CN106517080B - Improve the new method of nano-structure porous silicon physics micro-structure and optical characteristics stability - Google Patents
Improve the new method of nano-structure porous silicon physics micro-structure and optical characteristics stability Download PDFInfo
- Publication number
- CN106517080B CN106517080B CN201610889553.6A CN201610889553A CN106517080B CN 106517080 B CN106517080 B CN 106517080B CN 201610889553 A CN201610889553 A CN 201610889553A CN 106517080 B CN106517080 B CN 106517080B
- Authority
- CN
- China
- Prior art keywords
- porous silicon
- optical characteristics
- porous
- silicon
- stability
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00523—Etching material
- B81C1/00539—Wet etching
Abstract
The invention discloses a kind of new methods for improving porous silicon physics micro-structure and optical characteristics stability, it is after the completion of porous silicon film preparation, just using Peracetic acid and square-wave signal source is added to carry out oxidation processes the inner surface of porous silica material immediately, the silicon dangling bonds of porous silicon inner surface and si-h bond is made to be combined or replaced with the oxygen atom in Peracetic acid and form stable silicon oxygen bond film.The present invention can improve the stability of the physical strength of porous silicon film, physics micro-structure and optical characteristics；Be conducive to prepare the porous silicon thick film that physics micro-structure and optical characteristics are stablized；Be conducive to explore using porous silicon multilayer film in photonic device, it is possible to prepare the relatively strong and higher uniformity porous silicon multilayer device Porous Silicon Microcavity of stability.
Description
Technical field
The present invention relates to technical field of semiconductor, specifically a kind of stable nanoporous silicon microstructure and optics are special
The new method of property.
Background technology
Porous silicon material is found when electrochemical polishing treatment is carried out in hydrofluoric acid (HF) solution to silicon chip from Uhlir in 1956
Since material；Porous silica material in photoelectron material, optical device, solar cell and sensor technology etc. widely
It studies and applies, but it is porous silicon film to be badly in need of one of bottleneck problem solved（Especially thick film microporous silicon）Physics micro-structure and light
It is unstable to learn characteristic.Since its physics microstructural stability, uniformity and luminescent properties are effectively improved, make it
It is restricted in the application of industry.Porous silica material unstability is easily cracked or is collapsed, especially thick film microporous silicon materials
It is extremely unstable, limit its use scope.
According to related document report, porous silicon film cracking, collapse with physical arrangement it is unstable the reason of one of be surface tension
Carried out by.Porous silica material is a kind of spongiform hollow structure material, and surface area/volume ratio is flat up to per cubic centimeter 600
Square rice.In general, porous silica material inner surface is made of the dangling bonds or silicon-hydrogen bond of silicon, these are strong in air
Extremely unstable, the hydrogen atom easily caused in the dangling bonds or silicon-hydrogen bond of its inner surface silicon is combined with the atom in external environment
Or displacement, so as to cause porous silicon film cracking, collapse it is unstable with physical arrangement.Eliminate porous silicon inner surface silicon dangling bonds or
Silicon-hydrogen bond promotes porous silica material inner surface to form stable silicon-oxygen key structure, avoids the dangling bonds of porous silicon inner surface silicon
Or the ionic structure in the hydrogen atom and ambient enviroment in si-h bond recombinates or displacement generates intermolecular uneven internal stress, from
And obtain stable physical property, the reliable, characteristics of luminescence is stablized, in air can kept dry for a long time porous silicon film.
At this stage, the porous silicon film that physics micro-structure is stablized in order to obtain, the general method using post processing porous silicon film.
Had document report using cathode reduction process for treating surface, anode oxidizing process for treating surface, using hydrogen peroxide after
Reason technology, pentane seasoning, supercritical drying, freeze-drying ease up slow seasoning, these methods can make porous silicon film
Stablize, be preferred especially with supercritical drying.But these methods are complicated, fully do not carry out exhaustive oxidation to porous silicon surface, lead
It causes still unstable.
Invention content
In view of the deficiency of the prior art, present invention firstly provides use Peracetic acid（）And
Square-wave signal source post-processes porous silica material, it is therefore an objective to provide a kind of raising porous silica material physics micro-structure and optical characteristics
The new method of stability, to improve the stability of porous silica material physics micro-structure and optical characteristics.
The purpose of the present invention is achieved through the following technical solutions：Improve porous silica material physics micro-structure and optics
The new method of character constancy, which is characterized in that after porous silicon film is formed, immediately by corrosive liquid change into Peracetic acid and go from
The mixed liquor that sub- water is formed, wherein Peracetic acid are with deionized water volume ratio（1~5）：（49~99）, while by corrosion current
It changes square-wave signal source into, oxidation processes is carried out to porous silica material, oxidation treatment time is 5~30min；Then, by porous silicon
Film is put into the deionized water of isothermal and cleans, and is finally drying to obtain in air.
Preferably, the amplitude size of the square-wave signal source is -0.5~2V.
