CN117165905A - Liquid metal wetting regulation and control modified coating on surface of flexible substrate and preparation method thereof - Google Patents
Liquid metal wetting regulation and control modified coating on surface of flexible substrate and preparation method thereof Download PDFInfo
- Publication number
- CN117165905A CN117165905A CN202311010276.3A CN202311010276A CN117165905A CN 117165905 A CN117165905 A CN 117165905A CN 202311010276 A CN202311010276 A CN 202311010276A CN 117165905 A CN117165905 A CN 117165905A
- Authority
- CN
- China
- Prior art keywords
- flexible substrate
- coating
- liquid metal
- transition layer
- magnetron sputtering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000758 substrate Substances 0.000 title claims abstract description 69
- 238000000576 coating method Methods 0.000 title claims abstract description 59
- 239000011248 coating agent Substances 0.000 title claims abstract description 57
- 229910001338 liquidmetal Inorganic materials 0.000 title claims abstract description 54
- 238000009736 wetting Methods 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000000151 deposition Methods 0.000 claims abstract description 50
- 230000008021 deposition Effects 0.000 claims abstract description 41
- 230000007704 transition Effects 0.000 claims abstract description 36
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 29
- 238000004544 sputter deposition Methods 0.000 claims description 31
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 26
- 239000001301 oxygen Substances 0.000 claims description 26
- 229910052760 oxygen Inorganic materials 0.000 claims description 26
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 20
- 229910052751 metal Inorganic materials 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 20
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 16
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 10
- -1 polydimethylsiloxane Polymers 0.000 claims description 8
- 238000005530 etching Methods 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- 239000013077 target material Substances 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 239000002033 PVDF binder Substances 0.000 claims description 3
- 239000004642 Polyimide Substances 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 3
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 abstract description 26
- 229910052733 gallium Inorganic materials 0.000 abstract description 26
- 239000010409 thin film Substances 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 33
- 239000010410 layer Substances 0.000 description 27
- 230000008569 process Effects 0.000 description 13
- 238000009832 plasma treatment Methods 0.000 description 6
- 239000004020 conductor Substances 0.000 description 5
- 239000010408 film Substances 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000007480 spreading Effects 0.000 description 4
- 238000003892 spreading Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002346 layers by function Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000013473 artificial intelligence Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
The application provides a liquid metal wetting regulation modified coating on the surface of a flexible substrate and a preparation method thereof, wherein the liquid metal wetting regulation modified coating on the surface of the flexible substrate comprises a Ti transition layer arranged on the surface of the etched flexible substrate and a Cu coating arranged on the surface of the Ti transition layer. The application can solve the problem that the gallium-based liquid metal is difficult to prepare the thin film conductive element due to high surface tension; the gallium-based liquid metal wetting regulation and control can be realized by changing the deposition parameters of the magnetron sputtering Cu coating, and the preparation method is simple, low in cost and easy to realize large-scale manufacture.
Description
Technical Field
The application relates to the technical field of surface coatings, in particular to a modified coating for flexible substrate surface based on liquid metal wetting regulation and control and a preparation method thereof.
Background
At present, with the development of artificial intelligence, the internet of things and sensor technology, wearable equipment for vital sign and sports health detection shows a wide development prospect. The flexible circuit conductors and the electrodes are used as electronic functional devices of wearable equipment, and important functional materials such as sensors, display screens, batteries and the like, and in practical application, extreme working conditions such as large-range bending, stretching, random folding and the like are faced, so that the conductors and the electrodes can be freely stretched/contracted in a large deformation process, and signal transmission is completed. The existing flexible stretchable composite conductor, such as a stretchable composite conductor (carbon nano tube, graphene, metal nanowire, organic polymer film, composite material thereof and the like) prepared by loading an inextensible active material on a flexible stretchable material, has excellent stretchability and stretching recovery, but is limited by the material itself, and has lower conductivity and energy density; in addition, the stretchable conductor prepared based on the structural design (corrugated structure, island bridge structure, grid structure and the like) of the metal film material has high conductivity, but is difficult to maintain resistance stability in the stretching process and limited in the stretching direction, and the microstructure is easy to break and lose efficacy in the complex deformation process, so that the increasingly severe actual service performance requirements are difficult to meet.
