CN1436878A - Prepn of porous luminescent material - Google Patents
Prepn of porous luminescent material Download PDFInfo
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- CN1436878A CN1436878A CN 03115546 CN03115546A CN1436878A CN 1436878 A CN1436878 A CN 1436878A CN 03115546 CN03115546 CN 03115546 CN 03115546 A CN03115546 A CN 03115546A CN 1436878 A CN1436878 A CN 1436878A
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- porous silicon
- silicon
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- porous
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Abstract
The present invention is supersonic electrochemical etching process of preparing porous luminescent silicon material. The traditional porous silicon material preparing electrochemical processes, including DC current process and pulse current process, has some demerits resulting in porous silicon material with imperfect optical characteristics. The supersonic electrochemical etching process of the present invention has optimized etching condition, and can obtain porous silicon material with improved surface interface structure and optical characteristics.
Description
Technical field
The present invention is a kind of novel method that electrochemistry anodic corrosion legal system is equipped with porous silica material.
Background technology
Porous silicon, promptly the porous silicon materials are used as the structure sealing coat in the unicircuit at first, and this is owing to hole in the silicon post in the porous silicon layer exhausts, and the cause of very big resistance is arranged.Porous silicon did not cause people's too many concern at that time.Report for the first time the fifties from twentieth century and to find porous silicon and subsequent nearly 40 years, relevant article only has less than 200 pieces.Nineteen ninety Britain scientist L. T.Canham has found the characteristic of high-level efficiency visible emitting under the porous silicon room temperature, has opened up a new field for total silicon base photoelectricity is integrated, has caused a research boom in scientific circles very soon.People have not only carried out theory and experimental study to the fundamental characteristics of porous silicon, microstructure, formation mechanism, luminous mechanism and carrier transport mechanism etc. as the quantum sponge, and practical devices used carried out attempting widely and exploring, and obtained certain result, as photodiode (LED), silicon based opto-electronics subclass one-tenth, photo-detector, optical waveguides and transmitter etc.
It is galvanic corrosion that the preparation method of porous silicon has a variety of, the most frequently used methods, promptly silicon chip is passed to electric current as anode in the HF acid solution and carries out anodic oxidation.There will be two kinds of situations owing to the alive difference of institute in the HF acid solution for silicon, in current density greater than certain threshold value (with the type of silicon chip, resistivity and corrosive fluid concentration are relevant with factors such as compositions) time, silicon chip will be peeled off by electricity, and when being lower than this threshold value, silicon face will be made of the erratic composition that the silicon post (silicon grain) of countless nanometer scale is formed, and just said " quantum sponge " structure is referred to as porous silicon layer.
The fundamental method of preparation porous silicon is to adopt anode the anodic etching method method.A kind of self-regulating mechanism makes that in the porous silicon forming process, the reaction of corrosive fluid and silicon substrate mainly concentrates on the root in the hole of formation.Though the product that silicon substrate and HF reaction form still has arguement now, produces H in the reaction process
2SiF
6Or the compound of other ionic speciess of some fluosilicics and H
2Obtained certainly.When adopting traditional dc corrosion method corrosion of porous silicon, the fluosilicic compound of generation is deposited on the bottom in hole easily, and H
2Bubble is because surface tension is adsorbed on silicon post surface, and these have all hindered corrosive fluid and have infiltrated through bottom, silicon hole, make chemical reaction become slow and difficult.On the other hand, the reactive deposition thing causes silicon chip resistance to increase, and reaction current density diminishes, and this also is unfavorable for keeping certain reaction speed.The method of another preparation method---pulse corrosion prepares porous silicon, i.e. anodic corrosion process is not continuous but carry out the compartment of terrain.Do making reaction product in the intersegmental time of having a rest that does not add corrosion current, can from the silicon hole, diffuse out rice like this, keep the concentration of corrosive fluid in the hole.Though comparing dc corrosion, pulsed electrochemical etching has superiority, fluosilicic compound and H
2Bubble is to make corrosive fluid reach new balance in the bottom, hole by the mode that spreads naturally, if thereby can adopt mode initiatively to make reactant and H
2Bubble hightails the bottom in hole, will further improve and optimize the galvanic corrosion condition.
Summary of the invention
The objective of the invention is to develop a kind of simple and practical, respond well light-emitting porous silicon preparation methods.
