CN114351090A - Method for preparing flexible film with adjustable fold structure under high temperature condition and application thereof - Google Patents
Method for preparing flexible film with adjustable fold structure under high temperature condition and application thereof Download PDFInfo
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- CN114351090A CN114351090A CN202111391287.1A CN202111391287A CN114351090A CN 114351090 A CN114351090 A CN 114351090A CN 202111391287 A CN202111391287 A CN 202111391287A CN 114351090 A CN114351090 A CN 114351090A
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000000758 substrate Substances 0.000 claims abstract description 82
- 239000010445 mica Substances 0.000 claims abstract description 57
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 57
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052709 silver Inorganic materials 0.000 claims abstract description 8
- 239000004332 silver Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000000853 adhesive Substances 0.000 claims abstract description 3
- 230000001070 adhesive effect Effects 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims description 20
- 238000000137 annealing Methods 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000037303 wrinkles Effects 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000004544 sputter deposition Methods 0.000 claims description 4
- 239000002390 adhesive tape Substances 0.000 claims description 3
- 238000010494 dissociation reaction Methods 0.000 claims description 3
- 230000005593 dissociations Effects 0.000 claims description 3
- 238000004093 laser heating Methods 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 241001251094 Formica Species 0.000 claims description 2
- 239000000084 colloidal system Substances 0.000 claims description 2
- 239000010408 film Substances 0.000 description 59
- 239000010409 thin film Substances 0.000 description 10
- 238000012546 transfer Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 description 5
- 239000011737 fluorine Substances 0.000 description 5
- 229910052731 fluorine Inorganic materials 0.000 description 5
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- OMEXLMPRODBZCG-UHFFFAOYSA-N iron rhodium Chemical compound [Fe].[Rh] OMEXLMPRODBZCG-UHFFFAOYSA-N 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- -1 polydimethylsiloxane Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
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Abstract
The invention provides a method for preparing a flexible film with an adjustable fold structure under a high-temperature condition, which comprises the following steps: s1, mechanically dissociating a mica substrate, adhering the back of the mica substrate to the surface of a high-temperature sample support by using silver adhesive after a new surface is dissociated, and placing the mica substrate on a heating table for drying; s2, conveying the dried high-temperature sample support into a magnetron sputtering cavity, carrying out magnetron sputtering on a mica substrate, and growing a film; s3, pre-stretching the flexible substrate through a stretching die; s4, attaching the mica substrate on which the film grows on one side to a pre-stretched flexible substrate, drying, then mechanically stripping, controlling a stretching die to release pre-stretching to obtain the flexible film with the fold structure, and compared with the prior art, the film flexibilizing method is suitable for growing at high temperature and preparing the flexible film with the adjustable fold structure; the invention also provides an application of the flexible film with the adjustable and controllable fold structure in the field of electronics.
Description
Technical Field
The invention relates to the technical field of electronics, in particular to a method for preparing a flexible film with an adjustable fold structure under a high-temperature condition and application thereof, so as to prepare a flexible film with high growth temperature and regular fold structure.
Background
With the advent of flexible electronic, wearable, and implantable technologies, there is a need for flexibility in sensors. Magnetic sensors, a very important class of sensors, also face problems of flexibility. The flexibility of the functional layer magnetic film material of the magnetic sensor is required to be realized when the magnetic sensor is required to be flexible, and the flexibility of the magnetic sensor is realized by manufacturing a fold structure to stretch the film.
There are three main approaches to the preparation of flexible films with a pleated structure: (1) directly growing a film on a pre-stretched flexible substrate, and then releasing the pre-stretching to obtain a fold structure; (2) transferring the thin film by dissolving the sacrificial layer to prepare a wrinkled structure; (3) and (5) manually designing a fold structure. However, the above methods are only suitable for preparing flexible thin films grown at room temperature, and are not suitable for preparing flexible thin films grown at high temperature and having lattice parameters not matched with the sacrificial layer.