Liquid Metals (LMs) are a class of Metals/metal compounds with low melting points, which exhibit Liquid characteristics at or slightly above normal temperature, and thus have both Liquid flow deformability and excellent electrical conductivity properties of Metals. Wherein, gallium-based liquid metal, electricity (conductivity: 3.4-6.7X10) 4 S/cm), heat (thermal conductivity: 16.5-29.3W/mK), machineryAnd excellent fluid characteristics, and has low toxicity, safety and high stability, and has become one of ideal materials for preparing flexible electronic devices such as flexible communication base bands, stretchable circuits, stretchable electrodes and the like. However, the gallium-based liquid metal has high surface tension (the surface tension of EGaIn and GaInSn are respectively as high as 624mN/m and 534 mN/m) and is easy to oxidize, so that the wetting spreading of the gallium-based liquid metal on the surface of a flexible substrate is affected, the contact angle of the gallium-based liquid metal is generally over 135 DEG, the film forming property of the gallium-based liquid metal is poor, the gallium-based liquid metal cannot be directly prepared into a thin film device, and the technical problem of limiting the large-scale commercial application of the gallium-based liquid metal is formed.
At present, researchers have proposed various improved technical solutions. In the patent of CN104357795 a, "a method for spreading liquid in a large area by improving wettability of a liquid-solid surface", better wetting is achieved by processing a plurality of spherical or ellipsoidal holes of specific depth and defining a spatial distance on a non-wetting surface, and by injecting a metal droplet, the contact angle is < 90 °. But has the problems of high processing cost and difficult industrialized popularization; in the CN108754422 a patent, "a method for realizing gallium-based liquid metal spreading on the surface of a solid sheet", a continuous layer of Ga is deposited on the surface of a silicon wafer or copper sheet 2 O 3 The film is annealed to form a composite structure film, so that the gallium-based liquid metal is completely wetted. However, the proposal involves 480-550 ℃ annealing treatment, has complex process and limits the application on flexible substrates. Therefore, the development of the gallium-based liquid metal wetting modification and wetting regulation technology with simple process and low cost on the surface of the flexible substrate can accelerate the realization of the large-scale application of the gallium-based liquid metal wetting modification and wetting regulation technology on the flexible circuit.
Disclosure of Invention
In view of the above problems, the present application aims to provide a modified coating for controlling the surface of a flexible substrate based on liquid metal wetting and a preparation method thereof, so as to solve the problem that a gallium-based liquid metal is difficult to prepare a thin film conductive element due to high surface tension. The metal functional layers with different microstructures are prepared by changing the parameters during magnetron sputtering to realize the wetting regulation and control of gallium-based liquid metal, the contact angle range is 19-80 degrees, the process is simple, the cost is low, and the large-scale manufacturing is easy to realize.
The application provides a liquid metal wetting regulation modified coating on the surface of a flexible substrate, which comprises a Ti transition layer arranged on the surface of the etched flexible substrate and a Cu coating arranged on the surface of the Ti transition layer.
The application also provides a preparation method of the modified coating based on liquid metal wetting regulation on the surface of the flexible substrate, which comprises the following steps:
processing the surface of the flexible substrate by oxygen plasma to obtain a surface-activated flexible substrate;
depositing a Ti transition layer on the flexible substrate after surface activation through direct-current magnetron sputtering;
and depositing a Cu coating on the Ti transition layer by high-power magnetron sputtering.
According to the technical scheme, the surface of the flexible substrate provided by the application is based on the liquid metal wetting regulation modified coating and the preparation method, and compared with the prior art, the following beneficial effects can be obtained:
(1) And preparing a Ti transition layer of 10-50 nm and a Cu coating of 70-150 nm on the surface of the flexible substrate by a magnetron sputtering technology, so as to realize the wetting of gallium-based liquid metal on the surface of the flexible substrate.
