CN110470611A - A kind of on-line measuring device and method of gaN series film growth conditions - Google Patents
A kind of on-line measuring device and method of gaN series film growth conditions Download PDFInfo
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Abstract
The invention discloses the on-line measuring devices and method of a kind of gaN series film growth conditions, pass through contactless reflection spectrometry, gaN series semiconductive thin film can be obtained online at high temperature influences the parameter of Material growth, realizes the real time monitoring and film quality detection of process conditions during Material growth.The method can on-line real-time measuremen multiple parameters.The invention discloses a kind of devices for realizing this method, comprising: introduces quartzy optical waveguide in the reaction chamber window of growth gaN series thin-film material, light shines on sample and by signal collection into spectrometer;Nitrogen is passed through around quartzy optical waveguide to be contaminated to protect optical waveguide end face not deposit upper film material;It is light-blocking that graphite plate pedestal is placed between the substrate for growing film and heating furnace below, to prevent the luminous influence to reflectance spectrum test result of heating furnace.
Description
Technical field
The present invention relates to GaN system films under semiconductor material growing, solid-state spectroscopy field, in particular to a kind of high temperature
The online test method and device of growth conditions.
Technical background
As a kind of semiconductor material with wide forbidden band, the research and application of gaN series material are the forward positions of current semiconductor field
And hot spot.As microelectronics, the important novel semiconductor material in optoelectronic device applications field, GaN material and SiC, diamond
Equal semiconductors are known as third generation semiconductor material together.It has stronger valence link polarity and intensity, high thermal conductivity, high
Many excellent performances such as breakdown voltage, stable chemical property and strong capability of resistance to radiation, be develop high frequency field effect transistor,
High electron mobility transistor, high-power pulsed ion beams and the weight from visible ultraviolet band light emitting devices and sensitive detection parts
Want material.
GaN material series is a kind of ideal short-wave long light-emitting device material, and the band gap of GaN and its alloy is covered from red
Color is to ultraviolet spectral region.After Japan in 1991 develops homojunction GaN blue led, InGaN/AlGaN is bis- different
Matter knot ultra-brightness blue led, InGaN single quantum well GaN LED come out one after another.Currently, single quantum well GaN blue and green
LED has entered the mass production stage, to fill up the blank of blue led many years in the market.Blue luminescent device is highly dense
Information Access, the full light of degree CD are shown, there is huge application market in the fields such as laser printer.With to III group-III nitride
What material and device research and development worked deepens continuously, and InGaN hypervelocity blue and green light LED technology has been carried out commodity
Change, all investment huge fund is added to the competition ranks of exploitation blue-ray LED one after another for each major company, the present world and research institution.
The preparation method that gaN series material generallys use has conventional MOCVD (including APMOCVD, LPMOCVD), plasma
Enhance MOCVD (PE-MOCVD) and electron cyclotron resonace auxiliary MBE etc..Usual mocvd method growth gaN series material is in high temperature
Under, pass through the TMGa Ga decomposited and NH3Chemical reaction realize.Temperature be one of Material growth in MOCVD system extremely
Close important influence factor.Too high or too low for temperature, speed, length of soaking time of heating cooling rate etc. can all be influenced into
Film quality.Growth temperature is high, makes the kinetic energy of adatom with increase, and the probability across surface potential barrier increases, and is easy crystallization,
And reduce film defects, but it is excessively high when can reduce the purity of cubic phase.Growth temperature is low, then easily forms the thin of indefiniteness structure
Film.It grows in gaN series materials process, the working range of temperature is larger, and constant interval is 30~1100 DEG C.It to be in time each
Growth phase selects suitable growth temperature.And the speed of growth rate to crystalline property, defect and surface roughness all
There is larger impact.Constituent content can then significantly affect the forbidden bandwidth and photoelectric properties of gaN series semiconductive thin film.Thus grow temperature
Degree, growth rate and Ga1-xYxThe online Fast Calibration of N material Y constituent content x value to the growth course of GaN series thin film and
Quality monitoring important in inhibiting.
