the stainless steel sheet for 30 minutes under natural conditions to form a low-adhesion super-hydrophobic surface. The laser etching method is an advanced technology, and the controllable material surface structure can be obtained through a simple one-step method without ultra-clean room facilities or high-vacuum equipment. The technology can effectively reduce the test times on the premise of ensuring that the test reaches the expected result, and greatly improves the super-hydrophobic property and the manufacturing efficiency of the material compared with other technologies (such as a photoetching template method, a colloid assembly method, a chemical corrosion method and the like).

In the manufacturing experiment process, the micro-nano structure and the low surface energy of the material surface are two important factors forming the low-adhesion super-hydrophobic surface, wherein the micro-nano structure of the material surface is determined by the influence factor of the material during laser processing, so how to quickly and accurately determine the optimal influence factor can effectively reduce the experiment times and duration, and the low-adhesion super-hydrophobic surface meeting the requirements can be obtained.

Disclosure of Invention

The invention aims to provide a method for manufacturing a low-adhesion super-hydrophobic surface based on an orthogonal experiment, which can effectively reduce the experiment times, time and energy and obtain the low-adhesion super-hydrophobic surface with the symbol requirement.

The technical purpose of the invention is realized by the following technical scheme:

a method for manufacturing a low-adhesion super-hydrophobic surface based on an orthogonal experiment comprises the following steps:

step S1, determining four influence factors of the processing material, wherein the four influence factors are respectively speed, space, processing times and power;

step S2, determining different levels under four influence factors, wherein each influence factor has three levels;

step S3, determining L9 (3) based on each influence factor and level⁴) And performing experiments;

step S4, analyzing the experimental result by utilizing a range analysis method, and establishing an optimal scheme;

and step S5, checking whether the optimal scheme meets the requirement of low-adhesion super-hydrophobicity.

The step S3 is further configured to specifically include:

step S31, sequentially marking four influence factors of power, speed, space and processing times as A, B, C, D, sequentially marking three levels as 1, 2 and 3, and establishing L9 (3)⁴) The orthogonal table of (2);

step S32, convert the contents in the orthogonal table into each influence factor and its level representation.

The step S4 is further configured to specifically include:

step S41, based on the orthogonal table in the step S3, measuring by using a contact angle measuring instrument and a rolling angle measuring instrument to obtain an experimental result;

step S42, performing analysis and comparison by a range analysis method:

(1) determining the sizes of contact angles and rolling angles of the same influence factor at different levels;

(2) analyzing range, and determining range values of all the influence factors;

(3) determining an optimal scheme, namely determining the primary and secondary sequence of each influence factor according to the range value of each influence factor; and for the multi-index, determining an optimal scheme according to the weight ratio.

The invention has the beneficial effects that:

by making orthogonal empirical table L9 (3)⁴) And (4) carrying out 9 times of experiments in total, then analyzing the experimental data by using a range analysis method, and determining the primary and secondary properties of each influence factor so as to find an optimal experimental scheme. Compared with other experimental methods, the adopted orthogonal experimental table can not only ensure to obtain a better experimental scheme, but also effectively reduce the experimental times, experimental time and energy. The method has great guiding significance for other scientific research experiments and production.

Drawings

FIG. 1 is an analytical flow chart according to the present invention;

FIG. 2 is a table showing the settings of the shadow and the corresponding level according to the present invention;

FIG. 3 is a table setting orthogonal tables according to the present invention;

FIG. 4 is an experimental protocol in the present invention;

FIG. 5 is a graph showing the measurement results of contact angles and rolling angles in the present invention;

FIG. 6 is a line graph of contact angle and roll angle in the present invention;

FIG. 7 is an analysis table of the experimental structure in the present invention;

FIG. 8 is a schematic diagram illustrating the influence of various influencing factors on the contact angle according to the present invention; wherein (a) the effect of power on the contact angle; (b) the influence of speed on the contact angle; (c) the effect of the spacing on the contact angle; (d) influence of the number of machining times on the contact angle;

FIG. 9 is a schematic diagram showing the effect of various influencing factors on the roll angle in the present invention; wherein (a) the effect of power on roll angle; (b) the effect of speed on roll angle; (c) the influence of the pitch on the roll angle; (d) influence of the machining times on the roll angle;

FIG. 10 is a super-hydrophobic surface processed using orthogonal experiments to arrive at an optimal solution in accordance with the present invention; wherein (a) the contact angle prior to laser ablation; (b) laser machining and contact angle after stearic acid ethanol solution soaking.

Detailed Description

The invention is described in further detail below with reference to the accompanying drawings:

as shown in fig. 1, a method for manufacturing a low-adhesion superhydrophobic surface based on an orthogonal experiment comprises the following steps:

step S1, determining four influence factors of the processing material, wherein the four influence factors are respectively speed, space, processing times and power;

step S2, determining different levels under four influence factors, wherein each influence factor has three levels;

specifically, this embodiment uses a german fast laser (fast 5050) with a wavelength of 515 nm. The influence factors mainly comprise four factors of power, speed, space and processing times, and have different levels under different influence factors, and refer to the attached figure 2.

As can be seen from fig. 2, the use of a laser to create a superhydrophobic surface sets 4 influencing factors and 3 levels at each influencing factor. Then, if each impact factor and each level are tested one by one, a total of 3^4 ^ 81 tests are performed. Obviously, this requires excessive effort, materials, and time to be invested in a common experiment. Therefore, in this embodiment, the orthogonal experiment table is selected to be used for completing the experiment.

Step S3, determining L9 (3) based on each influence factor and level⁴) And performing experiments;

since this experiment coincided with a factor 4 3 level, L9 (3) was chosen⁴) And (4) an orthogonal table. By using the orthogonal table, only 9 experiments are needed to obtain a relatively accurate result.

The step S3 specifically includes the following steps:

s31, sequentially marking four influence factors of power, speed, space and processing times as A, B, C, D, sequentially marking three levels as 1, 2 and 3, and establishing L9 (3)⁴) The orthogonal table of (2); reference is made to figure 3.

As can be seen from fig. 3, the table in fig. 3 corresponds exactly to two features of the orthogonal table: (1) in each column, each level of each factor appears equally in the total number of trials. (2) Between any two factor columns, various levels match the number pairs in the ordered sequence (i.e. the left bundle is placed before and the right one after), and the number pairs in each pair appear equally. That is, the orthogonal table is consistent with the feature of "each factor and each level" matching balance.

Step S32, convert the contents in the orthogonal table into each influence factor and its level representation. Corresponding reference is made to fig. 4.

Step S4, analyzing the experimental result by utilizing a range analysis method, and establishing an optimal scheme;

the step S4 specifically includes the following steps:

step S41, based on the orthogonal table in the step S3, namely the attached figure 4, simultaneously applying the Young equation, and measuring by using a contact angle measuring instrument and a rolling angle measuring instrument to obtain an experimental result;

wherein the Young's equation is the basic theorem of wetting science of an ideal solid surface, and the expression is

γ_LVcosθ_Y＝γ_SV-γ_SL (1)

In the formula (1), the contact angle of the liquid droplet with the surface thereof is θ_YSurface tension (gamma) of solid-liquid interface_SL) Surface tension (gamma) of solid-gas interface_SV) And liquid-gas interfacial surface tension (gamma)_LV) Satisfies the formula (1).

Meanwhile, 9 sets of data were counted using a contact angle measuring instrument (OLS4000) and a rolling angle measuring instrument, and the obtained experimental data are shown in fig. 5 and 6.

Step S42, performing analysis and comparison by a range analysis method:

to obtain more accurate results, the results after the test must be analyzed. And (4) analyzing and comparing by using a visual analysis method (range analysis method) to draw an experimental conclusion.

(1) Determining the sizes of contact angles and rolling angles of the same influence factor at different levels;

taking FIG. 3 as an example, there are a total of 4 influencing factors, namely A (power), B (speed), C (velocity) ((C))The distance and D (number of processes) have an influence on the experimental results. First three levels A of A influencing factors are determined₁、A₂、A₃The influence on the contact angle and the roll angle. For the a influencing factor, a total of 9 experiments were performed. Let the contact angle be CA₁、CA₂、CA₃、CA₄、CA₅、CA₆、CA₇、CA₈、CA₉And roll angle SA₁、SA₂、SA₃、SA₄、SA₅、SA₆、SA₇、SA₈、SA₉. For the first level of the A influencing factor, the total contact angle is K₁＝CA₁+CA₂+CA₃Average contact angle k₁＝(CA₁+CA₂+CA₃) A/3; for the second level of the A influencing factor, the total contact angle is K₂＝CA₄+CA₅+CA₆Average contact angle k₂＝(CA₄+CA₅+CA₆) A/3; for the third level of the A influencing factor, the total contact angle is K₃＝CA₇+CA₈+CA₉Average contact angle k₃＝(CA₇+CA₈+CA₉) A/3; likewise, the total and average contact angles for each level of the impact factor can be calculated B, C. The magnitude of the roll angle of the influence factor on another experimental index can also be determined by the method.

Thus, A affects three levels A of factors₁、A₂、A₃Comparability was observed because in three experiments under a1 condition, B, C was at three levels and the three levels appeared the same number of times. In A₂、A₃All B, C were at three levels, and the three levels appeared the same number of times. Similarly, at the B, C influential factor, the other variables appeared the same number of times, and the respective influential factor levels were comparable throughout the experiment.