(2) By varying the parameters of the deposited Cu coating during magnetron sputtering, for example: the deposition air pressure, bias voltage, argon flow, metal target power density and the like can effectively regulate and control the plasma discharge characteristic by changing sputtering process parameters, so that the microstructure of the metal coating can be regulated and controlled, the wetting reaction characteristic between the Cu coating and the gallium-based liquid metal can be controlled, and the controllable spreading of the gallium-based liquid metal on the flexible substrate can be realized.
(3) The application has simple process, relatively economic cost and strong industrial popularization and implementation.
To the accomplishment of the foregoing and related ends, one or more aspects of the application comprise the features hereinafter fully described. The following description and the annexed drawings set forth in detail certain illustrative aspects of the application. These aspects are indicative, however, of but a few of the various ways in which the principles of the application may be employed. Furthermore, the application is intended to include all such aspects and their equivalents.
Drawings
Other objects and attainments together with a more complete understanding of the application will become apparent and appreciated by referring to the following description taken in conjunction with the accompanying drawings. In the drawings:
FIG. 1 is a schematic structural diagram of a surface modified coating of the present application.
Fig. 2 is a graph showing the effect of the gallium-based liquid metal wetting contact angle test on the PDMS sample with preferred parameters.
Fig. 3 is a graph of the effect of untreated control and gallium-based liquid metal wetting contact angle test.
Fig. 4 is a topography of Cu coating deposited on PDMS surface for examples 1-5, followed by examples 1-5.
Fig. 5 is an XRD pattern of Cu coating deposited on PDMS surface of examples 1 to 5.
Fig. 6 shows the wetting contact angle test results of the samples of examples 1 to 5 with gallium-based liquid metal.
The same reference numerals will be used throughout the drawings to refer to similar or corresponding features or functions.
Detailed Description
In order that the above objects, features and advantages of the application will be readily understood, a more particular description of the application will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the application. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the application described herein without departing from the scope or spirit of the application. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present application. The specification and examples of the present application are exemplary only.
Aiming at the problem that the thin film conductive element is difficult to prepare due to high surface tension of the gallium-based liquid metal, the application provides a liquid metal wetting regulation and control modified coating on the surface of a flexible substrate and a preparation method thereof, wherein the gallium-based liquid metal wetting regulation and control is realized by changing parameters in magnetron sputtering to prepare metal functional layers with different microstructures, the contact angle range is 19-80 degrees, the process is simple, the cost is low, and the large-scale manufacturing is easy to realize.
The application provides a liquid metal wetting regulation modified coating on the surface of a flexible substrate, which comprises a Ti transition layer arranged on the surface of the etched flexible substrate and a Cu coating arranged on the surface of the Ti transition layer.
In the application, a metal transition layer and a functional coating are prepared by magnetron sputtering, and an oxygen plasma etching treatment is adopted to treat a flexible substrate before deposition of the transition layer so as to remove surface impurities and realize surface activation, thereby improving the bonding force between the Ti transition layer and the flexible substrate; meanwhile, the Ti layer and the LMs do not react and wet, so that the LMs can be prevented from overflowing and diffusing; and the Ti transition layer and the surface Cu coating are firmly combined.
In addition, specific parameters of the sputtering process can be changed to effectively regulate and control the plasma discharge characteristic, the microstructure of the metal coating (Cu coating) can be regulated and controlled, and the wetting reaction characteristic between the Cu coating and the gallium-based liquid metal is controlled, so that the gallium-based liquid metal can be controllably spread on the flexible substrate.
In the present application, the flexible substrate may be Polydimethylsiloxane (PDMS), polyimide (PI), polyvinylidene fluoride (PVDF), polyethylene terephthalate (PET), polypropylene (PP), polymethyl methacrylate (PMMA), ultra thin glass, or the like, and preferably, the flexible substrate is Polydimethylsiloxane (PDMS). The magnetron sputtering parameters are regulated and controlled to comprise deposition pressure, substrate bias voltage, argon flow, metal target power density and the like.
