CN113387322A - Preparation method and application of uniform micro-nano film of liquid metal - Google Patents
Preparation method and application of uniform micro-nano film of liquid metal Download PDFInfo
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- CN113387322A CN113387322A CN202110484798.1A CN202110484798A CN113387322A CN 113387322 A CN113387322 A CN 113387322A CN 202110484798 A CN202110484798 A CN 202110484798A CN 113387322 A CN113387322 A CN 113387322A
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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
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B7/00—Microstructural systems; Auxiliary parts of microstructural devices or systems
- B81B7/0009—Structural features, others than packages, for protecting a device against environmental influences
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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
- 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
Abstract
The invention provides a preparation method and application of a uniform micro-nano film of liquid metal. The invention is based on the excellent wettability of the flexible material subjected to surface modification treatment on the liquid metal, and utilizes the methods of high-speed spin coating and multiple adhesion transfer printing to prepare the flexible liquid film which has uniform and consistent thickness and adjustable thickness and is different from the traditional rigid film, and the preparation method is simple and rapid. The uniform micro-nano film for the liquid metal provided by the invention expands the application range of the liquid metal and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of metal films, in particular to a preparation method and application of a uniform liquid metal micro-nano film.
Background
The metal film has the characteristics of good stability, excellent performance and the like, has great application value in the fields of dielectric, superconductivity, high resistance, ferroelectricity, piezoelectricity, pyroelectricity, electrocaloric card, electrostatic storage, photoelectricity, gas sensitivity and the like, and is also a hot point for researching functional films.
Researchers at home and abroad in recent years generally adopt methods such as magnetron sputtering, chemical vapor deposition, ion beam deposition, pulsed laser deposition, electron beam thermal evaporation, metal ion assisted sputtering and the like for preparing metal films, the methods generally require precise and expensive equipment and complex preparation and processing processes, and how to prepare high-quality films at lower temperature even at room temperature attracts the research interest of numerous researchers at home and abroad.
Liquid metal, as a unique advanced material with high fluidity, high conductivity and low toxicity, has been applied and developed in the fields of flexible electronics, biomedical treatment, additive manufacturing, national defense and military industry and the like. With the achievement of a series of major breakthroughs and progresses, the research of the basic and application technologies surrounding the room-temperature liquid metal gradually becomes the major scientific and technological frontier of international enthusiasm, and is bringing about subversive changes to the development of human high and new energy, electronic information, advanced manufacturing, flexible circuits, national defense and military safety, and biomedical health technologies.
In the field of liquid metal flexible electronics, regarding the fields of patterning drawing of liquid metal, liquid metal-based electronic devices, combination of liquid metal and flexible base materials and the like, liquid metal exerts the characteristic of flexible conduction. However, the existing liquid metal application has the problems of rough circuit preparation, low circuit manufacturing precision, poor stability and the like. In order to achieve more stable performance output of the liquid metal and to promote the liquid metal in more fields, the uniformity and thickness of the liquid metal film must be accurately controlled. In addition, after the preparation of the uniform liquid metal film is realized, the liquid metal film can be more fully applied to the fields of flexible microelectronics, biosensing, photoelectricity, additive manufacturing, heat transfer refrigeration and the like.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a preparation method of a uniform liquid metal micro-nano film. The invention also aims to provide the liquid metal uniform micro-nano film prepared by the method and application thereof.
Specifically, the invention provides the following technical scheme:
the invention provides a preparation method of a uniform liquid metal micro-nano film, which is characterized in that a flexible material is subjected to surface modification treatment, liquid metal is coated on the surface subjected to the surface modification treatment in a spinning mode, and the obtained liquid metal film is used as a seal to carry out at least one-time adhesion transfer printing on a substrate.
The invention discovers that the flexible material subjected to surface modification shows excellent wettability to the liquid metal, the liquid metal can be efficiently spread into a thin film in a spin coating mode, meanwhile, more sufficient and uniform transfer printing can be realized in adhesion transfer printing, the thickness of the liquid metal film after each adhesion transfer printing is reduced by half, and the liquid metal thin film with uniform thickness and adjustable thickness can be obtained by controlling the times of adhesion transfer printing.
