CN117658119A - Preparation method of ultra-flat nano film - Google Patents
Preparation method of ultra-flat nano film Download PDFInfo
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- CN117658119A CN117658119A CN202311661851.6A CN202311661851A CN117658119A CN 117658119 A CN117658119 A CN 117658119A CN 202311661851 A CN202311661851 A CN 202311661851A CN 117658119 A CN117658119 A CN 117658119A
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Abstract
The invention provides a preparation method of an ultra-flat nano film, which comprises the following steps: coating a transfer adhesive layer on the upper surface of the nanomaterial; placing the nanomaterial on the smooth surface of the target substrate, and enabling the lower surface of the nanomaterial to be attached to the smooth surface of the target substrate; removing the transfer adhesive layer; coating a dielectric layer on the upper surface of the nano material; etching the target substrate to obtain the ultra-flat nano film. The material of the transfer bonding layer comprises vaseline, paraffin or rosin, the nano material comprises graphene or boron nitride, and the material of the dielectric layer comprises epoxy resin or polyester resin. According to the method, the nanomaterial is in conformal contact with the target substrate with the smooth surface, the target substrate is removed after being closely adhered and conformal, and the ultra-flat graphene and boron nitride film can be obtained.
Description
Technical Field
The invention relates to the technical field of micro-nano material films, in particular to a preparation method of an ultra-flat nano film.
Background
Currently, nano-films have wide applications in semiconductor device fabrication, electronic devices and equipment, etc., such as graphene films. In the prior art, a CVD direct growth method or a transfer method is generally used to prepare a graphene film with high flatness. However, the two methods have the following disadvantages:
the direct growth method is limited by a target substrate (such as a monocrystalline copper substrate, a sapphire substrate, a silicon wafer and the like), and can only realize the growth of the graphene with high flatness on the fixed substrate, and the energy consumption is high.
In the transfer method, because of strong coupling effect with a transferred target substrate, wrinkles are always formed during the growth period, so that line defects are caused, the continuity of graphene is affected, the adhesive on the surface is difficult to clean, and the uniformity of preparation of a graphene device is limited; in addition, by directly coating a layer (film) on the surface of the graphene/growth substrate, the transferred graphene can be used for re-engraving the surface morphology of the copper foil, and the surface roughness is not easy to control.
Thus, there is a need for a method of preparing ultra-flat nano-films.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a preparation method of an ultra-flat nano film, which adopts the following technical scheme:
in a first aspect, a method for preparing an ultra-flat nano-film is provided;
in a first implementation, the method of preparing includes:
coating a transfer adhesive layer on the upper surface of the nanomaterial;
placing the nanomaterial on the smooth surface of the target substrate, and enabling the lower surface of the nanomaterial to be attached to the smooth surface of the target substrate;
removing the transfer adhesive layer;
coating a dielectric layer on the upper surface of the nano material;
etching the target substrate to obtain the ultra-flat nano film.
In combination with the first implementation manner, in a second implementation manner, the material of the transfer adhesive layer includes vaseline, paraffin or rosin;
coating a transfer adhesive layer on the upper surface of the nanomaterial, comprising: heating the transfer adhesive layer material to be molten, then uniformly coating the molten transfer adhesive layer material on the surface of the nano material by using a spin coater, and cooling;
or uniformly dripping the melted transfer bonding layer material liquid on the surface of the nano material until the liquid covers the surface of the nano material and overflows immediately, and cooling.
In combination with the first implementation manner, in a third implementation manner, after the transfer adhesive layer is coated on the upper surface of the nanomaterial, a layer of supporting framework is added on the surface of the transfer adhesive layer, and the supporting framework comprises a screen window net, a polytetrafluoroethylene plate and a PET film.
In combination with the first realizable mode, in a fourth realizable mode, the nanomaterial comprises graphene or boron nitride.
With reference to the first implementation manner, in a fifth implementation manner, the target substrate is in a rigid planar structure, and at least one of the upper and lower surfaces of the target substrate is a smooth surface; target substrates include silicon wafers and glass.
In combination with the first implementation, in a sixth implementation, the solvent is applied to the smooth surface of the target substrate before the nanomaterial is placed on the smooth surface of the target substrate; the solvent comprises deionized water, absolute ethanol solution diluted by deionized water, absolute ethanol or acetone;
the manner of applying the solvent includes immersing the target substrate in the solvent.
With reference to the first implementation manner, in a seventh implementation manner, removing the transfer adhesive layer includes:
the transfer bonding layer is melted by heating, then is put into normal hexane solution for water bath heating, is put into preheated petroleum ether solution for heating, and finally is dried by a nitrogen gun.
