CN112662999A - Preparation method of liquid metal film - Google Patents
Preparation method of liquid metal film Download PDFInfo
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- CN112662999A CN112662999A CN201910976345.3A CN201910976345A CN112662999A CN 112662999 A CN112662999 A CN 112662999A CN 201910976345 A CN201910976345 A CN 201910976345A CN 112662999 A CN112662999 A CN 112662999A
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- liquid metal
- evaporation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/20—Metallic material, boron or silicon on organic substrates
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/26—Vacuum evaporation by resistance or inductive heating of the source
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a preparation method of a liquid metal film. The method adopts a thermal evaporation technology, liquid metal is taken as an evaporation source to be evaporated and deposited on the surface of the substrate to form a liquid metal film, the evaporation and deposition process is carried out for multiple times in the process, gas is introduced between two adjacent times to oxidize the surface of the deposited liquid metal particles, the agglomeration of the liquid metal particles in the deposition process is favorably reduced, the dispersion uniformity of the liquid metal particles on the surface of the substrate is improved, and the film formed by multiple times of deposition has conductivity. In addition, the invention can control the thickness of the liquid metal film by setting evaporation parameters and/or regulating and controlling the deposition times, and the liquid metal film with the resistance from ohm to megaohm is obtained.
Description
Technical Field
The invention relates to the technical field of flexible electronics, in particular to a preparation method of a liquid metal film.
Background
Along with the improvement of living standard of people, the demand of flexible wearable equipment is also gradually increasing. The flexible conductive film is used as a part of various flexible device units, and has great significance for the realization of wearable equipment. In addition, research on electronic skins is emerging, and research on flexible circuits is of great significance to its development.
The existing flexible circuit preparation method mainly adopts conductive high polymer materials, hydrogel, nano materials and liquid metal. Among them, liquid metal materials are favored because of their fluid flexibility, high conductivity, non-toxicity, and the like. In addition, with the development of miniaturization of electronic devices, ultra-thin electronic skins and integrated miniaturized devices have become a research hotspot.
At present, the thickness of a film obtained by patterning liquid metal is higher, generally in the order of hundreds of micrometers, so that the thickness of a flexible circuit is larger, and miniaturization is not facilitated. For this reason, patent document CN106498348A proposes a method of forming a thin film of liquid metal by using a thermal evaporation technique, in which liquid metal is deposited on a surface of a flexible substrate by thermal evaporation using the liquid metal as an evaporation source. The method can enable the liquid metal to be deposited on the surface of the flexible substrate in an atomic scale, and is beneficial to reducing the thickness of the liquid metal film. However, because the liquid metal has a large surface tension, the liquid metal particles tend to roll on the surface of the substrate, and the liquid metal particles tend to agglomerate locally on the substrate during the deposition process and are difficult to spread uniformly on the whole surface of the substrate to form a continuous conductive film. For this reason, this patent document proposes a method of applying an electrostatic charge to the surface of a flexible substrate to reduce the surface tension of the liquid metal, but this method is complicated in process, difficult to control the amount of the applied electrostatic charge accurately, and inconvenient in experiment.
Disclosure of Invention
In view of the above technical situation, the present invention aims to provide a method for preparing a liquid metal thin film, which has a small thickness and continuous conductivity.
In order to achieve the technical purpose, the inventor discovers through a large number of experiments that in the process of forming a liquid metal film by evaporating liquid metal serving as an evaporation source to deposit liquid metal particles on the surface of a flexible substrate by adopting a thermal evaporation technology, the evaporation and deposition process of the liquid metal is divided into a plurality of times, and gas is introduced between two adjacent times to form an oxide layer on the surface of the liquid metal particles.
Namely, the technical scheme of the invention is as follows: a method for preparing liquid metal film, adopt the thermal evaporation technology, regard liquid metal as the evaporation source, evaporate and deposit on the flexible substrate surface, namely, the liquid metal particle that the evaporation source evaporates deposits on the flexible substrate surface; the method is characterized in that: the evaporation deposition process is carried out for multiple times, and gas is introduced between two adjacent evaporation depositions to oxidize the surface of the deposited liquid metal particles.
Preferably, during the evaporation and deposition process, vacuum is firstly pumped, and the vacuum degree is preferably 10-3-10-7Pa, high vacuum degree can ensure the cleanness of the cavity and more uniform film property.
The thickness and conductivity of the deposited liquid metal film can be controlled by controlling the evaporation parameters. Preferably, the heating time and heating power are controlled during evaporation so that the evaporation rate can be controlled from
The adjustment was made to 100 nm/s.
Preferably, the vapor deposition process is performed in two or more times.
Preferably, the gas is introduced to double the gas pressure to a standard atmospheric pressure.