Wherein the flexible material is selected from any one of PDMS (polydimethylsiloxane), Ecoflex (aliphatic aromatic random copolyester), POE (polyethylene octene), EVA (ethylene-vinyl acetate copolymer) and EPDM (ethylene propylene diene monomer).
Further, the surface modification treatment includes plasma treatment, acid solution treatment, alkali solution treatment, surface coating, or chemical vapor deposition.
Wherein, the plasma treatment refers to treating the flexible material with plasma, and the used process gas includes but is not limited to carbon dioxide, oxygen and nitrogen. Taking the process gas as an example of oxygen, the specific operation of the plasma treatment is as follows: putting the surface to be processed of the flexible material into a vacuum plasma cavity with the surface to be processed facing upwards, opening a vacuum pump, and vacuumizing the cavity; after the vacuum degree in the cavity is stabilized after waiting for 2-3 min, opening an oxygen inflow switch, and sending oxygen into the vacuum cavity; and waiting for 30-40 s, and opening a switch for plasma treatment after the vacuum cavity is filled with oxygen. Preferably, the plasma processing power is 60-100 kW, and the processing time is 15-20 s.
The acid solution treatment refers to the treatment of the flexible material by using acid solution with strong corrosive oxidizing property. The acid solution can be concentrated hydrochloric acid, concentrated sulfuric acid, a mixture of hydrogen peroxide and concentrated acid, and the like. As an example, the specific operation of the acid solution treatment is as follows: adding hydrogen peroxide (30 percent, AR) into sulfuric acid with the concentration of 98-100 percent, and preparing a surface treatment solution according to the volume ratio of 3: 7; and placing the surface to be treated of the flexible material in the surface treatment solution, shaking for 10-30 seconds, taking out and washing with deionized water.
The alkali solution treatment refers to the treatment of the flexible material by using alkali solution. The alkali liquor can be an alkali metal solution such as NaOH and KOH, or a mixture of ammonia water and hydrogen peroxide. As an example, the specific operation of the alkali solution treatment is as follows: and (3) placing the surface to be treated of the flexible material in a NaOH solution with the concentration of 1-5 mol/L, soaking for 0.5-2 h, taking out, and washing with deionized water.
The surface coating refers to coating PMA (propylene glycol methyl ether acetate) or ACM (polyacrylate) glue on the surface of the flexible material. As an example, the specific operation of surface coating is as follows: coating a layer of PMA glue on the surface to be treated of the flexible material; after coating, carrying out spin coating treatment, wherein the rotating speed of a spin coating machine is 100-20000 r/min; and drying the PMA glue.
The chemical vapor deposition is to deposit copper, silver, gold or tungsten on the surface of the flexible material. As an example, the specific operation of chemical vapor deposition is as follows: cleaning the surface to be treated of the flexible material according to a conventional cleaning method in the field, putting the surface to be treated into chemical vapor deposition equipment, and depositing copper on the surface to be treated after cleaning, wherein the thickness of the obtained copper metal layer is 30 nm-200 mu m.
Furthermore, the spin coating speed is 50-20000 r/min, and the thickness of the liquid metal film is 1 μm-5 mm.
In the invention, the liquid metal is any one of gallium, gallium-indium alloy, gallium-indium-tin alloy and bismuth-indium-tin-zinc alloy. The melting point of the liquid metal used in the present invention is less than 300 c, preferably less than 200 c. For liquid metal with melting point higher than room temperature, such as bismuth-based liquid metal, in the spin coating, the liquid metal is heated to be liquid in advance, and then the molten liquid metal is dipped for spin coating treatment.
Further, the adhesive transfer comprises: covering the substrate with the liquid metal film, and applying a pressure of 10-200 kPa for 1-10 s.
It can be understood that in order to realize smooth adhesion transfer printing of the liquid metal with the melting point higher than room temperature, the ambient temperature is increased in the adhesion transfer printing process, so that the ambient temperature is 5-10 ℃ higher than the melting point of the liquid metal.
