CN103474526B - Infrared LED preparation method based on black silicon material - Google Patents
Infrared LED preparation method based on black silicon material Download PDFInfo
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- CN103474526B CN103474526B CN201310313985.9A CN201310313985A CN103474526B CN 103474526 B CN103474526 B CN 103474526B CN 201310313985 A CN201310313985 A CN 201310313985A CN 103474526 B CN103474526 B CN 103474526B
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Abstract
The invention belongs to Si-based optoelectronics field, the preparation method of specially a kind of infrared LED based on silicon materials.The present invention etches p-type silicon substrate surface using femtosecond pulse in sulfur hexafluoride atmosphere, and infraluminescence energy level is both introduced in silicon crystal band gap, and and can enough forms the heavily doped n in surface+P is tied.By the way that luminous energy level is controlled sample quick thermal annealing process, and improve luminous intensity.One layer of indium tin oxide films for not only improving the enough transmitted infrared lights of conductive and can, surface indium extraction electrode are deposited on n-type area surface by the method for magnetron sputtering again.It is corresponding with front electrode, aluminium electrode is formed in silicon substrate back side p areas by evaporation coating, and then the efficient infrared LED of stable luminescence is made.The method that the present invention uses is simple, and the cost of material is low, and preparation technology is compatible with existing photoelectronic industry.Under forward bias, stronger and stable infraluminescence can be produced in 1.4 1.65 mu m wavebands.
Description
Technical field
The invention belongs to Si-based optoelectronics field, and in particular to a kind of making of the infrared LED based on black silicon material
Method.
Background technology
Silicon materials are had broad application prospects for semiconductor industry and market value.But due to silicon conduct in itself
Indirect bandgap material, its band band transition luminescence efficiency are very low.If the luminous efficiency of silica-base material can be improved ---
The luminous efficiency of optical communicating waveband near especially 1.5 μm, then play a positive role for light network and Guang Ji Chengdu.
In order to improve the luminous efficiency of silicon materials, scientific research personnel has had taken up various means.In the last few years, by black silicon material is had
Some physical properties and potential application value cause the extensive attention of people.
In existing document, black silicon is concentrated mainly on visible waveband as luminescent material, and rarely has the report of infrared band
Road.For the infrared LED of black silicon, the report of this respect is less.The reason for causing this respect mainly has at 2 points：It is firstly, since black
Silicon materials are started late as the research of luminescent material；Secondly as the irregularities of black silicon face, surface electrode are more difficult
Do, electronics is difficult to inject.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of efficient infrared based on black silicon material
LED preparation method.
The method that the present invention etches p-type silicon substrate surface using femtosecond pulse in sulfur hexafluoride atmosphere, both in silicon
Infraluminescence energy level is introduced in crystal bandgap, and can enough forms the heavily doped n in surface+- p is tied.At to sample rapid thermal annealing
Manage to control luminous energy level, and improve luminous intensity.It is existing in one layer of n-type area surface deposition by the method for magnetron sputtering again
Beneficial to the indium tin oxide films of the enough transmitted infrared lights of conductive and can, surface indium extraction electrode.It is corresponding with front electrode, pass through
Evaporation coating forms aluminium electrode in silicon substrate back side p areas, and then forms the efficient infrared LED of stable luminescence.
The specific make step of the present invention is as follows：
（1）Clean substrate：
It is substrate from p-type Si (100) single-chip that resistivity is 1~3 Ω cm.Substrate needs before femtosecond laser etching
Make cleaning treatment.
（2）The preparation and its annealing activation of black silicon：
P-type silicon substrate surface is performed etching in sulfur hexafluoride atmosphere using femtosecond pulse, in silicon crystal band gap
Middle introducing infraluminescence energy level, and form the heavily doped n in surface+- p is tied；Pass through 500-1100 DEG C again（It is preferred that 500-800 DEG C）
Quick thermal annealing process 2-5 minutes eliminate some non-radiative recombination centers, while activate and control luminous energy level, to improve hair
Luminous intensity and control luminous peak position；Luminescence band is 1.4-1.65 μm.
（3）LED makes：
In order to overcome the electrode fabrication problem that black silicon face irregularities are brought, first with magnetically controlled DC sputtering in black silicon table
The relatively low indium tin oxide films of one layer resistivity of length of looking unfamiliar, it not only improves the enough transmitted infrared lights of conductive and can.Again in indium oxide
Indium is pressed as positive electrode in tin thin film surface.One layer of aluminium is deposited in substrate back with evaporation coating machine, as back electrode.In order to ensure
The Ohmic contact of electrode, whole sample is in 300-350 DEG C of quick thermal annealing process 2-5 minute.So just form n+- p ties LED
Device.
