CN106544720A - A kind of new method for improving porous silicon longitudinal direction physical arrangement uniformity - Google Patents
A kind of new method for improving porous silicon longitudinal direction physical arrangement uniformity Download PDFInfo
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- CN106544720A CN106544720A CN201610946638.3A CN201610946638A CN106544720A CN 106544720 A CN106544720 A CN 106544720A CN 201610946638 A CN201610946638 A CN 201610946638A CN 106544720 A CN106544720 A CN 106544720A
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- porous silicon
- longitudinal direction
- hydrofluoric acid
- concentration
- physical arrangement
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
- C25F3/12—Etching of semiconducting materials
Abstract
The invention discloses a kind of new method that can improve porous silicon longitudinal direction physical arrangement uniformity.The method is, during porous silicon is prepared, a small amount of hydrofluoric acid to be gradually added in corrosive liquid, to increase concentration of the hydrofluoric acid in corrosive liquid.On the one hand, being caused by gradually increasing concentration of the hydrofluoric acid in corrosive liquid increases with corrosion depth in the vesicularity for going up porous silicon along the longitudinal direction and reduces；On the other hand, under the etching condition of normal constant current density, with the increase of corrosion depth, vesicularity becomes greatly or refractive index diminishes, two kinds of trend reach dynamic equilibrium, so that porous silicon film its being consistent property of vesicularity along the longitudinal direction, enhances the uniformity of longitudinal physical arrangement of porous silicon film inner surface.
Description
Technical field
The present invention relates to technical field of semiconductors, and in particular to a kind of raising porous silicon longitudinal direction physical arrangement uniformity it is new
Method.
Background technology
1956, Uhlir found that the presence of porous silicon when electrochemical polishing treatment is carried out in HF solution to Si pieces,
The various performances of porous silicon and its micropore number, size and be distributed closely related.Due to the special physical characteristic of porous silicon, light
Characteristic and electrology characteristic etc. are learned, such as there is very high resistivity 106Ω .cm, relatively low refractive index (1.1-3.1) and its luminous spy
Property.So far, porous silicon is mainly used in electroluminescence device, sensor, deielectric-coating and application biologically etc..1990
Year, Canham has found that porous silicon sends visible ray at room temperature, is that porous silicon research opens new epoch.Porous silica material will
Into the practical stage, prepare the porous silica material that micropore is evenly distributed, aperture and hole depth are controllable be future studies problem it
One.
According to relevant document report, the characteristic of porous silica material for example vesicularity, refractive index, physical thickness, uniformity, surface and
Interface flatness, aperture and micro-structural etc. are strongly depend on anodic attack parameter, and these corrosion parameters include the composition of corrosive liquid
Composition, the density of corrosion current, etching time, the type of silicon chip and resistivity etc..Draw the following conclusions from existing document：
Under the etching condition of constant current density, with the increase of corrosion depth, vesicularity becomes greatly or refractive index diminishes, so cause porous silicon
The inhomogeneities of physical arrangement along the longitudinal direction.
At this stage, it is in order to prepare the porous silicon film of porous silicon physical arrangement uniformity, general using the corrosion electricity that successively decreases
Improving porous silicon longitudinal direction physical arrangement uniformity, although these methods improve porous silicon longitudinal direction physics to method of current density etc.
Structural homogeneity, but the complexity of experimental facilities is increased, remain to be further improved.
The content of the invention
It is multiple using corrosion electric current density method etc. of successively decreasing equipment brought to the process of porous silicon uniformity at present in order to overcome
The defect that polygamy, longitudinal physical arrangement uniformity are remained to be further improved, it is an object of the invention to provide a kind of improve porous silicon
The new method of longitudinal physical arrangement uniformity.
For achieving the above object, the technical solution used in the present invention：It is a kind of to improve porous silicon longitudinal direction physical arrangement uniformity
Method, it is characterised in that during porous silicon is prepared, by gradually increase concentration of the hydrofluoric acid in corrosive liquid, realize
Following purpose：On the one hand, under the etching condition of normal constant current density, with the increase of corrosion depth, in porous silicon pores
Product is slack-off to hole external diffusion, while HF dies down to pore diffusion ability, so that bottom hole is particularly in porous silicon pores
HF concentration is not easy to return to initial concentration state, causes downward corrosive power to die down, and causes vesicularity to become big or refractive index change
It is little；On the other hand, with the gradually increase of hydrofluoric acid concentration in corrosive liquid, make in porous silicon pores, to be particularly the HF concentration of bottom hole
Initial concentration state is returned to easily, so as to cause porous silicon vesicularity to be consistent in a longitudinal direction.
