CN105092511A - Method for detecting content of substitutional carbon and interstitial oxygen in monocrystalline silicon - Google Patents
Method for detecting content of substitutional carbon and interstitial oxygen in monocrystalline silicon Download PDFInfo
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Abstract
The invention discloses a method for detecting the content of substitutional carbon and interstitial oxygen in monocrystalline silicon, and belongs to the field of semiconductor material examination and analysis. The method includes the steps that a reference silicon wafer and a sample silicon wafer are placed on a sample fixing rack for repeated transmission-reflection measuring accessories, and p-linear polarization infrared beams are used for executing N times of the transmission-reflection process; the p-linear polarization infrared beams arrive at an infrared detector, infrared absorption spectrograms are obtained, the difference value of the absorbance of the position where the absorption peak of the substitutional carbon and the interstitial oxygen on the infrared spectrogram of the sample silicon wafer is located and the absorbance of the position where the absorption peak of the substitutional carbon and the interstitial oxygen on the infrared spectrogram of the reference silicon wafer is located is calculated, namely the absorbance of the substitutional carbon and the interstitial oxygen in the sample silicon wafer is obtained; the concentration of the substitutional carbon and the interstitial oxygen can be obtained according to the one-time Brewster infrared transmission equation and the Lambert-Beer law. By the adoption of the method, the monocrystalline silicon with the thickness being 0.1-2.0 mm can be measured, and the measuring accuracy is high.
Description
Technical field
The present invention relates to semiconductor material Inspection and Analysis field, is a kind of method measured monocrystalline silicon and subrogate carbon and interstitial oxygen content in particular.
Background technology
Silicon is the maximum and most widely used semiconductor material of current output, and its output and consumption indicate research and development and the production level of a national electronics and solar industry.The production of high quality silicon material and detection technique and silicon-based devices new and high technology are mutually promoted.As 1) be the miracle in human history based on the semi-conductor industry of silicon, the every aspect of human lives has been changed in its appearance revolutionaryly, mobile phone like the shadow following the person from daily life, communication, computing machine and network thereof produce to intelligence and the control etc. of traffic system as digital machine bed, automobile, high ferro and aircraft is all based on silicon-chip technology, and every day, we came into contacts with by the device of with tens silicon.2) silicon solar cell is just in thriving rise, because fossil energy (oil, coal, rock gas etc.) can use totally in the near future, national governments all at the searching Green Sustainable energy, silicon solar cell due to the technology of maturation and reliable performance be the solar battery product of unique marketing on market.3) photoelectric technology based on silicon materials is predicted by continuation governance market even centuries decades, and emerging silicon-based devices is widely used in many fields such as biological detection, sensor, solar cell and molecular recognition.
The purity of crystal silicon has material impact to its electricity and mechanical property, and semiconductor electronics industry requires that crystal silicon material has very high purity (impurity concentration <1ppb).China's silicon materials and semi-conductor industry are started in the 1950's, middle 1960s achieves industrialization, the development of silicon solar cell industry at the beginning of 21 century drives the flourish of Chinese crystal silicon material industry, but crystal silicon manufacturer is also in development the stage to the grasp of purifying technique, the detection and control of the carbon in crystal silicon material, oxygen and metals content impurity becomes a difficult problem and the bottleneck of silicon materials industry.In addition, the ingot casting in silicon chip production run and pull-rod link also can introduce a large amount of carbon oxygen impurities.Impurity in crystal silicon material can have a strong impact on the fragment rate in the conversion efficiency of solar cell, semiconductor device yield and production run.Single (many) crystal silicon chips subrogate carbon and interstitial oxygen concentration impurity content directly affects and reduces physicochemical property and effect of silicon device, raising crystal silicon subrogates the sensitivity of carbon and the detection of interstitial oxygen concentration impurity content and accuracy is an instant job.
Be used for measuring the technology of subrogating carbon and interstitial oxygen concentration impurity content in crystal silicon at present and comprise gas fusing analysis, SIMS analysis, charged particle activation analysis, neutron activation analysis etc., and above-mentioned technology all needs to carry out pre-service to sample, bulk sample is pulverized or dissolves, thus there is certain environmental impact, work consuming consuming time, and apparatus expensive.In addition, above technology is all measure for the total amount of carbon in crystal silicon and oxygen, for the measurement (can more accurately judge Si wafer quality and performance) of subrogating carbon and interstitial oxygen concentration in monocrystalline silicon, the method that industrial community is happy to take is infrared absorption spectroscopy.Subrogate carbon to exist with the form of Si-C, its infrared absorption peak is at 605cm
-1; Interstitial oxygen concentration exists with the form of Si-O-Si, and infrared absorption peak is respectively at 1107cm
-1(by force), 513cm
-1(in) and 1718cm
-1(weak).According to Lambert-Beer law, infrared absorbance and the content of element proportional, can be expressed as follows:
A＝α·b·c，
Wherein, A represents absorbance; α represents absorptivity, and unit is cm
-1; B representative sample thickness, unit is that cm, c represent impurity concentration, and unit is at/cm
3.
Traditional infrared method, shown in the following equation of relation of the transmissivity of monocrystalline silicon, absorptivity and silicon wafer thickness:
ψ＝2πnbσ，
Wherein, T is the percent transmission of monocrystalline silicon; R is reflectivity; N is refractive index; σ is wave number, and unit is cm
-1.