Shown by SEM shape appearance figure, black silicon face pattern is needle-like, and its height is 4-6 μm, transmission
Electron microscope shape appearance figure shows that femtosecond pulse, which is processed inside the spicule to be formed, generates amorphous and crystalline state interface.
By quick thermal annealing process, the amorphous inside spicule and crystalline state interface can control.
The inventive method cost is low, and preparation technology is compatible with existing photoelectronic industry.Under forward bias, Neng Gou
1.4-1.65 mu m wavebands produce stronger and stable infraluminescence.
Brief description of the drawings
Fig. 1 is black silicon preparation system schematic diagram.
Fig. 2 is the electron scanning micrograph of black silicon face.
Fig. 3 is the transmission electron microscope photo of black silicon cross section.Wherein, before (a) annealing；(b) anneal 2 points for 500 DEG C
Clock.
Fig. 4 is black silicon LED structure schematic diagram.
Embodiment
It is further detailed to the manufacturing process of the efficient infrared LED of the present invention based on black silicon material below in conjunction with the accompanying drawings
Explanation.
（1）Clean substrate：
It is substrate from p-type Si (100) single-chip that resistivity is 1~3 Ω cm.Substrate needs before femtosecond laser etching
Make cleaning treatment.Cleaning procedure is as follows：
i）By silicon substrate film in acetone and a methanol successively each ultrasonic 5~6 minutes, to remove the organic of substrate surface
Thing.It is ultrasonic 5~6 minutes in deionized water again；
Ii after) being soaked 10 minutes in sulfuric acid and hydrogen peroxide mixed solution, with deionized water rinsing 5~6 minutes.Sulfuric acid and
The volume ratio of hydrogen peroxide is 1: 4；
Iii) in ammoniacal liquor, hydrogen peroxide, water mixed solution after 80 DEG C of water-baths 10 minutes, with 5~6 points of deionized water rinsing
Clock.Ammoniacal liquor, hydrogen peroxide, the volume ratio of water three are 1: 1: 4；
Iv) the immersion 60-80 seconds remove the oxide layer on surface in 5% hydrofluoric acid.Then rinsed well with deionized water
It is standby afterwards.
（2）The preparation and its annealing activation of black silicon：
As shown in figure 1, the silicon substrate after cleaning is quickly transferred on the sample stage of femtosecond laser system of processing intracavitary, first
Vacuumize process is carried out to intracavitary with mechanical pump molecular pump afterwards, vacuum is reached 10-4Pa magnitude.Again six are passed through toward intracavitary
Sulfur fluoride gas, control pressure is in 70 kPa or so femtosecond pulses（Ti sapphire laser, the nm of wavelength 800, repeat
The kHz of rate 1）Act on surface of silicon.Because sample stage drives sample to do the motion oriented under the drive of stepper motor, because
The etching of cycle light pulse is received on this silicon substrate, forms acicular texture as shown in Figure 2, its height is that 4-6 μm of passes through this
The simple step processing method of kind, both introduces infraluminescence energy level in silicon crystal band gap, and and can enough formed surface sulphur atom weight
The n mixed+- p is tied.Finally by sample in nitrogen and hydrogen mixture (H2: N2=5%:95%) more than 500 DEG C rapid thermal annealing 2- are kept in
5 minutes, it is therefore an objective to eliminate non-radiative recombination defect and activating radiation recombination luminescence centre, formed stable and efficient infrared
It is luminous.Fig. 3 is the transmission electron microscope photo of black silicon cross section.It can be seen that pass through quick thermal annealing process, needle-like
There occurs movement for amorphous and crystalline state interface inside thing.This is the committed step that can improve luminous intensity.
（3）LED makes：
First the relatively low indium tin oxide films of a layer resistivity are grown with magnetically controlled DC sputtering in black silicon face.Tin indium oxide
Film thickness is 700-800 nm, and sputter temperature is that 200 DEG C of not only improve conduction in the indium tin oxide films of black silicon face
The enough transmitted infrared lights of and can.Indium is pressed on indium tin oxide films surface again as positive electrode.One layer of aluminium is deposited with evaporation coating machine to exist
Substrate back, as back electrode.Thickness of electrode be 150 nm. in order to ensure the Ohmic contact of electrode, whole sample mixes in nitrogen hydrogen
Close 300-350 DEG C of quick thermal annealing process 2-5 minute in gas.So just form n+- p ties LED component, device architecture such as Fig. 4
It is shown.Whole device works under forward bias, can send the infrared waves band of stability and high efficiency, peak value is near 1.6 μm.
