CN111057999B - Method and equipment for preparing nano porous silicon dioxide film by continuous wave laser irradiation - Google Patents

Method and equipment for preparing nano porous silicon dioxide film by continuous wave laser irradiation Download PDF

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CN111057999B
CN111057999B CN201911307643.XA CN201911307643A CN111057999B CN 111057999 B CN111057999 B CN 111057999B CN 201911307643 A CN201911307643 A CN 201911307643A CN 111057999 B CN111057999 B CN 111057999B
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continuous wave
silicon
preparing
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silica film
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CN111057999A (en
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王楠
钟奇
谢雨江
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Shanghai Mifeng Laser Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/10Glass or silica
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58After-treatment
    • C23C14/5806Thermal treatment
    • C23C14/5813Thermal treatment using lasers

Abstract

The invention relates to the technical field of preparation of porous silicon dioxide films, in particular to a method and equipment for preparing a nano porous silicon dioxide film by continuous wave laser irradiation. Compared with the prior art, the invention has the advantages that: the method can avoid using chemical reagents causing environmental pollution as much as possible, and can ensure the cleanliness of the film; the uniformity of the pore size of the nanoporous silica film can be precisely controlled.

Description

Method and equipment for preparing nano porous silicon dioxide film by continuous wave laser irradiation
Technical Field
The invention relates to the technical field of preparation of porous silicon dioxide films, in particular to a method and equipment for preparing a nano porous silicon dioxide film through continuous wave laser irradiation.
Background
The nano porous silicon dioxide film has the characteristics of low density, adjustable refractive index, low dielectric constant, high thermal stability and the like, and can be applied to the fields of optical films, dielectric materials, sensors, filters and the like. The preparation technology of the nano porous silicon dioxide becomes the key research point of the material world at home and abroad at present. The method for preparing the nano porous silicon dioxide film by using the sol-gel method, evaporation, sputtering and other methods is widely applied to industrial production due to the characteristics of low cost, good repeatability and the like. However, on one hand, the method adopts chemical reagents, and the recovery of waste liquid in the production can cause potential environmental pollution problems; on the other hand, the method may also have the problem of film cracking during the drying process; in addition, the method can not provide effective guarantee for the uniformity of the size of the nanometer pores and the cleanliness of the thin film, and the application of the method in the field of integrated circuits is limited. The invention adopts a brand new method to irradiate the silicon-rich silicon oxide film through the continuous wave laser to prepare the nano porous silicon dioxide film, which can accurately control the uniformity of the pore size of the nano porous silicon dioxide film and ensure the high cleanliness of the film.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides a method and equipment for preparing a nano porous silica film by continuous wave laser irradiation, which are used for accurately controlling the uniformity of the pore size of the nano porous silica film.
In order to achieve the purpose, the method for preparing the nano porous silicon dioxide film through continuous wave laser irradiation is designed, a silicon-rich silicon dioxide film is fixed on a moving platform arranged in a closed metal cavity, a quartz window is arranged on one side of the metal cavity, which is perpendicular to the moving direction of the moving platform, a focusing lens is used for focusing a laser spot of continuous wave laser on the surface of the silicon-rich silicon dioxide film through the quartz window, nitrogen airflow is continuously introduced into the metal cavity, nano holes with different densities are obtained by controlling the moving speed of the moving platform, and the nano holes with different thicknesses are obtained by controlling the laser power.
The invention also has the following preferable technical scheme:
the method also comprises the following preparation steps of the silicon-rich silicon oxide film: step a, cleaning molten glass; and b, taking the molten glass as a substrate, and depositing the silicon-rich silicon oxide film.
The step a specifically comprises the following steps: the molten glass was immersed in an isopropanol solution for ultrasonic cleaning.
The step a further comprises: and taking out the molten glass after the ultrasonic cleaning is finished, and drying the molten glass by using nitrogen.
The diameter of the molten glass adopted in the step a is 20mm, and the thickness of the molten glass is 2 mm.