Disclosure of Invention
The invention provides a film flexibility method which is suitable for growing at high temperature and has adjustable and controllable fold structure in order to overcome the defects of the prior art.
The invention provides a method for preparing a flexible film with an adjustable fold structure under a high-temperature condition, which comprises the following steps:
s1, mechanically dissociating a mica substrate, adhering the back of the mica substrate to the surface of a high-temperature sample support by using silver adhesive after a new surface is dissociated, and placing the mica substrate on a heating table for drying;
s2, conveying the dried high-temperature sample support into a magnetron sputtering cavity, carrying out magnetron sputtering on a mica substrate and growing a film, wherein the magnetron sputtering comprises the following steps: vacuumizing, annealing the mica substrate, adjusting the temperature to the growth temperature of a sample, introducing argon, pre-sputtering, formally growing a film, annealing the film, cooling and sampling;
s3, pre-stretching the flexible substrate through a stretching die;
and S4, attaching the mica substrate on which the film grows on one side to the pre-stretched flexible substrate, putting the mica substrate into an oven, heating, taking out the mica substrate, cooling, mechanically stripping the mica substrate, and controlling a stretching die to release the pre-stretching to obtain the flexible film with the fold structure.
Compared with the prior art, the method for preparing the flexible film with the controllable fold structure under the high-temperature condition has the following advantages: (1) the film is directly grown on the surface of the mica substrate by a direct transfer method, the method is simple, high lattice matching degree is not required, and a sacrificial layer is not required to be prepared; (2) the invention adopts the mica substrate which can resist the high temperature of 1100 ℃, can prepare the flexible film with high growth temperature and stable performance, and the growth temperature of the film is not limited by the flexible substrate; (3) by using the method of the invention, a flexible film with a larger area can be prepared, and the film can be kept complete after transfer and has the properties basically consistent with those before transfer; (4) the flexible film prepared by the invention is of a regular wavy fold structure, and the wavelength and the amplitude of the wavy fold structure can be regulated and controlled by changing the thickness of the film, the cooling mode of the film after annealing and the pre-stretching proportion of the flexible substrate.
Preferably, the mica substrate of step S1 is mechanically dissociated in a water bath, and since the mica substrate has a book-like structure and can be peeled off and completely cleaved, in order to obtain a new surface with good flatness, the knife edge used for dissociation should be parallel to the mica substrate.
Further, in step S1, the center of the high temperature sample holder is a 10mm × 10mm square of SiC, and the mica substrate is attached to the SiC surface with silver paste.
Further, during magnetron sputtering in step S2, the back of SiC is heated by laser, and the mica substrate is kept at a high temperature during the growth of the film by utilizing the good thermal conductivity of SiC and silver paste.
Further, the initial vacuum degree of the magnetron sputtering chamber in the step S2 is 5 × 10-8torr～5×10-9the heating source for mica substrate annealing and film annealing is laser heating, the substrate annealing temperature is 500-700 ℃, and the film growsThe temperature is 500-600 ℃, the annealing temperature of the film is 600-800 ℃, the target and the substrate are obliquely sputtered at 30-60 ℃ during the growth of the film, the high-temperature sample holder is kept rotating at 10 revolutions per minute during the growth of the film, the high-temperature sample holder is kept rotating at 1 revolution per minute during the annealing of the film, and the cooling speed is 0.2 ℃/second-0.6 ℃/second.
Further, the cooling manner in step S4 includes water cooling and air cooling.
Preferably, the pre-stretching in step S3 is performed after clamping both ends of the flexible substrate.
Further, the mica substrate mechanical peeling of step S4 is to perform mechanical peeling of the mica substrate on the back of the film using an adhesive tape.
Further, the releasing pre-stretching of step S4 is to hold one end of the flexible substrate fixed, and to remove the flexible film after slowly releasing the other end of the flexible substrate.