Preferably, in etching time, the incrementss of above-mentioned hydrofluoric acid solution are dense for hydrofluoric acid in corrosion Initial Corrosion liquid
The 2%-20% of degree, and at the uniform velocity hydrofluoric acid is added in corrosive liquid.
Compared with prior art, the beneficial effect that the present invention possesses：By at the uniform velocity adding a small amount of hydrogen fluorine in corrosive liquid
Acid, causes concentration of the hydrofluoric acid in corrosive liquid gradually to increase so as to during porous silicon is prepared, on the one hand, due to system
Hydrofluoric acid is gradually added in corrosive liquid during standby, hydrofluoric acid concentration is increasing in causing corrosion liquid, and contains in corrosive liquid
Hydrofluoric acid concentration is higher, and the vesicularity of porous silicon is less, and porous silicon vesicularity has the trend for diminishing in a longitudinal direction；The opposing party
Face, under the etching condition of constant current density, with the increase of corrosion depth, vesicularity becomes greatly or refractive index diminishes, in certain bar
Under part, the two reaches dynamic equilibrium, so as to cause porous silicon vesicularity to be consistent in a longitudinal direction.
Specific embodiment
With reference to specific embodiment, the present invention is further illustrated.Described below, is only the preferable reality of the present invention
Example is applied, the restriction of other forms is not done to the present invention, any those skilled in the art are possibly also with the present invention
Disclosed technology contents are changed to the Equivalent embodiments of equal change.Therefore every content without departing from the present invention program, according to
Following examples are made with simple modification or equivalent variations according to the technical spirit of the present invention, all should be fallen in protection scope of the present invention
It is interior.
Embodiment one
The method of this raising porous silicon longitudinal direction physical arrangement uniformity of the present invention, specifically includes following steps：
1st, connect circuit：Corrosive liquid is placed with etching tank, the one end in etching tank is provided with silicon chip, in etching tank
The other end is provided with platinized platinum, and silicon chip and platinized platinum are immersed in corrosive liquid, are externally provided with constant-current source in etching tank；Constant-current source is to pass through
What TekVisa AFG3101 AWGs were produced, the positive pole of the constant-current source is connected with silicon chip by wire, constant-current source
Negative pole is connected with platinized platinum by wire, and during work, the both positive and negative polarity of current source forms current loop by corrosive liquid.
2nd, from type be P100, silicon chip that resistivity is 0.01 Ω .cm as electrochemical corrosion anode, thin platinized platinum
As the negative electrode of electrochemical corrosion；Silicon chip and thin platinized platinum carry out galvano-cautery in being fully immersed in electrolytic etching liquid, and etching time is
4min.Electrolytic etching liquid is by hydrofluoric acid：Absolute ethyl alcohol and deionized water are with volume ratio as 1:1:2 preparations.It is many at 4 minutes
In the silicon preparation process of hole, hydrofluoric acid is uniformly added in electrolytic etching liquid, the hydrofluoric acid in corrosive liquid：Absolute ethyl alcohol and deionization
Water volume ratio is from 1:1:2 reach 1.08:1:2.
3rd, for the convenience for studying a question, we have selected two groups of experiments, and its experiment parameter and corresponding data are as follows：
| Numbering | Corrosion current（mA/cm2） | Etching time (Min) | Vesicularity | Porous silicon thickness (μm) |
| ⑴ | 5 | 4 | 54% | ~1.30 |
| ⑵ | 10 | 4 | 56% | ~2.50 |
4th, according to pertinent literature and with reference to above-mentioned experiment condition, obtain the vesicularity of formed two panels porous silicon film respectively about
For 54%, 56%, thickness is respectively about 1.30 μm, 2.50 μm；
5th, prepare after finishing, using deionized water rinsing, be finally dried in atmosphere；
6th, porous silicon sample is analyzed research by reflectance spectrum, photoluminescence spectrum and SEM；
7th, finished product is after the assay was approved.