Infrared spectrum can detect the content of the trace element such as carbon, oxygen with no damage, simple, quick, and can feed back to production line in time to adjust manufacturing parameter, therefore is subject to the favor of silicon materials upstream and downstream producer.In the infrared absorption measurement crystal silicon of current employing, the world of carbon, oxygen impurities content and national standard method are: under normal temperature, and the monocrystalline silicon piece of the double side chemical mechanical polishing of thickness 2.0mm (diameter 1cm) is measured as the mode of sample, infrared light vertical incidence and single transmission.But following 2 measurements that have impact on carbon in crystal silicon, oxygen impurities content: the silicon substrate that 1) solar battery sheet modular manufacture manufacturer is general is at present that thick (thin silicon wafer can reduce costs 0.1mm ~ 0.2mm, but thin silicon wafer also more easily causes fragmentation in process of production, the two is selected, and it is excellent), very strong interference peaks is produced when using standard method to measure 0.1mm ~ 0.2mm thin silicon wafer, disturb the measurement of useful signal, therefore easily there is the dispute to buying thin crystal silicon chip quality of materials in cell piece modular manufacture manufacturer with ingot casting and manufacturer of cutting into slices.2) when the content of carbon, oxygen impurities is at below 0.1ppm, the infrared absorption measurement error of the single vertical incidence of standard law is large, and particularly the measurement of carbon needs to use difference spectrum, and the Signal-to-Noise collected is low, is difficult to distinguish signal and noise.People wait in expectation and occur that a kind of new signal to noise ratio (S/N ratio) is good, data redundancy is high, experimental implementation is easy, also economical and practical outstanding method.
Chinese invention patent, application number: 200610097859.4, publication number: CN1975386A, disclose a kind of infrared spectrometer multiple transmission-reflection measuring attachement, it comprises two parallel plane mirrors, sample holder is had between two plane mirrors, sample silicon chip is fixed between two plane mirrors by sample holder, and it is parallel with plane mirror, when measuring, the infrared light that infrared spectrometer is launched and plane mirror are that an incident angle enters between two plane mirrors, multiple reflections is carried out between two plane mirrors, sample strip then by infrared light repeatedly trans-reflective measure, through entering the detecting device of infrared spectrometer to the infrared light after sample repeatedly trans-reflective measurement.The infrared spectrometer multiple transmission-reflection measuring attachement of this invention, adopts repeatedly the method for trans-reflective to improve the signal to noise ratio (S/N ratio) of collection of illustrative plates.Simple to operate, do not need total reflection crystal sample being carried out to special process and costliness, measurement result is reproducible.Except can detecting the micro constitutent on surface, the micro constitutent that also may be used in material bodies is measured.Its weak point is, can only carry out qualitative experiment research, can not quantitatively calculate, and cannot explain and subtract interference mechanism.
Summary of the invention
1. invent the technical matters that will solve
Be the content of subrogating carbon and interstitial oxygen concentration of the crystal silicon thin slice of 0.2 ~ 2.0mm for thickness measurable in prior art, but immeasurability thickness is the problem of subrogating carbon and interstitial oxygen content of the crystal silicon thin slice of 0.1mm ~ 0.2mm, the present invention proposes a kind of method measured monocrystalline silicon and subrogate carbon and interstitial oxygen content.It can detect thickness be the crystal silicon thin slice of 0.1mm ~ 0.2mm subrogate carbon and interstitial oxygen content, the detectability of an order of magnitude is reduced than prior art, improve the precision of an order of magnitude, achieve Measurement accuracy, there is very large advantage in practicality, economy etc.
2. technical scheme
For achieving the above object, technical scheme provided by the invention is:
Measure the method that monocrystalline silicon subrogates carbon and interstitial oxygen content, the steps include:
(A), twin polishing and the surperficial no marking of parallel reference silicon chip and sample silicon chip, removing Surface Oxygen SiClx;
(B), reference silicon chip and sample silicon chip are placed on the sample holder of the multiple transmission-reflection measuring attachement of infrared spectrometer respectively;
(C) p linear polarization infrared beam, is used, projecting light path is as follows: light beam is with brewster angle incidence and all through silicon chip → metallic mirror surface reflection → brewster angle incidence and all through silicon chip → metallic mirror surface reflection, light repeats above-mentioned transmission and reflection process for N time in silicon chip;
(D), after above-mentioned N transmission and reflection process, N is integer, p linear polarization infrared beam arrives infrared detector, when obtaining taking air as reference in monocrystalline silicon impurity subrogate carbon and interstitial oxygen concentration absorption peak strengthen after infared spectrum, the infared spectrum of sample silicon chip finds the absorbance of the absorption peak position of subrogating carbon and interstitial oxygen concentration, the infrared light collection of illustrative plates of reference silicon chip finds the absorbance of the absorption peak position of subrogating carbon and interstitial oxygen concentration, the absorbance using sample silicon chip to subrogate the absorption peak position of carbon and interstitial oxygen concentration deducts the absorbance of subrogating the absorption peak position of carbon and interstitial oxygen concentration of reference silicon chip, namely the absorbance of subrogating carbon and interstitial oxygen concentration in sample silicon chip is obtained,
(E), according to single Brewster infrared transmission equation and Lambert-Beer law, obtain final transmissivity and the proportionate relationship of subrogating carbon or interstitial oxygen content, converse the concentration of subrogating carbon or interstitial oxygen concentration according to the transmissivity obtained thus;
Wherein, single Brewster infrared transmission equation:
R
s: polarized light reflectivity; α: absorption coefficient; ψ: the phase transformation caused during light transmission sample one time; T
b: the transmittance during transmission of single Brewster angle, %; b
b: the light path passing silicon chip when representing single brewster angle incidence;
Lambert-Beer law:
Infrared absorbance and the content of element proportional, be expressed as follows:
A＝α·b·c,
Wherein A represents absorbance; α represents absorptivity, and unit is cm
-1; B representative sample thickness, unit is cm; C represents impurity concentration, and unit is at/cm
3.