The substrate material is not limited and may be a flexible substrate. The flexible substrate material is not limited and includes Polydimethylsiloxane (PDMS), PI, PET, PVC, and the like.
The liquid metal includes, but is not limited to, one or more of gallium (Ga) -indium (In) -tin (Sn), Ga-In alloy, and gallium (Ga).
The gas is not limited and includes one or more of oxygen, air, chlorine and the like.
Preferably, the vapor deposition process is performed in two or more times. With the increase of times, the flatness, compactness and conductivity of the whole liquid metal film are improved.
Compared with the prior art, the evaporation and deposition steps of the liquid metal are carried out intermittently, gas is introduced in the intermittent process to oxidize the surface of the deposited liquid metal particles to form a shell structure, so that the agglomeration of the liquid metal particles in the deposition process is reduced, the dispersion uniformity of the liquid metal particles on the surface of the substrate is improved, and the film formed by multiple depositions has conductivity. The reason for this is that after multiple depositions, the liquid metal particles are in contact with each other, and the liquid metal, the oxide layer and the liquid metal form a resistor-capacitor series-parallel structure, which results in a structure of a josephson junction and an electron tunneling effect. In addition, the invention can control the thickness of the liquid metal film by setting evaporation parameters and/or regulating and controlling the deposition times to obtain the liquid metal film with the thickness of hundreds of nanometers to micrometers, thereby obtaining the liquid metal film with the resistance of ohm to megaohm, and realizing the regulation and control of the liquid metal composite film from a conductor to a semiconductor.
Drawings
FIG. 1 is a schematic diagram of a first thermal evaporation deposition of a liquid metal film in example 1 of the present invention.
FIG. 2 is a schematic view of the gas introduced after the first thermal evaporation to deposit the liquid metal thin film in example 1 of the present invention.
FIG. 3 is a schematic diagram of a second thermal evaporation process for depositing a liquid metal film in example 1 of the present invention.
FIG. 4 is a schematic diagram of a liquid metal film formed on the surface of a flexible substrate according to example 1 of the present invention.
Fig. 5 is an enlarged view of fig. 4.
FIG. 6 is a schematic diagram of a liquid metal thin film formed on the surface of a flexible substrate according to comparative example 1 of the present invention.
Fig. 7 is a graph showing the electrical conductivity of the liquid metal thin film produced in example 1 of the present invention when it is subjected to tensile deformation.
FIG. 8 is a schematic diagram of a liquid metal film formed on the surface of a flexible substrate in example 2 of the present invention.
Detailed Description
The invention will be described in further detail with reference to the following examples of the drawings, which are intended to facilitate the understanding of the invention and are not intended to limit the invention in any way
Wherein the reference numerals are: the device comprises a liquid metal evaporation boat 1, a flexible substrate 2, a vacuum cover 3, a liquid metal film 4 growing for the first time and a liquid metal film 5 growing for the second time.
Comparative example 1:
in the embodiment, the flexible substrate PDMS is used as the substrate material, and the PDMS has good stretchability, bendability and elasticity. The liquid metal is a Ga-In-Sn alloy.
In this embodiment, a thermal evaporation technology is adopted, and liquid metal particles are thermally evaporated from liquid metal as an evaporation source and deposited on the surface of the flexible substrate, specifically as follows:
as shown in fig. 1, an evaporation boat 1 and a flexible substrate 2 are placed in a closed cavity, 0.3ml of liquid metal is pumped and placed in the evaporation boat 1 to be used as an evaporation material, and the following operations are carried out:
(1) starting a mechanical pump to vacuumize the cavity until the vacuum degree reaches 10-4When Pa, the evaporation boat 1 is electrically heated, and the heating parameters are set as follows: the voltage is 2V, the current is changed between 180A and 200A, the voltage indication is kept unchanged, the liquid metal is heated and evaporated, liquid metal particles are deposited on the substrate, the evaporation is stopped after 5min, and a layer of liquid metal particles covers the substrate to form a first deposited liquid metal film 4;
(2) as shown in fig. 2, gas is introduced into the cavity, the surface of the liquid metal particles is oxidized, and the introduction of the gas is stopped after 3 min;
(3) as shown in fig. 3, the step (1) is repeated, and liquid metal particles are continuously deposited on the surface of the substrate processed by the step (2), so as to form a second deposited liquid metal film 5.
The surface topography of the liquid metal film prepared on the surface of the flexible substrate by the above method is shown in fig. 4 and 5.
Comparative example 1:
this example is a comparative example to example 1 above.
In this embodiment, the substrate material and the liquid metal are exactly the same as those in embodiment 1.