Optical means is as a kind of lossless, quick, convenient, detection means that can be online, in thin-film material growth monitoring
It is widely used.But common practice only detects film growth rate or thickness with laser interference or spectrum.And
In thin film growth process other than this parameter of growth rate, growth temperature and the two factors of component influence the performance of material
It is bigger.The practical growth temperature (and temperature in nonambient environment) and component that material itself is how effectively monitored online contain
Amount is a difficult problem.Currently used thermometry has glass liquid thermometer, resistance thermometer, thermocouple
Contact thermography, infrared radiation temperature, fibre optic temperature sensor etc..Although there is numerous temperature measuring devices, technically very at
It is ripe, but it is function-specific, growth rate and component can not be measured simultaneously, and can only use mostly in traditional occasion, be but difficult to
Solve the temperature detection problems under certain specific demands and specific environment.
Though the technological means of existing monitoring film growth at present, such as Shanghai Inst. of Technical Physics, Chinese Academy of Sciences Wang Shanli
Et al. propose with ellipsometry and infrared radiation temperature technical monitoring HgCdTe growth key parameter method, but it is ellipse partially
Method has specific requirement, measurement and calculating ratio since the uniformity requirement to film thickness is relatively high, to incidence and the angle of reflection of detection light
It is more complex, (see " Wang Shanli, in the real-time monitoring research of the molecular beam epitaxy HgCdTe Material growth parameter such as Mei Fang it is infrared with
Millimeter wave journal [J] .1998,17 (4): 287-291. "), the monitoring technology of gaN series film growth conditions is had not been reported.
Summary of the invention
The present invention proposes that the on-line measuring device of gaN series film growth conditions, in particular to one kind are based under a kind of high temperature
Reflectance spectrum monitors growth temperature, growth rate and the Ga of gaN series material at high temperature on-line simultaneously1-xYxN material Y component contains
Measure this three big method and device thereof for influencing Material growth condition of x value.
The method of the present invention is to utilize reflected spectrum interference peak principle relevant to film thickness, at any time by interference peaks
Change the growth rate to determine film;Using the forbidden bandwidth of semiconductor principle relevant to temperature, obtained by gaN series material
The variation of its forbidden bandwidth out is established thin in gaN series according to the functional relation between the forbidden bandwidth and temperature of gaN series material
The forbidden band of gaN series film growth temperature, material Y constituent content x value and real-time growth material in film growth temperature fluctuation range
Normalized optical constant data library between width.Go out Ga by computation of table lookup1-xYxThe real time temperature and Ga of N Material growth1-xYxN
The Y constituent content x value of material.Reference spectra is compared simultaneously, the calibration error of test macro is eliminated, so that growth rate, growth
Temperature measurement accuracy is higher.
Specific method the following steps are included:
(1) respectively to interference peaks in gaN series material reflectance spectrum with the variation relation of film thickness, ABSORPTION EDGE with temperature
Variation relation, forbidden bandwidth are with Ga1-xYxThe variation relation of N material Y constituent content x value carries out experiment test and fitting, obtains pair
Thus the functional relation answered establishes gaN series film growth temperature in gaN series film growth temperature fluctuation range, Ga1- xYxNormalized optical constant data library between N material Y constituent content x value and the forbidden bandwidth of real-time growth material.
Establish the database method particularly includes: 1 μm of thickness is chosen under the 773K (500 degrees Celsius) demarcated in advance
The reflectance spectrum of gaN series film is as reference spectra, so that the calibration error of test macro is eliminated, so that growth rate, growth
Temperature measurement accuracy is higher;By the difference of reflectance spectrum and this reference spectra ABSORPTION EDGE during measurement Material growth, obtain
The difference of forbidden bandwidth and reference thin film forbidden bandwidth in growth course, the letter varied with temperature using gaN series film forbidden band width
Number relational expression calculates Current Temperatures and the difference of 773K, to obtain current growth temperature;For gaN series multi-element compounds material
Material, including InGaN, AlGaN and AlInGaN choose the InGaN of the In content 0.1 demarcated in advance, Al content 0.1 respectively
AlGaN, In and Al content are respectively the reflectance spectrum of 0.1 AlInGaN respectively as reference spectra, using reflecting in growth course
The difference of spectrum and reference spectra obtains the difference of forbidden bandwidth and reference thin film forbidden bandwidth in growth course, according to
The forbidden bandwidth and Ga of InGaN, AlGaN and AlInGaN1-xYxFunctional relation between N material Y constituent content x value obtains current
Difference between growth material and reference material is to obtain the Ga of current growth material1-xYxN material Y constituent content x value.
(2) the anti-of the GaN system thin-film material of 1 μ m-thick of thickness under 773K (500 degrees Celsius, other temperature can also with) is chosen
Penetrating spectrum is reference spectra, is calibrated by functional relation obtained in step 1 spectral measurement system, to eliminate test
The error of system;
(3) on-line measurement obtains the real-time reflectance spectrum in thin film growth process;
(4) the real-time reflectance spectrum that will acquire is transmitted directly to computer, calculates spectral interference peak by data processing
Amount of movement and material forbidden bandwidth and forbidden bandwidth variable quantity.
(5) be fitted to obtain the thickness of film in growth course by reflectance spectrum during Material growth, by film thickness with
The variation of film growth time obtains film growth rate;
(6) it by the difference of reference spectra ABSORPTION EDGE in reflectance spectrum during Material growth and step 2, was grown
The difference of forbidden bandwidth and reference thin film forbidden bandwidth in journey, the functional relation varied with temperature using gaN series film forbidden band width
Formula calculates Current Temperatures and the difference of 773K, to obtain current growth temperature;For gaN series multi-element compounds material, packet
Include InGaN, AlGaN and AlInGaN, choose respectively the InGaN of In content 0.1, Al content 0.1 that have demarcated in advance AlGaN,
In and Al content are respectively the reflectance spectrum of 0.1 AlInGaN respectively as reference spectra, using reflectance spectrum in growth course with
The difference of reference spectra obtains the difference of forbidden bandwidth and reference thin film forbidden bandwidth in growth course, according to InGaN, AlGaN
With the forbidden bandwidth and Ga of AlInGaN1-xYxFunctional relation between N material Y constituent content x value calculates current growth material
Compositional difference between reference material obtains current Ga1-xYxThe Y constituent content x value of N material.Thus it can establish thin in gaN series
GaN series film growth temperature in film growth temperature fluctuation range, Ga1-xYxN material Y constituent content x value and real-time growth material
Forbidden bandwidth between normalized optical constant data library.
(7) in gaN series thin-film material growth course, the ABSORPTION EDGE of material is determined by reflectance spectrum, then passes through ABSORPTION EDGE
Calculate its forbidden bandwidth;Normalized optical constant library by inquiring gaN series material obtains arrives Material growth temperature in real time, can be used for
Instruct the adjusting and control of film growth temperature.
(8) in gaN series thin-film material growth course, the ABSORPTION EDGE of material is determined by reflectance spectrum, then passes through ABSORPTION EDGE
Calculate its forbidden bandwidth;Normalized optical constant library by inquiring gaN series material obtains the content x value of the Y component of material.
The method of the present invention also proposes a kind of device for realizing above method, specifically includes:
Quartzy optical waveguide 3 is introduced in the window of the MOCVD reaction chamber 5 of growth gaN series thin-film material, by itself and reaction chamber
It is closed between cavity wall;Quartzy 3 outer end of optical waveguide is connect by optical fiber 2 with spectrometer 1;It is nitrogen around quartz optical waveguide 3
Feed channel 4, being passed through the inert gases such as nitrogen in test process is influenced with protecting optical waveguide end face not by deposition reaction;Substrate 8
It is light-blocking to prevent the luminous influence to reflectance spectrum test result of heating furnace that graphite plate pedestal is placed between heating furnace 10;Reaction
Gas 6 deposits gaN series film grown layer 7 on substrate 8.