The Ti transition layer is prepared by Direct Current Magnetron Sputtering (DCMS), and the thickness of the Ti transition layer is 10-50 nm. The Cu coating is prepared by high-power magnetron sputtering (HiPIMS), and the thickness of the Cu coating is 70-200 nm.
The application also provides a preparation method of the modified coating based on liquid metal wetting regulation on the surface of the flexible substrate, which comprises the following steps:
s1: processing the surface of the flexible substrate by oxygen plasma to obtain a surface-activated flexible substrate;
s2: depositing a Ti transition layer on the flexible substrate after surface activation through direct-current magnetron sputtering;
s3: and depositing a Cu coating on the Ti transition layer by high-power magnetron sputtering.
In the present application, the flexible substrate is loaded onto a sample stage and placed into a deposition chamber during the surface treatment of the flexible substrate by oxygen plasma;
adjusting the etching environment of the deposition chamber, wherein the vacuum is 1×10 -3 Under Pa, the oxygen flow is 10-30 sccm, and the chamber air pressure is 2-2.7 Pa;
etching the surface of the flexible substrate by oxygen plasma; wherein, the output power of the pulse power supply is 30-90W, and the etching treatment time is 30-120 s.
Wherein, before the magnetron sputtering is carried out on the surface-activated flexible substrate;
adjusting the sputtering environment of the deposition chamber, wherein the vacuum is 1×10 -3 Under Pa, the flow rate of argon is 10-30 sccm, and the pressure of a cavity is 0.5-2.5 Pa;
and performing sputtering self-cleaning on the Cu target and the Ti target by direct-current magnetron sputtering, wherein the output power of a direct-current power supply of the metal target is 100W, and cleaning for 3-5min.
Wherein, in the process of depositing the Ti transition layer on the flexible substrate after surface activation by direct current magnetron sputtering,
and performing Ti target sputtering deposition on the surface-activated flexible substrate by adopting the direct-current magnetron sputtering to form a Ti transition layer with the thickness of 10-50 nm, wherein the sputtering power is 100W, the rotation speed of the sample stage is 120Hz, and the deposition time is 30-60 s.
In the process of depositing a Cu coating on the Ti transition layer through high-power magnetron sputtering, adopting the high-power magnetron sputtering to perform Cu target sputtering deposition on the Ti transition layer to form a Cu coating with the thickness of 70-200 nm, wherein the rotation speed of the sample stage is 120Hz, the negative bias voltage is 0-200V, and the power density of the target material is 2-6W/cm 2 Pulse frequency is 200-600 Hz, pulse width is 100 mu s, and deposition time is 5-12 min. The specific process comprises the following steps:
step 1: loading the flexible substrate onto a sample stage, then placing the sample stage into a deposition chamber, and evacuating to 1×10 -3 And (3) introducing oxygen gas with the flow rate of 10-30 sccm below Pa, opening a flow control valve, setting the pressure of the chamber to be 2-2.7 Pa, and then performing plasma treatment, wherein the output power of the applied pulse power supply is 30-90W, and the treatment time is 30-120 s.
Step 2: closing the oxygen gas and evacuating the deposition chamber to 1X 10 -3 And (3) introducing argon gas with the flow of 10-30 sccm below Pa, opening a flow control valve, setting the pressure of a chamber to be 0.5-2.5 Pa, adopting DCMS to sputter and self-clean a Cu target and a Ti target, enabling the output power of a metal target direct current power supply to be 100W, cleaning for 3min, and closing the power supply.
Step 3: and (3) performing Ti target sputtering by using a DCMS, wherein the sputtering power is 100W, the sample stage rotates at a rotating speed of 120Hz, the deposition time is 30-90 s, and the thickness of the Ti transition layer is 10-50 nm.