Preferably, in described step (A), the physical dimension of reference silicon chip and sample silicon chip, i.e. length × wide × thick the same, length × wide >=2cm × 1cm, thickness 0.1mm ~ 2.0mm.
Preferably, the length of reference silicon chip and sample silicon chip should make the incidence point at p linear polarization infrared beam center and eye point all at silicon chip surface instead of bounding edge, and forms integer time transmission.
Preferably, in described step (A), the surface flatness <1 μm of reference silicon chip and sample silicon chip.
Preferably, free from foreign meterly in described reference silicon chip carbon and interstitial oxygen concentration is subrogated.
Preferably, during measurement, the temperature of spectrometer sample chamber should control at 25 ± 5 DEG C.
Preferably, the thickness difference of reference silicon chip and sample silicon chip is within ± 0.5%, and sample surfaces flatness is less than 1/4 of the wavelength of incident infrared light, and to avoid the impact of silicon crystal lattice vibration in carbon absorption band, the transmissivity at absorption peak place is not less than 20%.
Preferably, described reference silicon chip and sample silicon chip are p-type silicon chip or n-type silicon chip, the resistivity > 0.5 Ω .cm of described p-type silicon chip, the resistivity > 0.1 Ω .cm of described n-type silicon chip.
Preferably, when adopting said method measured resistivity lower than n-type silicon chip lower than 1 Ω .cm of the p-type silicon chip of 3 Ω .cm or resistivity, the resistivity of reference silicon chip is equal with the resistivity of sample silicon chip.
3. beneficial effect
Adopt technical scheme provided by the invention, compared with existing known technology, there is following remarkable result:
(1) the present invention uses p linear polarization infrared beam, projecting light path is as follows: light beam is with brewster angle incidence and all through silicon chip → metallic mirror surface reflection → brewster angle incidence and all through silicon chip → metallic mirror surface reflection, light repeats above-mentioned transmission and reflection process for N time in silicon chip, the incidence point at p linear polarization infrared beam center and eye point are all at silicon chip surface instead of bounding edge, and form integer time transmission, to reduce the scattering of infrared light, strengthen detection signal strength, regulate the guide-lighting mirror in MTR annex two sides, the signal intensity detected is made to reach maximum, the absorption peak of subrogating carbon and interstitial oxygen concentration is amplified, thus improve the measuring accuracy of subrogating carbon and interstitial oxygen content, an order of magnitude is improve than the existing world and domestic standard, be applicable to the monocrystalline silicon that the intrinsic-OR of all kinds is low-doped,
(2) the present invention uses P polarized light when brewster angle incidence, do not produce reflection, also reflection is not produced in silicon chip inside, light all through, film interference phenomenon can not be there is, so the incidence of Brewster angle (74 °) contributes to reducing the interference fringe caused due to the inner multipath reflection of silicon chip, to measure the silicon chip that thickness is 0.1mm ~ 0.2mm;
(3) the present invention uses p linear polarization infrared beam, through N transmission and reflection process, arrive infrared detector, the incidence point at p linear polarization infrared beam center and eye point are all at silicon chip surface instead of bounding edge, and form integer time transmission, to reduce the scattering of infrared light, strengthen detection signal strength, regulate the guide-lighting mirror in MTR annex two sides, the signal intensity detected is made to reach maximum, infrared light collection of illustrative plates after being amplified, due to the amplification of signal, detectability can be reduced an order of magnitude, because the improvement of current silicon chip production technology, oxygen and carbon content in the silicon chip produced is in continuous reduction, be necessary the detectability expanding original examination criteria, the present invention is that the detectability expanding original examination criteria provides foundation,
(4) the present invention uses MTR annex, and Jin Jing makes together with reflected light meets with transmitted light, and crest adds trough and offsets, thus weakens or eliminate thin film interference effects.P polarized light, when brewster angle incidence, does not produce reflection, does not also produce reflection in silicon chip inside, light all through, film interference phenomenon can not be there is, so, 0.1mm ~ 0.2mm silicon chip just can be used as sample, reduce sampling quantity, save experimental cost;
(5) the present invention is from accompanying drawing 6 and accompanying drawing 7, the interstitial oxygen concentration obtained is measured very good with the relevance of subrogating carbon absorption coefficient with MTR infra-red sepectrometry (being called for short MTR-IR) and traditional infrared spectroscopic methodology (being called for short IR), so MTR-IR method and can be subrogated carbon and measures the interstitial oxygen concentration of industrial silicon chip of solar cell;
(6) prior art can only carry out qualitative experiment research, can not quantitatively calculate, and cannot explain and subtract interference mechanism, and the invention solves quantitative computational problem, can be used in quantitative examination, and it subtracts interference mechanism with mathematical model quantitative interpretation;
(7) signal to noise ratio (S/N ratio) of the method for the invention is good, data redundancy is high, experimental implementation is easy, economical and practical.
