CN1800830A - Spectrum detection method for instructing plasma assisted semiconductor material preparation - Google Patents
Spectrum detection method for instructing plasma assisted semiconductor material preparation Download PDFInfo
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- CN1800830A CN1800830A CN 200510016509 CN200510016509A CN1800830A CN 1800830 A CN1800830 A CN 1800830A CN 200510016509 CN200510016509 CN 200510016509 CN 200510016509 A CN200510016509 A CN 200510016509A CN 1800830 A CN1800830 A CN 1800830A
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Abstract
The invention relates to a method to determine plasma component with spectral detection technique and guide plasma assist device to dope semiconductor material. Wherein, measuring the RF plasma emission spectrum with spectrograph, analyzing chemical component of plasma; adjusting gas source flow to change pressure of growth chamber, adjusting RF power to boost the benefit component increasing and reduce bad effect from other component; selecting optimal experiment condition to prepare the N-doped P-type ZnO. This invention can learn and control the chemical component real time, improves material repeatability, and takes an important step forwardly to realize ZnO-base luminescent device.
Description
Technical field
The invention belongs to technical field of semiconductor, relate to and utilize the spectrographic detection technology to determine that plasma components instructs the method for plasma Assisted Preparation doped semiconductor materials.
Background technology
Over past ten years,, become a focus of semiconductor laser device research in the message area because short wavelength laser diode (LD), laser instrument and related device thereof have higher storage density and read or write speed faster.ZnO is the semiconductor material with wide forbidden band of direct band gap, energy gap is 3.37eV under the room temperature, and exciton bind energy is up to 60meV, hot ionization energy 26meV is a lot of greatly than room temperature, that is to say that exciton can not be ionized yet under room temperature or higher temperature, realize high efficiency Laser emission therefore easilier in room temperature.At present, the research work of zno-based light emitting diode and laser instrument such as p type ZnO, the preparation of ZnO p-n junction and characteristic research still are in the junior stage.Owing to there is stronger self compensation mechanism in the ZnO film, make to be difficult to obtain the carrier concentration height, resistivity is low, and the p type ZnO material of good reproducibility becomes the difficult point and the focus of present research work.
A lot of seminar both domestic and external has carried out number of research projects to it, employed doped source is mainly I family and V group element, wherein the nitrogen element is very desirable adulterant, and its ionic radius and oxonium ion radius are more or less the same, and the replace oxygen case can form effective single acceptor level.Last century the nineties, in the research of II-IV ZnSe material, the nitrogen that utilizes plasma to activate of success has prepared p type ZnSe, and has prepared the LD of ZnSe base, LED based on this.So in the research of ZnO, nitrogen still is to receive much concern and most promising doped chemical, a lot of in the world seminar have carried out a large amount of work (Appl.Phys.Lett.Vol 81 (2002) 1830-1832, Journal of CrystalGrowth 209 (2001) 526-531).But the result is unsatisfactory, has difficulty transition, the problem of repeatable difference.
The molecular beam epitaxy (P-MBE) that plasma is auxiliary in experimentation, utilizes radio frequency plasma to activate the required gas source of growth, provides effective IV family and doped chemical to prepare p type ZnO.In the process of carrying out p type doped growing, can use N
2Or NO provides N element.With N
2Or in the NO feeding plasma, activate, it is decomposed, the N atom of formation can substitute the O case in intrinsic ZnO, form to be subjected to major defects.But for N
2, its ionization energy is higher, and the chemical constitution in the plasma is complicated, and N is arranged
2Decompose the N atom that the back forms, the N molecule of activated state, the N of activated state
2Ion, electronics etc.For NO, in plasma, be decomposed to form N atom and O atom, be combined into N after the N atom is collided simultaneously
2, N
2Be difficult to decompose, so have the N atom in the NO plasma, the N molecule of activated state, the N of activated state
2Ion, O atom, electronics etc.N
2Substitute the O case in ZnO, can form two alms giver's defectives, the P type is mixed compensates (Phys.Rev.Lett.86,5723 (2001)), is the unfavorable factor of doped growing, and therefore isoionic chemical composition is the important parameter of experiment.
Summary of the invention
The present invention utilizes the light emission spectrum of spectrum detection technique article on plasma to monitor in real time, analyzes the chemical composition of plasma, and purpose provides a kind of optical spectrum detecting method that instructs plasma assisted semiconductor material preparation.