Step 4: the HiPIMS is adopted to carry out Cu target sputtering, the sample stage rotates at the rotation speed of 120Hz, the sample stage is loaded with 0-200V negative bias, the sputtering power is 40-120W, the pulse frequency is 200-600 Hz, the pulse width is 100 mu s, the deposition time is 5-12 min, and the thickness of the Cu functional coating is 70-200 nm.
In the present application, preferably, in step 1, the flexible substrate is Polydimethylsiloxane (PDMS); the deposition air pressure in the step 2 is 0.5Pa; in the step 4, the negative bias voltage is 100V, and the target power density is 5W/cm 2 The deposition time was 7min.
The preparation method is simple and controllable, is easy to treat at low temperature in a large area, can solve the problem that the liquid metal on the surface of the flexible substrate is difficult to pattern due to the fact that spherical liquid drops are easy to form due to high surface energy, and has wide application prospects in the fields of liquid metal-based flexible electronic information and intelligent devices.
Specific examples in the present application are as follows:
example 1
Step 1: the flexible substrate PDMS is loaded onto a sample stage, which is then placed into a deposition chamber and evacuated to 1X 10 -3 And (3) introducing oxygen with the gas flow rate of 30sccm below Pa, opening a flow control valve, setting the pressure of the chamber to be 2.7Pa, performing oxygen plasma treatment, and setting the output power to be 60W and the treatment time to be 90s.
Step 2: closing oxygen and evacuating the chamber to 1X 10 -3 And (3) introducing argon with the gas flow of 30sccm below Pa, opening a flow control valve, setting the chamber air pressure to be 0.5Pa, adopting DCMS to sputter and self-clean a Cu target and a Ti target, cleaning a metal target material with the output power of a direct current power supply of 100W for 3min, and turning off the power supply.
Step 3: and (3) performing Ti target sputtering by using a DCMS, wherein the sputtering power is 100W, the sample stage rotates at a rotating speed of 120Hz, the deposition time is 30s, and the thickness of the Ti transition layer is about 10nm.
Step 4: cu target sputtering is carried out by HiPIMS, the sample stage rotates at the rotation speed of 120Hz, the sample stage is not loaded with negative bias voltage, and the power density is 5W/cm 2 The pulse frequency is 400Hz, the pulse width is 100 mu s, the deposition time is 7.4min, and the thickness of the Cu coating is about 100nm.
Example 2
Step 1: the flexible substrate PDMS is loaded onto a sample stage, which is then placed into a deposition chamber and evacuated to 1X 10 -3 And (3) introducing oxygen with the gas flow rate of 30sccm below Pa, opening a flow control valve, setting the pressure of a chamber to be 2.7Pa, performing oxygen plasma treatment, and applying a pulse power supply with the output power of 60W for 90s.
Step 2: closing oxygen and evacuating the chamber to 1X 10 -3 Argon with the gas flow of 30sccm below Pa is introduced, a flow control valve is opened, the chamber air pressure is set to be 1.0Pa, DCMS is adopted to sputter and self-clean a Cu target and a Ti target, and the output power of a metal target direct current power supply is 100W, cleaning for 3min, and turning off the power supply.
Step 3: and (3) performing Ti target sputtering by using a DCMS, wherein the sputtering power is 100W, the sample stage rotates at a rotating speed of 120Hz, the deposition time is 30s, and the thickness of the Ti transition layer is about 10nm.
Step 4: cu target sputtering is carried out by HiPIMS, the sample stage rotates at the rotation speed of 120Hz, the sample stage is not loaded with negative bias voltage, and the power density is 5W/cm 2 The pulse frequency is 400Hz, the pulse width is 100 mu s, the deposition time is 6.5min, and the thickness of the Cu coating is about 100nm.
Example 3
Step 1: the flexible substrate PDMS is loaded onto a sample stage, which is then placed into a deposition chamber and evacuated to 1X 10 -3 And (3) introducing oxygen with the gas flow rate of 30sccm below Pa, opening a flow control valve, setting the pressure of a chamber to be 2.7Pa, performing oxygen plasma treatment, and applying a pulse power supply with the output power of 60W for 90s.