The step b specifically comprises the following steps: the silicon-rich silicon oxide film is prepared by an ion sputtering method, monocrystalline silicon is used as a target material, argon is used as a sputtering gas, oxygen is used as a reaction gas, the silicon-rich silicon oxide films with different oxygen contents are prepared by adjusting the flow rate of the oxygen, and the thickness of the silicon-rich silicon oxide film is adjusted by controlling the sputtering time.
And b, using monocrystalline silicon with the diameter of 40mm and the thickness of 2mm as a target material to prepare the silicon-rich silicon oxide film with the oxygen content of 75% and the thickness of 545 nm.
And a continuous wave diode laser with the wavelength of 405nm is adopted to obtain the continuous wave laser, and laser spots are focused to the surface of the silicon-rich silicon oxide film through a quartz window by a focusing lens of 10 times.
The density of the laser power is more than or equal to 1.16 ∙ 105 W/cm2
The invention also relates to equipment for the method for preparing the nano porous silicon dioxide film by continuous wave laser irradiation, which comprises a closed metal cavity, wherein a moving platform is arranged in the metal cavity, the metal cavity is respectively provided with an air inlet and an air outlet at two sides of the moving direction of the moving platform for nitrogen airflow to pass through, a quartz window is arranged at one side of the metal cavity perpendicular to the moving direction of the moving platform, and a focusing lens is arranged at the outer side of the quartz window and used for focusing laser spots of continuous wave laser to the surface of the silicon-rich silicon oxide film through the quartz window and an air passage for introducing nitrogen airflow into the metal cavity.
Compared with the prior art, the invention has the advantages that:
1. compared with the existing sol-gel method for preparing the nano porous silicon dioxide film, the method has obvious advantages. On one hand, the sol-gel method adopts chemical reagents, which can cause potential environmental pollution in the later waste liquid recovery process; on the other hand, the residue of the chemical agent also causes contamination of the thin film, thereby limiting its application in the field of integrated circuits. The technology for preparing the nano porous silicon dioxide film by laser irradiation can avoid using chemical reagents causing environmental pollution as far as possible and can ensure the cleanliness of the film.
2. Compared with other technologies for preparing the nano porous silicon dioxide film, the method can accurately control the uniformity of the pore size of the nano porous silicon dioxide film. Because the method is based on the phase transition mechanism of continuous wave laser irradiation induced silicon-rich silicon oxide, the nano-pores of the film are formed due to the evaporation and vaporization of the silicon nanoparticles formed in the early stage. Therefore, the size of the silicon nanoparticles formed at the beginning will directly determine the size of the pores of the nano-silica. The uniformity of the silicon nano particles is controlled to realize the accurate control of the uniformity of the pore size of the nano porous silicon dioxide film, and reliable technical support is provided for the future application of the nano porous silicon dioxide film in the field of integrated circuits.
Drawings
FIG. 1 is a schematic diagram of a method for preparing a nanoporous silica film by continuous wave laser irradiation according to the invention in one embodiment.
FIG. 2 is a structural view and a schematic view of a film composition of a sample prepared by the method of the present invention in one embodiment.
FIG. 3 is a schematic thickness diagram of nano-holes obtained at different laser power densities by the method of the present invention according to one embodiment.
In the figure: 1. the device comprises a continuous wave laser 2, a focusing lens 3, a quartz window 4, a silicon-rich silicon oxide film 5, a fused glass substrate 6 of the silicon-rich silicon oxide film and a moving platform.
Detailed Description
The principles and construction of such a method and apparatus will be apparent to those skilled in the art from the following further description of the invention, taken in conjunction with the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the embodiment, the method fixes a silicon-rich silicon oxide film on a moving platform arranged in a closed metal cavity, the metal cavity is respectively provided with an air inlet and an air outlet at two sides of the moving direction of the moving platform for nitrogen gas flow to pass through, in the embodiment, the moving direction of the moving platform in figure 1 is the up-down direction, namely the upper side and the lower side of the metal cavity are respectively provided with the air inlet and the air outlet, the metal cavity is provided with a quartz window at one side perpendicular to the moving direction of the moving platform, namely the left side of the metal cavity in the demonstration market of the present market is provided with the quartz window, the silicon-rich silicon oxide film is fixed at the left side of the moving platform, a focusing lens is used for focusing a laser spot of continuous wave laser to