CN100353572C - Preparation method of blue light-emitting diode - Google Patents
Preparation method of blue light-emitting diode Download PDFInfo
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- CN100353572C CN100353572C CNB2004100245965A CN200410024596A CN100353572C CN 100353572 C CN100353572 C CN 100353572C CN B2004100245965 A CNB2004100245965 A CN B2004100245965A CN 200410024596 A CN200410024596 A CN 200410024596A CN 100353572 C CN100353572 C CN 100353572C
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000010703 silicon Substances 0.000 claims abstract description 46
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 45
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000006056 electrooxidation reaction Methods 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 17
- 238000005516 engineering process Methods 0.000 claims description 15
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 15
- 238000002161 passivation Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 abstract description 8
- 150000002500 ions Chemical class 0.000 abstract description 7
- 238000011282 treatment Methods 0.000 abstract description 3
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 23
- 239000000463 material Substances 0.000 description 17
- 229910010271 silicon carbide Inorganic materials 0.000 description 17
- 229910021426 porous silicon Inorganic materials 0.000 description 16
- 238000000137 annealing Methods 0.000 description 12
- 239000013078 crystal Substances 0.000 description 12
- -1 rare earth ion Chemical class 0.000 description 11
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 11
- 238000004020 luminiscence type Methods 0.000 description 10
- 235000012239 silicon dioxide Nutrition 0.000 description 10
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- 229910052691 Erbium Inorganic materials 0.000 description 7
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
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- 238000004435 EPR spectroscopy Methods 0.000 description 1
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- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
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Abstract
The present invention provides a preparation method of a blue light-emitting diode. The preparation method has the following steps: a. firstly, carbonic ions with the energy of 20 to 50 keV and the amount of 5*10<16>ions/cm<2> are injected into N-type monocrystal silicon with the specific resistance of 30 to 50 omega. Cm; b. the N-type monocrystal silicon injected with the carbonic ions is put in a tubular furnace, is input with hydrogen or nitrogen or argon and is passivated at the temperature of 800 to 1100 DEG C for 20 to 90 minutes; c. subsequently, electrochemical corrosion is carried out for 10 to 50 minutes under constant pressure at the current density of 20 to 100 mA/cm<2>; d. finally, the blue light-emitting diode is obtained through regular silicon planar process treatment. The gas flow of the input hydrogen or nitrogen or argon is from 1000 to 2500 ml/min, and the corrosive liquor of the electrochemical corrosion is prepared from 1 share of hydrochloric acid and 1 to 5 shares of ethanol by weight.
Description
Technical field
The present invention relates to the electron luminescence device, relate to a kind of light-emitting diode more specifically.
Background technology
Blue light is one of three-primary colours in the panchromatic demonstration.And information transmission and information processing are of great importance.It is not only the necessary technology of silica-based panchromatic demonstration, and can improve the resolution of capacity and the laser printer and the laser scanner of light storage device.So people carry out the research of blue light material by persistence for a long time always.The research and development of blue diode LED are started in early seventies, are to adopt halide crystal growth method growing GaN to begin one's study by people such as the H.P.Marvska of the U.S. and Pankove.Thereafter PANASONIC technical research institute researchs and develops, but does not reach application level.Japan Synesis Company of Toyota adopts the MOCVDLPE technology to carry out the research of GaN blue led from nineteen ninety.GaN blue led in nineteen ninety-five produces reaches the highest level in the world.Siemens and electrical machinery of Japanese sanyo company adopt LPE technological development SiC blue led, and luminous intensity reaches 6mcd and 12mcd respectively.But GaN and SiC are not silicon base luminous materials, and technology and silicon planner technology are incompatible, and cost is also higher.Integrated from integrated solid-state demonstration and photoelectron, all require the silica-based blue led of development.Because the high development and the critical role of microelectric technique can only be that the photoelectron integrated technology is developed on the basis with it, otherwise economically with technical all be unacceptable.As the basic material of microelectric technique, silicon is difficult to replace.The research of silicon base luminous material at present mainly concentrates on preparation low-dimensional silicon luminescent material aspect, as porous silicon, nano-silicon, silicon/silicon dioxide super crystal lattice material and rare earth ion doped etc.
