CN102435596A - Method and device for testing light emission spectrum in hot filament chemical vapor deposition - Google Patents
Method and device for testing light emission spectrum in hot filament chemical vapor deposition Download PDFInfo
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- CN102435596A CN102435596A CN2011102650833A CN201110265083A CN102435596A CN 102435596 A CN102435596 A CN 102435596A CN 2011102650833 A CN2011102650833 A CN 2011102650833A CN 201110265083 A CN201110265083 A CN 201110265083A CN 102435596 A CN102435596 A CN 102435596A
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Abstract
The invention relates to a method and a device for testing a light emission spectrum in hot filament chemical vapor deposition, belonging to the technical field of spectrum research. The method is characterized in that: radio frequency drive is used for generating a luminescent element in the gas phase of preparing a silicon film by hot filament chemical vapor deposition, the light emission spectrum of the radio frequency driven hot filament chemical vapor deposition is tested and analyzed by a double slit device, optical fibers, and a spectrometer, the gas phase process characteristics are recognized, and the film preparation is guided. The spectrum emitted by the device herein can explain the relationship between changes of gas pressure, gas flow and other deposition parameters and microcrystal silicon film deposition rate and microstructure, and is one of effective methods of researching HWCVD gas phase process. The method and device has the advantages of simple operation, easy realization, and repeated and reliable data, and can be applied in film preparation technology by hot filament chemical vapor deposition in solar cell, microelectronics and other fields.
Description
Technical field
The present invention relates to the method for testing and the device thereof of light emission spectrum in a kind of hot-wire chemical gas-phase deposition process, belong to the spectral investigation technical field.
Background technology
Hot-wire chemical gas-phase deposition (hereinafter to be referred as HWCVD) is the common technology of film preparation; Owing to have the advantage that device structure is simple, decomposing gas abundant, high concentration atom H helps the film crystallization and do not have ion bom bardment, make it in the preparation of low-cost silicon-film solar-cell, have good application prospect.Obtain high deposition rate, high-quality microcrystalline silicon film, must study the gas phase reaction process of film growth, understand Thin Film Deposition in depth, disclose the relation of reaction primitive concentration in film microstructure and photoelectric characteristic and the gas phase.
Yet,, less relatively to the experimental study of HWCVD gas-phase reaction dynamic process because no luminous primitive among the HWCVD is difficult for directly measurement.The luminous technology of using in the research at present of indirect induction that mainly contains: single photon ionization (SPI; Single-photo ionization) and LIF (LIF; Laser Induced Fluorescence) technology;, HWCVD detects Si, SiH3, primitives such as Si2HX in preparing the gas phase of silicon thin film.But, be difficult to detect the signal of H owing to the photon energy quantitative limitation.Mass spectrometer is unique technology of directly measuring of can realizing, but the mass spectrometer apparatus expensive, and what analyze usually is residual gas, with the gaseous environment of film growth certain difference is arranged.Above technology has certain help to the gas phase reaction process of understanding HWCVD, but because equipment cost and technical difficulty etc. make practical application receive certain restriction.
Summary of the invention
The objective of the invention is to propose the method for testing and the device thereof of light emission spectrum in a kind of hot-wire chemical gas-phase deposition process, to be used for the research of HWCVD gas phase reaction process.On the basis of HWCVD high temperature heated filament decomposition gas; Adopt radio frequency (rf) to excite and produce luminous primitive; Utilize light emission spectrum appearance (OES) to measure the light emission spectrum that rf excites HWCVD (rf-HWCVD); Through the research that different primitive spectral intensities are changed, the gas phase reaction process of understanding HWCVD, guiding material preparation.