With reference to the first implementation manner, in an eighth implementation manner, the material of the dielectric layer includes epoxy resin or polyester resin;
coating a dielectric layer on the upper surface of the nanomaterial, comprising: and coating liquid epoxy resin or polyester resin on the upper surface of the graphene in a spin coating/drop coating/doctor blade coating/rolling mode, and standing to completely solidify the graphene.
With reference to the first implementation manner, in a ninth implementation manner, after the dielectric layer is coated on the upper surface of the nanomaterial, an additional support film is placed on the upper surface of the dielectric layer; the material of the additional support film comprises polytetrafluoroethylene, PET or sapphire.
In a second aspect, there is provided an ultra-flat nano-film, which is prepared by any one of the first to ninth realizable modes provided in the first aspect, and includes an ultra-flat graphene film and an ultra-flat boron nitride film.
According to the technical scheme, the beneficial technical effects of the invention are as follows:
the ultra-flat graphene and boron nitride film can be obtained by conformally contacting the nanomaterial with a target substrate with a smooth surface, closely attaching the nanomaterial to the target substrate, and removing the target substrate. Factors influencing the performance of the device, such as residual glue and wrinkles on the surfaces of graphene and boron nitride, are avoided, and the surface of the obtained film is smooth and clean. The process steps are few, the method is simple and easy to operate, and the nano film with the smooth surface is obtained in a macroscopic mode, so that compared with microscopic growth, the method is more amplified and operable.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. Like elements or portions are generally identified by like reference numerals throughout the several figures. In the drawings, elements or portions thereof are not necessarily drawn to scale.
FIG. 1 is a flow chart of an embodiment of the present invention for preparing an ultra-flat nano-film;
FIG. 2 is a schematic diagram of a process for preparing an ultra-flat graphene film according to an embodiment of the present invention;
reference numerals:
1-transfer adhesive layer, 2-graphene, 3-target substrate, 4-dielectric layer, 5-additional support film.
Detailed Description
Embodiments of the technical scheme of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for more clearly illustrating the technical aspects of the present invention, and thus are merely examples, and are not intended to limit the scope of the present invention.
It is noted that unless otherwise indicated, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention pertains.
Examples
The embodiment provides a preparation method of an ultra-flat nano film, which comprises the following steps of: the prepared nano material, the transfer bonding layer, the target substrate, and the additional support film and the medium layer.
In this embodiment, for the prepared nanomaterial, the material includes graphene and boron nitride, and the shape and size of the nanomaterial are not limited, for example, single-layer or multi-layer graphene can be used; the nanometer material can be selected from self-supporting films or copper foil.
The transfer adhesive layer is not limited in its implementation form, and a substance that releases the nano-film stress by utilizing the difference in thermal expansion coefficient, such as vaseline, paraffin, rosin, or the like, may be used. In a specific embodiment, when the transfer adhesive layer is solid, it is necessary to pretreat it in the following manner: and (5) placing part of the bonding layer for transferring in a container, heating in a water bath, and finishing pretreatment after the bonding layer is melted.
The target substrate is a rigid plane with a smooth surface, the material and the size of the target substrate are not limited, and the materials such as silicon chips, glass and the like are exemplified, and the size of the target substrate is determined according to the ultra-flat nano-film prepared according to the requirement. Preferably, at least one of the upper and lower surfaces of the target substrate is a smooth surface having a surface roughness of less than 10 nanometers.
Dielectric layer: acid-resistant epoxy resins may be used, as well as highly corrosion-resistant polyester resins, such as epoxy resins and ethylenically unsaturated monoacid addition reactants. The dielectric layer is used for fixing the graphene structure in the preparation process and provides a supporting effect for the graphene film. Epoxy resin is used as a common resin matrix, has the characteristics of excellent adhesive property, mechanical strength, heat resistance, dielectric property and the like, and can be cured under ultraviolet irradiation; and the material has inertia in strong acid and strong corrosive solution, and is a good dielectric layer material.
As shown in fig. 1, the preparation of the ultra-flat nano-film is performed as follows:
s1, coating a transfer bonding layer on the upper surface of the nano material
Transfer bond layer with solid petrolatum, nanomaterial with graphene is illustrated: and (3) taking a proper amount of solid vaseline into a beaker, and heating in a water bath at 60-70 ℃ until the solid vaseline is melted. And then uniformly coating the melted Vaseline on the surface of the graphene by using a spin coater, or directly uniformly dripping the melted Vaseline liquid on the surface of the graphene until the Vaseline liquid covers the surface of the graphene and overflows immediately, and cooling to obtain the transfer bonding layer/graphene composite structure.