The invention does not strictly limit the substrate for adhering and transferring, and can be mutually infiltrated with the liquid metal, namely, flexible or rigid materials of which the contact angle of the liquid metal on the substrate is less than 90 degrees can be used. Preferably, the substrate is PVC (polyvinyl chloride), PET (polyester resin), metallic copper, silver, gold, wood board, graphite plate, PTFE, silicon wafer, PVA (polyvinyl alcohol), cellulose membrane, sodium chloride crystal substrate, or a flexible material subjected to surface modification treatment in the present invention.
Further, when the substrate is a water-soluble material such as a sodium chloride crystal substrate, a PVA film or a cellulose film, the method further comprises a step of dissolving the film obtained by the adhesion transfer to the substrate in water. Therefore, the independent liquid metal uniform micro-nano film can be obtained.
Further, the thickness of the uniform micro-nano film of the liquid metal is 10 nm-5 mm.
The invention also provides the liquid metal uniform micro-nano film prepared by any one of the methods.
The invention also provides application of the liquid metal uniform micro-nano film in the fields of flexible microelectronics, biosensing, photoelectricity, additive manufacturing and heat transfer refrigeration.
The invention has the beneficial effects that:
1. the invention discloses a method for preparing a micro-nano flexible liquid metal film with uniform thickness and adjustable thickness by utilizing a high-speed spin coating and multiple adhesion transfer printing method based on excellent wettability of a flexible material subjected to surface modification treatment on liquid metal.
2. The spin coating and the adhesive transfer printing in the method can be carried out at a lower temperature even at room temperature, and the method has the advantages of simple and quick operation, and the flexible material subjected to surface modification can be repeatedly used, so that the production cost is reduced.
3. The uniform micro-nano film for the liquid metal provided by the invention expands the application range of the liquid metal, and particularly the application of the liquid metal in the fields of flexible microelectronics, biosensing, photoelectricity, additive manufacturing, heat transfer refrigeration and the like. The uniform micro-nano film of the liquid metal also has more application possibilities, and provides a material foundation with high reliability and high stability for the application of the liquid metal material.
Drawings
FIG. 1 is a flow chart of a method for preparing a uniform micro-nano film of liquid metal according to the present invention;
FIG. 2 is a cross-sectional view of a uniform nano-film of liquid metal prepared by four transfers in example 1 of the present invention;
fig. 3 is a surface view of a liquid metal uniform micro-nano film prepared by secondary transfer printing in embodiment 3 of the present invention, a: sectional view, b: surface topography SEM picture;
FIG. 4 is a cross-sectional view of a uniform micro-nano film of liquid metal prepared by five times of transfer printing in example 4 of the present invention;
fig. 5 is a macroscopic view of an incomplete liquid metal film prepared by using PDMS spin coating without surface treatment in comparative example 1 of the present invention.
Detailed Description
The following examples illustrate the properties of the materials of the invention in terms of their preparation and their isolation. It should be understood by those skilled in the art that the examples are only for the purpose of facilitating understanding of the present invention and should not be construed as specifically limiting the present invention.
The starting materials used in the examples are all commercially available. The means used in the following examples are all technical means known in the art unless otherwise specified.
The liquid metal used in the following examples was prepared according to the following procedure, exemplified by gain 24.5:
(a) the method comprises the following steps of mixing metal gallium with purity of 99.9% and indium according to a mass ratio of 75.5: 24.5 weighing and then putting into a beaker;
(b) placing the beaker on a heating constant-temperature magnetic stirrer, setting the heating temperature to 80 ℃, setting the rotating speed to 200r/min, and simultaneously placing a magnetic stirrer;
(c) after the indium block is dissolved, the metal liquid is continuously stirred for 10min, so that the indium block and the metal liquid are completely mixed into a homogeneous phase.
Other liquid metal alloys can be prepared by changing the mass ratio of the metals of gallium, indium, tin and bismuth.