Step 2: closing oxygen and evacuating the chamber to 1X 10 -3 And (3) introducing argon with the gas flow of 30sccm below Pa, opening a flow control valve, setting the chamber air pressure to be 1.5Pa, adopting DCMS to sputter and self-clean a Cu target and a Ti target, cleaning a metal target material by using a direct current power supply with the output power of 100W for 3min, and turning off the power supply.
Step 3: and (3) performing Ti target sputtering by using a DCMS, wherein the sputtering power is 100W, the sample stage rotates at a rotating speed of 120Hz, the deposition time is 30s, and the thickness of the Ti transition layer is about 10nm.
Step 4: cu target sputtering is carried out by HiPIMS, the sample stage rotates at the rotation speed of 120Hz, the sample stage is not loaded with negative bias voltage, and the power density is 5W/cm 2 The pulse frequency is 400Hz, the pulse width is 100 mu s, the deposition time is 6min, and the thickness of the Cu coating is about 100nm.
Example 4
Step 1: the flexible substrate PDMS is loaded onto a sample stage, which is then placed into a deposition chamber and evacuated to 1X 10 -3 And (3) introducing oxygen with the gas flow rate of 30sccm below Pa, opening a flow control valve, setting the pressure of a chamber to be 2.7Pa, performing oxygen plasma treatment, and applying a pulse power supply with the output power of 60W for 90s.
Step 2: closing oxygen and evacuating the chamber to 1X 10 -3 And (3) introducing argon with the gas flow of 30sccm below Pa, opening a flow control valve, setting the chamber air pressure to be 2.0Pa, adopting DCMS to sputter and self-clean a Cu target and a Ti target, cleaning a metal target material with the output power of a direct current power supply of 100W for 3min, and turning off the power supply.
Step 3: and (3) performing Ti target sputtering by using a DCMS, wherein the sputtering power is 100W, the sample stage rotates at a rotating speed of 120Hz, the deposition time is 30s, and the thickness of the Ti transition layer is about 10nm.
Step 4: cu target sputtering is carried out by HiPIMS, the sample stage rotates at the rotation speed of 120Hz, the sample stage is not loaded with negative bias voltage, and the power density is 5W/cm 2 The pulse frequency is 400Hz, the pulse width is 100 mu s, the deposition time is 6.9min, and the thickness of the Cu coating is about 100nm.
Example 5
Step 1: the flexible substrate PDMS is loaded onto a sample stage, which is then placed into a deposition chamber and evacuated to 1X 10 -3 And (3) introducing oxygen with the gas flow rate of 30sccm below Pa, opening a flow control valve, setting the pressure of a chamber to be 2.7Pa, performing oxygen plasma treatment, and applying a pulse power supply with the output power of 60W for 90s.
Step 2: closing oxygen and evacuating the chamber to 1X 10 -3 And (3) introducing argon with the gas flow of 30sccm below Pa, opening a flow control valve, setting the chamber air pressure to be 2.5Pa, adopting DCMS to sputter and self-clean a Cu target and a Ti target, cleaning a metal target material by using a direct current power supply with the output power of 100W for 3min, and turning off the power supply.
Step 3: and (3) performing Ti target sputtering by using a DCMS, wherein the sputtering power is 100W, the sample stage rotates at a rotating speed of 120Hz, the deposition time is 30s, and the thickness of the Ti transition layer is about 10nm.
Step 4: cu target sputtering is carried out by HiPIMS, the sample stage rotates at the rotation speed of 120Hz, the sample stage is not loaded with negative bias voltage, and the power density is 5W/cm 2 The pulse frequency is 400Hz, the pulse width is 100 mu s, the deposition time is 7min, and the thickness of the Cu coating is about 100nm.
Comparative example
The comparative examples differ from examples 1-5 in that the contact angle of gallium-based liquid metal EGaIn on PDMS samples (as shown in fig. 3) was tested directly using a contact angle tester without depositing the surface modified coatings of examples 1-5. In examples 1 to 5, the same sample was tested for contact angle at 3 points (as shown in fig. 2) to ensure accuracy of experimental data.