After above-mentioned technical proposal and device, the invention has the following advantages that
(1) this method is composed using contactless optical reflection, is had the advantages that lossless, quick, real-time;
(2) this method can obtain actual temperature, growth rate and the Ga during Material growth simultaneously1-xYxN material Y
This three big key condition for influencing Material growth of constituent content x value, it is ensured that the real time monitoring of process conditions during Material growth;
(3) this method and its device are simple and easy to do, low in cost, good reliability and can carry out Fast Calibration;
(4) it is not limited to gaN series column semiconductor material, the method for the present invention is pervasive partly to be led in on-line real time monitoring calibration is various
Growth rate, growth temperature and Ga during body Material growth1-xYxN material Y constituent content x value, is especially suitable for various semiconductors
The commercial production conditions of material monitor.
Detailed description of the invention
Attached drawing 1 is a kind of on-line measuring device of gaN series film growth conditions, in which:
1 is spectrometer;
2 be spectrometer optical fiber;
3 quartzy optical waveguides;
4 be nitrogen and its pipeline, to protect quartzy optical waveguide end face not influenced by reaction gas;
5 be MOCVD reaction chamber cavity wall;
6 be reaction gas;
7 be gaN series film grown layer;
8 be substrate;
9 be graphite plate pedestal;
10 be heating furnace.
Attached drawing 2 is the reflectance spectrum of the GaN material of experiment measurement at different temperatures, it can be seen that with the liter of temperature
Apparent red shift has occurred in height, ABSORPTION EDGE.
Attached drawing 3 is the forbidden bandwidth variation with temperature relationship obtained by experiment measurement GaN material reflectance spectrum.
Attached drawing 4 is the reference light spectrogram for having demarcated the reflectance spectrum of 1 μm of thickness of GaN film under 773K (500 degrees Celsius)
And the real-time reflectance spectrum figure measured after growth 5min.
Attached drawing 5 is the film reflector spectrogram measured in real time.
The Al that attached drawing 6 is 1 μm of thickness under the 773K (500 degrees Celsius) demarcated0.1Ga0.9The reflectance spectrum figure of N thin film and
The reflectance spectrum figure surveyed at 773K.
Attached drawing 7 is the Al being fitted by the reflectance spectrum of experiment measurementxGa1-xThe relationship that N forbidden bandwidth changes with x value
Figure.
Specific embodiment
For the contents of the present invention, technical solution and advantage is more clearly understood, below in conjunction with attached drawing 1 and attached drawing 2, respectively
GaN and Al is prepared with mocvd method in LED manufacturing processxGa1-xFor N material, a specific embodiment of the invention is made detailed
Explanation.These embodiments are merely to illustrate the present invention, but the present invention is not limited only to following embodiment.
Embodiment 1:
Firstly, respectively to interference peaks in GaN film reflectance spectrum with the mobile relationship of film thickness, ABSORPTION EDGE with temperature
Variation relation carries out theoretical calculation and experimental fit, obtains corresponding functional relation.
Attached drawing 2 is that the reflectance spectrum of the GaN material of measurement at different temperatures is tested in vacuum environment.It can be seen that
Apparent red shift has occurred in (290K-823K) as the temperature rises, ABSORPTION EDGE.The absorption of material is searched out by reflectance spectrum
Side, then its forbidden bandwidth is calculated by ABSORPTION EDGE, so that fitting obtains the relationship that GaN material forbidden bandwidth varies with temperature
Formula.By the measurement to interference peak position and its amount of movement under different film thicknesses, digital simulation obtains the thickness of film and does
The relational expression between peak position is related to, the optical constant under each growth temperature is obtained, establishes standard database.