The invention also provides an application of the flexible film with the adjustable and controllable fold structure in the electronic field, namely a method for preparing the flexible film with the adjustable and controllable fold structure under the high-temperature condition is applied to the electronic field.
Drawings
FIG. 1 is a schematic diagram of a transfer process for preparing a flexible FeRh film with an adjustable fold structure according to the present invention;
FIG. 2 is a M-T curve diagram of a flexible FeRh film with controllable corrugated structure prepared by the present invention;
FIG. 3 is an atomic force microscope surface topography map of the flexible FeRh thin film with the controllable wrinkle structure prepared by the invention.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
Example one
The method for preparing the flexible FeRh film with the controllable fold structure at the high temperature comprises the following steps:
s1, under an optical microscope, mechanically dissociating a 5mm multiplied by 0.2mm artificial fluorine crystal mica substrate in a water bath by using a surgical blade, keeping a knife edge used in dissociation parallel to the mica substrate, blowing dry moisture on the surface of the mica substrate by using a nitrogen gun after dissociating a new surface, adhering the reverse side of the mica substrate to the surface of a 10mm multiplied by 10mm SiC square at the center of a high-temperature sample holder by using silver glue, enabling the newly dissociated surface to face upwards for growing a film, drying on a heating table at the drying temperature of 120 ℃, cleaning the surface of the substrate again by using the nitrogen gun after drying, and simultaneously ensuring that the mica substrate is firmly adhered;
s2, conveying the dried high-temperature sample holder into a magnetron sputtering cavity, and vacuumizing the magnetron sputtering cavity to a vacuum degree of 8 multiplied by 10-8torr, then starting a laser heating source to heat the back of the SiC, and utilizing the good heat conduction performance of the SiC and the silver colloid to heat the mica substrate and keep the temperature at 600 ℃ for annealing; after the mica substrate is annealed, adjusting laser to control the temperature of the mica substrate to be 550 ℃, opening an argon valve to introduce argon, starting a power supply to carry out pre-sputtering, keeping the F eRh (iron rhodium) target material and the mica substrate to be arranged in an inclined way at 45 degrees during sputtering, keeping a high-temperature sample holder to rotate at 10 revolutions per minute, formally growing the FeRh film, adjusting the gas flow and the rotating speed of a molecular pump to keep the air pressure of a cavity at 1.4-2torr; after the FeRh film is grown, adjusting the temperature of the mica substrate to 700 ℃, keeping the high-temperature sample holder to rotate at 1 r/min, and annealing the FeRh film; after the FeRh film is annealed, cooling to room temperature at a cooling rate of 0.4 ℃/second, and finally sampling to obtain the FeRh film;
s3, clamping two ends of a PDMS (polydimethylsiloxane) flexible substrate through a stretching mold, and then pre-stretching to obtain pre-strain of the PDMS flexible substrate (as shown in figure 1);
and S4, attaching the Mica (Mica) substrate on one surface on which the FeRh film (film) grows to a pre-stretched PDMS flexible substrate, putting the PDMS flexible substrate into an OVEN (OVEN), heating, taking out, cooling, mechanically stripping the Mica substrate and the FeRh film by using an adhesive tape, controlling a stretching die to keep one end of the flexible substrate fixed, slowly releasing the other end of the flexible substrate, and then taking down the flexible FeRh film to obtain the flexible FeRh film with the folded structure.
