CN111606299B - A kind of film for controlling droplet shape and its preparation method and application - Google Patents
A kind of film for controlling droplet shape and its preparation method and application Download PDFInfo
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- 229910052719 titanium Inorganic materials 0.000 claims abstract description 73
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000002184 metal Substances 0.000 claims abstract description 70
- 229910052751 metal Inorganic materials 0.000 claims abstract description 69
- 238000000034 method Methods 0.000 claims abstract description 47
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 12
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 10
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B7/00—Microstructural systems; Auxiliary parts of microstructural devices or systems
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B7/00—Microstructural systems; Auxiliary parts of microstructural devices or systems
- B81B7/04—Networks or arrays of similar microstructural devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
- B81C1/00031—Regular or irregular arrays of nanoscale structures, e.g. etch mask layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00134—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems comprising flexible or deformable structures
- B81C1/00158—Diaphragms, membranes
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Abstract
本发明公开了一种用于控制液滴形状的薄膜及其制备方法与应用。所述用于控制液滴形状的薄膜的制备方法，包括：提供衬底；在所述衬底上沉积钛金属层；采用激光直写技术在所述钛金属层上刻写图案，得到图案化的钛金属层；对所述图案化的钛金属层进行湿法刻蚀，得到具有悬切结构的薄膜。本发明所制备的用于控制液滴形状的薄膜上形成有带有尖锐边缘的悬切结构，对液体具有强钉扎效应，从而提高微液滴形状稳健性。
The invention discloses a thin film for controlling the shape of droplets and a preparation method and application thereof. The method for preparing a thin film for controlling the shape of droplets includes: providing a substrate; depositing a titanium metal layer on the substrate; using laser direct writing technology to write a pattern on the titanium metal layer to obtain a patterned Titanium metal layer; performing wet etching on the patterned titanium metal layer to obtain a thin film with an overhanging structure. A cantilever structure with sharp edges is formed on the film for controlling the shape of the droplet prepared by the invention, which has a strong pinning effect on the liquid, thereby improving the robustness of the shape of the microdroplet.
Description
Technical Field
The invention relates to the technical field of micro-nano processing, in particular to a thin film for controlling the shape of liquid drops and a preparation method and application thereof.
Background
The shape of the droplets as commonly seen is typically on the order of millimeters to the naked eye, approaching a sphere, and the smaller the droplet, the more spherical the shape. Since the surface layer of the liquid has surface tension, the liquid surface tends to shrink under the action of the surface tension, and among various objects having the same volume and having various shapes, the surface area of the spherical object is the smallest, so that the liquid drop is spherical. Therefore, it is difficult to control the shape of the droplet, especially the shape of the micro-droplet, to obtain droplets having other shapes such as triangle, square, etc.
With the development of microfluidic technology, the droplet shape control technology has a very wide application prospect in the aspects of droplet-based printing technology, protein or DNA detection, manufacturing of LED displays and the like. At present, hydrophilic and hydrophobic composite patterns are mostly prepared by processing, so that the shape of liquid drops is controlled. However, in the aspect of shape control of liquid drops, the two-dimensional hydrophilic-hydrophobic composite pattern in the prior art has key technical bottlenecks such as easy overflow of liquid at boundaries, poor boundary overflow control and the like. In applications such as droplet microflow control, droplet shape control in biomedicine, and the like, liquid collapse and overflow at boundaries will be the most destructive, and therefore inhibiting liquid from spreading in non-target directions, preventing boundary overflow is a key issue in the field of droplet shape control at present.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a thin film for controlling the shape of liquid droplets, and a preparation method and application thereof, and aims to improve the robustness of the prepared thin film for controlling the shape of liquid droplets.
A method for preparing a thin film for controlling a shape of a droplet, comprising:
providing a substrate;
depositing a titanium metal layer on the substrate;
writing a pattern on the titanium metal layer by adopting a laser direct writing technology to obtain a patterned titanium metal layer;
and carrying out wet etching on the patterned titanium metal layer to obtain the film with the overhang structure.
The preparation method of the film for controlling the shape of the liquid drop is characterized in that the substrate is a glass sheet.
The preparation method of the film for controlling the shape of the liquid drop is characterized in that the deposition process for depositing the titanium metal layer comprises one of a magnetron sputtering method, an ion sputtering method, an electron beam evaporation method, a thermal evaporation method and a laser pulse method.
The preparation method of the film for controlling the shape of the liquid drop is characterized in that the thickness of the titanium metal layer is 20-200 nm.
The preparation method of the film for controlling the shape of the liquid drop is characterized in that the pattern comprises one or more of a circle, an ellipse, a trapezoid, a pentagon, a hexagon, a rectangle and a triangle.
The preparation method of the film for controlling the shape of the liquid drop is characterized in that the writing parameters of the laser direct writing technology are as follows: the laser power is 1-10 mW; the pulse width of the laser is 0.1-10 ms.
The preparation method of the film for controlling the shape of the liquid drop is characterized in that the etching liquid adopted by the wet etching is a hydrogen fluoride solution with the mass fraction of 5-7%.
The preparation method of the film for controlling the shape of the liquid drop is characterized in that the wet etching time is 30-120 min.
A film for controlling the shape of liquid droplets, wherein the film is prepared by the preparation method of the film for controlling the shape of liquid droplets.
Use of a film for controlling the shape of droplets as described above, wherein the film for controlling the shape of droplets is used to control the shape of droplets comprising one or more of water, ethylene glycol, hexadecane.
Has the advantages that: the invention directly processes patterns with various shapes on the titanium metal layer by a laser direct writing technology, and then obtains the film for controlling the shapes of liquid drops by subsequent wet etching. The prepared film for controlling the shape of the liquid drop is provided with the overhang cutting structure with sharp edges, and has strong pinning effect on the liquid, so that the robustness of the shape of the micro liquid drop is improved, the liquid can be effectively inhibited from diffusing in a non-target direction, and the boundary overflow is prevented. In addition, the preparation method of the film for controlling the shape of the liquid drop does not need a mask in the whole processing process, and the process is very simple and convenient.
Drawings
Fig. 1 is an SEM image of a thin film for controlling droplet shape according to the present invention.
Fig. 2 is a schematic structural diagram of a film for controlling the shape of a droplet according to the present invention.
Wherein, 1-a substrate; 2-a titanium metal layer; 3-titanium dioxide layer.
Detailed Description
The present invention provides a thin film for controlling the shape of liquid droplets, and a preparation method and an application thereof, and the present invention is further described in detail below in order to make the objects, technical solutions, and effects of the present invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A method for preparing a thin film for controlling a shape of a droplet, comprising:
s100, providing a substrate;
s200, depositing a titanium metal layer on the substrate;
s300, writing a pattern on the titanium metal layer by adopting a laser direct writing technology to obtain a patterned titanium metal layer;
s400, performing wet etching on the patterned titanium metal layer to obtain the film with the overhang structure.
The laser direct writing technology has the characteristics of high processing resolution and good flexibility, and can process more dense and more accurate patterns on various patterns of a bottom material based on the laser direct writing technology, so that accurate control on various shapes of nano-liter liquid drops is realized.
The invention directly preprocesses various shapes and patterns on the metal titanium metal layer by a laser direct writing technology, and then obtains the film for controlling the shape of the liquid drop by subsequent wet etching, wherein the film for controlling the shape of the liquid drop is formed with a suspension cutting structure with a sharp edge, and has strong pinning effect on the liquid, thereby controlling the shape of the micro liquid drop more stably, effectively inhibiting the liquid from diffusing in a non-target direction and preventing the boundary from overflowing. In addition, the preparation method of the film for controlling the shape of the liquid drop does not need a mask in the whole processing process, and the process is very simple and convenient.