In some embodiments, when transferring large-area graphene, a layer of supporting framework, such as a screen mesh, a polytetrafluoroethylene plate, PET (polyethylene terephthalate) and the like, can be added on the surface of the transfer adhesive layer, and preferably the screen mesh. By adding the supporting framework, a certain mechanical force can be provided as a support, and the preparation of a large-area film is facilitated.
And for the grapheme with the back, for example, the back is a copper foil, the grapheme coated with the transfer bonding layer is put into ferric trichloride etching solution to be etched for 1h, the surface of the copper foil is washed by clear water in the period, and the process is repeated for three times for 2-3min each time, so that the effect of removing the back copper foil is achieved. In a specific embodiment, feCl is contained in the ferric trichloride etching solution 3 The concentration of (2) was 1mol/L and the mass fraction of HCL was 5%.
In some embodiments, in order to remove the back more thoroughly, the back of the graphene/copper foil may also be sealed with tape upwards before the transfer of the adhesive layer is applied, and the back of the graphene/copper foil is etched by a reactive ion etcher. After etching, continuously flushing the residual etching liquid on the surface of the graphene with clear water, and then carrying out the operation of the subsequent steps. The step of coating the transfer bonding layer is used for releasing graphene stress in subsequent operation, so that the prepared graphene film is flatter, and warping caused by internal attractive force is reduced.
In this step, the thickness of the transfer bond layer is in the order of millimeters, typically 1-2mm.
S2, placing the nano material on the smooth surface of the target substrate to enable the lower surface of the nano material to be attached to the smooth surface of the target substrate
And placing the graphene coated with the transfer bonding layer on the smooth surface of the target substrate, and attaching the graphene to the smooth surface of the target substrate to obtain the transfer bonding layer/graphene/target substrate composite structure.
In some embodiments, in order to make the graphene more tightly fit to the smooth surface of the target substrate, a solvent may be applied to the smooth surface of the target substrate before the graphene is placed on the smooth surface of the target substrate. The solvent is selected from low surface tension liquid with certain volatility, such as deionized water, absolute ethanol solution diluted by deionized water (volume ratio of water to absolute ethanol is 1:1), absolute ethanol, and acetone; preferably, diluted absolute ethanol is used as the solvent.
S3, removing the transfer bonding layer
In a specific embodiment, the transfer adhesive layer is taken as vaseline, and the target substrate is taken as a silicon wafer for illustration: and heating the transfer bonding layer/the graphene/the target substrate by using a heating table to melt Vaseline, respectively putting n-hexane and petroleum ether for 1h after residual liquid between the graphene and the silicon wafer is baked, and drying by using a nitrogen gun to obtain the graphene/target substrate composite structure.
After the treatment of this step, the upper surface of the graphene is not smooth, and in general, the upper surface of the graphene will have wrinkles, residual impurity particles, and the like.
S4, coating a dielectric layer on the upper surface of the nano material
In a specific embodiment, the dielectric layer is exemplified by epoxy resin: and (3) coating the acid-resistant and corrosion-resistant liquid epoxy resin on the upper surface of the graphene by using a spin coater (or using a dropping/blade coating/rolling mode), and standing to completely solidify the graphene to obtain the dielectric layer/graphene/target substrate composite structure.
In some embodiments, a certain pressure can be applied downwards to the cured dielectric layer, so that the lower surface of the graphene is tightly attached to the smooth surface of the target substrate; the manner of the pressure application treatment is not limited, and weight pressing or pressing treatment using a tablet press may be selected.
In this step, the thickness of the dielectric layer is typically less than 2mm.
S5, etching the target substrate to obtain the ultra-flat nano film
The manner of etching the target substrate is not limited, and the target substrate is exemplified by a silicon wafer: placing the dielectric layer/graphene/target substrate composite structure into hydrofluoric acid, and etching the target substrate; after all the target substrates are corroded, an ultra-flat graphene film with a dielectric layer/graphene composite structure (the thickness of single-layer graphene is only about 0.3nm, and self-support is difficult to realize under the action of no dielectric layer) is obtained, and in the dielectric layer/graphene composite structure, the lower surface of graphene is smooth.