the surface of the silicon-rich silicon oxide film through the quartz window, and simultaneously continuously introducing the nitrogen gas flow into the metal cavity along the moving direction of the moving platform, the nano holes with different densities can be obtained by controlling the moving speed of the moving platform, and the moving speed of the moving platform can influence whether the irradiation area can be completely changed into the nano holes, for example, if the moving speed is too high (the laser irradiation time is short), although the nano holes can be generated, the number is not large enough; if the moving speed is small (laser irradiation time is short), the film in the entire laser irradiation area becomes a nano-pore. The nano holes with different thicknesses are obtained by controlling the laser power.
Examples
First, molten glass is cleaned: molten glass with a diameter of 20mm and a thickness of 2mm was immersed in an isopropanol solution with a concentration of 99.9% for ultrasonic cleaning for 5 minutes, and was taken out and blown dry with nitrogen.
Then, preparing the silicon-rich silicon oxide film by adopting an ion sputtering method: high-purity monocrystalline silicon with the diameter of 40mm and the thickness of 2mm is used as a target material, high-purity argon is used as sputtering gas, high-purity oxygen is used as reaction gas, the sputtering temperature is room temperature, silicon-rich silicon oxide films with different oxygen contents are prepared by adjusting the flow of the oxygen, the thickness of the film is adjusted by controlling the sputtering time, and finally the silicon-rich silicon oxide film with the oxygen content of 75% and the thickness of 545nm is obtained.
After the silicon-rich silicon oxide film is prepared, irradiating the silicon-rich silicon oxide film by laser: as shown in fig. 1, will be based on the enrichment of a molten glass substrateThe silicon oxide film sample is placed on a moving platform capable of accurately controlling the position of the sample, the moving platform is placed in a metal cavity with a quartz window, and the diameter of the quartz window of the metal cavity is 50 mm, and the thickness of the quartz window of the metal cavity is 2 mm. The stable nitrogen gas flow is continuously introduced into the cavity, high-purity nitrogen gas is adopted for the stable nitrogen gas flow, the stable gas flow is continuously introduced into the metal cavity and formed, the gas flow range is 20 sccm to 100 sccm, a continuous wave diode laser with the wavelength of 405nm is adopted, a laser spot is focused on a film sample through a quartz window by a 10-time focusing lens, the diameter of the laser spot is about 6 um, the moving speed of a sample position control platform is 50 um/s, and the laser power density is 1.75 × 105W/cm2, finally obtaining the nano-porous silica film.
In a preferred embodiment, it is believed that the laser power density has a preferred threshold value, above which nanopores can be created, and below which nanopores are difficult to create, through experimentation. Through multiple experiments, the critical value of the laser power density for generating the nano holes is 1.16 ∙ 105W/cm2, above which nano holes are generated, and below which nano holes are not generated. Too high a laser power can cause the formation of nanoholes to extend longitudinally along the depth of the film until the area of the film that is being lased becomes nanoholes. For further illustration, we present the power density at different values (1.22 ∙ 10)5 W/cm2 (a)、1.4∙105 W/cm2(b)、1.75∙105W/cm2 (c)) nanohole formation thickness, as shown in fig. 3, the thickness of the nanohole region increases with increasing laser power density, which further increases the laser power density, which results in the entire film region becoming nanohole.
And after the preparation of the nano porous silicon dioxide film is finished, confirming the structural components of the nano porous silicon dioxide film. Preparing a transmission electron microscope cross-section sample by adopting a focused ion beam technology, and preparing a gold nano-layer with the thickness of 5nm by a vacuum evaporation method before preparing the transmission electron microscope cross-section sample so as to prevent the transmission electron microscope sample from being influenced by the discharge phenomenon in the working environment of the focused ion beam technology; the structure of the sample is observed by a scanning transmission electron microscope technology, as shown in fig. 2, a silicon-rich silicon oxide film forms a porous structure (white part) after being irradiated by laser, and the components of the film are further measured by an energy-dispersive X-ray spectroscopy technology, and the components of the film are consistent with those of the substrate due to the fact that the substrate is SiO2, so that the formation of the nano-porous silicon dioxide is determined. It should be noted here that the Au, Pt and C components on the sample surface are introduced during the preparation of the transmission electron microscope sample by the focused ion beam technique, and are not introduced during the laser irradiation process and the preparation process of the silicon-rich silicon oxide film.