In the embodiment, the FeRh film is directly grown on the surface of the artificial fluorine crystal mica substrate by a direct transfer method, the method is simple, high lattice matching degree is not required, and a sacrificial layer is not required to be prepared; the fluorine crystal mica belongs to silicate artificial mica crystal, is prepared by smelting mica crystal in platinum crucible under strict process condition and material ratio at 1500 deg.C, and has chemical formula of KMg3(AlSi3O10)F2Does not contain (OH) -and replaces (OH) -hydroxyl by F-fluorine, has excellent electric insulation performance and high temperature resistance, can resist high temperature of 1100 ℃; the fluorine crystal mica has a book-shaped structure, can be peeled off and completely cleaved, and can be peeled to 0.02 mm at the thinnest; the flatness is very good and can reach the atomic level; the composite material is not easy to deform, can bear larger pressure, and has higher tensile strength and compression strength; the product is not aged, is not easy to break and is not easy to adsorb impurities; the invention adopts the mica substrate which can resist the high temperature of 1100 ℃, can prepare the flexible film with high growth temperature and stable performance, and the growth temperature of the film is not limited by the flexible substrate. By using the method of the invention, a flexible film with a larger area can be prepared, and the film can be kept complete after transfer and has the properties basically consistent with those before transfer; the flexible film prepared by the invention is of a regular wavy fold structure, and the wavelength and the amplitude of the wavy fold structure can be regulated and controlled by changing the thickness of the film, the cooling mode of the film after annealing and the pre-stretching proportion of the flexible substrate.
Test example 1
The flexible FeRh thin film obtained in the first embodiment is tested to obtain an M-T curve, as shown in FIG. 2, the flexible FeRh thin film shows a first-order phase change around room temperature, the use requirement is met, and the flexibility of the thin film which needs to grow at high temperature is realized.
Test example two
And (4) preparing different types of flexible FeRh thin films according to the method in the first embodiment, observing the micro-topography of the different types of flexible FeRh thin films by observing the flexibility effect of different cooling modes on the FeRh thin films with different thicknesses in the step S4, and obtaining the surface topography map of the atomic force microscope. As shown in fig. 3, the corrugated shape of the Fe Rh film is regular wave-shaped. Specifically, fig. 3-1 and 3-4 show that the cooling manner has a regulating effect on the specific wrinkle appearance of the flexible ferah film, and the faster the cooling speed is, the smaller the wavelength and amplitude of the wavy wrinkle appearance are; fig. 3-1, 3-2, and 3-3 show that the greater the thickness of the flexible ferah film, the greater the wavelength and amplitude of the wavy fold topography, and that this trend is also shown by the data of fig. 3-4, 3-5, and 3-6. In addition, the larger the pre-stretching ratio, the larger the wavelength and amplitude of the wavy fold morphology.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present disclosure, and such changes and modifications will fall within the scope of the present invention.
Claims (10)
1. A method for preparing a flexible film with an adjustable fold structure under high temperature conditions is characterized by comprising the following steps:
s1, mechanically dissociating a mica substrate, adhering the back of the mica substrate to the surface of a high-temperature sample support by using silver adhesive after a new surface is dissociated, and placing the mica substrate on a heating table for drying;
s2, conveying the dried high-temperature sample support into a magnetron sputtering cavity, carrying out magnetron sputtering on a mica substrate and growing a film, wherein the magnetron sputtering comprises the following steps: vacuumizing, annealing the mica substrate, adjusting the temperature to the growth temperature of a sample, introducing argon, pre-sputtering, formally growing a film, annealing the film, cooling and sampling;
s3, pre-stretching the flexible substrate through a stretching die;
and S4, attaching the mica substrate on which the film grows on one side to the pre-stretched flexible substrate, putting the mica substrate into an oven, heating, taking out the mica substrate, cooling, mechanically stripping the mica substrate, and controlling a stretching die to release the pre-stretching to obtain the flexible film with the fold structure.
2. The method for preparing a flexible film with a controllable folding structure under high temperature conditions according to claim 1, wherein the mica substrate of step S1 is mechanically dissociated in a water bath, and the knife edge used for dissociation should be parallel to the mica substrate.
3. The method for preparing a flexible film with a controllable corrugation structure under high temperature conditions as claimed in claim 1, wherein the central part of the high temperature sample holder in step S1 is a square SiC block of 10mm x 10mm, and the mica substrate is adhered to the SiC surface by silver colloid.