In this embodiment, a liquid metal film is deposited on the surface of a substrate, the deposition method is basically the same as that in embodiment 1, and the specific process is as follows:
as shown in fig. 1, an evaporation boat 1 and a flexible substrate 2 are placed in a closed cavity, 0.3ml of liquid metal is pumped and placed in the evaporation boat 1 to be used as an evaporation material, and the following operations are carried out:
(1) starting a mechanical pump to vacuumize the cavity until the vacuum degree reaches 10-4When Pa, the evaporation boat 1 is electrically heated, and the heating parameters are set as follows: the voltage is 2V, the current is changed from 180A to 200A, the voltage indication is kept unchanged, the liquid metal is heated and evaporated, liquid metal particles are deposited on the substrate, the evaporation is stopped after 10min, and the liquid metal particles cover the substrate to form a liquid metal film.
The surface topography of the liquid metal film produced on the surface of the flexible substrate by the above method is shown in fig. 6.
Comparing fig. 4 with fig. 6, it can be seen that: in comparative example 1, the liquid metal film formed by continuously evaporating and depositing the liquid metal without introducing gas is agglomerated in the dispersion process, and the conductive particles are dispersed and isolated and have a long distance from each other, and the resistance of the liquid metal film is tested to find that the liquid metal film is in a completely non-conductive state; in example 1, the shape distribution of the secondarily deposited liquid metal film formed by introducing gas and intermittently evaporating and depositing the liquid metal is more uniform, the distance between the conductive particles is closer, the resistance of the liquid metal film is tested, the liquid metal film is found to be conductive, and the conductivity of the liquid metal film can be controlled by controlling parameters such as the evaporation amount and the evaporation time.
The flexible substrate obtained by the treatment of example 1 was stretched, and the liquid metal thin film on the surface of the substrate was subjected to a current of 2mA, and the electrical properties of the liquid metal thin film were tested, as shown in fig. 7, it was revealed that the conductivity of the liquid metal thin film was stable, the stretching amount thereof was up to 50% or more, and the conductivity change of the liquid metal thin film was 5.56%.
Example 2:
this example is a comparative example to example 1 above.
In this embodiment, the substrate material and the liquid metal are exactly the same as those in embodiment 1.
In this embodiment, a liquid metal film is deposited on the surface of a substrate, the deposition method is basically the same as that in embodiment 1, and the specific process is as follows:
as shown in fig. 1, an evaporation boat 1 and a flexible substrate 2 are placed in a closed cavity, 0.3ml of liquid metal is pumped and placed in the evaporation boat 1 to be used as an evaporation material, and the following operations are carried out:
(1) starting a mechanical pump to vacuumize the cavity until the vacuum degree reaches 10-4When Pa, the evaporation boat 1 is electrically heated, and the heating parameters are set as follows: the voltage is 2V, the current is changed between 180A and 200A, the voltage indication is kept unchanged, the liquid metal is heated and evaporated, liquid metal particles are deposited on the substrate, the evaporation is stopped after 5min, and a layer of liquid metal particles covers the substrate to form a first deposited liquid metal film 4;
(2) as shown in fig. 2, gas is introduced into the cavity, the surface of the liquid metal particles is oxidized, and the introduction of the gas is stopped after 3 min;
(3) and (3) repeating the steps (1) and (2), and continuously depositing liquid metal particles on the surface of the substrate treated in the step (2) to form a liquid metal film deposited for the second time.
(4) And (4) repeating the step (1), and continuously depositing liquid metal particles on the surface of the substrate processed in the step (3) to form a liquid metal film deposited for the third time.
The surface topography of the liquid metal film produced on the surface of the flexible substrate by the above method is shown in fig. 8.
Comparing fig. 5 with fig. 8, it can be seen that: the average thickness of the liquid metal film subjected to secondary deposition is 5 microns, and the surface of the liquid metal film is of a relief structure; compared with the secondary deposition, the average thickness of the liquid metal film deposited in the third time is 7 microns, the surface is smoother and more uniform, the liquid metal globules are distributed more compactly on the whole, and the conductivity is enhanced accordingly.
The embodiments described above are intended to illustrate the technical solutions of the present invention in detail, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modification, supplement or similar substitution made within the scope of the principles of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing liquid metal film, which adopts thermal evaporation technology and takes liquid metal as an evaporation source, the evaporation source is evaporated and deposited on the surface of a flexible substrate, and is characterized in that: the evaporation and deposition process is carried out for multiple times, and gas is introduced between two adjacent times to oxidize the surface of the deposited liquid metal particles.
2. The method of claim 1, wherein: firstly, vacuumizing in the evaporation deposition process;
preferably, the degree of vacuum is 10-3-10-7Pa。
3. The method of claim 1, wherein: the gas is introduced to double the gas pressure until the gas pressure reaches a standard atmospheric pressure.