Er-doped silicon is luminous:
Impurity can be introduced the complex centre in silicon.But the impurity in the silicon, except the alms giver, led and defect state, be non-radiation recombination center mostly.And rare earth elements such as erbium have unique electronic state, and its emission wavelength is at 1.54 μ m, are in just in the wave-length coverage of low loss window of silex glass fiber, have potential using value.There is (Er3+) in erbium in silicon with positive trivalent form, and the light emission is to be caused by the transition between the 4f attitude of erbium internal layer, and the 4f attitude is by the 5s of outer shell, the 5p attitude shields, and parent residing with it is also irrelevant, for example at Si, GaAs, the luminescent properties among the GaP after the er-doped is basic identical.Therefore can mix erbium in the required material as luminescence center with deterministic nature.The common method that erbium is mixed in the silicon has ion implantation, diffusion method and molecular beam epitaxy etc.Wherein the most frequently used is ion implantation.Preparation er-doped silicon has certain difficulty technically.Because the atomic weight of erbium is very big,, need to use the high energy implanter for it is mixed in the silicon.Though people have carried out big quantity research to the characteristic of er-doped silicon, er-doped silicon luminescent material is failed practicability so far.Main cause is that the solid solubility of erbium in silicon is too low, luminous intensity too a little less than, realize light amplification and make relatively difficulty of laser.But because of its emission wavelength and optical fiber are complementary, people are still carrying out pilot study.
Isoelectronic center is luminous:
The another kind of method of silicon being carried out modification is the defect luminescence center of introducing in silicon, but the compound of most of defect center is non-radiative compound, do not have the characteristics of luminescence.Yet the isoelectronic center defective is a kind of luminescence center.Mix element of the same clan with it such as C in silicon, Ge or Sn etc. such as can form at the electron luminescence center.Such as obtaining the infrared light emission of 1.28 μ m in silicon, mixing carbon.This luminescence center is complicated impurity--defective assembly, and it is made up of two carbon atoms and a silicon interstitial atom, is called the G center again.The light emission characteristic of isoelectronic center has obtained explanation in theory in the silicon, can detect the infrared light emission spectra experimentally, and its wavelength drops on the spread fiber low-loss band, and using value is arranged.But waiting electron luminescence center luminous efficiency lower, is 1% only when 77K, has got long long way to go from practicality.
Porous silicon luminescence:
Though it is luminous that the body silicon materials are difficult for, when the silicon materials size was reduced to nanoscale, silicon can be luminous.Porous silicon luminescence is wherein representational example.Nineteen ninety Canham obtains red emission when the porous silica material that research obtains with hydrofluoric acid corrosion silicon.Porous silicon is that electrochemical corrosion forms.Its surface topography is the coralliform porous body.High resolution electron microscopy the analysis showed that porous silicon is to be piled up by the little crystal grain of some nano-scales to form, and each little crystal grain itself still keeps the ordered structure of crystal.For Luminescence in Porous Silicon mechanism, exist different views always.Conclude to get up to be divided into three major types.The first kind is a quantum limitation effect.In the porous silicon crystal grain of nano-scale, because quantum limitation effect, one side band gap broadening, push emission wavelength to visible-range, original on the other hand non-direct band gap turns to direct band gap, the probability of vertical transition has in other words increased, and luminous efficiency is increased, so at room temperature obtain strong VISIBLE LIGHT EMISSION.Second class is that amorphous silicon is luminous.When monocrystalline silicon was corroded porous silicon crystal grain into nano-scale, little crystal grain is noncrystal with avalanche, and was luminous by the magnetic tape trailer transition in amorphous silicon.The 3rd class is the multiple model relevant with the surface.Quantum limitation effect is accepted by increasing people, and people admit that also surface and interface play an important role in the Luminescence in Porous Silicon process simultaneously.The formation of porous silicon is to utilize electrochemical corrosion, and electrochemical corrosion course is subjected to the conduction type of silicon crystal, the influence of resistivity and crystal perfection.These character of silicon crystal can be effectively injected by ion and are controlled and change, so ion injects the effective means that becomes control porous silicon luminescence character.Ion injects can control luminous intensity significantly, can also change emission wavelength within the specific limits.Regrettably porous silicon is used does not have breakthrough so far.There are several problems to hinder the application of porous silicon.The firstth, the luminosity instability.Second light emitting region is confined to ruddiness and green glow, is difficult to obtain blue emission.