4. The method for preparing the flexible film with the controllable wrinkle structure under the high temperature condition as claimed in claim 3, wherein during the magnetron sputtering in the step S2, the SiC back side is heated by laser, and the mica substrate is kept at a high temperature during the growth of the film.
5. The method for preparing the flexible film with the controllable corrugated structure under the high temperature condition as claimed in claim 1, wherein the initial vacuum degree of the magnetron sputtering chamber in the step S2 is 5 x 10-8torr～5×10-9the heating source for mica substrate annealing and film annealing is laser heating, the substrate annealing temperature is 500-700 ℃, the film growth temperature is 500-600 ℃, the film annealing temperature is 600-800 ℃, the target and the substrate are obliquely sputtered at 30-60 ℃ during film growth, the high-temperature sample holder is kept to rotate at 10 r/min during film growth, the high-temperature sample holder is kept to rotate at 1 r/min during film annealing, and the cooling speed is 0.2-0.6 ℃/sec.
6. The method for preparing a flexible film with a controllable corrugated structure under high temperature conditions according to claim 1, wherein the cooling manner in step S4 includes water cooling and air cooling.
7. The method for preparing a flexible film with a controllable corrugation structure under high temperature conditions according to claim 1, wherein the pre-stretching of step S3 is performed after clamping two ends of the flexible substrate.
8. The method for preparing the flexible film with the controllable wrinkle structure under the high temperature condition according to claim 1, wherein the mica substrate mechanical peeling of the step S4 is to perform mechanical peeling on the mica substrate on the back of the film by using an adhesive tape.
9. The method for preparing the flexible film with the controllable corrugation structure under the high temperature condition as claimed in claim 1, wherein the releasing pre-stretching of step S4 is to keep one end of the flexible substrate fixed, and to remove the flexible film after slowly releasing the other end of the flexible substrate.
10. Use of a flexible film with a controllable corrugated structure in the electronic field, wherein the method of preparing a flexible film with a controllable corrugated structure under high temperature conditions according to any one of claims 1 to 9 is applied in the electronic field.
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| CN202111391287.1A CN114351090A (en) | 2021-11-23 | 2021-11-23 | Method for preparing flexible film with adjustable fold structure under high temperature condition and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117604461A (en) * | 2023-11-29 | 2024-02-27 | 成光新材料科技(无锡)有限公司 | Preparation method of epitaxial pleated film |
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| US20150197058A1 (en) * | 2014-03-26 | 2015-07-16 | Sourabh Kumar Saha | Wrinkled surfaces with tunable hierarchy and methods for the preparation thereof |
| CN106877732A (en) * | 2017-03-17 | 2017-06-20 | 中国科学院半导体研究所 | Friction generator and preparation method based on fold conductive film, integrated morphology |
| CN113594357A (en) * | 2020-04-30 | 2021-11-02 | 南京理工大学 | ABO3Flexible stretchable single crystal film and preparation method thereof |
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2021
- 2021-11-23 CN CN202111391287.1A patent/CN114351090A/en active Pending
Patent Citations (3)
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| US20150197058A1 (en) * | 2014-03-26 | 2015-07-16 | Sourabh Kumar Saha | Wrinkled surfaces with tunable hierarchy and methods for the preparation thereof |
| CN106877732A (en) * | 2017-03-17 | 2017-06-20 | 中国科学院半导体研究所 | Friction generator and preparation method based on fold conductive film, integrated morphology |
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Non-Patent Citations (1)
| Title |
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| "Preparation and magnetic properties of wrinkled FeRh flexible films", 《AIP ADVANCES》, vol. 10, no. 2, 24 February 2020 (2020-02-24), pages 2 * |
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| CN117604461A (en) * | 2023-11-29 | 2024-02-27 | 成光新材料科技(无锡)有限公司 | Preparation method of epitaxial pleated film |
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