Compared with prior art, the invention has the following features and advances：The present invention is to form porous silicon film in anodic attack
Afterwards, by using Peracetic acid（）With deionized water mixed liquor and square-wave signal source method, on the one hand,
During additional square wave positive voltage, make hydrogen atom and mistake in the dangling bonds or silicon-hydrogen bond of the silicon atom of porous silica material inner surface
Oxygen atom in fluoroacetic acid molecule combines or displacement；On the other hand, outside plus during square wave negative voltage, porous silicon inner surface lacks portion
Unstable atom is divided to be ionized to form dangling bonds, in cycles, so as to form stable silicon-oxygen key film, improves porous silicon film
Physics micro-structure and optical characteristics stability, be conducive to prepare the porous silicon thick film that physics micro-structure and optical characteristics are stablized；
Be conducive to explore the porous silicon multilayer film after stability in use, uniformity and interface flatness improve for realizing in photonic device
Scheme, it is possible to prepare and realize the relatively strong or higher uniformity porous silicon multilayer device of stability or Porous Silicon Microcavity.
Specific embodiment
In conjunction with specific embodiment, next the present invention is further elaborated.The present invention is only preferred embodiment, and simultaneously
Not all embodiment, therefore any technical solution without departing from present inventive concept should all be within the scope of the present invention.
Embodiment one
One of method for improving nano-structure porous silicon physics micro-structure and optical characteristics stability, this method include following step
Suddenly：
1st, after the completion of prepared by porous silica material, corrosive liquid is changed into Peracetic acid immediately（）It is mixed with deionized water
Close liquid；Meanwhile change corrosion current source into the square wave of additional 10 hertz（- 0.5~2V）Signal source carries out porous silica material
Oxidative work-up, oxidation treatment time are 10 minutes；
2nd, post processing mixed liquor is by Peracetic acid（）﹕ deionized waters are prepared by 1 ﹕ 49 of volume ratio；
3rd, the temperature of aftertreatment fluid is room temperature；For the convenience to study a question, we have selected two groups of experiments, experiment ginseng
Number and corresponding data are as follows：
4th, according to pertinent literature and with reference to above-mentioned experiment condition, the vesicularity point of formed two panels porous silicon film is obtained
Not Yue Wei 52%, 55%, thickness is respectively about 0.50 μm, 0.80 μm；
5th, after the completion of handling, porous silicon film is immersed in the deionized water solution synthermal with post-processing blended liquid phase,
Then it is rinsed using deionized water, finally dried in air；
6th, porous silicon sample is analyzed and researched by reflectance spectrum, photoluminescence spectrum and SEM；
7th, it is after the assay was approved finished product.
Embodiment two
The two of the method for nano-structure porous silicon physics micro-structure and optical characteristics stability are improved, this method includes following step
Suddenly：
1st, after the completion of prepared by porous silica material, corrosive liquid is changed into Peracetic acid immediately（）It is mixed with deionized water
Close liquid；Meanwhile change corrosion current source into the square wave of additional 20 hertz（- 0.5~2V）Signal source carries out porous silica material
Oxidative work-up, oxidation treatment time are 15 minutes；
2nd, post processing mixed liquor is by Peracetic acid（）﹕ deionized waters are prepared by 1 ﹕ 99 of volume ratio；
3rd, the temperature of aftertreatment fluid is room temperature；For the convenience to study a question, we have selected two groups of experiments, experiment ginseng
Number and corresponding data are as follows：
4th, according to pertinent literature and with reference to above-mentioned experiment condition, the vesicularity point of formed two panels porous silicon film is obtained
Not Yue Wei 56%, 58%, thickness is respectively about 1.2 μm, 1.5 μm；
5th, after the completion of handling, porous silicon film is immersed in the deionized water solution synthermal with post-processing blended liquid phase,
Then it is rinsed using deionized water, finally dried in air；
6th, porous silicon sample is analyzed and researched by reflectance spectrum, photoluminescence spectrum and SEM；
7th, it is after the assay was approved finished product.