4. The method of claim 1, wherein: the gas comprises one or more of oxygen, air and chlorine.
5. The method of claim 1, wherein: the substrate is a flexible substrate.
6. The method of claim 5, wherein: the flexible substrate material comprises one or more of PDMS, PI, PET and PVC.
7. The method of claim 1, wherein: the liquid metal comprises one or more of gallium, gallium-indium alloy and gallium-indium-tin alloy.
8. A method for preparing a liquid metal film according to any one of claims 1 to 7, characterized in that: the liquid metal film has continuous conductivity.
9. A method for preparing a liquid metal film according to any one of claims 1 to 7, characterized in that: the thickness and the resistance of the liquid metal film are controlled by controlling the evaporation parameters and/or the evaporation deposition times.
10. The method of claim 8, wherein: the thickness and the resistance of the liquid metal film are controlled by controlling the evaporation parameters and/or the evaporation deposition times.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910976345.3A CN112662999A (en) | 2019-10-15 | 2019-10-15 | Preparation method of liquid metal film |
| PCT/CN2019/127249 WO2021072968A1 (en) | 2019-10-15 | 2019-12-21 | Method for preparing liquid metal thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910976345.3A CN112662999A (en) | 2019-10-15 | 2019-10-15 | Preparation method of liquid metal film |
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| CN112662999A true CN112662999A (en) | 2021-04-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201910976345.3A Withdrawn CN112662999A (en) | 2019-10-15 | 2019-10-15 | Preparation method of liquid metal film |
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| CN (1) | CN112662999A (en) |
| WO (1) | WO2021072968A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113387322A (en) * | 2021-04-30 | 2021-09-14 | 中国科学院理化技术研究所 | Preparation method and application of uniform micro-nano film of liquid metal |
| CN116023824A (en) * | 2023-01-18 | 2023-04-28 | 上海宇叠智能科技有限公司 | Conductive ink and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5165954A (en) * | 1986-09-02 | 1992-11-24 | Microbeam, Inc. | Method for repairing semiconductor masks & reticles |
| CN102071405A (en) * | 2010-12-03 | 2011-05-25 | 湖南大学 | Polysilicon film preparation method |
| CN106498348A (en) * | 2016-12-12 | 2017-03-15 | 中国科学院宁波材料技术与工程研究所 | A kind of use liquid metal prepares the method and apparatus of flexible electronic circuit |
| CN110017923A (en) * | 2019-05-13 | 2019-07-16 | 中国科学院宁波材料技术与工程研究所 | A kind of flexible sensor and preparation method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009249703A (en) * | 2008-04-08 | 2009-10-29 | Sumitomo Metal Mining Co Ltd | Method for producing metal thin film-laminated board and vacuum film deposition device |
| US10057981B2 (en) * | 2015-06-10 | 2018-08-21 | Industry Foundation Of Chonnam National University | Stretchable circuit board and method of manufacturing the same |
| US11059098B2 (en) * | 2017-06-09 | 2021-07-13 | SAFI-Tech, Inc. | Direct printing and writing using undercooled metallic core-shell particles |
| CN108629421B (en) * | 2018-04-08 | 2019-10-11 | 北京梦之墨科技有限公司 | A kind of liquid metal quantum processor |
-
2019
- 2019-10-15 CN CN201910976345.3A patent/CN112662999A/en not_active Withdrawn
- 2019-12-21 WO PCT/CN2019/127249 patent/WO2021072968A1/en active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5165954A (en) * | 1986-09-02 | 1992-11-24 | Microbeam, Inc. | Method for repairing semiconductor masks & reticles |
| CN102071405A (en) * | 2010-12-03 | 2011-05-25 | 湖南大学 | Polysilicon film preparation method |
| CN106498348A (en) * | 2016-12-12 | 2017-03-15 | 中国科学院宁波材料技术与工程研究所 | A kind of use liquid metal prepares the method and apparatus of flexible electronic circuit |
| CN110017923A (en) * | 2019-05-13 | 2019-07-16 | 中国科学院宁波材料技术与工程研究所 | A kind of flexible sensor and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113387322A (en) * | 2021-04-30 | 2021-09-14 | 中国科学院理化技术研究所 | Preparation method and application of uniform micro-nano film of liquid metal |
| CN116023824A (en) * | 2023-01-18 | 2023-04-28 | 上海宇叠智能科技有限公司 | Conductive ink and preparation method and application thereof |
| CN116023824B (en) * | 2023-01-18 | 2023-09-01 | 上海宇叠智能科技有限公司 | Conductive ink and preparation method and application thereof |
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| WO2021072968A1 (en) | 2021-04-22 |
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Application publication date: 20210416 |