The thin film for controlling the shape of the liquid drop is an overhang-cut structure with sharp edges, remarkable anisotropy on the liquid can be shown, the strong pinning effect of the overhang-cut edges can inhibit the liquid drop from spreading in the vertical direction, and the liquid drop is easier to wet along the direction of the parallel edges.
In the laser direct writing process, the titanium metal layer converts the absorbed laser beam energy into heat energy and causes the corresponding surface of the titanium metal layer to be oxidized, so that a titanium metal oxide (titanium dioxide) pattern structure is generated on the surface of the titanium metal layer, and the patterned titanium metal layer is obtained. The etching rates of titanium dioxide and metal titanium generated in the laser scanning area in the hydrogen fluoride diluted solution are obviously different, namely, the titanium dioxide formed in the laser scanning area has good etching resistance, and the titanium metal layer can be quickly corroded by the etching solution. And etching the patterned titanium metal layer by using a wet etching technology so as to obtain a shape pattern structure with a sharp edge, namely preparing the film for controlling the shape of the liquid drop.
Theoretically, patterns with any shapes can be obtained by processing on the titanium metal layer through a laser direct writing technology. The preparation method has the advantages that: precise control of the size of the pattern and arbitrary designability of the shape.
In S100, the substrate is used for depositing titanium metal oxide. Optionally, the substrate is a silicon substrate, a silicon carbide substrate, or the like.
Optionally, the substrate of the present invention is a base that can be corroded in an etching solution. After the etching liquid finishes etching the titanium metal layer, the substrate is further etched, and the thin film with the cantilever structure or the suspended cutting structure and used for controlling the shape of the liquid drop can be obtained by controlling the etching time. In one embodiment of the invention, the substrate is a glass sheet. And controlling the wet etching process, and corroding the glass substrate by the dilution of the hydrogen fluoride to form a cantilever beam structure. Therefore, in the etching process, the glass sheet is used as a substrate, so that the etching depth can be improved, and the formation of an overhang cutting structure is facilitated. The glass sheet substrate is particularly suitable for being applied to the condition that the thickness of the titanium metal layer is not thick, and the purpose of improving the etching depth is achieved.
In S200, the deposition process according to the present invention is to form a titanium metal layer on a substrate, and in one embodiment of the present invention, the deposition process for depositing the titanium metal layer includes one of a magnetron sputtering method, an ion sputtering method, an electron beam evaporation method, a thermal evaporation method, and a laser pulse method.
In one embodiment of the present invention, the thickness of the titanium metal layer is 20 to 200 nm. Experiments show that the thickness of the titanium metal layer is not lower than 20nm, the etching difficulty of the etching liquid is increased to a certain extent, and the thickness of the titanium metal layer exceeds 200nm, so that the etching time is increased and the waste of the titanium metal is caused.
In S300, laser scanning is performed on the titanium metal layer by the laser direct writing technique, and a laser scanning area generates heat, so that a titanium dioxide pattern is formed by oxidizing titanium metal. It will be appreciated that the laser direct writing technique is used to write a pattern in the titanium metal layer, which is actually a titanium dioxide layer having a certain thickness. And because the titanium dioxide layer is formed by laser scanning oxidation, the oxidation effect of the surface of the titanium dioxide layer is better than that of the part below the surface of the titanium dioxide layer, and the specific expression is that the width of the upper surface of the titanium dioxide layer is wider than that of the lower bottom surface of the titanium dioxide layer, so that the prepared suspended cutting structure presents a sharp edge.
The pattern is anisotropic to the liquid drop, namely, the anisotropic structure to the liquid drop can be prepared through the pattern, so that the aim of controlling the shape of the liquid drop is fulfilled. In one embodiment of the invention, the pattern comprises one or more of a circle, an ellipse, a trapezoid, a pentagon, a hexagon, a rectangle, a triangle. Furthermore, the pattern may also comprise an asymmetric pattern, for example a trapezoid, a pentagon, a hexagon, a rectangle, a triangle or a patch with missing corners. Alternatively, the pattern may be an array pattern formed by repeating one or more of a circle, an ellipse, a trapezoid, a pentagon, a hexagon, a rectangle, and a triangle, for example, a pattern in which a plurality of rectangles are equally spaced. For example, a metal titanium layer (Ti film) is deposited on a glass substrate by electron beam evaporation, and a laser beam is used to process different anisotropic patterns on the surface of the titanium layer, such as square, rectangle, ellipse, pentagon, hexagon, etc.