Ultrasonic electrochemical anode preparation porous silica material method of the present invention is extremely simple.The cleaning of a slice single-sided polishing is treated that the corrosive silicon chip puts into the etching tank of a tetrafluoroethylene.Then etching tank is put into a ultrasonic generator.In etching tank, add the corrosive fluid that contains HF, in ultrasonic generator, add less water, for etching tank connects electrode.Signal generator with a cover computer control provides electric current for reaction process.Change corrosion electric current density and time.Carry out galvanic corrosion simultaneously, open the power supply of ultra-sonic generator, carry out ultrasonic erosion in the lump.
Ultrasonic frequency of the present invention with 20-200KHZ for well.
The ultrasonic erosion time can finish simultaneously with the galvanic corrosion time, as the case may be, decided on the corrosion sample thickness, generally 5 seconds-5 hours scopes.
Because modern silicon technology all concentrates on the little silicon chip and carries out, etching tank can be put into ultra-sonic generator and carry out ultrasonic erosion, just can obtain good porous silica material simultaneously in galvanic corrosion, technology is simple and convenient.The present invention can directly insert galvanic corrosion grooves such as dc corrosion groove or pulse corrosion groove in the ultra-sonic generator.
Adopt the porous silica material of ultrasonic electrochemical anodic corrosion method preparation to have equally distributed surface arrangement, smooth silicon layer interface the more important thing is that the porous silicon of this method preparation has good optical characteristics.Through a large amount of experiments, the result proves that ultrasonic anodic corrosion method is a kind of novel method of effective preparation light-emitting porous silicon material.The inventive method is simple and easy to realize that cost is not high that product performance are better.
Description of drawings
Fig. 1 is the sample surfaces SEM figure that adopts the dc corrosion method to obtain.
Fig. 2 is the sample surfaces SEM figure that adopts the ultrasonic erosion method to obtain.
Fig. 3 is a ultrasonic erosion method processing unit synoptic diagram.
Among the above-mentioned figure, the 1st, ultra-sonic generator, the 2nd, etching tank, the 3rd, sample, the 4th, HF electrolytic solution, the 5th, bolt.
Embodiment
To have the pulsed current etching tank now and put into ultrasonic generator, put certain water gaging in the ultrasonic generator, carry out the pulsed current corrosive and open ultrasonic generator simultaneously and carry out simultaneously, select the ultrasonic 33KHZ that is for use, because silicon chip is thinner, selecting the ultrasonic erosion time is 5 minutes.Its result such as Fig. 2.
Selecting frequency respectively according to different silicon wafer thicknesses is 25KHZ, 30KHZ, 180KHZ, and the time is to carry out ultrasonic erosion in 5 seconds, 1 hour, 5 hours, prepares the sample that surface interface structure and optical characteristics all are significantly increased.
Claims (4)
1, a kind of light-emitting porous silicon preparation methods is characterized in that placing etching tank ultrasound environments to prepare porous silicon, adds in the galvanic corrosion porous silicon that promptly ultrasound condition prepares the light-emitting porous silicon material.
2, light-emitting porous silicon preparation methods according to claim 1 is characterized in that frequency of ultrasonic is 20-200KHZ.
3, light-emitting porous silicon preparation methods according to claim 1 is characterized in that the ultrasonic erosion time is 5 seconds-5 hours.
4, light-emitting porous silicon preparation methods according to claim 1 is characterized in that the galvanic corrosion groove inserted and carries out ultrasonic erosion in the ultra-sonic generator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03115546 CN1436878A (en) | 2003-02-27 | 2003-02-27 | Prepn of porous luminescent material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03115546 CN1436878A (en) | 2003-02-27 | 2003-02-27 | Prepn of porous luminescent material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1436878A true CN1436878A (en) | 2003-08-20 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03115546 Pending CN1436878A (en) | 2003-02-27 | 2003-02-27 | Prepn of porous luminescent material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1436878A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974880B (en) * | 2006-11-16 | 2010-05-12 | 天津大学 | Dual bath apparatus for porous silicon preparing electrochemical process |
| CN102134737A (en) * | 2011-04-28 | 2011-07-27 | 上海理工大学 | Method for preparing porous silicon |
| TWI470822B (en) * | 2005-01-11 | 2015-01-21 | Semileds Corp | Light emitting diodes (leds) with improved light extraction by roughening |
-
2003
- 2003-02-27 CN CN 03115546 patent/CN1436878A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI470822B (en) * | 2005-01-11 | 2015-01-21 | Semileds Corp | Light emitting diodes (leds) with improved light extraction by roughening |
| CN1974880B (en) * | 2006-11-16 | 2010-05-12 | 天津大学 | Dual bath apparatus for porous silicon preparing electrochemical process |
| CN102134737A (en) * | 2011-04-28 | 2011-07-27 | 上海理工大学 | Method for preparing porous silicon |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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