Accompanying drawing explanation
Fig. 1 the present invention calculates light path schematic diagram during transmissivity;
The variation relation figure of interference fringe amplitude wave number when Fig. 2 theoretical modeling vertical incidence, the transmission of Brewster angle single, multiple trans-reflective;
Fig. 3 test obtain natural light vertical incidence, the transmission of Brewster angle single, multiple trans-reflective time interference fringe change contrast;
Fig. 4 test obtain p polarized light vertical incidence, the transmission of Brewster angle single, multiple trans-reflective time interference fringe change contrast;
Carbon oxygen content difference spectrum in 200 μm of monocrystalline silicon pieces that Fig. 5 MTR-IR method records;
Fig. 6 MTR-IR method (N=10) and vertical incidence IR method are measured 0.5mm thick monocrystalline silicon piece intermediate gap oxygen and are subrogated the collection of illustrative plates contrast of carbon;
Figure 78 sample is respectively with the monocrystalline silicon interstitial oxygen concentration absorption coefficient associated diagram that MTR-IR method and the measurement of vertical incidence IR method obtain;
Figure 88 sample subrogates carbon absorption coefficient associated diagram with the monocrystalline silicon that MTR-IR method and the measurement of vertical incidence IR method obtain respectively;
The change of N value and monocrystalline silicon interstitial oxygen concentration when Fig. 9 uses MTR-IR method, subrogate carbon absorbance correspondence variation relation figure;
Figure 10 MTR-IR method and vertical incidence IR method are measured monocrystalline silicon interstitial oxygen concentration and subrogate carbon detectability comparison diagram;
Figure 11 is trans-reflective (MTR) annex and infrared light path schematic diagram repeatedly.
Embodiment
For understanding content of the present invention further, the multiple transmission-reflection measuring attachement of request for utilization infrared spectrometer number disclosed in 200610097859.4, the present invention is described in detail by reference to the accompanying drawings.
Embodiment 1
For measure Chinese Shanghai Jun He Electron Material Co., Ltd produce monocrystalline silicon subrogate carbon and interstitial oxygen content, content of the present invention is described in detail in detail.Sample silicon wafer thickness is 100 μm, and silicon chip is cut into rectangle, 1.6cm × 5cm, and crystal formation is <100>, and doping type is N-shaped, phosphorus doping, and resistivity is the silicon chip of 15 Ω cm, is called for short CZ silicon chip; Not carbon containing oxygen in reference silicon chip, resistivity is 3000 Ω cm, all the other are the same with sample silicon chip, be called for short FZ silicon chip, the thickness difference of reference silicon chip and sample silicon chip is within ± 0.5%, and sample surfaces flatness is less than 1/4 of the wavelength of incident infrared light, to avoid the impact of silicon crystal lattice vibration in carbon absorption band, the transmissivity at absorption peak place is not less than 20%, to reduce the scattering of infrared light.The multiple transmission-reflection measuring attachement of application number infrared spectrometer disclosed in 200610097859.4, be called for short MTR annex, this Infrared survey annex is applicable to all business FTIR spectrum instrument, except non-designated, general use DTGS detecting device.Because carbon, oxygen absorption band and silicon crystal lattice absorption of vibrations bands of a spectrum all can become with the change of sample temperature, the temperature of optical spectrometer sample room controls at 25 ± 5 DEG C.Detect the step of subrogating carbon and interstitial oxygen content in monocrystalline silicon as follows:
A, sample silicon chip and reference silicon chip are all placed on Piranha solution, namely volume ratio is that in the concentrated sulphuric acid of 3:1 and 30% hydrogen peroxide mixed solution, then digestion takes out silicon chip be placed in NH to wash organic impurities for 15 minutes
3.H
2o:H
2o:H
2o
230 minutes are boiled in the mixed solution of=1:1:1, then room temperature is cooled to, with being stored in water outlet after pure water rinsing, before measuring silicon chip is soaked in 0.5%HF solution 1 minute to remove the passivation layer of silicon face, then use nitrogen fluidized drying, two-sidedly carry out chemically mechanical polishing, ensure silicon chip surface smoothness <1 μm, two-sided parallel, surperficial no marking, to reduce the scattering of infrared light.
B, open infrared spectrometer and its workstation, regulate the catoptron of MTR annex, catoptron direction is made to become the angle of 74 ° (namely incident angle is Brewster angle) with p linear polarization ruddiness incident direction, reference silicon chip is placed on the sample holder of MTR annex, MTR annex is fixed on FTIR sample holder of Infrared spectrometer, to carry out N transmission and reflection process to reference silicon.Figure 11 is repeatedly trans-reflective infrared spectrum schematic diagram, is followed successively by Jin Jing, silicon chip and Jin Jing, p linearly polarized light from top to bottom incident from left side.
C, projecting light path are as follows: light beam is with brewster angle incidence and all through silicon chip → metallic mirror surface reflection → brewster angle incidence and all through silicon chip → metallic mirror surface reflection, light repeats above-mentioned transmission and reflection process for N time in silicon chip, N is integer, the incidence point at p linear polarization infrared beam center and eye point are all at silicon chip surface instead of bounding edge, and form integer time transmission, to reduce the scattering of infrared light, detection signal strength, regulate the guide-lighting mirror in MTR annex two sides, make the signal intensity detected reach maximum.
D, experimentally requirement, arrange experiment parameter.
E, after DTGS detecting device is stable, take air as background, measure and obtain reference silicon chip infared spectrum.
F, taking-up MTR annex, put into sample silicon chip between two gold medal mirrors, makes one end of silicon chip be 5mm apart from infrared light incidence point, ensure that first incidence point of infrared light is at silicon chip surface with this; Two guide-lighting mirrors (multiple transmission-reflection measuring attachement see application number infrared spectrometer disclosed in 200610097859.4) can all around be moved, and obtain maximum luminous flux to make DTGS detecting device.Incident angle remains on 74 °, is that 0.225 vernier adjustment knob regulates, tightens gib screw and fix silicon chip after regulating by the minimum scale of on annex.