The present invention instructs plasma assisting growth semiconductor material by obtaining isoionic light emission spectrum.
For realizing above-mentioned target, the present invention advances multimode optical fiber with the optically-coupled of radio frequency plasma emission and draws, and utilizes its spectrum of spectrometer measurement.From spectrogram, can observe the O atom (777.4,843nm), the N atom (744.2,746.8,821,869nm), N
2(337.1,380.5,580.4nm), N
2* (357.6nm), N
2 +(391.4, glow peak 427.8nm).When carrying out the growth of p type ZnO, the O atom in the plasma, N atom are effective constituent, and growth has adverse effect to all the other compositions to material.
The ion trap trap that the present invention is derived from band by radio frequency plasma is realized separating of neutral molecule or atom and charged particle.Then need to improve the ionization level of gas for the N of molecular state, make it to be converted into atomic form.After adopting the spectrographic detection technology, can reflection spectral component very directly perceived, obtain the corresponding relation of plasma components and each experiment condition, improve the controllability and the repeatability of testing.Practice shows, reduces gas flow, improves growth room's vacuum tightness, increases radio-frequency power and helps to improve the gas ionization level.
For understanding the present invention better, be described in detail operating process.
When the growing P-type semiconductor, cleaned Sapphire Substrate is fixed on indium in the molybdenum holder of the auxiliary molecular beam epitaxy of plasma, move into pretreatment chamber, utilize mechanical pump, molecular pump and ionic pump that pretreatment chamber's vacuum tightness is evacuated to 10
-7Below the mbar, underlayer temperature is raised to 800 ℃, degass 30-40 minute.The molybdenum holder is moved into the growth room, close ionic pump, utilize mechanical pump, molecular pump to keep growth room's vacuum.By flowmeter and leakage valve gas flow is controlled.Gas is fed the radio frequency plasma source generator, increase plasma source power, the gas build-up of luminance also reaches highlighted pattern.
Because the light-emitting window of radio frequency plasma rifle is not a horizontal positioned, be the simplification optical system for testing, and get rid of the influence of veiling glare in the laboratory that the light that the present invention launches plasma quartz glass lens focus is drawn by φ 0.9mm silica fibre.Adopting quartz material mainly is to cause the spectrum distortion for the signal of avoiding ultraviolet band is partially absorbed.Adopt dual grating light spectrometer measuring light emission spectrum, and analyze the component of plasma according to the relative intensity of the characteristic spectral line of various molecules (or atom).Can change the ionization level of gas by adjustments of gas flow, growth room's vacuum tightness and plasma source power, make it to reach the required condition of experiment.With purity be 99.9999% Metal Zn as electron gun, the Zn source temperature is 245 ℃, opens the ion trap trap, opens Zn source shutter, growth ZnO.
The present invention can understand the also chemical composition of regulating and controlling plasma in real time by the light emission spectrum of spectrometer measurement plasma, and especially the quality and the controllability of doped growing have vital role to improving plasma assisting growth semiconductor material.
Embodiment
Embodiment 1, utilizes oxygen, nitrogen mixture to be growth source and doped source growth N doped p type ZnO
Before the growth, growth room's vacuum is evacuated to 5 * 10
-8Below the mbar.With the c-Al that disposes
2O
3(0001) the substrate specimen holder of packing into is increased to 450 ℃ with growth temperature, and the Zn source temperature rises to 245 ℃, and this moment, Zn source line was 5 * 10
-5Mbar.With oxygen, by flowmeter control, the control oxygen flow is 0.30sccm to the flow of nitrogen respectively, and nitrogen flow is 0.15sccm, and this moment, growth room's vacuum tightness was 6 * 10
-6Mbar.Regulate radio frequency plasma source generator power, power setting is 300W, and this moment, the gas ionization level was high and stable, was optimal experimental conditions.Through growth in 2 hours, prepare p type ZnO film.ZnO film is measured through X-ray diffraction, show and grow the measured ZnO film of crystalline on the Sapphire Substrate, the Hall measuring instrument of use Lakeshore company utilizes the electrical properties of vanderburg method measuring samples, and the resistivity that obtains sample is 6 Ω cm, and carrier concentration is 10
18Cm
-3, mobility is 1cm
2/ Vs.