The method of testing of light emission spectrum in the hot-wire chemical gas-phase deposition process that the present invention proposes may further comprise the steps:
(1) between the ground-electrode and high-frequency electrode of the setting parallel to each other of vacuum cavity; Place one or more heated filament; Make heated filament be parallel to two electrodes; Distance between heated filament and the ground-electrode is 3～6 centimetres, and the distance between heated filament and the high-frequency electrode is 1～3 centimetre, on the vacuum chamber body wall, quartz window is set;
(2) making the vacuum tightness in the vacuum cavity is 1 * 10
-3Handkerchief～1 * 10
-5Handkerchief makes the hot-wire temperature reach 1600～2200 ℃;
(3) mixed gas that in vacuum chamber, feeds silane and hydrogen is as reacting gas; The ratio of silane and hydrogen is: silane: hydrogen=1: 0～1: 50; The air pressure of reacting gas is 0.3～300 handkerchief, applies radio-frequency power to high-frequency electrode, makes radio-frequency power greater than 0.01 watt/centimetre
2, less than 0.1 watt/centimetre
2, between two parallel poles, produce the plasma aura;
(4) make the outgoing from the quartz window of vacuum cavity of above-mentioned plasma aura, and through a double aperture slit device, to slacken bias light;
(5) make from the aura of double aperture slit device outgoing,, obtain emission spectrum figure through optical fiber introducing light emission spectrum appearance;
(6) radio-frequency power of high-frequency electrode is reduced to 0, repeat (4) and (5), obtain the bias light spectrogram;
(7) background spectrum that deduction step (6) obtains from the spectrogram that step (5) obtains obtains hot-wire chemical gas-phase deposition emission spectrum figure.
The proving installation of light emission spectrum comprises vacuum cavity, ground-electrode, high-frequency electrode, heated filament, double aperture slit device and spectrometer in the hot-wire chemical gas-phase deposition process that the present invention proposes; Described ground-electrode and high-frequency electrode place in the vacuum cavity, and ground-electrode and high-frequency electrode are parallel to each other; Described heated filament places between ground-electrode and the high-frequency electrode; Have quartz window on the described vacuum chamber body wall, described double aperture slit device places a side of quartz window; Described spectrometer links to each other with the double aperture slit device through optical fiber.
The method of testing and the device thereof of light emission spectrum in the hot-wire chemical gas-phase deposition process that the present invention proposes, its advantage is:
1, the method for testing and the device thereof of light emission spectrum in the hot-wire chemical gas-phase deposition process of the present invention adopt conventional radio-frequency technique, impel the HWCVD gas phase process to produce luminous primitive, and be easy to operate, helps measuring in real time.
2, the present invention adopts conventional light emission spectrum technology to study the luminous spectrum of the HWCVD of radio-frequency drive, and data repeat reliable.
3, the method for testing and the device thereof of light emission spectrum in the hot-wire chemical gas-phase deposition process of the present invention; Be not limited to the kind of reactant gas source and the frequency of excitation power source, can be used for the research of adopting different sources of the gas and different plasma frequency to prepare the gas phase process of different materials.
Description of drawings
Fig. 1 is the structural representation of the proving installation of light emission spectrum in the hot-wire chemical gas-phase deposition process that proposes of the present invention.
Fig. 2 is the emission spectrum figure of an embodiment test of the inventive method, wherein, (a) is the light emission spectrum figure that has bias light, (b) is the bias light spectrogram, (c) is the light emission spectrum figure of background correction light.
Among Fig. 1, the 1st, vacuum cavity, the 2nd, ground-electrode, the 3rd, high-frequency electrode, the 4th, heated filament, the 5th, quartz window, the 6th, double aperture slit device, the 7th, optical fiber, the 8th, spectrometer.