Claims (1)
1. a kind of preparation method of the infrared LED based on black silicon material, it is characterised in that concretely comprise the following steps：
（1）Clean substrate：
It is substrate from p-type Si (100) single-chip that resistivity is 1~3 Ω cm, cleaning treatment is carried out to it；
（2）The preparation and its annealing activation of black silicon：
P-type silicon substrate surface is performed etching in sulfur hexafluoride atmosphere using femtosecond pulse, drawn in silicon crystal band gap
Enter infraluminescence energy level, and form the heavily doped n in surface+- p is tied；Pass through 500-1100 DEG C of quick thermal annealing process 2-5 minutes again
To eliminate non-radiative recombination center, while activate and control luminous energy level, to improve luminous intensity and control luminous peak position；It is luminous
Wave band is 1.4-1.65 μm；
（3）LED makes：
Indium oxide layer tin thin film is grown in black silicon face with magnetically controlled DC sputtering first, to be advantageous to conductive and transmit infrared
Light；Indium is pressed on indium tin oxide films surface again as positive electrode；One layer of aluminium is deposited in substrate back with evaporation coating machine, as the back of the body
Electrode；, then will be integrally in 300-350 DEG C of quick thermal annealing process 2-5 minute, to ensure in order to ensure the Ohmic contact of electrode
The Ohmic contact of electrode, so as to form n+- p ties LED component.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104900752A (en) * | 2015-04-14 | 2015-09-09 | 中国电子科技集团公司第四十四研究所 | Black silicon layer preparation method and black silicon PIN photoelectric detector preparation method |
| CN105609412A (en) * | 2016-03-23 | 2016-05-25 | 云南大学 | Rapid annealing preparation method of Al-Si<+> ohmic contact electrode |
| CN117525233B (en) * | 2024-01-05 | 2024-04-12 | 南昌凯迅光电股份有限公司 | Small-size red light LED chip and manufacturing method thereof |
Citations (4)
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|---|---|---|---|---|
| CN101824653A (en) * | 2009-03-04 | 2010-09-08 | 中国科学院半导体研究所 | Method for manufacturing black silicon material by scanning and irradiation of light source of broad-pulse laser |
| CN102735939A (en) * | 2012-07-11 | 2012-10-17 | 电子科技大学 | Method for measuring ohmic contact resistivity between black silicon material and metal electrodes |
| CN102842651A (en) * | 2012-09-18 | 2012-12-26 | 电子科技大学 | Black silicon structure and manufacturing method thereof |
| CN102976326A (en) * | 2012-12-17 | 2013-03-20 | 南开大学 | Method for preparing sulfur-doped silicon nano-particles |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102017088B (en) * | 2008-01-31 | 2013-08-07 | 哈佛大学校长及研究员协会 | Engineering flat surfaces on materials doped via pulsed laser irradiation |
| JP2013102058A (en) * | 2011-11-08 | 2013-05-23 | Toshiba Corp | Led light source |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101824653A (en) * | 2009-03-04 | 2010-09-08 | 中国科学院半导体研究所 | Method for manufacturing black silicon material by scanning and irradiation of light source of broad-pulse laser |
| CN102735939A (en) * | 2012-07-11 | 2012-10-17 | 电子科技大学 | Method for measuring ohmic contact resistivity between black silicon material and metal electrodes |
| CN102842651A (en) * | 2012-09-18 | 2012-12-26 | 电子科技大学 | Black silicon structure and manufacturing method thereof |
| CN102976326A (en) * | 2012-12-17 | 2013-03-20 | 南开大学 | Method for preparing sulfur-doped silicon nano-particles |
Non-Patent Citations (2)
| Title |
|---|
| Infrared absorption by sulfur-doped silicon formed by femtosecond laser irradiation;C.H. CROUCH,et al;《Appl. Phys. A》;20040623;第79卷;第1635-1641页 * |
| Sulfur-doped black silicon formed by metal-assist chemical etching and ion implanting;Kong Liu，et al;《Appl Phys A》;20130406;第114卷;第765-768页 * |
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