(2) Analyzing range, and determining range values of all the influence factors;

best level A_MAXTo and fromPoor level A_MINThe difference is called the range, and is denoted by R. For example, for factor A, the range R is A_MAX-A_MINWe also calculated the difference of the B, C factors in this way.

(3) Determining an optimal scheme, namely determining the primary and secondary sequence of each influence factor according to the range value of each influence factor; and for the multi-index, sorting is carried out according to the weight ratio.

We also determined the effect of each influencing factor on the experimental results. Specifically, the magnitude of the range between the levels of the various influence factors is compared, and which influence factor has a large range is the primary influence factor, and which influence factor has a small range is the secondary influence factor. And when the optimal scheme is judged, sequencing each scheme according to the primary and secondary of each influence factor. For the multi-index experiment, the advantages and disadvantages of each scheme can be judged according to the weight ratio. The determined optimal solution must comply with the definition of superhydrophobicity. The results refer to FIG. 7.

From fig. 7, 4 range differences can be obtained: 10 (power), 3.3 (speed), 2.8 (pitch), 2.8 (number of machining). According to the size of the 4 pole difference numbers. The influence of the individual influencing factors on the contact angle and the sliding angle can be determined from fig. 8 and 9. The range of power is 10, which indicates that the power effect on the size of the contact is the most important, followed by the speed and pitch, and finally the number of processes. From the analysis, it is seen that the a factor (power) takes the third level well, while both the B factor (speed) and the C factor (pitch) take the second level well. As regards the number of processes, the effect it has on the experimental results is minimal, if from the point of view of saving time it is appropriate to choose the second level, since this level factor not only fulfils the requirements of superhydrophobicity (the contact angle must be greater than or equal to 150 °), but for careful consideration and for better results it is still chosen level 3. In summary, the primary and secondary impact factors for the experimental index of contact angle are A, B, C, D. For the roll angle, the primary and secondary factors are D, A, C, B.

The contact angle and the rolling angle are two important indexes of low-adhesion super-hydrophobicity, and in order to determine an optimal scheme, the weight ratio of each of the two experiment indexes is set to be 0.5. Ranking the various impact factors for contact angle: 1(A), 2(B), 3(C) and 4 (D). The roll angle has the following respective influence factors: 1(D), 2(A), 3(C) and 4 (B). And (3) performing weight ratio calculation on the ranking, wherein the obtained result is as follows:

influencing factor A1 × 0.5+2 × 0.5 ═ 1.5

Influencing factor B2 × 0.5+4 × 0.5 ═ 3

Influencing factor C3 × 0.5+3 × 0.5 ═ 3

Influence factor D1 × 0.5+4 × 0.5 ═ 2.5

The four impact factors are ranked A, D, B, C according to the calculation. Where B and C are ranked equally, but the B effect factor is placed before the C effect factor to allow for increased speed and reduced time of the experiment. According to fig. 4, for the a influencing factor, the contact angle size will only meet the requirement at level 3, at which the roll size is 3.8 °, so selecting level 3 is the optimal choice under the a influencing factor; for the B influencing factor, both the roll angle and the contact angle at level 2 are most preferred; for the D impact factor, the roll angle requirement is also met only at 3 levels, selecting D3 as the most preferred; as for the C influencing factor, either level 2 or level 3 is chosen as desired, but the contact angle at level 2 is critical, so level 3 is more suitable. Finally, we choose the scheme: a. the₃B₂C₃D₃Namely, the selected scheme is that the power is 60%, the speed is 100mm/s, the interval is 60um, and the processing times are 4 times.

And step S5, checking whether the optimal scheme meets the requirement of low-adhesion super-hydrophobicity.

Optimal scheme A selected by utilizing orthogonal experiment₃B₂C₃D₃Performing an experiment, wherein the superhydrophobic surface processed by the optimal scheme is obtained by an orthogonal experiment in fig. 10, wherein (a) in fig. 10 is a contact angle which is not measured by laser ablation and has a size of 102.5 degrees; (b) is a contact angle image measured after the stearic acid ethanol solution is soaked for 60min, and the contact angle is measured to be 161.3 degrees. The rolling angle is measured to be 1.8 degrees by using a rolling angle measuring instrument,meets the requirement of a super-hydrophobic surface with low adhesiveness.

In this example, the best solution for producing a low adhesion superhydrophobic surface using 304 stainless steel was found and established using orthogonal experimental methods. By making orthogonal empirical table L9 (3)⁴) And (3) carrying out 9 times of experiments, analyzing the experimental data by using an intuitive analysis method (range analysis method), and determining the primary and secondary properties of each influence factor so as to find an optimal experimental scheme. Compared with other experimental methods, the adopted orthogonal experimental table can not only ensure to obtain a better experimental scheme, but also effectively reduce the experimental times, experimental time and energy. The method has great guiding significance for other scientific research experiments and production.

The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of the appended claims.