Attached drawing 3 is the relationship that the GaN forbidden bandwidth obtained by the reflectance spectrum of experiment measurement varies with temperature.By to this
It is as follows that relationship progress linear fit obtains forbidden bandwidth variation with temperature relational expression:
Eg(eV)=3.56637-6.70071 × 10-4T(K)
Secondly, build such as the reflective spectral measure system in attached drawing 1, and according to functional relation obtained in the previous step to being
System is calibrated.Introduce quartzy optical waveguide in the MOCVD reaction chamber window of growth GaN, by its between reaction chamber cavity wall it is closed,
Quartzy optical waveguide lumen outer end is connected on spectrometer.Intracavitary optical waveguide end face is set to be parallel to the lining of epitaxial growth GaN material
Reflected light signal is coupled into waveguide to greatest extent to improve the signal-to-noise ratio of measure spectrum by bottom.Lead to around optical waveguide
Entering nitrogen is influenced with protecting optical waveguide end face not by deposition reaction.
Such as 4 solid line of attached drawing, the reflectance spectrum for having demarcated 1 μm of thickness of GaN film under 773K (500 degrees Celsius) is reference light
Spectrum.During Material growth, the reflectance spectrum of on-line measurement GaN film.
4 dotted line of attached drawing is to grow the real-time reflectance spectrum measured after 5min, is transmitted directly to computer, passes through fitting
Obtain growing film with a thickness of 1150nm, growth rate 0.5nm/s.
By the difference of reflectance spectrum during Material growth and reference spectra ABSORPTION EDGE, it is wide to obtain forbidden band in growth course
The difference of degree and reference thin film forbidden bandwidth: attached drawing 5 is that the film reflector measured in real time is composed, forbidden bandwidth 3.0544eV,
Go out the difference of forbidden bandwidth under Current Temperatures and 773K using the functional relation the Fitting Calculation that GaN film forbidden band width varies with temperature
Different is 0.006eV, by tabling look-up to obtain current growth temperature to be 768K.
Embodiment 2:
Firstly, respectively to AlxGa1-xIn N thin film reflectance spectrum interference peaks with the mobile relationship of film thickness, ABSORPTION EDGE with
The variation relation of temperature, forbidden bandwidth carry out theoretical calculation and experimental fit with the variation relation of Al component, obtain corresponding letter
Number relational expression.AlxGa1-xN thin film forbidden bandwidth is as follows with the variation relation of component:
Eg(x)=(1-x) Eg(GaN)-xEg(AlN)-bx(1-x)
Wherein, b=1eV, Eg(GaN)=3.5eV, Eg(AlN)=6.1eV
Secondly, build such as the reflective spectral measure system in attached drawing 1, and according to functional relation obtained in the previous step to being
System is calibrated.In growth AlxGa1-xThe MOCVD reaction chamber window of N introduces quartzy optical waveguide, by it between reaction chamber cavity wall
Closed, quartzy optical waveguide lumen outer end is connected on spectrometer.Intracavitary optical waveguide end face is set to be parallel to epitaxial growth AlxGa1- xReflected light signal is coupled into waveguide to greatest extent to improve the signal-to-noise ratio of measure spectrum by the substrate of N material.Around light wave
Surrounding catheter, which is passed through nitrogen, to be influenced with protecting optical waveguide end face not by deposition reaction.
The Al that 6 solid line of attached drawing is 1 μm of thickness under the 773K (500 degrees Celsius) demarcated0.1Ga0.9The reflectance spectrum of N thin film,
It is as reference spectra, forbidden bandwidth 3.45eV.During Material growth, on-line measurement AlxGa1-xThe reflected light of N thin film
Spectrum.
Attached drawing 7 is the Al being fitted by the reflectance spectrum of experiment measurementxGa1-xThe relationship that N forbidden bandwidth changes with x value.
6 dotted line of attached drawing is to survey reflectance spectrum at 773K, and the real-time reflectance spectrum that will acquire is transmitted directly to computer, calculates its taboo
Bandwidth is 2.638eV, utilizes AlxGa1-xIt is wide that N thin film component x value with the functional relation of forbidden bandwidth calculates current forbidden band
The difference of degree and calibration forbidden bandwidth 2.45eV are 0.188eV, table look-up to obtain current x value to be 0.082.