Claims (10)

1. A method for preparing a nano-porous silica film by continuous wave laser irradiation, characterized in that the method comprises: fixing the silicon-rich silicon oxide film on a moving platform arranged in a closed metal cavity, wherein a quartz window is arranged on one side of the metal cavity perpendicular to the moving direction of the moving platform, focusing a laser spot of continuous wave laser on the surface of the silicon-rich silicon oxide film through the quartz window by using a focusing lens, continuously introducing nitrogen airflow into the metal cavity, obtaining nano holes with different densities by controlling the moving speed of the moving platform, and obtaining the nano holes with different thicknesses by controlling the laser power.
2. The method for preparing a nanoporous silica film by continuous wave laser irradiation as claimed in claim 1 wherein the method further comprises the step of preparing a silicon-rich silica film:
step a, cleaning molten glass;
and b, taking the molten glass as a substrate, and depositing the silicon-rich silicon oxide film.
3. The method for preparing a nanoporous silica film by continuous wave laser irradiation as claimed in claim 2, wherein the step a specifically comprises: the molten glass was immersed in an isopropanol solution for ultrasonic cleaning.
4. The method for preparing a nanoporous silica film by continuous wave laser irradiation as claimed in claim 3 wherein the step a further comprises: and taking out the molten glass after the ultrasonic cleaning is finished, and drying the molten glass by using nitrogen.
5. The method for preparing a nanoporous silica film by continuous wave laser irradiation as claimed in claim 2, wherein the step b specifically comprises: the silicon-rich silicon oxide film is prepared by an ion sputtering method, monocrystalline silicon is used as a target material, argon is used as a sputtering gas, oxygen is used as a reaction gas, the silicon-rich silicon oxide films with different oxygen contents are prepared by adjusting the flow rate of the oxygen, and the thickness of the silicon-rich silicon oxide film is adjusted by controlling the sputtering time.
6. The method for preparing a nanoporous silica film by continuous wave laser irradiation as claimed in claim 2 wherein the molten glass used in step a has a diameter of 20mm and a thickness of 2 mm.
7. The method for preparing a nanoporous silica film by continuous wave laser irradiation as defined in claim 2, wherein the step b is performed by using single crystal silicon with a diameter of 40mm and a thickness of 2mm as a target material to prepare a silicon-rich silica film with an oxygen content of 75% and a thickness of 545 nm.
8. The method for preparing a nanoporous silica film by irradiation of a continuous wave laser as claimed in claim 1, wherein the continuous wave laser is obtained by using a continuous wave diode laser with a wavelength of 405nm, and the laser spot is focused to the surface of the silica-rich silica film through a quartz window by a focusing lens of 10 times.
9. The method for preparing a nanoporous silica film by continuous wave laser irradiation as claimed in claim 1 wherein the densification of the laser power is such thatDegree of 1.16 x 10 or more5 W/cm2
10. The apparatus for preparing a nanoporous silica film by continuous wave laser irradiation as claimed in claim 1, wherein the apparatus comprises a closed metal cavity, the inside of the metal cavity is provided with a moving platform, the metal cavity is respectively provided with an air inlet and an air outlet at two sides of the moving platform in the moving direction for nitrogen gas to pass through, the metal cavity is provided with a quartz window at one side perpendicular to the moving direction of the moving platform, a focusing lens is arranged at the outer side of the quartz window for focusing the laser spot of the continuous wave laser to the surface of the silicon-rich silica film through the quartz window, and an air passage for introducing nitrogen gas flow into the metal cavity.
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