In some embodiments, in order to facilitate industrial application, for example, to prepare a large-area ultra-flat graphene film, after the dielectric layer is coated on the upper surface of the nanomaterial in step S4, an additional support film may be placed on the upper surface of the dielectric layer for standing and curing, and then a certain pressure is applied downward to the additional support film, so that the lower surface of the nanomaterial is more tightly adhered to the smooth surface of the target substrate; the manner of the pressure application treatment is not limited, and weight pressing or pressing treatment using a tablet press may be selected. The additional support film may be selected from highly corrosion resistant polyesters, typically adducts of epoxy resins and ethylenically unsaturated monoacids such as polytetrafluoroethylene, PET, sapphire, and the like; in some embodiments, the polytetrafluoroethylene support membrane may be optionally wrapped in a roll or sheet. Taking the dielectric layer as epoxy resin and the additional support film as PET as an example for illustration: the prepared ultra-flat graphene film is of a graphene/epoxy resin/PET composite structure, and can be directly used as a transparent conductive film for application test.
The following is the actual preparation process of the ultra-flat nano film:
example 1 preparation of ultra-Flat graphene film
The vaseline adopts vaseline with 99% purity, and is heated in water bath at 70deg.C for 20min to melt. And (3) placing the graphene/copper foil on a heating table, setting the temperature of the heating table to be 50 ℃, slowly coating the vaseline solution which is melted into liquid on the surface of the copper foil on which the graphene grows until the surface of the graphene/copper foil is covered by the vaseline liquid and overflows, and cooling for tens of seconds at room temperature to solidify the vaseline without continuously adding the vaseline.
Sticking the cut screen mesh (the area is slightly larger than the area of the sample to be transferred) on the surface of solidified vaseline, and adding 1mol/L FeCl 3 Etching in etching solution for 1h, removing back bottom for 2-3 times, wherein the time interval for removing back bottom and the rinsing time of clear water can be maintained at about 2-3 min. Washing with clear water to directly pinch one corner of the screen window net, washing with deionized water, preparing water diluted absolute ethanol solution (volume ratio is 1:1), cleaning in ultrasonic cleaner for 15-30min, and removing bubbles in the solution. And meanwhile, soaking the silicon wafer in the prepared ethanol solution, and waiting for lamination.
And after etching, lifting the graphene/vaseline composite structure from the etching liquid by one corner of the handheld screen window net, continuously flushing the etching liquid remained on the surface of the graphene with clear water, and then attaching the graphene on the smooth surface of the silicon wafer. And vertically placing the bonded Vaseline/graphene/silicon wafer composite structure for 1h, fully leaving residual liquid between bonding interfaces, and then placing the bonded Vaseline/graphene/silicon wafer composite structure in an oven for heating at 30 ℃ for 24h.
Taking out the Vaseline/graphene/silicon wafer composite structure, and removing the screen window net. And placing the Vaseline/graphene/silicon wafer composite structure with the screen window mesh removed on a heating table at 50 ℃ until the Vaseline is changed into a liquid state again. The silicon wafer is vertically placed so that redundant vaseline is left under the action of gravity and then is placed into normal hexane solution, and the silicon wafer is heated in water bath at 60 ℃ for 1h; then put into the preheated petroleum ether solution and heated for 1h at 90 ℃. And taking out the silicon wafer from which the vaseline is removed from the petroleum ether, flushing the surface of the silicon wafer with clean petroleum ether and absolute ethyl alcohol respectively, and finally drying by a nitrogen gun to obtain the graphene/silicon wafer composite structure.
And coating transparent epoxy resin on the surface of graphene of the graphene/silicon wafer composite structure, and covering a layer of PET film on the surface of the epoxy resin. And irradiating the PET side for 30min or more by an ultraviolet lamp to ensure the epoxy resin to be fully cured.
And (3) putting the PET/epoxy resin/graphene/silicon wafer composite structure into a hydrofluoric acid solution with the concentration of 10% -50%, etching at the temperature of 50 ℃ for about 3 hours until the silicon wafer is completely corroded and disappears, taking out the PET/epoxy resin/graphene composite structure, putting into deionized water for soaking, washing and drying to obtain the smooth ultra-flat graphene film.
Example 2 preparation of ultra-Flat boron nitride film
Paraffin wax with 99% purity is heated in 90 deg.c water bath for 20min to melt. Meanwhile, the glass sheet is soaked in the prepared ethanol solution to wait for lamination.
The molten paraffin was coated on the surface of the boron nitride film using a spin coater, and then boron nitride was attached to the smooth surface of the glass sheet. And vertically placing the bonded paraffin/boron nitride/glass sheet composite structure for 1h, fully leaving residual liquid between bonding interfaces, and then placing the bonded paraffin/boron nitride/glass sheet composite structure in an oven for heating at 30 ℃ for 24h.