G, again MTR annex to be fixed on FTIR sample holder of Infrared spectrometer, to carry out N transmission and reflection process to sample silicon chip; Repeat step c ~ e, scanning samples, obtains sample silicon chip infared spectrum.
H, the reference silicon chip infared spectrum obtained and sample silicon chip infared spectrum are processed and calculated, obtain the relative content of subrogating carbon Cs and interstitial oxygen concentration Oi.According to single Brewster infrared transmission equation and Lambert-Beer law, obtain final transmissivity and the proportionate relationship of subrogating carbon or interstitial oxygen content, converse the concentration of subrogating carbon or interstitial oxygen concentration according to the transmissivity obtained thus.
All measuring processs are all with reference to ASTMF1391, and arranging infrared spectrometer scan method is on a workstation with 4cm
-1wave number, scanning times can fix between 10 ~ 200 per sample, and during each measurement one batch sample, measuring reference silicon chip must be identical with the scanning times of sample silicon chip, and scanning wave-number range is 400cm
-1~ 4000cm
-1.Measure two groups of samples altogether, often group comprises 12 samples.Each sample uses repeatedly trans-reflective method (N=10) and the incident method of Brewster angle single to survey 4 times continuously respectively, repeatedly trans-reflective method measuring method is shown in step a ~ h, after each measurement all by silicon chip slightly mobile some distances to ensure the diverse location of measurement point at this silicon chip, so obtain with the Brewster angle single incidence method of single transmission and repeatedly trans-reflective infrared spectrum (abbreviation MTR-IR) method to measure in each sample 4 and 40 different points respectively.
Subrogate the computation process of carbon
I, be respectively d with the thickness of vernier caliper measurement sample silicon chip and reference silicon chip
mand d
r;
II, sample silicon wafer thickness d
mwith reference silicon wafer thickness d
rratio be multiplied by the absorption spectra of reference silicon chip;
III, deduct the normalized absorption spectrum of reference silicon chip by the absorption spectra of sample silicon chip;
605cm in IV, reading difference spectrum
-1the maximal value at carbon peak, place;
V, this point add each 2 points totally 5 points around, as parabola of fit, and the wave number at para-curve summit place and absorbance A
c,Pdetermined;
VI, to difference spectrum carry out baseline fitting, baseline two ends wave-number range is respectively 550cm
-1~ 570cm
-1, 630cm
-1~ 650cm
-1;
VII, the reading wave number at para-curve summit place and the absorbance A at corresponding baseline place
c,B;
VII、
The absorption coefficient on para-curve summit
c, Pwith baseline absorbance factor alpha
c, Bcalculate respectively by following formula;
P polarized light:
T
MTR-C,P＝exp(-α
c,pNb
B)，
T
MTR-C,B＝exp(-α
c,BNb
B)，
Wherein T
mTRfor monocrystalline silicon uses the percent transmission of MTR-IR method; b
bfor Brewster angle single incident light is through the light path of silicon chip; b
mTRfor using the MTR-IR method time through the light path of silicon chip; N is the number of times that light passes silicon chip.
The absorption coefficient of subrogating carbon is calculated as follows:
α
C＝α
C，P-α
C，B；
The concentration of subrogating carbon (uses C
crepresent, capitalization C represents concentration, and small letter c subrogates carbon) absorption coefficient that equals to subrogate carbon is multiplied by typical coefficient,
C
C＝0.82×10
17·α
C；
Subrogate the concentration C of carbon
cbe multiplied by machine revision coefficient FC again, be generally 1,
CC＝FC×CC。
The computation process of interstitial oxygen concentration
Carbon oxygen content in 100 μm of silicon chips that table 1MTR-IR method is measured
1), d is respectively with the thickness of vernier caliper measurement sample silicon chip and reference silicon chip
mand d
r;
2), sample silicon wafer thickness d
mwith reference silicon wafer thickness d
rratio be multiplied by the absorption spectra of reference silicon chip;
3) normalized absorption spectrum of reference silicon chip, is deducted by the absorption spectra of sample silicon chip;
4) 1107cm in difference spectrum, is read
-1the maximal value at oxygen peak, place;
5), this point add each 2 points totally 5 points around, as parabola of fit, the wave number at para-curve summit place and absorbance A
o,Pdetermined;
6), to difference spectrum carry out baseline fitting, baseline two ends wave-number range is 900cm
-1~ 1000cm
-1, 1200cm
-1~ 1300cm
-1;
7), the wave number at para-curve summit place and the absorbance A at corresponding baseline place is read
o,B;
8)、
The absorption coefficient on para-curve summit
o, Pwith baseline absorbance factor alpha
o, Bcalculate respectively by following formula;
P polarized light:
T
MTR-O,P＝exp(-α
O,PNb
B)，
T
MTR-O,B＝exp(-α
O,BNb
B)，
Wherein, T
mTRfor monocrystalline silicon uses the percent transmission of MTR-IR method; b
bfor Brewster angle single incident light is through the light path of silicon chip; b
mTRfor using the MTR-IR method time through the light path of silicon chip; N is the number of times that light passes silicon chip.
The absorption coefficient of interstitial oxygen concentration is calculated as follows:
α
o=α
o, Pone α
o, B;
The absorption coefficient that the concentration of interstitial oxygen concentration equals interstitial oxygen concentration is multiplied by typical coefficient,
C
O＝3.14×10
17·α
O；
Interstitial oxygen concentration C
obe multiplied by machine revision coefficient FO again, be generally 1,
C
O＝FO×C
O，
Table 1 is carbon oxygen content in 100 μm of monocrystalline silicon for using MTR-IR method detect thickness.
Embodiment 2
Sample silicon wafer thickness is 200 μm, the remainder of sample silicon chip and reference silicon wafer parameters, detection method and step with embodiment 1, carbon oxygen content in 200 μm of silicon chips that table 2 is measured for MTR-IR method.
Brewster angle subtract interference effect
Figure 11 is repeatedly trans-reflective (MTR) annex and infrared light path schematic diagram, Fig. 1 is the light path schematic diagram of P polarized light transmission reflection, Jin Jing is followed successively by from top to bottom in Fig. 1, silicon chip and Jin Jing, the lower left corner in figure, in incident ray and figure, p polarized light incides silicon chip surface with Brewster angle (namely 74 °), golden mirror through top in silicon chip arrival figure reflects, arrive on Figure below gold mirror through silicon chip and be reflected back silicon chip, through said process, incident ray is through silicon wafer N time, and order of reflection is also N on two golden mirrors, N is integer, in Fig. 1, N is respectively 1, 2, 3 and 4, then DTGS detecting device is arrived, weak peak in interference fringe is not only fuzzy spectrum, and decrease the accuracy of quantitative measurment.P polarized light, when brewster angle incidence, does not produce reflection, does not also produce reflection in silicon chip inside, light all through, film interference phenomenon can not be there is.So the incidence of Brewster angle contributes to reducing the interference fringe caused due to the inner multipath reflection of silicon chip, provides possibility for carrying out thin slice measurement.
Table 2MTR-IR method measures the carbon oxygen content in 200 μm of silicon chips
Interference effect is subtracted, wherein n=3.42, α=39.5cm when Fig. 2 is the natural light of theoretical modeling
-1, b=0.020cm, b
b=0.0208cm, b
mTR=0.1664cm, Brewster angle is 74 °, N=8.When Brewster angle single is incident, R
p=0, R
s=0.70, owing to interfering the amplitude reflecting the transmittance caused only to affect s polarized light, and the projectile energy of maximum half, and p polarized light is only relevant with thickness, by interfering reflections affect, so oscillator intensity is bound to reduce.Fig. 2 is the variation relation figure of interference fringe amplitude wave number when using vertical incidence method, Brewster angle single transmission beam method, multiple trans-reflective (MTR) method respectively.T=0.058 during vertical incidence, T during Brewster angle single transmission beam method
bt during=0.029, MTR-IR method
mTR=0.0025, so in theory, Brewster angle single transmission beam method can reduce interference fringe amplitude 2 times than vertical incidence method, and MTR-IR method compares vertical incidence can reduce interference fringe amplitude 23 times, and MTR-IR method compares Brewster angle single transmission beam method can reduce interference fringe amplitude 11 times.
Subtract interference effect when Fig. 3 is the natural light of measuring, sample length is 5cm, n=3.42, N=8, b=0.020cm, b
b=0.0208cm, b
mTR=0.1664cm, brewster angle incidence angle is 74 °; Interference fringe change when measuring 0.020cm thin silicon wafer respectively to vertical incidence method, Brewster angle single transmission beam method, multiple trans-reflective (MTR) method contrasts.The signal to noise ratio (S/N ratio) of the incident method of single Brewster is 10 times of vertical incidence IR method, and MTR-IR method is 5 times of the incidence of single Brewster, therefore the signal to noise ratio (S/N ratio) of MTR-IR method is 50 times of vertical incidence IR method.The actual amplitude of vertical incidence IR method is 0.056, and theoretical value is 0.058; The actual amplitude of the incident method of single Brewster is 0.028, and theoretical value is 0.029; The actual amplitude of MTR-IR method is 0.002, and theoretical value is 0.0025; The ratio that the incident IR method of MTR-IR method Relative vertical reduces with the interference fringe Oscillation Amplitude of the incident method of single Brewster conforms to substantially with theoretical modeling above.The reason that the theoretical value of MTR-IR method is larger than actual value may be do not consider integrating sphere effect in theoretical modeling.The infrared absorption pattern of the 0.020cm silicon chip using vertical incidence method, Brewster angle single transmission beam method, multiple trans-reflective (MTR) method to record when Fig. 4 is p polarized light respectively.Wherein multiple trans-reflective (MTR) method collection of illustrative plates has no interference fringe and signal increase, so select P polarized light incident.
Fig. 5 is the carbon oxygen difference spectrum in 200 μm of silicon chips recording of MTR-IR method, and sample silicon chip is the same with reference silicon wafer thickness, and reference silicon chip is carbon containing oxygen not, b=0.02cm, incident angle=74 °, N=8.
Although can to the smoothing process of interference fringe spectrum, doing like this can derivative spectomstry portion deforms.Compared with vertical incidence, Brewster angle single transmission beam method obviously can reduce interference fringe, and the spectrum recorded by MTR-IR method does not only have visible interference fringe, and is exaggerated useful signal.MTR-IR method reduces the mechanism of interference fringe except brewster angle incidence, also has a major reason to be exactly integrating sphere effect (i.e. destructive interference).In MTR annex, Jin Jing makes together with reflected light meets with transmitted light, and crest adds trough and offsets, thus weakens or eliminate thin film interference effects.So, comparatively thin silicon wafer just can be used as sample, to reduce sampling quantity, save experimental cost.Obtain the high-quality spectrum for quantitative test, just should avoid in the measurements occurring interference.Because vertical incidence IR method only employs a transmission, for weak peak, because of peak shape less thus be easy to the interference fringe caused by the multiple reflections in thin silicon wafer cover.
With traditional vertical incidence IR method measure 100 μm, 200 μm of silicon chips time, due to the existence of thin film interference fringes, therefore vertical incidence IR method can not to compared with thin silicon wafer intermediate gap oxygen with subrogate carbon content and measure.The relative standard deviation that the incident IR method of conventional vertical is surveyed interstitial oxygen concentration that thickness of sample is 2mm and subrogated carbon is ± and 2%, and MTR-IR method surveys the maximum relative standard deviation 0.988% of interstitial oxygen concentration that thickness of sample is 100 μm, 200 μm, subrogate the maximum relative standard deviation 1.991% of carbon, not only meet the requirements, from thickness of sample, the reappearance of MTR-IR method is far superior to vertical incidence IR method.In fact vertical incidence IR method cannot be measured comparatively thin silicon wafer at all, let alone result.Can be found out by upper table, MTR-IR method not only can be measured comparatively thin silicon wafer, and also meets relevant national standard requirement in reappearance.Industrial solar silicon wafers is generally thin silicon wafer, so can directly measure by MTR-IR method, facilitates the needs that commercial production detects.
Embodiment 3
Except the thickness of sample and reference silicon chip is except 450 μm, all the other parameters, detection method and step are with embodiment 1.In Fig. 6, MTR-examples representative MTR-IR method measures the spectrogram of sample silicon chip; IR-examples representative vertical incidence IR method measures the spectrogram of sample silicon chip, and sample length is 5cm, n=3.42, N=10, b=0.0450cm, b
b=0.0469cm, b
tMR=0.469cm, incident angle=74 °.Fig. 6 gives the MTR-IR method of same silicon chip and the infrared spectrum of vertical incidence IR method, by comparing, can find out, the sample absorbance of MTR-IR method is always greater than vertical incidence IR method, especially at interstitial oxygen concentration crest 1107cm
-1with subrogate carbon crest 605cm
-1place, MTR-IR method and the contrast of vertical incidence IR method on peak height or peak area are fairly obvious, and in vertical incidence IR method, peak width at half height degree is larger, and the error of calculation is larger.As can be seen from Figure 6, at 1107cm
-1and 605cm
-1place, although MTR-IR method peak heights adds, peak width at half height degree does not become, and the increase of peak height does not cause the increase of the error of calculation in other words.Because incident light there occurs reflection repeatedly and transmission in multiple trans-reflective annex, whole optical path length increases, adding Jin Jing makes reflected light first again enter silicon chip, light energy absorption is increased, according to Lambert-Beer law, the signal that detecting device is collected obtains amplification and absorbance increases.From quantitative angle, absorbance is larger, and relative error will be less, and correspondingly measurement result is just more accurate, so result can be more accurate.Because silicon crystal lattice is at 610cm
-1near have stronger vibration, it is lower to add carbon content, can affect the absorption peak 605cm subrogating carbon
-1observation, so need fused silicon chip to eliminate the impact of silicon crystal lattice as reference.
For same silicon chip, MTR-IR method spectral quality has raising clearly, and demonstrating MTR-IR method has higher sensitivity with subrogating in carbon than vertical incidence IR method at measurement clearance oxygen.But the real advantage that MTR-IR method compares vertical incidence IR method is not only that it can record the spectrogram having stronger interstitial oxygen concentration He subrogate carbon signal, and pass through the sampled point quantity of increase by 10 times, relevant interstitial oxygen concentration can be obtained and subrogate the more real information of carbon.
1107cm from Fig. 6
-1and 605cm
-1the integral area ratio at neighbouring peak, MTR-integral area/IR-integral area=9 ~ 10, the interstitial oxygen concentration ratio calculated is between 9 ~ 10, and substitutional carbon concentrations ratio is between 7 ~ 8.In general, ft-ir measurement carbon content is more difficult than measuring oxygen content.Reason has three: one to be that silicon crystal lattice is at 610cm
-1near have a very strong absorption peak, with 605cm
-1the carbon peak superposition at place together, will extract little carbon peak from very strong large peak, want accurate quantitative analysis very difficult; Two is in general silicon chip more than a carbon content order of magnitude lower than oxygen content; Three are peak width at half height degree of carbon is 7cm
-1, and general instrumental resolution adopts 4cm
-1, both differences are comparatively near, are also one of reasons causing error.Due to the amplification of signal, detectability can be reduced an order of magnitude, because the improvement of current silicon chip production technology, the oxygen and carbon content in the silicon chip of production, in continuous reduction, is necessary the detectability expanding original examination criteria.
In order to calibrate this method, by MTR-IR method and vertical incidence IR method, 8 silicon chip samples are measured respectively.From Fig. 7 and Fig. 8, the interstitial oxygen concentration obtained with MTR-IR method and the measurement of vertical incidence IR method is very good with the relevance of subrogating carbon absorption coefficient.So MTR-IR method and can be subrogated carbon and measures the interstitial oxygen concentration of industrial silicon chip of solar cell.
In Fig. 9, sample length is 5cm, n=3.42, b=0.0450cm, incident angle is 74 °, and when N value changes in 6 ~ 12 scopes, N value often increases by 1, and absorbance increases by 0.1, interstitial oxygen concentration absorbance and N value proportional, namely N value is larger, and the absorbance of interstitial oxygen concentration is larger.Although the variation tendency of subrogating carbon is the same with interstitial oxygen concentration, when N=11,12 time, the absorbance of subrogating carbon is changed to 0.13, somewhat bigger than normal.Grey square in Figure 10 refers to the detectability of the interstitial oxygen concentration using vertical incidence IR method, gray triangles refers to the detectability of subrogating carbon using vertical incidence IR method, black bars refers to the detectability using MTR-IR method interstitial oxygen concentration, black pentagram refers to use MTR-IR method to subrogate the detectability of carbon, as can be seen from Figure 10, for the silicon chip of 2.0mm, the detectability 1 × 10 of vertical incidence IR method interstitial oxygen concentration
16at.cm
-3, subrogate the detectability 5 × 10 of carbon
15atcm
-3; And the detectability 5 × 10 of MTR-IR method interstitial oxygen concentration
14atcm
-3, the detection of subrogating carbon is limited to 1.25 × 10
14atcm
-3; MTR-IR method significantly improves interstitial oxygen concentration and subrogates the detectability of carbon, reaches 10 respectively
14atcm
-3left and right.