Embodiment two
The method of this raising porous silicon longitudinal direction physical arrangement uniformity of the present embodiment, specifically includes following steps：
1st, connect circuit：Corrosive liquid is placed with etching tank, the one end in etching tank is provided with silicon chip, in etching tank
The other end is provided with platinized platinum, and silicon chip and platinized platinum are immersed in corrosive liquid, are externally provided with constant-current source in etching tank；Constant-current source is to pass through
What TekVisa AFG3101 AWGs were produced, the positive pole of the constant-current source is connected with silicon chip by wire, constant-current source
Negative pole is connected with platinized platinum by wire, and during work, the both positive and negative polarity of current source forms current loop by corrosive liquid.
2nd, from type be P100, silicon chip that resistivity is 0.01 Ω .cm as electrochemical corrosion anode, thin platinized platinum
As the negative electrode of electrochemical corrosion；Silicon chip and thin platinized platinum carry out galvano-cautery in being fully immersed in electrolytic etching liquid, and etching time is
3min, electrolytic etching liquid are by hydrofluoric acid：Absolute ethyl alcohol and deionized water are with volume ratio as 1:1:2 preparations.It is many at 3 minutes
In the silicon preparation process of hole, hydrofluoric acid is uniformly added in electrolytic etching liquid, the hydrofluoric acid in corrosive liquid：Absolute ethyl alcohol and deionization
Water volume ratio is from 1:1:2 reach 1.05:1:2.
3rd, for the convenience for studying a question, we have selected two groups of experiments, and its experiment parameter and corresponding data are as follows：
| Numbering | Corrosion current（mA/cm2） | Etching time (Min) | Vesicularity | Porous silicon thickness (μm) |
| ⑴ | 10 | 3 | 55% | ~1.7 |
| ⑵ | 15 | 3 | 57% | ~2.5 |
4th, according to pertinent literature and with reference to above-mentioned experiment condition, obtain the vesicularity of formed two panels porous silicon film respectively about
For 55%, 57%, thickness is respectively about 1.7 μm, 2.5 μm；
5th, prepare after finishing, using deionized water rinsing, be finally dried in atmosphere；
6th, porous silicon sample is analyzed research by reflectance spectrum, photoluminescence spectrum and SEM；
7th, finished product is after the assay was approved.
Claims (2)
1. a kind of new method for improving porous silicon longitudinal direction physical arrangement uniformity, it is characterised in that during porous silicon is prepared,
By gradually increasing concentration of the hydrofluoric acid in corrosive liquid, following purpose is realized：On the one hand, in the corruption of normal constant current density
Under the conditions of erosion, with the increase of corrosion depth, the product in porous silicon pores is slack-off to hole external diffusion, while HF is to pore diffusion
Ability dies down, so that the HF concentration of particularly bottom hole is not easy to return to initial concentration state in porous silicon pores, causes downwards
Corrosive power dies down, and causes vesicularity change greatly or refractive index diminishes；On the other hand, with hydrofluoric acid in corrosive liquid concentration by
It is cumulative to add, make the HF concentration of particularly bottom hole in porous silicon pores easily return to initial concentration state, so as to cause porous silicon many
Cell size is consistent in a longitudinal direction.
2. the method for improving porous silicon longitudinal direction physical arrangement uniformity according to claim 1, it is characterised in that in corrosion
In time, the incrementss of hydrofluoric acid solution are the 2%-20% for corroding hydrofluoric acid concentration in Initial Corrosion liquid, and are at the uniform velocity increased.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112142054A (en) * | 2020-10-23 | 2020-12-29 | 浙江大学 | Biodegradable porous silicon particles and application thereof in aspect of promoting vascularization |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN105264654A (en) * | 2013-01-07 | 2016-01-20 | 威廉马歇莱思大学 | Combined electrochemical and chemical etching processes for generation of porous silicon particulates |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105264654A (en) * | 2013-01-07 | 2016-01-20 | 威廉马歇莱思大学 | Combined electrochemical and chemical etching processes for generation of porous silicon particulates |
Non-Patent Citations (2)
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| 田云龙: "阳极氧化多孔结构的研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112142054A (en) * | 2020-10-23 | 2020-12-29 | 浙江大学 | Biodegradable porous silicon particles and application thereof in aspect of promoting vascularization |
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Application publication date: 20170329 |