In a word, above-mentioned several silica-base materials generally can only send infrared light, ruddiness or green purple light, and difficulty is sent blue light, so can not satisfy the integrated luminous shortwave requirement of photoelectricity.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, providing a kind of is that the cost of substrate is low with the silica-base material, the preparation method of blue LED easy to prepare.
Purpose of the present invention can realize by following technical measures:
A, earlier to inject energy in resistivity is the n type single crystal silicon of 30-50 Ω cm be 20～50keV, 5 * 10
16Ions/cm
2Carbon ion; B, the n type single crystal silicon that will inject carbon ion again place tube furnace, feed hydrogen or nitrogen or argon gas, carry out passivation at 800～1100 ℃ and 20～90 minutes under the condition; C and then be 20～100mA/cm in constant voltage and current density
2Carry out electrochemical corrosion 10～50 minutes under the condition, handle through conventional silicon planner technology at last, get goods.
Purpose also can realize by following technical measures:
The gas flow of described feeding hydrogen or nitrogen or argon gas is 1000～2500ml/min; The corrosive liquid of described electrochemical corrosion is by hydrochloric acid: ethanol=1: 1～5 weight portions are formed; In tube furnace, feed hydrogen and carry out passivation, better effects if.
Technical finesse route of the present invention is:
(1) carbon ion is injected monocrystalline silicon with various dose, after suitable annealing and electrochemical treatments, measure its electroluminescence characters.
(2) use electron paramagnetic resonance, X-ray diffraction, the micro-structural of multiple technologies analytic samples such as Fuli's leaf infrared absorption spectroscopy.
(3) with defective and the damage of study sample after different heat treatment and electrochemical treatments such as Rutherford backscattering and trench technology, secondary ion mass spectroscopy, transmission electron microscope and twin crystal X-ray diffractions.
(4) utilize the computer simulation carbon ion to inject the situation of monocrystalline silicon,, ion is injected the luminescence mechanism of monocrystalline silicon and study in conjunction with experimental result.
(5) utilize the injection of aforementioned optimization, annealing and electrochemical conditions are prepared the silica-based silicon carbide nano material of the high characteristics of luminescence.
(6) adopt Au/Si (C)/P-Si/Al structure, develop the blue LED of high brightness.
The present invention at first finishes preparation novel silicon base nanometer silicon carbide luminescent material, adopts electrochemical corrosion to form the silicon-based nano silicon-carbide particle, in conjunction with adopting conventional silicon planner technology to prepare blue LED.
The analysis of FTIR infrared transmission is measured with Nicolet 710 FTISs and is obtained.The RIGAKU D-Max-RB type X-ray diffractometer that the sample crystalline structure is produced in Japan is measured and is obtained.This diffractometer adopts Cu target Ka line as x-ray source, and operating voltage is 40KV, and operating current is 1000mA.Morphology analysis adopts HITACHI-8010 type scanning electron microscopy to carry out.The photoluminescence spectrum of all samples is measured by Edingburger FLS920 spectral fluorometer and is obtained.
Carbon is injected into annealing in the silicon and forms β-SiC.Can directly form nano SiC than cold spot area.High dose can form continuous SiC layer after injecting.But both all can not be directly luminous.Continuous SiC layer belongs to body β-SiC, is non-direct band gap material, and nature can not be luminous.Nanometer β-SiC is not luminous to be that silicon band gap is that 1.12eV is also narrower than the band gap (2.2eV) of β-SiC because they are embedded in the silicon.Even excitation electron is arranged among β-SiC, can be directly not compound and luminous, but transfer in the contiguous silicon medium yet, through non-radiative compound and disappear.So it is luminous to make carbon inject the β-SiC that forms, and need make pantostrat become nanocrystal, again nanocrystal is applied quantum limit, promptly around nano SiC crystal grain, set up high potential barrier, make it to produce quantum limitation effect.Simple and effective approach is to make it porous, so the inventor adopts and preparation porous silicon similar methods, uses electrochemical corrosion, makes carbon implanted layer porous, and this has just satisfied quantum limitation effect, obtains blue emission.The blue emission of porous SiC is very stable, under up to 850 ℃ temperature oxidation after 30 minutes luminescent spectrum do not have any drift.This and porous silicon form sharp contrast, and porous silicon is at room temperature deposited in the air, and the characteristics of luminescence i.e. significantly drift.
Carbon injects the major progress that the porous SiC blue light emitting material is silicon base luminous material research.This is to obtain stable strong blue emission first on silica-based.This also is ion implantation technique once successful application in silicon base luminous material research.
The present invention is that substrate preparation goes out the silica-based blue led of high brightness with the n type single crystal silicon, can realize that silicon photoelectricity is integrated, also can reduce cost simultaneously.
Adopt silica-base material to prepare the blue led luminescent device, characteristics such as it is low to have a cost, easy to prepare.And compatible with silicon planner technology, can realize that silicon photoelectricity is integrated.If can develop the high-brightness blue light-emitting diode, and and redness and the green LED sold in the market combine, can make the LED field possess three primary colors.Thereby can constitute polychrome, panchromatic light-emitting diode display spare.These devices can be widely used in household appliances, measuring instrument, and indoor and outdoor information shows, advertising, communication apparatus etc.Characteristics such as this product has that volume is little, the response time is short, luminous efficiency is high, energy-conservation, long service life.
Blue LED of the present invention after tested, its key technical indexes is as follows:
Peak luminous wavelength: 467 ± 4nm
11 γ spectrum half breadth :≤36nm
12 γ luminous intensity: 〉=700mcd
Test condition:
Measuring current: 20mA
Temperature: 20 ℃
Humidity: 45%
Air pressure: 100kPa
Embodiment
Embodiment 1:
Adopting resistivity is that the n type single crystal silicon of 30 Ω cm is a substrate, the injection energy be 50keV (kiloelectron-volt), 5 * 10
16Ions/cm
2The carbon ion of (ounce/square centimeter); The n type single crystal silicon sample that injects carbon ion is inserted tube furnace anneals, during annealing, earlier sample is placed quartz boat, again quartz boat is put into the quartz ampoule of tube furnace, pass to highly purified flowing hydrogen (or nitrogen or argon gas) and carry out surface passivation, gas flow is controlled at 2500ml/min (ml/min), and annealing temperature is 1100 ℃, and annealing time is 20 minutes; Adopting 20V constant voltage instrument control power supply, is 70mA/cm in current density
2Carry out electrochemical corrosion 10 minutes under the condition; Corrosive liquid is according to hydrochloric acid: ethanol=weight portion preparation in 1: 5; Corrosion current is 100mA/cm
2, and in conjunction with adopting conventional silicon planner technology to be prepared into blue LED.
Embodiment 2:
Adopting resistivity is that the n type single crystal silicon of 50 Ω cm is a substrate, the injection energy be 20keV (kiloelectron-volt), 5 * 10
16Ions/cm
2The carbon ion of (ounce/square centimeter); The n type single crystal silicon sample that injects carbon ion is inserted tube furnace anneals, during annealing, earlier sample is placed quartz boat, again quartz boat is put into the quartz ampoule of tube furnace, pass to highly purified flowing hydrogen (or nitrogen or argon gas) and carry out surface passivation, gas flow is controlled at 1000ml/min (ml/min), and annealing temperature is controlled to be 800 ℃, and annealing time is 80 minutes; Adopting 50V constant voltage instrument control power supply, is 20mA/cm in current density
2Carry out electrochemical corrosion 50 minutes under the condition; Corrosive liquid is according to hydrochloric acid: ethanol=weight portion preparation in 1: 3; Corrosion current is 20mA/cm
2, and in conjunction with adopting conventional silicon planner technology to be prepared into blue LED.
Embodiment 3:
Adopting resistivity is that the n type single crystal silicon of 40 Ω cm is a substrate, the injection energy be 30keV (kiloelectron-volt), 5 * 10
16Ions/cm
2The carbon ion of (ounce/square centimeter); The n type single crystal silicon sample that injects carbon ion is inserted tube furnace anneals, during annealing, earlier sample is placed quartz boat, again quartz boat is put into the quartz ampoule of tube furnace, pass to highly purified flowing hydrogen (or nitrogen or argon gas) and carry out surface passivation, gas flow is controlled at 1500ml/min (ml/min), and annealing temperature is 950 ℃, and annealing time is 60 minutes; Adopting 30V constant voltage instrument control power supply, is 100mA/cm in current density
2Carry out electrochemical corrosion 30 minutes under the condition; Corrosive liquid is according to hydrochloric acid: ethanol=weight portion preparation in 1: 1; Corrosion current is 50mA/cm
2, and in conjunction with adopting conventional silicon planner technology to be prepared into blue LED.
Claims (2)
1, a kind of preparation method of blue LED is characterized in that:
A, earlier to inject energy in resistivity is the n type single crystal silicon of 30-50 Ω cm be 20～50keV, 5 * 10
16Ions/cm
2Carbon ion;
B, the n type single crystal silicon that will inject carbon ion again place tube furnace, feed hydrogen or nitrogen or argon gas and carry out passivation, and passivation temperature is 800～1100 ℃, and passivation time is 20～90 minutes;
C and then be 20～100mA/cm in constant voltage and current density
2Reach by hydrochloric acid under the condition: carried out electrochemical corrosion 10～50 minutes in the electrochemical corrosive liquid that ethanol=1: 1～5 weight portions are formed, handle through conventional silicon planner technology at last, get goods.
2, the preparation method of a kind of blue LED according to claim 1 is characterized in that described passivation gas flow is 1000～2500ml/min.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5397429A (en) * | 1993-09-14 | 1995-03-14 | University Of Florida | Method of manufacturing photoluminescing porous silicon using spark erosion |
| CN1142875A (en) * | 1993-12-06 | 1997-02-12 | 英国国防部 | porous semiconductor material |
| US6056868A (en) * | 1998-05-22 | 2000-05-02 | Cheah; Kok Wei | Rare earth doping of porous silicon |
| US6103540A (en) * | 1993-09-09 | 2000-08-15 | The United States Of America As Represented By The Secretary Of The Navy | Laterally disposed nanostructures of silicon on an insulating substrate |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6103540A (en) * | 1993-09-09 | 2000-08-15 | The United States Of America As Represented By The Secretary Of The Navy | Laterally disposed nanostructures of silicon on an insulating substrate |
| US5397429A (en) * | 1993-09-14 | 1995-03-14 | University Of Florida | Method of manufacturing photoluminescing porous silicon using spark erosion |
| CN1142875A (en) * | 1993-12-06 | 1997-02-12 | 英国国防部 | porous semiconductor material |
| US6056868A (en) * | 1998-05-22 | 2000-05-02 | Cheah; Kok Wei | Rare earth doping of porous silicon |
Non-Patent Citations (1)
| Title |
|---|
| 激发波长和电化学腐蚀对注碳外延硅荧光特性的影响 王强，李忠，李玉国，石礼伟，郭兴龙.纳米材料与结构 2004 * |
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