Claims (6)
1. a kind of on-line measuring device of gaN series film growth conditions, device includes spectrometer (1), optical fiber (2), quartzy light
Waveguide (3), nitrogen pipeline (4), reaction chamber (5), reaction gas (6), gaN series film grown layer (7), substrate (8), graphite plate
Pedestal (9), heating furnace (10).Its method characteristic is:
Quartzy optical waveguide (3) is introduced in the window of the reaction chamber (5) of growth gaN series thin-film material, by itself and reaction chamber cavity wall
Between it is closed;Quartzy optical waveguide (3) outer end is connect by optical fiber (2) with spectrometer (1);Around quartz optical waveguide (3)
It is influenced with protecting optical waveguide end face not by deposition reaction to be passed through nitrogen in nitrogen pipeline (4) test process;Substrate (8) with plus
It is light-blocking to prevent the luminous influence to reflectance spectrum test result of heating furnace that graphite plate pedestal (9) is placed between hot stove (10);Instead
Gas (6) is answered to deposit gaN series film grown layer (7) on substrate (8).
2. a kind of online test method of the on-line measuring device based on gaN series film growth conditions described in claim 1,
It is characterized in that method is as follows:
Using reflectance spectrum simultaneously on-line checking gaN series semiconductive thin film growth rate at high temperature, growth temperature and
Ga1-xYxThis three big condition for influencing film growth quality of N material Y constituent content x value, to ensure technique in thin film growth process
The real-time control of condition and film quality;Its main operational steps are as follows:
1) gaN series film growth temperature in gaN series film growth temperature fluctuation range, Ga are established1-xYxN material Y component contains
Measure the normalized optical constant data library between x value and the forbidden bandwidth of real-time growth material;
2) it utilizes the acquisition of information film growth thickness of reflectance spectrum and calculates growth rate;
3) information for utilizing reflectance spectrum obtains the exact temperature of Material growth by calculating and tabling look-up;
4) information for utilizing reflectance spectrum, by calculating the content x value with the Y component for obtaining material of tabling look-up.
3. a kind of on-line checking dress based on gaN series film growth conditions described in claim 1 according to claim 2
The online test method set, which is characterized in that the method for building up of normalized optical constant data library described in step 1) is as follows: by
The functional relation that the forbidden bandwidth of gaN series material varies with temperature obtains the real-time growth temperature of material, according in certain temperature
Lower gaN series InGaN, AlGaN and AlInGaN multi-element compounds material forbidden bandwidth and Ga1-xYxN material Y constituent content x value it
Between functional relation calculate the content of material, thus establish the gaN series film in gaN series film growth temperature fluctuation range
Growth temperature, Ga1-xYxNormalized optical constant number between N material Y constituent content x value and the forbidden bandwidth of real-time growth material
According to library.
4. a kind of on-line checking dress based on gaN series film growth conditions described in claim 1 according to claim 2
The online test method set, which is characterized in that film growth rate calculation method described in step 2) is as follows: using being grown
The interference peaks in reflectance spectrum formed between film and substrate obtain the real-time growth thickness of film, and pass through film and grow
Thickness changes with time to calculate the growth rate of thin-film material.
5. a kind of on-line checking dress based on gaN series film growth conditions described in claim 1 according to claim 2
The online test method set, which is characterized in that the definite method for acquiring temperature of Material growth described in step 3) is as follows: passing through
Reflectance spectrum determines the ABSORPTION EDGE of material, calculates its taboo in gaN series film growth temperature fluctuation range by ABSORPTION EDGE
Bandwidth;By inquiring the normalized optical constant library of gaN series material, the exact temperature of Material growth is obtained in real time, for instructing
The adjusting and control of film growth temperature.
6. a kind of on-line checking dress based on gaN series film growth conditions described in claim 1 according to claim 2
The online test method set, which is characterized in that the content x value of calculating and the Y component for obtaining material of tabling look-up described in step 4)
Method it is as follows: determine the ABSORPTION EDGE of material by reflectance spectrum, it calculated in gaN series film growth temperature by ABSORPTION EDGE
Forbidden bandwidth in fluctuation range;Normalized optical constant library by inquiring gaN series material obtains the content x of the Y component of material
Value.
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