The surface morphology changes of examples 1 to 5 can be seen from fig. 4, and the crystal structure changes of examples 1 to 5 can be seen from fig. 5, and the wettability of the liquid metal is realized by adjusting the microstructure of the Cu coating according to the surface morphology changes and the crystal structure changes.
Although the present disclosure is disclosed above, the scope of protection of the present disclosure is not limited thereto. Various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the disclosure, and these changes and modifications will fall within the scope of the application.
Claims (10)
1. The modified coating is characterized by comprising a Ti transition layer arranged on the surface of the etched flexible substrate and a Cu coating arranged on the surface of the Ti transition layer.
2. The liquid metal wetting control modified coating based on a flexible substrate surface of claim 1, wherein the flexible substrate surface is etched with an oxygen plasma.
3. The liquid metal wetting control modified coating-based flexible substrate surface of claim 1, wherein the flexible substrate is polydimethylsiloxane, polyimide, polyvinylidene fluoride, polyethylene terephthalate, polypropylene, polymethyl methacrylate, or ultra thin glass.
4. The flexible substrate surface-based liquid metal wetting regulation modification coating according to claim 1, wherein the Ti transition layer is prepared by direct current magnetron sputtering and has a thickness of 10-50 nm.
5. The flexible substrate surface-based liquid metal wetting regulation modified coating of claim 1, wherein the Cu coating is prepared using high power magnetron sputtering and the Cu coating has a thickness of 70-200 nm.
6. A method of preparing a liquid metal wetting control modified coating on a flexible substrate surface according to any one of claims 1 to 5, comprising the steps of:
processing the surface of the flexible substrate by oxygen plasma to obtain a surface-activated flexible substrate;
depositing a Ti transition layer on the flexible substrate after surface activation through direct-current magnetron sputtering;
and depositing a Cu coating on the Ti transition layer by high-power magnetron sputtering.
7. The method for preparing a modified coating for controlling the wetting of a flexible substrate surface based on liquid metal according to claim 6,
during the treatment of the surface of the flexible substrate by oxygen plasma,
loading the flexible substrate onto a sample stage and into a deposition chamber;
adjusting the etching environment of the deposition chamber, wherein the vacuum is 1×10 -3 Under Pa, the oxygen flow is 10-30 sccm, and the chamber air pressure is 2-2.7 Pa;
etching the surface of the flexible substrate by oxygen plasma; wherein, the output power of the pulse power supply is 30-90W, and the etching treatment time is 30-120 s.
8. The method for preparing a liquid metal wetting control modified coating on a surface of a flexible substrate according to claim 7, wherein the surface-activated flexible substrate is subjected to magnetron sputtering prior to the surface-activated flexible substrate;
adjusting the sputtering environment of the deposition chamber, wherein the vacuum is 1×10 -3 The flow rate of argon gas is 10-30 sccm under Pa, and the chamber pressure is 0.5~2.5Pa;
And performing sputtering self-cleaning on the Cu target and the Ti target by direct-current magnetron sputtering, wherein the output power of a direct-current power supply of the metal target is 100W, and cleaning for 3-5min.
9. The method for preparing a modified coating based on liquid metal wetting regulation on a flexible substrate surface according to claim 8, wherein, during deposition of the Ti transition layer on the surface-activated flexible substrate by DC magnetron sputtering,
and performing Ti target sputtering deposition on the surface-activated flexible substrate by adopting the direct-current magnetron sputtering to form a Ti transition layer with the thickness of 10-50 nm, wherein the sputtering power is 100W, the rotation speed of the sample stage is 120Hz, and the deposition time is 30-60 s.