Embodiment
The method of testing of light emission spectrum in the hot-wire chemical gas-phase deposition process that the present invention proposes may further comprise the steps:
(1) between the ground-electrode and high-frequency electrode of the setting parallel to each other of vacuum cavity; Place one or more heated filament; Make heated filament be parallel to two electrodes; Distance between heated filament and the ground-electrode is 3～6 centimetres, and the distance between heated filament and the high-frequency electrode is 1～3 centimetre, on the vacuum chamber body wall, quartz window is set;
(2) making the vacuum tightness in the vacuum cavity is 1 * 10
-3Handkerchief～1 * 10
-5Handkerchief makes the hot-wire temperature reach 1600～2200 ℃;
(3) mixed gas that in vacuum chamber, feeds silane and hydrogen is as reacting gas; The ratio of silane and hydrogen is: silane: hydrogen=1: 0～1: 50; The air pressure of reacting gas is 0.3～300 handkerchief, applies radio-frequency power to high-frequency electrode, makes radio-frequency power greater than 0.01 watt/centimetre
2, less than 0.1 watt/centimetre
2, between two parallel poles, produce the plasma aura;
(4) make the outgoing from the quartz window of vacuum cavity of above-mentioned plasma aura, and through a double aperture slit device, to slacken bias light;
(5) make from the aura of double aperture slit device outgoing,, obtain emission spectrum figure through optical fiber introducing light emission spectrum appearance;
(6) radio-frequency power of high-frequency electrode is reduced to 0, repeat (4) and (5), obtain the bias light spectrogram;
(7) background spectrum that deduction step (6) obtains from the spectrogram that step (5) obtains obtains hot-wire chemical gas-phase deposition emission spectrum figure.
The proving installation of light emission spectrum in the hot-wire chemical gas-phase deposition process that the present invention proposes, its structure is as shown in Figure 1, comprises vacuum cavity 1, ground-electrode 2, high-frequency electrode 3, heated filament 4, double aperture slit device and spectrometer.Ground-electrode 2 places in the vacuum cavity 1 with high-frequency electrode 3, and ground-electrode 2 is parallel to each other with high-frequency electrode 3.Heated filament 4 places between ground-electrode 2 and the high-frequency electrode 3.Have quartz window 5 on the wall of vacuum cavity 1.Double aperture slit device 6 places a side of quartz window 5.Spectrometer links to each other with the double aperture slit device through optical fiber.
According to the light reflection spectrum that the inventive method obtains, can be used to analyze each luminous primitive (Si* (254 nanometers, 288 nanometers) for example, SiH* (414 nanometer), H
β(488 nanometer), H
α(656 nanometer)) spectral intensity with the variation of deposition parameter, in conjunction with the analysis of luminous primitive rate equation, the gas phase process of understanding HWCVD plays directive function to film preparation.
The principle of the inventive method is to adopt radio frequency to excite the primitive that generates among the HWCVD, makes it luminous, studies the gas phase process of HWCVD with this.Therefore in the experimentation, guarantee that the adding of radio frequency is not influential to heater current, so heated filament will be in floating potential with respect to radio-frequency electrode; In addition, luminous except impelling primitive, radio frequency also can make decomposing gas, therefore, will guarantee in the experiment that heated filament plays a major role to the decomposition of gas, and the effect of radio frequency mainly is to produce luminous primitive.Main primitive in that can detect and silane and the hydrogen gas plasma luminous between the 200-800 nanometer, the spectral range of therefore measuring is between 200～800 nanometers.
Below introduce one embodiment of the present of invention:
(1) between the ground-electrode and high-frequency electrode of the setting parallel to each other of vacuum cavity; Place two heated filaments; Make heated filament be parallel to two electrodes; Distance between heated filament and the ground-electrode is 4.5 centimetres, and the distance between heated filament and the high-frequency electrode is 1.5 centimetres, on the vacuum chamber body wall, quartz window is arranged.
(2) making the vacuum tightness in the vacuum cavity is 1 * 10
-4Handkerchief, it is 1900 ℃ that the hot-wire temperature is reached.
(3) mixed gas that in vacuum chamber, feeds silane and hydrogen is as reacting gas; The ratio of silane and hydrogen is: silane: hydrogen=1: 2.45, and total gas flow rate 28sccm, the air pressure of reacting gas are 7.5 handkerchiefs; Apply radio-frequency power to high-frequency electrode, make that radio-frequency power is 0.05 watt/centimetre
2, between two parallel poles, produce the plasma aura.