Taking out the paraffin/boron nitride/glass sheet composite structure, and placing the paraffin/boron nitride/glass sheet composite structure on a heating table at 90 ℃ until the paraffin is changed into a liquid state again. The glass sheet was placed vertically so that excess paraffin remained under the force of gravity, and then placed in an n-hexane solution and heated in a water bath at 60℃for 1 hour. And taking out the glass sheet from which the paraffin is removed from the n-hexane, flushing the surface of the glass sheet by using clean n-hexane and absolute ethyl alcohol respectively, and finally drying by using a nitrogen gun to obtain the boron nitride/glass sheet composite structure.
And (3) coating polyester resin on the surface of boron nitride of the boron nitride/glass sheet composite structure, then putting the polyester resin/boron nitride/glass sheet composite structure into 10% -50% hydrofluoric acid solution, etching at 50 ℃ for about 3 hours until the glass sheet is completely corroded and disappears, taking out the polyester resin/boron nitride/composite structure, putting into deionized water for soaking, washing and drying to obtain the smooth ultra-flat boron nitride film.
By adopting the technical scheme of the embodiment, the ultra-flat graphene and boron nitride film can be obtained by contacting the nanomaterial with the target substrate with a smooth surface in a conformal manner, closely attaching the nanomaterial to the target substrate, and removing the target substrate. Factors influencing the performance of the device, such as residual glue and wrinkles on the surfaces of graphene and boron nitride, are avoided, and the surface of the obtained film is smooth and clean. The process steps are few, the method is simple and easy to operate, and the nano film with the smooth surface is obtained in a macroscopic mode, so that compared with microscopic growth, the method is more amplified and operable.
The preparation method can be suitable for preparing devices by films made of various different transparent materials, for example, the transparent graphene film can be widely applied to various scenes such as transparent conductive films, luminous OLED devices, flexible display screens and the like.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention, and are intended to be included within the scope of the appended claims and description.
Claims (10)
1. The preparation method of the ultra-flat nano film is characterized by comprising the following steps:
coating a transfer adhesive layer on the upper surface of the nanomaterial;
placing the nanomaterial on the smooth surface of the target substrate, and enabling the lower surface of the nanomaterial to be attached to the smooth surface of the target substrate;
removing the transfer adhesive layer;
coating a dielectric layer on the upper surface of the nano material;
etching the target substrate to obtain the ultra-flat nano film.
2. The method according to claim 1, wherein the material of the transfer adhesive layer comprises vaseline, paraffin or rosin;
coating a transfer adhesive layer on the upper surface of the nanomaterial, comprising: heating the transfer adhesive layer material to be molten, then uniformly coating the molten transfer adhesive layer material on the surface of the nano material by using a spin coater, and cooling;
or uniformly dripping the melted transfer bonding layer material liquid on the surface of the nano material until the liquid covers the surface of the nano material and overflows immediately, and cooling.
3. The preparation method according to claim 1, wherein after the transfer adhesive layer is coated on the upper surface of the nanomaterial, a layer of supporting framework is added on the surface of the transfer adhesive layer, and the supporting framework comprises a screen mesh, a polytetrafluoroethylene plate and a PET film.
4. The method of claim 1, wherein the nanomaterial comprises graphene or boron nitride.
5. The method of claim 1, wherein the target substrate is a rigid planar structure, and at least one of the upper and lower surfaces of the target substrate is a smooth surface; the target substrate comprises a silicon wafer and glass.
6. The method of claim 1, wherein the solvent is applied to the smooth surface of the target substrate prior to the nanomaterial being placed on the smooth surface of the target substrate; the solvent comprises deionized water, absolute ethanol solution diluted by deionized water, absolute ethanol or acetone;
the manner of applying the solvent includes immersing the target substrate in the solvent.
7. The method of manufacturing according to claim 1, wherein removing the transfer adhesive layer comprises:
the transfer bonding layer is melted by heating, then is put into normal hexane solution for water bath heating, is put into preheated petroleum ether solution for heating, and finally is dried by a nitrogen gun.
8. The method of claim 1, wherein the dielectric layer comprises an epoxy or polyester resin;
coating a dielectric layer on the upper surface of the nanomaterial, comprising: and coating liquid epoxy resin or polyester resin on the upper surface of the graphene in a spin coating/drop coating/doctor blade coating/rolling mode, and standing to completely solidify the graphene.
9. The method of claim 1, wherein the additional support film is placed on the upper surface of the dielectric layer after the dielectric layer is coated on the upper surface of the nanomaterial; the material of the additional support film comprises polytetrafluoroethylene, PET or sapphire.
10. An ultra-flat nano film, which is characterized by being prepared by the method of any one of claims 1-9, comprising an ultra-flat graphene film and an ultra-flat boron nitride film.
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