In one embodiment of the invention, the processing resolution of the laser direct writing technology is 100-500nm, which substantially meets the requirements for preparing various films for controlling the shapes of liquid drops. Optionally, the processing resolution of the laser direct writing technology is one of 200nm, 300nm and 400 nm.
In an embodiment of the present invention, the writing parameters of the laser direct writing technology are: the laser power is 1-10 mW; the pulse width of the laser is 0.1-10 ms. Optionally, the writing parameters of the laser direct writing technology are: the laser power is 6 mW; the laser pulse width is 1 ms. Tests show that under the conditions, a layer of titanium dioxide pattern can be successfully inscribed on the surface of the titanium metal layer, and the titanium dioxide layer has a certain thickness, so that a thin film with a sharp edge and used for controlling the shape of liquid drops can be formed by etching. Optionally, the thickness of the titanium dioxide layer is 10-30 nm.
The etching liquid provided by the invention aims to etch titanium metal but cannot etch titanium dioxide metal oxide on the surface, so that a suspended cutting structure with a narrow lower part and a wide upper part (the upper surface is wider than the lower bottom surface) is formed. In one embodiment of the present invention, the etching solution used in the wet etching is a hydrogen fluoride solution (HF solution). Therefore, the etching solution provided by the invention is an etching solution capable of selectively etching titanium metal and titanium dioxide, and is not limited to the hydrogen fluoride solution.
The concentration of the etching liquid can influence the etching speed of the titanium metal, and further influence the final etching effect. In one embodiment of the present invention, the etching solution used in the wet etching is a hydrogen fluoride solution with a mass fraction of 5-7%. Optionally, the hydrogen fluoride solution with the mass fraction of 6% ensures the uniformity of etching.
In one embodiment of the present invention, the wet etching time is 30-120min, for example 100 min. Experiments show that the etching process comprises two processes of titanium metal etching and substrate etching, and the etching speeds of the two processes are different for hydrogen fluoride solution, specifically, the etching time for titanium metal etching and the etching time for substrate etching are respectively 85min and 15min, so that a suspended cutting structure with uniform appearance and sharp edges is obtained.
As shown in fig. 1 and 2, a film for controlling the shape of droplets is prepared by the method for preparing a film for controlling the shape of droplets as described above. The surface of the film used to control the shape of the droplets has sharp edges, forming an undercut structure. Specifically, the film for controlling the shape of the liquid drop comprises: the structure comprises a substrate 1, a titanium metal layer 2 formed on the substrate 1 and a titanium dioxide layer 3 formed on the titanium metal layer 2, wherein the width of the titanium dioxide layer 3 is larger than that of the titanium metal layer 2, and the titanium dioxide layer has an overhang structure with a wide upper part and a narrow lower part, or the titanium dioxide layer 3 extends outwards relative to the titanium metal layer 2; and the titanium dioxide layer 3 has good etching resistance, so that sharp titanium dioxide edges are formed at two side edges of the overhang structure. Therefore, the film for controlling the shape of the liquid drop has a strong pinning effect on the liquid, so that the shape of the micro liquid drop is more stably controlled, the liquid can be effectively inhibited from diffusing in a non-target direction, and the boundary overflow is prevented.
The invention also provides the use of a film as described above for controlling the shape of a droplet, wherein the droplet comprises one or more of water, ethylene glycol, hexadecane. In particular, water, ethylene glycol and hexadecane were distributed on the resulting anisotropic surface with sharp edges, enabling control of the droplet shape. For example, a water droplet is dropped onto a square pattern of thin film for controlling the shape of the droplet, and the droplet can spread along the square pattern and be pinned at the sharp edge of the square pattern.