(4) make the outgoing from the quartz window of vacuum cavity of above-mentioned plasma aura, and through a double aperture slit device, to slacken bias light; The double aperture slit device is for adopting the metal aluminium flake of 2 millimeters thick, black plastic-blasting, the rectangular box that the line cutting is combined to form then.On two opposite faces of box, a slit is arranged respectively, slit length is 2 centimetres, and width is 0.5 millimeter, and 10 centimetres at the interval of two slits is parallel to each other, shown in 6 among Fig. 1.
(5) make from the aura of double aperture slit device outgoing; Introduce light emission spectrum appearance (monochromator (Micro HR) and the charge-coupled device (Synapsa TM CCD) produced by French Horiba Jobin Yvon constitute) through optical fiber; Obtain emission spectrum figure; Spectral range is between 200～800 nanometers, shown in Fig. 2 (a).Can tell SiH* (414nm) in this spectrum, H
α(656nm) luminous, but because bias light is very strong, luminous being difficult to of other primitives told.
(6) radio-frequency power of high-frequency electrode is reduced to 0, repeat (4) and (5), obtain not having the bias light spectrogram of luminescence of plasma, spectral range is between 200～800 nanometers, shown in Fig. 2 (b).
(7) background spectrum that deduction step (6) obtains from the spectrogram that step (5) obtains obtains hot-wire chemical gas-phase deposition emission spectrum figure, and spectral range is between 200～800 nanometers, shown in Fig. 2 (c).In Fig. 2 (c), can see the luminous signal of following luminous primitive: Si* (254 nanometer), Si* (288 nanometer), SiH* (414 nanometer), H
α(656 nanometer), H
β(486 nanometer) and H
2(570-640 nanometer).
(8) change experiment condition; Repeating step (5)-(7); Can obtain of the variation of each luminous signal along with experiment parameter (for example deposition pressure, gas flow, silane and hydrogen ratio etc.); And compare with the performance of film of preparation under the same conditions, analyze gas phase process, instruct the preparation of high-quality thin-film.
More than concrete parameter be to illustrate and realize object lesson of the present invention, can not be in order to limit the protection domain that this claim is confirmed.
Claims (2)
1. the method for testing of light emission spectrum in the hot-wire chemical gas-phase deposition process is characterized in that this method of testing may further comprise the steps:
(1) between the ground-electrode and high-frequency electrode of the setting parallel to each other of vacuum cavity; Place one or more heated filament; Make heated filament be parallel to two electrodes; Distance between heated filament and the ground-electrode is 3～6 centimetres, and the distance between heated filament and the high-frequency electrode is 1～3 centimetre, on the vacuum chamber body wall, quartz window is set;
(2) making the vacuum tightness in the vacuum cavity is 1 * 10
-3Handkerchief～1 * 10
-5Handkerchief makes the hot-wire temperature reach 1600～2200 ℃;
(3) mixed gas that in vacuum chamber, feeds silane and hydrogen is as reacting gas; The ratio of silane and hydrogen is: silane: hydrogen=1: 0～1: 50; The air pressure of reacting gas is 0.3～300 handkerchief, applies radio-frequency power to high-frequency electrode, makes radio-frequency power greater than 0.01 watt/centimetre
2, less than 0.1 watt/centimetre
2, between two parallel poles, produce the plasma aura;
(4) make the outgoing from the quartz window of vacuum cavity of above-mentioned plasma aura, and through a double aperture slit device, to slacken bias light;
(5) make from the aura of double aperture slit device outgoing,, obtain emission spectrum figure through optical fiber introducing light emission spectrum appearance;
(6) radio-frequency power of high-frequency electrode is reduced to 0, repeat (4) and (5), obtain the bias light spectrogram;
(7) background spectrum that deduction step (6) obtains from the spectrogram that step (5) obtains obtains hot-wire chemical gas-phase deposition emission spectrum figure.
2. the proving installation of light emission spectrum in the hot-wire chemical gas-phase deposition process is characterized in that this device comprises vacuum cavity, ground-electrode, high-frequency electrode, heated filament, double aperture slit device and spectrometer; Described ground-electrode and high-frequency electrode place in the vacuum cavity, and ground-electrode and high-frequency electrode are parallel to each other; Described heated filament places between ground-electrode and the high-frequency electrode; Have quartz window on the described vacuum chamber body wall, described double aperture slit device places a side of quartz window; Described spectrometer links to each other with the double aperture slit device through optical fiber.
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| CN103635004A (en) * | 2013-12-13 | 2014-03-12 | 南开大学 | Method for measuring ion species and number density distribution of plasma |
| CN105744711A (en) * | 2016-04-15 | 2016-07-06 | 中国人民解放军装甲兵工程学院 | Thermal ionization plasma generation test device and density test and control methods |
| CN105744712A (en) * | 2016-04-15 | 2016-07-06 | 中国人民解放军装甲兵工程学院 | Closed bomb vessel for plasma diagnosis and density control method thereof |
| CN108982378A (en) * | 2018-07-31 | 2018-12-11 | 浙江大学 | Plasma components spatial distribution method for real-time measurement and its device based on light spectrum image-forming |
| CN109207948A (en) * | 2018-09-30 | 2019-01-15 | 大连理工大学 | A method of for reaction magnetocontrol sputtering Detection of Stability and control |
| CN112746259A (en) * | 2020-12-30 | 2021-05-04 | 尚越光电科技股份有限公司 | Method for controlling content of magnetron sputtering coating impurities through plasma glow spectrum |
| CN115466939A (en) * | 2022-10-10 | 2022-12-13 | 中国科学院上海微系统与信息技术研究所 | Light modulation chemical vapor deposition device and method for modulating film growth temperature by using same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102809553A (en) * | 2012-08-04 | 2012-12-05 | 重庆特瑞尔分析仪器有限公司 | Multi-gas concentration qualitative quantitative measuring device and measuring method thereof |
| CN103635004A (en) * | 2013-12-13 | 2014-03-12 | 南开大学 | Method for measuring ion species and number density distribution of plasma |
| CN105744711A (en) * | 2016-04-15 | 2016-07-06 | 中国人民解放军装甲兵工程学院 | Thermal ionization plasma generation test device and density test and control methods |
| CN105744712A (en) * | 2016-04-15 | 2016-07-06 | 中国人民解放军装甲兵工程学院 | Closed bomb vessel for plasma diagnosis and density control method thereof |
| CN105744711B (en) * | 2016-04-15 | 2018-01-23 | 中国人民解放军装甲兵工程学院 | A kind of thermal ionization plasma generation test device and its density measurement and control method |
| CN105744712B (en) * | 2016-04-15 | 2019-04-09 | 中国人民解放军装甲兵工程学院 | A kind of closed bomb vessel and its density control method for plasma diagnostics |
| CN108982378A (en) * | 2018-07-31 | 2018-12-11 | 浙江大学 | Plasma components spatial distribution method for real-time measurement and its device based on light spectrum image-forming |
| CN109207948A (en) * | 2018-09-30 | 2019-01-15 | 大连理工大学 | A method of for reaction magnetocontrol sputtering Detection of Stability and control |
| CN112746259A (en) * | 2020-12-30 | 2021-05-04 | 尚越光电科技股份有限公司 | Method for controlling content of magnetron sputtering coating impurities through plasma glow spectrum |
| CN115466939A (en) * | 2022-10-10 | 2022-12-13 | 中国科学院上海微系统与信息技术研究所 | Light modulation chemical vapor deposition device and method for modulating film growth temperature by using same |
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Application publication date: 20120502 |