Example 1
The process of the method for preparing a uniform micro-nano film of liquid metal provided by this embodiment is shown in fig. 1. The method specifically comprises the following steps:
1) uniformly mixing basic components of PDMS and a curing agent according to a mass ratio of 10:1, floating bubbles in a mixed solution to the surface and breaking the bubbles by using a vacuumizing mode, pouring the mixed solution into a culture dish with a polished silicon wafer placed in advance, baking the culture dish on a heating plate at 75 ℃ for about two hours, and stripping after curing to obtain PDMS with an extremely smooth surface;
2) placing the PDMS with the smooth surface facing upwards in an oxygen plasma treatment instrument with the power of 86kW and the treatment time of 18 s;
3) dipping the PDMS after the oxygen plasma treatment with the liquid metal material, putting the PDMS on a spin coater, and performing spin coating at 2000r/min for 4min to obtain a liquid metal film with the thickness of 8 mu m;
4) adhering and transferring the PDMS treated in the step 3) and the PDMS obtained in the step 2), pressing for 3s under the pressure of 10kPa, and separating the PDMS to obtain a liquid metal film with the thickness reduced by half;
5) repeating the step 4) for a total of four times, a uniform liquid metal film having a thickness of 500nm can be obtained (see fig. 2). FIG. 2 is a cross-sectional view of the obtained liquid metal film, and it can be seen that the obtained liquid metal film has good uniformity.
Example 2
The preparation method of the uniform micro-nano film of the liquid metal provided by the embodiment comprises the following steps:
1) uniformly mixing basic components of PDMS and a curing agent according to a mass ratio of 10:1, floating bubbles in a mixed solution to the surface and breaking the bubbles by using a vacuumizing mode, pouring the mixed solution into a culture dish with a polished silicon wafer placed in advance, baking the culture dish on a heating plate at 75 ℃ for about two hours, and stripping after curing to obtain PDMS with an extremely smooth surface;
2) placing the PDMS with the smooth surface facing upwards in an oxygen plasma treatment instrument with the power of 80kW and the treatment time of 20 s;
3) dipping the PDMS after the oxygen plasma treatment with the liquid metal material, putting the PDMS on a spin coater, and performing spin coating at 10000r/min for 5min to obtain a liquid metal film with the thickness of 2 mu m;
4) adhering and transferring the PDMS treated in the step 3) and the PDMS obtained in the step 2), pressing for 5s by using 20kPa, and separating the PDMS to obtain a liquid metal film with the thickness reduced by half;
5) repeating the step 4) for 1 time to obtain a uniform liquid metal film with the thickness of 1 mu m.
This example produced a liquid metal film with a thickness of 1 μm (surface topography see FIG. 3). Fig. 3a is a cross-sectional view of the obtained liquid metal film, and fig. 3b is a SEM image of the surface topography of the obtained liquid metal film, and it can be seen from fig. 3 that the prepared liquid metal film not only has a uniform thickness, but also has a uniform distribution of the liquid metal on the liquid metal film.
Example 3
The preparation method of the uniform micro-nano film of the liquid metal provided by the embodiment comprises the following steps:
1) uniformly mixing basic components of PDMS and a curing agent according to a mass ratio of 10:1, floating bubbles in a mixed solution to the surface and breaking the bubbles by using a vacuumizing mode, pouring the mixed solution into a culture dish with a polished silicon wafer placed in advance, baking the culture dish on a heating plate at 75 ℃ for about two hours, and stripping after curing to obtain PDMS with an extremely smooth surface;
2) placing the PDMS with the smooth surface facing upwards in an oxygen plasma treatment instrument with the power of 80kW and the treatment time of 20 s;
3) dipping the PDMS subjected to the oxygen plasma treatment with a liquid metal material, putting the PDMS on a spin coater, and performing spin coating at 5000r/min for 3min to obtain a liquid metal film with the thickness of 4 microns;
4) adhering and transferring the PDMS treated in the step 3) and the PDMS obtained in the step 2) to obtain a liquid metal film with the thickness reduced by half;
5) repeating the step 4) for 1 time to obtain a uniform liquid metal film with the thickness of 1 mu m.
Adhering and transferring the PDMS treated in the step 3) and a sodium chloride crystal substrate, and dissolving the sodium chloride crystal substrate to obtain the independent liquid metal flexible micro-nano film.