In growth course,, determine growth conditions thus with the chemical composition of spectrophotometer plasma.Used kaleidophon is equipped with the C31034 type photomultiplier that the Radio Corporation of America (CRA) makes, and carries semiconductor refrigeration system and can improve signal to noise ratio (S/N ratio), gets rid of noise effect.
Embodiment 2, utilize nitric oxide gas that growth source and doped source growth N doped p type ZnO are provided
Selecting the nitrogen monoxide flow is 0.40sccm, and substrate is c-Al
2O
3And, regulate experiment condition at any time (0001), according to results of spectral measurements.By results of spectral measurements, determine that growth room's pressure is 6 * 10
-6Mbar, radio-frequency power are 300W, and growth temperature is 450 ℃, 245 ℃ of Zn source temperatures, and Zn source line is 5 * 10
-5Mbar.Through growth in 2 hours, obtain p type ZnO film sample.The electrical properties of measuring samples, resistivity are 0.8 Ω cm, and carrier concentration is 2 * 10
18Cm
-3, mobility is 5cm
2/ Vs.
Find that by embodiments of the invention 2 the nitrogen monoxide ionization level will be higher than the ionization level of oxygen, nitrogen mixture.
Claims (3)
1, a kind of optical spectrum detecting method that instructs plasma assisted semiconductor material preparation is characterized in that adopting following concrete steps:
When a) growing cleaned Sapphire Substrate is fixed in the molybdenum holder with indium, is placed on the specimen holder, utilize mechanical pump, molecular pump and ionic pump that end vacuum is carried on the back by the growth room and be extracted into 10
-7Below the mbar, make underlayer temperature be raised to 800 ℃, degassed 30 minutes;
B) with purity be the nitrogen of 99.9999% Metal Zn, 99.999% oxygen and 99.9999% or 99.99% nitrogen monoxide as source material, the Zn source temperature is 245 ℃, Zn source line is 5 * 10
-5Mbar takes into account Lou valve control with gas source by flow and enters the radio frequency plasma source generator, increases plasma source power, and the gas build-up of luminance also reaches highlighted pattern;
C) light that plasma is launched is drawn by optical fiber, uses the spectrometer measurement light emission spectrum, analyzes its component; Ionization level by adjustments of gas flow, growth room's vacuum tightness and plasma source power change gas makes it to reach the required condition of experiment;
D) open the ion trap trap, open plasma source and Zn source shutter are grown; Monitor the plasma component in the growth course in real time, keep the stability of experiment condition.
2, the optical spectrum detecting method that instructs plasma assisted semiconductor material preparation according to claim 1, it is characterized in that the light that plasma is launched quartz glass lens focus, draw by φ 0.9mm silica fibre, with dual grating light spectrometer measuring light emission spectrum.
3, the optical spectrum detecting method that instructs plasma assisted semiconductor material preparation according to claim 1 and 2, the power setting that it is characterized in that the radio frequency plasma source generator is 300W.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101413115B (en) * | 2007-10-19 | 2010-08-25 | 财团法人工业技术研究院 | Method for plasma assisted film deposition |
| CN110470611A (en) * | 2019-07-10 | 2019-11-19 | 中国科学院上海技术物理研究所 | A kind of on-line measuring device and method of gaN series film growth conditions |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0964074A3 (en) * | 1998-05-13 | 2001-02-07 | Axcelis Technologies, Inc. | Ion implantation control using optical emission spectroscopy |
| US6632747B2 (en) * | 2001-06-20 | 2003-10-14 | Texas Instruments Incorporated | Method of ammonia annealing of ultra-thin silicon dioxide layers for uniform nitrogen profile |
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2005
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101413115B (en) * | 2007-10-19 | 2010-08-25 | 财团法人工业技术研究院 | Method for plasma assisted film deposition |
| CN110470611A (en) * | 2019-07-10 | 2019-11-19 | 中国科学院上海技术物理研究所 | A kind of on-line measuring device and method of gaN series film growth conditions |
| CN110470611B (en) * | 2019-07-10 | 2022-08-16 | 中国科学院上海技术物理研究所 | On-line detection device and method for growth conditions of GaN-based thin film |
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| CN100405045C (en) | 2008-07-23 |
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