10. The method for preparing a modified coating based on liquid metal wetting regulation on a flexible substrate surface according to claim 9, wherein during deposition of a Cu coating on the Ti transition layer by high-power magnetron sputtering,
performing Cu target sputtering deposition on the Ti transition layer by adopting the high-power magnetron sputtering to form a Cu coating with the thickness of 70-200 nm, wherein the rotation speed of the sample stage is 120Hz, the negative bias voltage is 0-200V, and the power density of the target material is 2-6W/cm 2 Pulse frequency is 200-600 Hz, pulse width is 100 mu s, and deposition time is 5-12 min.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202311010276.3A CN117165905A (en) | 2023-08-11 | 2023-08-11 | Liquid metal wetting regulation and control modified coating on surface of flexible substrate and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202311010276.3A CN117165905A (en) | 2023-08-11 | 2023-08-11 | Liquid metal wetting regulation and control modified coating on surface of flexible substrate and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN117165905A true CN117165905A (en) | 2023-12-05 |
Family
ID=88940337
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202311010276.3A Pending CN117165905A (en) | 2023-08-11 | 2023-08-11 | Liquid metal wetting regulation and control modified coating on surface of flexible substrate and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN117165905A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN118308699A (en) * | 2024-04-09 | 2024-07-09 | 华南理工大学 | Preparation method of ultralow-stress metal film |
-
2023
- 2023-08-11 CN CN202311010276.3A patent/CN117165905A/en active Pending
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN118308699A (en) * | 2024-04-09 | 2024-07-09 | 华南理工大学 | Preparation method of ultralow-stress metal film |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN108249424B (en) | Preparation method of bromine-doped high-conductivity ultrathin graphene film | |
Latthe et al. | Self-cleaning and superhydrophobic CuO coating by jet-nebulizer spray pyrolysis technique | |
US9388050B2 (en) | Production method for a graphene thin film | |
CN117165905A (en) | Liquid metal wetting regulation and control modified coating on surface of flexible substrate and preparation method thereof | |
KR101777016B1 (en) | Metal grid-Silver nanowire mixed transparent electrodes and the preparation method of metal grid using polymeric nanofiber mask | |
CN109911888B (en) | Preparation method and application of defect-free disordered-layer stacked graphene nano-film | |
CN108517696B (en) | Preparation method of patterned flexible conductive graphene cloth | |
Kim et al. | Electric properties and surface characterization of transparent Al-doped ZnO thin films prepared by pulsed laser deposition | |
KR101504956B1 (en) | Preparation of Liquid Crystal Alignment Layer with Graphene | |
CN109267027B (en) | WO with island-shaped nanoparticle structure3Preparation method of electrochromic film | |
US11572279B2 (en) | Two-dimensional material nanosheets with large area and controllable thickness and general preparation method therefor | |
CN106637085A (en) | Hydrophobic thin film as well as preparation method and application thereof | |
CN112410729B (en) | Ultrathin liquid metal film, preparation method and application | |
CN110422841B (en) | Method for realizing layer-by-layer growth of AB accumulation type double-layer graphene through asymmetric oxygen and sulfur channels with planar structures | |
KR102691697B1 (en) | Method for manufacturing flexible microsupercapacitor, and large area flexible microsupercapacitor provided with polymer buffer layer | |
CN109402566B (en) | Method for preparing flexible vanadium oxide film by two-step method | |
KR101905139B1 (en) | Method and apparatus for controlling actuation of liquid using electrowetting phenomenon | |
CN113005432B (en) | Method for depositing ZnO functional layer in patterned mode, strain sensor and preparation method of strain sensor | |
CN112038481B (en) | Heavy rare earth doped ZnO columnar crystal preferred orientation piezoelectric film material and preparation method thereof | |
CN109378267B (en) | Molybdenum sulfide film and preparation method thereof | |
TW202224025A (en) | Field effect transistor and method for making the smae | |
CN112531112A (en) | Ultrahigh-gain organic thin film transistor and preparation method thereof | |
CN110592548A (en) | Suede CuO composite structure film and preparation method thereof | |
CN115011922B (en) | Graphene film and method for converting in-situ amorphous carbon into graphene film | |
TWI762149B (en) | Field effect transistor and method for making the smae |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |