CN100369202C - Method for preparing nano-silicone base lighting composite film - Google Patents
Method for preparing nano-silicone base lighting composite film Download PDFInfo
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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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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 present invention relates to a kind of method for preparing nano-silicone base lighting composite film.
Background technology
The exploration of silica-based high-efficiency light-emitting film is a focus of studying in past 10 years and even several years in the future with preparation, and the luminous silica-base material of efficient adjustable visible light all band can be applicable to technical fields such as optical interconnection, optical communication and the demonstration of total silicon plane.But, since structure and chemical instability and with the problems such as poor compatibility of existing semiconductor processes, still there is certain distance in silicon base luminous material apart from production application.
The method of using at present for preparing the silicon base luminescence film has in the world: PECVD method (plasmaenhanced chemical vapor deposition), heated filament CVD method (hot filamentassisted chemical vapor deposition), atmospheric pressure CVD method (atmosphericpressure chemical vapor deposition), LPCVD method (1ow pressure chemicalvapor deposition) and ion implantation etc.These methods have under hot conditions growth or need characteristics such as high annealing, are unfavorable for and existing semiconductor technology compatibility.
Summary of the invention
The object of the present invention is to provide a kind of method that under cryogenic conditions, prepares nano-silicone base lighting composite film.
For achieving the above object, a kind of method for preparing nano-silicone base lighting composite film of the present invention may further comprise the steps:
1, according to known method substrate is carried out handling early stage after, earlier substrate was boiled under the boiling situation 2-20 minute with deionized water, remove the solid carbon dioxide branch after, again substrate is fixed on the lower surface of the top crown of capacitor plate; Capacitor plate is positioned at the vacuum chamber that capacitance coupling plasma strengthens chemical vapour deposition (CVD) (PECVD) system; Described substrate is monocrystalline silicon piece or quartz glass;
2, with the top crown ground connection of capacitor plate, the radiofrequency signal of radio-frequency power less than 40W is added on the bottom crown, the lower surface of mist from the bottom crown of capacitor plate evenly, slowly entered between the two-plate; Regulate distance and operating air pressure size between the upper and lower pole plate, make two-plate edge and outside discharge off, evenly discharge between pole plate.
Wherein,
Known method described in the step 1 is specially: adopt acetone, alcohol, deionized water to distinguish ultrasonic 10 minutes successively.
Capacitor plate in the step 1 is: the top crown of capacitor plate and bottom crown are the circle of diameter greater than 6cm, and bottom crown is fixedly mounted on the ceramic base; The center of top crown is provided with groove, and the shape of this groove and size are complementary with substrate; The two boards that bottom crown staggers for the double deck screen shape.
Mist in the step 2 is silane (SiH
4), nitrogen (N
2) and hydrogen (H
2) mist, gas purity is 99.99%.
Mist in the step 2 can also be silane (SiH
4), nitrous oxide (N
2O) and hydrogen (H
2) mist or be silane (SiH
4), oxygen (O
2) and hydrogen (H
2) mist, gas purity is 99.99%.
In order in preparation process, to reach better effect, in step 1, after substrate carried out handling early stage, earlier substrate was boiled under the boiling situation 2-20 minute with deionized water, remove the solid carbon dioxide branch after, again substrate is fixed on the lower surface of the top crown of capacitor plate.
The top crown of the capacitor plate in the step 2 and the distance between the bottom crown are 2.0-2.5cm, and operating air pressure is adjustable between 25-150Pa, and radio-frequency power is 35W.
Compared with prior art, a kind of method for preparing nano-silicone base lighting composite film provided by the invention, its advantage is: temperature is controlled at and is lower than 50 ℃ in the whole process of preparation, this temperature helps the survival of silicon nanoparticle in oxide isolation, the minimum silicon nanoparticle that is obtained can be less than 2.0nm, and the density of particle can reach 2.2 * 10
13/ cm
2Utilize this technology to obtain adjustable luminescence generated by light in the full spectral limit of visible light, obtained strong royal purple light especially smoothly, luminous efficiency up 10%.
Description of drawings
Fig. 1 is the embodiment of the invention 1 nanometer Si-in-SiN
1.0The transmission electron microscope photo of luminous laminated film;
Fig. 2 is nanometer Si-in-SiN
xLuminous laminated film is with [N
2]/[SiH
4] fluorescence spectrum that changes of value;
Fig. 3 is the embodiment of the invention 2 nanometer Si-in-SiO
1.27The transmission electron microscope photo of luminous laminated film;
Fig. 4 is nanometer Si-in-SiO
xThe fluorescence spectrum figure that luminous laminated film changes with the X value.
Embodiment
Prepare in the method for nano-silicone base lighting composite film in the present invention, the design of employed capacitor plate is: capacitor plate comprises parallel relative upper and lower pole plate, bottom crown is fixedly mounted on the ceramic base, two-plate is the circle of diameter greater than 6cm, there is a groove center at the lower surface of top crown, the shape of groove and size are provided with according to substrate, the two boards that bottom crown staggers for the double deck screen shape, and the distance between the pole plate can be adjusted as required.
Embodiment 1 preparation nanometer Si-in-SiN
x(x=1.0) luminous laminated film
1, monocrystalline silicon piece is adopted acetone, alcohol, deionization distinguish ultrasonic 10 minutes successively; Monocrystalline silicon piece was boiled under the boiling situation 2 minutes with deionized water; Dry up the remaining moisture content on the monocrystalline silicon piece, monocrystalline silicon piece is fixed in the groove of lower surface of top crown of capacitor plate with the mask sheet then, guarantee that monocrystalline silicon piece is loosening; Capacitor plate is put into the vacuum chamber that capacitance coupling plasma strengthens chemical vapour deposition (CVD) (PECVD) system;
2,, purity is 99.99% high purity silane (SiH with the top crown ground connection of capacitor plate
4), high-purity hydrogen (H
2) and high pure nitrogen (N
2) in mixing chamber, fully mix, the gas outlet of mixing chamber is connected together mutually with the intimate of bottom crown, gas outlet by mixing chamber imports the lower surface of mist from the bottom crown of capacitor plate, gas is through the bottom crown of the double deck screen shape that staggers mutually, evenly enter lentamente between bottom crown and the top crown, the distance between the two-plate is 2.0cm; Radiofrequency signal is added on the bottom crown, the radio-frequency (RF) energy input is set at 35W, operating air pressure is regulated between 25-150Pa, make two-plate edge and outside discharge off, evenly discharge between pole plate, the temperature of monocrystalline silicon piece is controlled at and is lower than 50 ℃, and growth is grown more than 10 minutes or repeatedly, can obtain nanometer Si-in-SiN
1.0Luminous laminated film.
Temperature all is controlled in and is lower than 50 ℃ in the above-mentioned whole process of preparation, this temperature helps the survival of silicon nanoparticle in oxide isolation, as can be known, the silicon nanoparticle average-size is 1.8nm in the photo of being obtained by transmission electron microscope among Fig. 1, and the density of particle is 1.07 * 10
13/ cm
2Use the PTI-710 fluorescence spectrophotometer, excite (excitation wavelength can be shorter or longer), at room temperature measure, by regulating high purity silane (SiH with He-Cd laser 325nm wavelength or xenon lamp 325nm wavelength
4) and high pure nitrogen (N
2) flow-rate ratio can obtain the different Si-in-SiN of X value
xLaminated film, nanometer Si-in-SiN
xLuminous laminated film has adjustable luminescence generated by light in the full spectral limit of visible light, has obtained strong royal purple light especially smoothly, and luminous efficiency can reach 10%.Fig. 2 is when adopting method of the present invention, with [N
2]/[SiH
4] fluorescence spectrum that changes of value, wherein [N
2]/[SiH
4] value big more, the X value is more little; As can be seen from Figure 2, the X value more little luminous will red shift, otherwise blue shift.Therefore adopt the method can prepare from infrared to the continuously adjustable light-emitting film of ultraviolet.The emission wavelength difference, efficient can be slightly different.
Embodiment 2 preparation nanometer Si-in-SiO
x(x=1.78) luminous laminated film
1, monocrystalline silicon piece is adopted acetone, alcohol, deionization distinguish ultrasonic 10 minutes successively, monocrystalline silicon piece was boiled under the boiling situation 20 minutes with deionized water; Dry up the remaining moisture content on the monocrystalline silicon piece, monocrystalline silicon piece is fixed in the groove of lower surface of top crown of capacitor plate with the mask sheet then, guarantee that monocrystalline silicon piece is loosening; Capacitor plate is positioned at the vacuum chamber that capacitance coupling plasma strengthens chemical vapour deposition (CVD) (PECVD) system;
2,, purity is 99.99% high purity silane (SiH with the top crown ground connection of capacitor plate
4), high-purity hydrogen (H
2) and high-purity nitrous oxide (N
2O) fully mix at mixing chamber, the gas outlet of mixing chamber is connected together mutually with the intimate of bottom crown, gas outlet by mixing chamber imports the lower surface of mist from the bottom crown of capacitor plate, gas is through the bottom crown of the double deck screen shape that staggers mutually, evenly enter lentamente between bottom crown and the top crown, the distance between the two-plate is 2.5cm; Radiofrequency signal is added on the bottom crown, and the radio-frequency (RF) energy input is set at 40W, and operating air pressure is regulated between 25-150Pa, make two-plate edge and outside discharge off, evenly discharge between pole plate, the temperature of monocrystalline silicon piece is controlled at and is lower than 50 ℃, repeatedly growth can obtain nanometer Si-in-SiO
1.27Luminous laminated film.Wherein, the nitrous oxide (N in the mist
2O) can also use oxygen (O
2) replace.