The invention provides an anisotropic pattern with a suspended cutting edge, which realizes various shape control on liquid drops, and can remarkably improve the robustness and flexibility of liquid drop control based on the pinning effect of the suspended cutting structure edge on liquid. Based on the micro-nano structure obtained by the method, macro liquid drops in conventional micro-fluidic can be controlled, nano liquid drops can be controlled by adjusting the surface machining size, and the single liquid drop can be controlled in any shape and the composite liquid drop array can be controlled by the designed anisotropic pattern structure with sharp edges. That is, the invention provides a method based on droplet shape control, which solves the problems of poor robustness and easy collapse of droplets in the existing micro-droplet control method.
The technical solution of the present invention will be described below by specific examples.
Example 1
The method comprises the following steps: a100 nm titanium metal layer 2 is deposited on a glass sheet substrate 1 by a magnetron sputtering deposition process.
Step two: and (3) writing the rectangular array pattern on the 100nm titanium metal layer 2 by a laser direct writing technology to obtain a patterned titanium metal layer. Wherein, the writing parameters of the laser direct writing technology are as follows: the laser power is 6 mW; the laser pulse width is 1 ms.
Step three: and immersing the obtained patterned film into a hydrogen fluoride diluent with the mass fraction of 6% for 100min to obtain the film for controlling the shape of the liquid drop in a rectangular array pattern.
Step four: the water drops are dropped onto a film for controlling the shape of the drops in a rectangular array pattern, and the drops can be spread along the rectangular pattern and pinned to the sharp edges of the rectangular pattern.
Example 2
The method comprises the following steps: and depositing a 20nm titanium metal layer 2 on the glass substrate 1 by a magnetron sputtering deposition process.
Step two: and (3) writing the square array pattern on the 20nm titanium metal layer 2 by a laser direct writing technology to obtain a patterned titanium metal layer. Wherein, the writing parameters of the laser direct writing technology are as follows: the laser power is 6 mW; the laser pulse width is 1 ms.
Step three: and immersing the obtained patterned titanium metal layer into a hydrogen fluoride diluent with the mass fraction of 5% for 60min to obtain the film with a rectangular array pattern and used for controlling the shape of the liquid drop.
Step four: and dripping water drops on the film for controlling the shapes of the water drops in the rectangular array pattern, wherein the water drops can spread along the rectangular pattern and are pinned at the sharp edges of the rectangular pattern, and the water drops do not collapse within 1 h.
Example 3
The method comprises the following steps: a200 nm titanium metal layer 2 is deposited on a glass sheet substrate 1 by a magnetron sputtering deposition process.
Step two: and (3) writing the rectangular array pattern on the 200nm titanium metal layer 2 by a laser direct writing technology to obtain a patterned titanium metal layer. Wherein, the writing parameters of the laser direct writing technology are as follows: the laser power is 6 mW; the laser pulse width is 1 ms.
Step three: and immersing the obtained patterned titanium metal layer into 8% hydrogen fluoride diluent by mass for 150min to obtain a rectangular pattern array with sharp edges.
Step four: and dripping water drops on the film for controlling the shapes of the water drops in the rectangular array pattern, wherein the water drops can spread along the rectangular pattern and are pinned at the sharp edges of the rectangular pattern, and the water drops do not collapse within 1 h.
The invention solves the problems of poor stability and easy collapse of the liquid drops in the existing micro-liquid drop control method. Compared with other processing modes, the invention has strong pinning effect on liquid and improves the robustness of the shape of the micro-droplet by preparing the suspension cutting structure. The invention directly processes patterns with various shapes on the titanium metal film by a laser direct writing technology, and then obtains the film for controlling the shape of the liquid drop by subsequent wet etching, and the film for controlling the shape of the liquid drop is formed with a suspended cutting structure with a sharp edge. Therefore, the preparation method of the film for controlling the shape of the liquid drop is very simple and convenient, and a mask is not needed in the whole processing process.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (9)
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