Example 4
The preparation method of the uniform micro-nano film of the liquid metal provided by the embodiment specifically comprises the following steps:
1) heating POE elastic plastic balls with the melting point of 80 ℃ to 100 ℃, pouring the heated melt into a metal container in which a polished silicon wafer is placed in advance, placing the metal container in a heating box with the temperature of 100 ℃ to anneal to room temperature, and stripping after solidification to obtain POE with an extremely smooth surface;
2) and (3) putting the POE with the smooth surface facing upwards into concentrated hydrochloric acid with the concentration of 2mol/L, and soaking for 1 h. Then taking out, washing with deionized water, and airing;
3) dipping the liquid metal material in the air-dried POE, and putting the POE on a spin coater to spin at 2000r/min for 5min to obtain a liquid metal film with the thickness of 8 mu m;
4) adhering and transferring the POE treated in the step 3) with a PVC substrate, applying 20kPa pressure to press for 5s, and separating the POE from the PVC substrate to obtain a liquid metal film with the thickness reduced by half;
5) repeating the step 4) five times, and obtaining a uniform liquid metal film with the thickness of 250nm (see figure 4). FIG. 4 is a cross-sectional view of the obtained liquid metal film, and it can be seen that the obtained liquid metal film has good uniformity.
Comparative example 1
The spin coating process provided in this comparative example is different from that of example 2 only in that step 2) is omitted, i.e., the PDMS with the extremely smooth surface obtained in step 1) is dipped in the liquid metal material and then placed on a spin coater for spin coating.
It was found that the spin coating was not successful, and the liquid metal film on the PDMS surface which was not subjected to the surface modification treatment was incomplete (see fig. 5, it can be seen that the liquid metal film on the PDMS surface was incomplete and uniform).
Comparative example 2
The adhesive transfer process provided by this comparative example is different from example 1 only in that the substrate used in the adhesive transfer process is PDMS which is not subjected to the surface modification treatment, i.e., in step 4), the PDMS treated in step 3) is subjected to adhesive transfer with the PDMS obtained in step 1).
It can be found that the transfer printing is not successful, and only a small amount of liquid metal remains on the untreated PDMS substrate, so that the purpose of obtaining a complete and uniform film by spin coating cannot be achieved.
The above examples are only for describing the preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims (10)
1. A preparation method of a uniform micro-nano film of liquid metal is characterized in that surface modification treatment is carried out on a flexible material, the liquid metal is coated on the surface after the surface modification treatment in a spinning mode, and at least one time of adhesion transfer printing is carried out on a substrate by taking the obtained liquid metal film as a seal.
2. The method for preparing the liquid metal uniform micro-nano film according to claim 1, wherein the flexible material is selected from any one of PDMS, Ecoflex, POE, EVA and EPDM;
and/or the substrate is selected from PVC, PET, copper, silver, gold, wood board, graphite board, PTFE, silicon chip, PVA film, cellulose film, sodium chloride crystal substrate or flexible material subjected to surface modification treatment.
3. The method for preparing the liquid metal uniform micro-nano film according to claim 1 or 2, wherein the surface modification treatment comprises plasma treatment, acid solution treatment, alkali solution treatment, surface coating or chemical vapor deposition.
4. The method for preparing the uniform micro-nano film of the liquid metal according to claim 1, wherein the spin coating speed is 50 to 20000r/min, and the thickness of the liquid metal film is 1 μm to 5 mm.
5. The method for preparing the uniform micro-nano film of the liquid metal according to claim 1, wherein the liquid metal is selected from any one of gallium, gallium-indium alloy, gallium-indium-tin alloy and bismuth-indium-tin-zinc alloy.
6. The method for preparing the uniform micro-nano film of liquid metal according to claim 1, wherein the adhering and transferring comprises: covering the substrate with the liquid metal film, and applying a pressure of 10-200 kPa for 1-10 s.
7. The method for preparing a liquid metal uniform micro-nano film according to any one of claims 1 to 6, further comprising a step of dissolving the film obtained by adhering and transferring to a substrate in water.
8. The method for preparing a liquid metal uniform micro-nano film according to claim 1, wherein the thickness of the liquid metal uniform micro-nano film is 10nm to 5 mm.
9. The liquid metal uniform micro-nano film prepared by the method of any one of claims 1 to 8.
10. The use of the uniform micro-nano liquid metal film of claim 9 in flexible microelectronics, biosensing, photovoltaics, additive manufacturing, and heat transfer refrigeration applications.
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Application publication date: 20210914 |