Temperature all is controlled in and is lower than 50 ℃ in the above-mentioned whole process of preparation, this temperature helps the survival of silicon nanoparticle in oxide isolation, as can be known, the silicon nanoparticle average-size is 3.0nm in the photo of being obtained by transmission electron microscope from Fig. 3, and the density of particle is 4.0 * 10
12/ cm
2Use the PTI-710 fluorescence spectrophotometer, excite (excitation wavelength can be shorter or longer), at room temperature measure, by regulating high purity silane (SiH with He-Cd laser 325nm wavelength or xenon lamp 325nm wavelength
4) and high-purity nitrous oxide (N
2O) flow-rate ratio can obtain the different Si-in-SiO of X value
xLaminated film, nanometer Si-in-SiO
xLuminous laminated film is realized adjustable luminescence generated by light in the full spectral limit of visible light.As shown in Figure 4, the X value more little luminous will red shift, otherwise blue shift.Therefore can prepare from infrared to the continuous light-emitting film of ultraviolet.The emission wavelength difference, efficient can be slightly different.
The monocrystalline silicon piece that is adopted among the embodiment 1 and 2 also can substitute with quartz glass.In addition, when adopting this method to prepare the silicon base luminescence laminated film, the substrate that when the conventional vacuum growing film, is adopted, for example: sapphire, magnesia crystal, simple glass sheet etc. all are suitable for as the backing material in the inventive method.
Claims (8)
1. method for preparing nano-silicone base lighting composite film may further comprise the steps:
(1) according to known method substrate is carried out handling early stage after, earlier substrate was boiled under the boiling situation 2-20 minute with deionized water, remove the solid carbon dioxide branch after, again substrate is fixed on the lower surface of the top crown of capacitor plate; Capacitor plate is positioned at the vacuum chamber that capacitance coupling plasma strengthens chemical gas-phase deposition system; Described substrate is monocrystalline silicon piece or quartz glass;
(2) with the top crown ground connection of capacitor plate, the radiofrequency signal of radio-frequency power less than 40W is added on the bottom crown, the lower surface of mist from the bottom crown of capacitor plate at the uniform velocity, slowly entered between the two-plate; Regulate distance and operating air pressure size between the upper and lower pole plate, make two-plate edge and outside discharge off, evenly discharge between pole plate; Wherein, the top crown of described capacitor plate and bottom crown are the circle of diameter greater than 6cm, and described bottom crown is fixedly mounted on the ceramic base; The center of described top crown is provided with groove, and the shape of this groove and size are complementary with described substrate; The two boards that described bottom crown staggers for the double deck screen shape.
2. method according to claim 1 is characterized in that: the known method described in the step (1) is distinguished ultrasonic 10 minutes successively for adopting acetone, alcohol, deionized water.
3. according to the described method of claim 1, it is characterized in that: described operating air pressure is 25-150Pa.
4. according to the described method of claim 1, it is characterized in that: described radio-frequency power is 35W.
5. method according to claim 4 is characterized in that: the top crown of described capacitor plate and the distance between the bottom crown are 2.0-2.5cm.
6. according to one of them described method of claim 1 to 5, it is characterized in that: described mist is the mist of silane, nitrogen and hydrogen, and gas purity is 99.99%.
7. according to one of them described method of claim 1 to 5, it is characterized in that: described mist is the mist of silane, nitrous oxide and hydrogen, and gas purity is 99.99%.
8. according to one of them described method of claim 1 to 5, it is characterized in that: described mist is the mist of silane, oxygen and hydrogen, and gas purity is 99.99%.
Priority Applications (1)
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|---|---|---|---|
| CNB2005100681511A CN100369202C (en) | 2005-04-29 | 2005-04-29 | Method for preparing nano-silicone base lighting composite film |
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|---|---|---|---|
| CNB2005100681511A CN100369202C (en) | 2005-04-29 | 2005-04-29 | Method for preparing nano-silicone base lighting composite film |
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| CN100369202C true CN100369202C (en) | 2008-02-13 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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2005
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Patent 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 |
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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