Claims (1)
1. improve the new method of porous silicon physics micro-structure and optical characteristics stability, which is characterized in that formed in porous silicon film
Afterwards, corrosive liquid is changed into the mixed liquor that Peracetic acid and deionized water are formed, wherein Peracetic acid and deionized water volume immediately
Than being 1 ~ 5：49 ~ 99, while change corrosion current into square-wave signal source, the amplitude size of the square-wave signal source is -0.5 ~ 2V,
Oxidation processes are carried out to porous silica material, oxidation treatment time is 5 ~ 30min；Then, by porous silicon film be put into isothermal go from
It cleans in sub- water, is finally drying to obtain in air.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610889553.6A CN106517080B (en) | 2016-10-12 | 2016-10-12 | Improve the new method of nano-structure porous silicon physics micro-structure and optical characteristics stability |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610889553.6A CN106517080B (en) | 2016-10-12 | 2016-10-12 | Improve the new method of nano-structure porous silicon physics micro-structure and optical characteristics stability |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106517080A CN106517080A (en) | 2017-03-22 |
| CN106517080B true CN106517080B (en) | 2018-07-10 |
Family
ID=58331529
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610889553.6A Active CN106517080B (en) | 2016-10-12 | 2016-10-12 | Improve the new method of nano-structure porous silicon physics micro-structure and optical characteristics stability |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106517080B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1436879A (en) * | 2003-02-27 | 2003-08-20 | 复旦大学 | Prepn of porous liminescent material |
| CN102874746A (en) * | 2012-10-11 | 2013-01-16 | 湖南文理学院 | Method capable of improving uniformity of porous silicon film physical micro-structure and optical characteristics |
| CN103288087A (en) * | 2013-05-28 | 2013-09-11 | 浙江大学 | Surface modification process for improving luminance and dispersity of porous silicon |
| CN104900488A (en) * | 2015-04-29 | 2015-09-09 | 湖南文理学院 | Novel method for stabilizing physical microstructure of porous silicon film |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6589883B2 (en) * | 2000-03-29 | 2003-07-08 | Georgia Tech Research Corporation | Enhancement, stabilization and metallization of porous silicon |
-
2016
- 2016-10-12 CN CN201610889553.6A patent/CN106517080B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1436879A (en) * | 2003-02-27 | 2003-08-20 | 复旦大学 | Prepn of porous liminescent material |
| CN102874746A (en) * | 2012-10-11 | 2013-01-16 | 湖南文理学院 | Method capable of improving uniformity of porous silicon film physical micro-structure and optical characteristics |
| CN103288087A (en) * | 2013-05-28 | 2013-09-11 | 浙江大学 | Surface modification process for improving luminance and dispersity of porous silicon |
| CN104900488A (en) * | 2015-04-29 | 2015-09-09 | 湖南文理学院 | Novel method for stabilizing physical microstructure of porous silicon film |
Non-Patent Citations (2)
| Title |
|---|
| "A Novel Technology for Post-Treating of Porous Silicon Thick Films in H2O2";Long Yongfu等;《半导体学报》;20030630;第24卷(第6期);第574-578页，正文第2部分 * |
| "NANO SCALE POROUS SILICON MICROCAVITY OPTICAL SENSOR DEVICE FOR THE DETECTION OF METHYL PARATHION";P.N.PATEL，et al.;《Digest Journal of Nanomaterials and Biostructures》;20121231;第7卷(第4期);p1817-1823，正文第3部分 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106517080A (en) | 2017-03-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhang et al. | Bamboo shoot nanotubes with diameters increasing from top to bottom: Evidence against the field-assisted dissolution equilibrium theory | |
| Zhang et al. | Rapid growth of TiO2 nanotubes under the compact oxide layer: Evidence against the digging manner of dissolution reaction | |
| Zhou et al. | Debunking the effect of water content on anodizing current: Evidence against the traditional dissolution theory | |
| CN102874746B (en) | Method capable of improving uniformity of porous silicon film physical micro-structure and optical characteristics | |
| Tsuchiya et al. | Electrochemical formation of porous superlattices on n-type (1 0 0) InP | |
| CN106348616B (en) | A kind of preparation method of SiO2/TiO2 antireflective coating | |
| CN106531626A (en) | Novel method for improving uniformity of porous silicon radial physical microstructure | |
| CN107860760A (en) | Graphene oxide/silver nano-grain/pyramid PMMA three-dimension flexibles Raman enhancing substrate and preparation method and application | |
| CN106517080B (en) | Improve the new method of nano-structure porous silicon physics micro-structure and optical characteristics stability | |
| Kim et al. | Sensing characteristics of the organic vapors according to the reflectance spectrum in the porous silicon multilayer structure | |
| Kizil et al. | Surface plasma characterization of polyimide films for flexible electronics | |
| CN104176944A (en) | Method for modifying OTS self-assembled film on glass substrate | |
| CN104900488B (en) | A kind of method of the stable porous silicon film physics micro-structural of energy | |
| Shi et al. | Fabrication of two-layer nanotubes with the pear-like structure by an in-situ voltage up anodization and the application as a drug delivery platform | |
| CN105908159A (en) | A preparing method of a g-C3N4/FTO composite clear electrically conductive film | |
| CN102732879A (en) | Preparation method of titanium-dioxide-base conducting film | |
| CN107698793A (en) | A kind of method for using fibroin to prepare polystyrene inverse opal photonic crystal for filling liquid | |
| Lai et al. | Fabrication and corrosion behavior of fresh porous silicon in sodium hydroxide solution | |
| CN109264664B (en) | Al (aluminum)2O3Preparation method of hollow spherical shell array | |
| Karbassian et al. | Luminescent porous silicon prepared by reactive ion etching | |
| Wu et al. | Acrylic acid grafted porous polycarbonate membrane with smart hydrostatic pressure response to pH | |
| Anitha et al. | Fabrication of hierarchical porous anodized titania nano-network with enhanced active surface area: Ruthenium-based dye adsorption studies for dye-sensitized solar cell (DSSC) application | |
| CN106206252B (en) | In the method for surface of semiconductor substrates one-step method chemical graft organic film | |
| CN106298496A (en) | A kind of improve porous silicon longitudinal direction physical arrangement and the method for optical characteristics uniformity | |
| CN106409705B (en) | The method for improving porous silicon radial direction physics micro-structure uniformity |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |