CN100369202C - Method for preparing nano-silicone base lighting composite film - Google Patents
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- CN100369202C CN100369202C CNB2005100681511A CN200510068151A CN100369202C CN 100369202 C CN100369202 C CN 100369202C CN B2005100681511 A CNB2005100681511 A CN B2005100681511A CN 200510068151 A CN200510068151 A CN 200510068151A CN 100369202 C CN100369202 C CN 100369202C
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- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 229920001296 polysiloxane Polymers 0.000 title 1
- 239000007789 gas Substances 0.000 claims abstract description 24
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims abstract description 16
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000008878 coupling Effects 0.000 claims abstract description 5
- 238000010168 coupling process Methods 0.000 claims abstract description 5
- 238000005859 coupling reaction Methods 0.000 claims abstract description 5
- 239000003990 capacitor Substances 0.000 claims description 26
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 13
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 10
- 229910000077 silane Inorganic materials 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 8
- 239000001272 nitrous oxide Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 abstract description 8
- 238000004020 luminiscence type Methods 0.000 abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 5
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 239000011856 silicon-based particle Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 230000005284 excitation Effects 0.000 description 4
- 229910004205 SiNX Inorganic materials 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- 238000005424 photoluminescence Methods 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 230000004083 survival effect Effects 0.000 description 3
- 235000005811 Viola adunca Nutrition 0.000 description 2
- 240000009038 Viola odorata Species 0.000 description 2
- 235000013487 Viola odorata Nutrition 0.000 description 2
- 235000002254 Viola papilionacea Nutrition 0.000 description 2
- 238000001505 atmospheric-pressure chemical vapour deposition Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000004050 hot filament vapor deposition Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 229910004797 SiO1.27 Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The present invention discloses a method for preparing nano silicon base luminescence composite films. The present invention uses a capacity coupling plasma enhancing chemical vapor deposition system, a lower pole plate of electroplate pole plates is in a double-layer screen-shapes inlet structure, the distance between the two pole plates is 2.0 to 2.5cm, radio frequency signals are added on the lower pole plate, and an upper pole plate is connected with the ground. The present invention adopts a 99.99% of mixed gas of pure silicane, nitrogen gas and hydrogen gas as a predecessor, and substrate single crystal silicon chips are placed on the pole plates. In this way, the present invention ensures the film preparation under small power (35W) radio frequency input, the substrate temperature is controlled below 50 DEG C, silicon particles easily survive in the composite films which grow on a substrate under the low temperature, the particle sizes are less than 2.0 nm, and the number density of the particles can reach 2.2*10<13>/cm<2>. The method can be used for preparing the high efficiency luminescence composite films with adjustable ranges from red light to purple light, the luminous efficiency can reach 10%, and the present invention has the advantages of simple production devices, economy, no pollution and high reliability.
Description
Technical Field
The invention relates to a method for preparing a nano silicon-based luminescent composite film.
Background
The exploration and preparation of the silicon-based high-efficiency luminescent film are a hot point of research in the past decade and even in the future years, and the silicon-based material capable of efficiently adjusting visible light full-waveband luminescence can be applied to the technical fields of optical interconnection, optical communication, full-silicon planar display and the like. However, due to the problems of structural and chemical instability, poor compatibility with the existing semiconductor process, and the like, the silicon-based luminescent material still has a certain distance from the practical production and application.
The methods currently used internationally for preparing silicon-based luminescent films include: PECVD (plasma enhanced chemical vapor deposition), hot filament CVD (hot filament CVD), atmospheric pressure CVD (atmospheric pressure CVD), LPCVD (1 w pressure chemical vapor deposition), ion implantation, and the like. These methods have the characteristics of growing under high temperature conditions or requiring high temperature annealing, and are not compatible with the existing semiconductor process.
Disclosure of Invention
The invention aims to provide a method for preparing a nano silicon-based luminescent composite film under a low-temperature condition.
In order to achieve the above purpose, the invention provides a method for preparing a nano silicon-based luminescent composite film, which comprises the following steps:
1. firstly, boiling the substrate for 2-20 minutes under the boiling condition by using deionized water after the substrate is subjected to pretreatment according to a known method, removing moisture, and then fixing the substrate on the lower surface of an upper plate of a capacitor plate; the capacitor plate is positioned in a vacuum chamber of a capacitance coupling Plasma Enhanced Chemical Vapor Deposition (PECVD) system; the substrate is a monocrystalline silicon wafer or quartz glass;
2. grounding the upper electrode plate of the capacitor electrode plate, adding a radio-frequency signal with the radio-frequency power less than 40W to the lower electrode plate, and uniformly and slowly introducing the mixed gas between the two electrode plates from the lower surface of the lower electrode plate of the capacitor electrode plate; the distance between the upper polar plate and the lower polar plate and the working pressure are adjusted, so that no discharge exists at the edges and the outer sides of the two polar plates, and the discharge is uniform between the polar plates.
Wherein,
the known method described in step 1 specifically is: acetone, alcohol and deionized water are sequentially and respectively subjected to ultrasonic treatment for 10 minutes.
The capacitor plate in step 1 is: the upper pole plate and the lower pole plate of the capacitor pole plate are both circular with the diameter larger than 6cm, and the lower pole plate is fixedly arranged on the ceramic base; a groove is arranged at the center of the upper polar plate, and the shape and the size of the groove are matched with those of the substrate; the lower polar plate is two staggered plates in a double-layer sieve shape.
The mixed gas in the step 2 is Silane (SiH)4) Nitrogen (N)2) And hydrogen (H)2) The gas purity of the mixed gas of (2) was 99.99%.
The mixed gas in step 2 may also be Silane (SiH)4) Nitrous oxide (N)2O) and hydrogen (H)2) Or Silane (SiH)4) Oxygen (O)2) And hydrogen (H)2) The gas purity of the mixed gas of (2) was 99.99%.
In order to achieve a better effect in the preparation process, in the step 1, after the substrate is subjected to pretreatment, the substrate is boiled for 2-20 minutes by deionized water under the boiling condition, and after moisture is removed, the substrate is fixed on the lower surface of the upper electrode plate of the capacitor electrode plate.
In the step 2, the distance between the upper polar plate and the lower polar plate of the capacitor polar plate is 2.0-2.5cm, the working air pressure is adjustable between 25-150Pa, and the radio frequency power is 35W.
Compared with the prior art, the method for preparing the nano silicon-based luminescent composite film has the advantages that: the temperature in the whole preparation process is controlled to be lower than 50 ℃, the temperature is favorable for the survival of the nano silicon particles in an oxidizing medium, the obtained minimum nano silicon particles can be less than 2.0nm, and the density of the particles can reach 2.2 multiplied by 1013/cm2(ii) a By utilizing the technology, the photoluminescence adjustable in the full spectrum range of visible light is obtained, especially the strong blue-violet light is successfully obtained, and the luminous efficiency reaches 10 percent to the maximum.
Drawings
FIG. 1 shows an example of 1 nm Si-in-SiN1.0A transmission electron microscope photograph of the luminescent composite film;
FIG. 2 is nano Si-in-SiNxLuminous composite film random [ N ]2]/[SiH4]A fluorescence spectrum of the change in value;
FIG. 3 shows nanometer Si-in-SiO in example 2 of the present invention1.27A transmission electron microscope photograph of the luminescent composite film;
FIG. 4 is nano Si-in-SiOxFluorescence spectrum of the luminescent composite film changing with X value.
Detailed Description
In the method for preparing the nano silicon-based luminescent composite film, the design of the used capacitor plate is as follows: the capacitor plate comprises an upper plate and a lower plate which are opposite in parallel, the lower plate is fixedly installed on the ceramic base, the two plates are circular, the diameter of each plate is larger than 6cm, a groove is formed in the center of the lower surface of the upper plate, the shape and the size of the groove are arranged according to the substrate, the lower plate is a double-layer sieve-shaped staggered plate, and the distance between the plates can be adjusted as required.
EXAMPLE 1 preparation of Nano Si-in-SiNx(x ═ 1.0) light-emitting composite film
1. Sequentially and respectively carrying out ultrasonic treatment on a monocrystalline silicon wafer for 10 minutes by adopting acetone, alcohol and deionized water; boiling the monocrystalline silicon piece for 2 minutes by using deionized water under the boiling condition; drying residual moisture on the monocrystalline silicon piece, and fixing the monocrystalline silicon piece into a groove on the lower surface of an upper polar plate of a capacitor polar plate by using a mask piece to ensure that the monocrystalline silicon piece is not loosened; putting the capacitor plate into a vacuum chamber of a capacitive coupling Plasma Enhanced Chemical Vapor Deposition (PECVD) system;
2. grounding the upper plate of the capacitor plate, and adding high-purity Silane (SiH) with purity of 99.99%4) High purity hydrogen (H)2) And high purity nitrogen (N)2) The mixed gas is introduced from the lower surface of the lower pole plate of the capacitor pole plate through the gas outlet of the mixing chamber, the gas uniformly and slowly enters between the lower pole plate and the upper pole plate through the lower pole plate in a double-layer sieve shape which is staggered with each other, and the distance between the two pole plates is 2.0 cm; applying radio frequency signal to the lower polar plate, setting the radio frequency energy input to 35W, regulating the working pressure between 25-150Pa to make the edges and outer sides of the two polar plates have no discharge, uniformly discharging between the polar plates, controlling the temperature of the monocrystalline silicon wafer to be lower than 50 ℃, and growing for more than 10 minutes or for multiple times to obtain the nano Si-in-SiN1.0A luminescent composite film.
The temperature is controlled to be lower than 50 ℃ in the whole preparation process, which is favorable for the survival of the nano silicon particles in the oxidation medium, as can be seen from the picture taken by a transmission electron microscope in figure 1,the average size of the nano silicon particles is 1.8nm, and the density of the particles is 1.07 x 1013/cm2(ii) a Measurement was carried out at room temperature using a PTI-710 fluorescence spectrometer with excitation by a He-Cd laser at a wavelength of 325nm or a xenon lamp at a wavelength of 325nm (the excitation wavelength may be shorter or longer), by adjusting high purity Silane (SiH)4) And high purity nitrogen (N)2) The flux ratio of (A) can obtain Si-in-SiN with different X valuesxComposite film, nano Si-in-SiNxThe luminescent composite film has adjustable photoluminescence in the whole visible light spectrum range, especially successfully obtains strong blue-violet light, and the luminous efficiency can reach 10%. FIG. 2 is a graph showing the following [ N ] when the method of the present invention is employed2]/[SiH4]Fluorescence spectrum of change of value, where [ N ]2]/[SiH4]The larger the value, the smaller the X value; as can be seen from FIG. 2, the smaller the X value, the red-shifted luminescence, and the blue-shifted luminescence, respectively. Therefore, the method can be used for preparing the luminescent film which is continuously adjustable from infrared to ultraviolet. The efficiency will be slightly different for different wavelengths of emitted light.
EXAMPLE 2 preparation of Nano Si-in-SiOx(x-1.78) luminescent composite film
1. Sequentially and respectively carrying out ultrasonic treatment on the monocrystalline silicon piece for 10 minutes by adopting acetone, alcohol and deionized water, and boiling the monocrystalline silicon piece for 20 minutes under the boiling condition by using deionized water; drying residual moisture on the monocrystalline silicon piece, and fixing the monocrystalline silicon piece into a groove on the lower surface of an upper polar plate of a capacitor polar plate by using a mask piece to ensure that the monocrystalline silicon piece is not loosened; the capacitor plate is positioned in a vacuum chamber of a capacitance coupling Plasma Enhanced Chemical Vapor Deposition (PECVD) system;
2. grounding the upper plate of the capacitor plate, and adding high-purity Silane (SiH) with purity of 99.99%4) High purity hydrogen (H)2) And high purity nitrous oxide (N)2O) fully mixing in a mixing chamber, wherein an air outlet of the mixing chamber is tightly connected with the outer surface of a lower polar plate, mixed gas is introduced from the lower surface of the lower polar plate of the capacitor polar plate through the air outlet of the mixing chamber, the gas uniformly and slowly enters between the lower polar plate and an upper polar plate through the lower polar plate in a double-layer sieve shape which is staggered with each other, and the distance between the two polar plates is 2.5 cm; radio frequency signalAdding the solution to the lower plate, setting the input of radio frequency energy at 40W, adjusting the working pressure between 25 Pa and 150Pa to ensure that no discharge exists at the edge and the outer side of the lower plate, uniformly discharging between the plates, controlling the temperature of the monocrystalline silicon wafer to be lower than 50 ℃, and growing for multiple times to obtain the nano Si-in-SiO1.27A luminescent composite film. Wherein nitrous oxide (N) in the mixed gas2O) oxygen (O) may also be used2) Instead of it.
The temperature during the whole preparation process is controlled to be lower than 50 ℃, which is favorable for the survival of the nano silicon particles in the oxidation medium, as can be seen from the photograph taken by a transmission electron microscope in FIG. 3, the average size of the nano silicon particles is 3.0nm, and the density of the particles is 4.0 × 1012/cm2(ii) a Measurement was carried out at room temperature using a PTI-710 fluorescence spectrometer with excitation by a He-Cd laser at a wavelength of 325nm or a xenon lamp at a wavelength of 325nm (the excitation wavelength may be shorter or longer), by adjusting high purity Silane (SiH)4) And high purity nitrous oxide (N)2O) can obtain Si-in-SiO with different X valuesxComposite film, nano Si-in-SiOxThe light-emitting composite film realizes adjustable photoluminescence in the whole visible light spectrum range. As shown in FIG. 4, the smaller the value of X, the red-shifted luminescence will occur, whereas the blue-shifted luminescence will occur. Therefore, the infrared to ultraviolet continuous luminescent film can be prepared. The efficiency will be slightly different for different wavelengths of emitted light.
The single crystal silicon wafer used in examples 1 and 2 may be replaced with quartz glass. In addition, when the method is adopted to prepare the silicon-based luminous composite film, the substrate adopted in the common vacuum growth of the film is as follows: sapphire, magnesium oxide crystals, ordinary glass flakes, and the like are suitable as substrate materials in the method of the present invention.
Claims (8)
1. A method for preparing a nano silicon-based luminescent composite film comprises the following steps:
(1) firstly, boiling the substrate for 2-20 minutes under the boiling condition by using deionized water after the substrate is subjected to pretreatment according to a known method, removing moisture, and then fixing the substrate on the lower surface of an upper plate of a capacitor plate; the capacitance polar plate is positioned in a vacuum chamber of the capacitance coupling plasma enhanced chemical vapor deposition system; the substrate is a monocrystalline silicon wafer or quartz glass;
(2) grounding the upper electrode plate of the capacitor electrode plate, adding a radio-frequency signal with the radio-frequency power less than 40W to the lower electrode plate, and slowly introducing the mixed gas between the two electrode plates from the lower surface of the lower electrode plate of the capacitor electrode plate at a constant speed; adjusting the distance between the upper and lower polar plates and the working pressure to ensure that no discharge exists at the edges and the outer sides of the two polar plates and the discharge is uniform between the polar plates; the capacitor comprises a capacitor plate, a ceramic base and a capacitor base, wherein the upper plate and the lower plate of the capacitor plate are both circular with the diameter larger than 6cm, and the lower plate is fixedly arranged on the ceramic base; a groove is arranged in the center of the upper polar plate, and the shape and the size of the groove are matched with those of the substrate; the lower polar plate is two staggered plates in a double-layer sieve shape.
2. The method of claim 1, wherein: the known method in the step (1) adopts acetone, alcohol and deionized water to respectively perform ultrasonic treatment for 10 minutes in sequence.
3. The method of claim 1, wherein: the working air pressure is 25-150 Pa.
4. The method of claim 1, wherein: the radio frequency power is 35W.
5. The method of claim 4, wherein: the distance between the upper polar plate and the lower polar plate of the capacitor polar plate is 2.0-2.5 cm.
6. Method according to one of claims 1 to 5, characterized in that: the mixed gas is the mixed gas of silane, nitrogen and hydrogen, and the purity of the gas is 99.99 percent.
7. Method according to one of claims 1 to 5, characterized in that: the mixed gas is the mixed gas of silane, nitrous oxide and hydrogen, and the purity of the gas is 99.99%.
8. Method according to one of claims 1 to 5, characterized in that: the mixed gas is the mixed gas of silane, oxygen and hydrogen, and the purity of the gas is 99.99 percent.
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| CN100449810C (en) * | 2006-12-30 | 2009-01-07 | 浙江大学 | Silicon based MgxZn1-xO ultraviolet electroluminescent device and method for producing the same |
| CN101942649A (en) * | 2010-10-21 | 2011-01-12 | 韩山师范学院 | Method for constructing high-density nano-silicon structure at low temperature |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000003415A1 (en) * | 1998-07-13 | 2000-01-20 | Applied Komatsu Technology, Inc. | Rf matching network with distributed outputs |
| CN1442883A (en) * | 2003-02-28 | 2003-09-17 | 浙江大学 | Method of preparing high effect silicon base luminuous film on silicon sheet |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000003415A1 (en) * | 1998-07-13 | 2000-01-20 | Applied Komatsu Technology, Inc. | Rf matching network with distributed outputs |
| CN1442883A (en) * | 2003-02-28 | 2003-09-17 | 浙江大学 | Method of preparing high effect silicon base luminuous film on silicon sheet |
Non-Patent Citations (1)
| Title |
|---|
| 纳米Si-SiOx和Si-SiNx复合薄膜的低温制备及其发光特性. 纪爱玲，马利波，刘瀓，王永谦；.物理学报，第53卷第11期. 2004 * |
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