Embodiment 4
Except sample and reference silicon wafer thickness are except 2.0mm, all the other parameters, detection method and step are with embodiment 1, and monocrystalline silicon interstitial oxygen concentration is identical with embodiment 3 with detectability relation with the relevance of subrogating carbon measurement result.
Embodiment 5
Except the boron doped p type crystal silicon that sample and reference silicon wafer thickness are 100 μm, all the other parameters, detection method and step are with embodiment 1, and monocrystalline silicon interstitial oxygen concentration is identical with embodiment 3 with detectability relation with the relevance of subrogating carbon measurement result.
Embodiment 6
Except the boron doped p type crystal silicon that sample and reference silicon wafer thickness are 200 μm, all the other parameters, detection method and step are with embodiment 1, and monocrystalline silicon interstitial oxygen concentration is identical with embodiment 3 with detectability relation with the relevance of subrogating carbon measurement result.
Embodiment 7
Except the boron doped p type crystal silicon that sample and reference silicon wafer thickness are 450 μm, all the other parameters, detection method and step are with embodiment 1, and monocrystalline silicon interstitial oxygen concentration is identical with embodiment 3 with detectability relation with the relevance of subrogating carbon measurement result.
Embodiment 8
Except the boron doped p type crystal silicon that sample and reference silicon wafer thickness are 2.00mm, all the other parameters, detection method and step are with embodiment 1, and monocrystalline silicon interstitial oxygen concentration is identical with embodiment 3 with detectability relation with the relevance of subrogating carbon measurement result.
Embodiment 9
Sample silicon chip is p-type, resistivity is 0.6 Ω cm, reference silicon chip is p-type, resistivity is also 0.6 Ω cm, because resistivity is that the free-carrier Absorption of the p-type silicon chip of 0.6 Ω cm is comparatively serious, therefore when testing, the resistivity of reference silicon chip should be consistent with the resistivity of sample silicon chip as far as possible, to ensure to deduct the transmitted spectrum of sample silicon chip after reference silicon chip spectrum at 1600cm
-1the transmitance at place is 100% ± 0.5%.The remainder of sample silicon chip and reference silicon wafer parameters, detection method and step are with embodiment 1, and monocrystalline silicon interstitial oxygen concentration is identical with embodiment 3 with detectability relation with the relevance of subrogating carbon measurement result.
Embodiment 10
Sample silicon chip is p-type, resistivity is 2.9 Ω cm, reference silicon chip is p-type, resistivity is also 2.9 Ω cm, because resistivity is that the free-carrier Absorption of the p-type silicon chip of 2.9 Ω cm is comparatively serious, therefore when testing, the resistivity of reference silicon chip should be consistent with the resistivity of sample silicon chip as far as possible, to ensure that the transmitted spectrum deducting sample after reference spectrum is at 1600cm
-1the transmitance at place is 100% ± 0.5%.The remainder of sample silicon chip and reference silicon wafer parameters, detection method and step are with embodiment 1, and monocrystalline silicon interstitial oxygen concentration is identical with embodiment 3 with detectability relation with the relevance of subrogating carbon measurement result.
Embodiment 11
Sample silicon chip is N-shaped, resistivity is 0.2 Ω cm, reference silicon chip is N-shaped, resistivity is also 0.2 Ω cm, because resistivity is that the free-carrier Absorption of the n-type silicon chip of 0.2 Ω cm is comparatively serious, therefore when testing, the resistivity of reference silicon chip should be consistent with the resistivity of sample silicon chip as far as possible, to ensure that the transmitted spectrum deducting sample after reference spectrum is at 1600cm
-1the transmitance at place is 100% ± 0.5%.The remainder of sample silicon chip and reference silicon wafer parameters, detection method and step are with embodiment 1, and monocrystalline silicon interstitial oxygen concentration is identical with embodiment 3 with detectability relation with the relevance of subrogating carbon measurement result.
Embodiment 12
Sample silicon chip is N-shaped, resistivity is 0.9 Ω cm, reference silicon chip is N-shaped, resistivity is also 0.9 Ω cm, because resistivity is that the free-carrier Absorption of the n-type silicon chip of 0.9 Ω cm is comparatively serious, therefore when testing, the resistivity of reference silicon chip should be consistent with the resistivity of sample silicon chip as far as possible, to ensure that the transmitted spectrum deducting sample after reference spectrum is at 1600cm
-1the transmitance at place is 100% ± 0.5%.The remainder of sample silicon chip and reference silicon wafer parameters, detection method and step are with embodiment 1, and monocrystalline silicon interstitial oxygen concentration is identical with embodiment 3 with detectability relation with the relevance of subrogating carbon measurement result.
Schematically above be described the present invention and embodiment thereof, this description does not have restricted, and also just one of the embodiments of the present invention shown in accompanying drawing, actual structure is not limited thereto.So, if those of ordinary skill in the art enlightens by it, when not departing from the invention aim, designing the frame mode similar to this technical scheme and embodiment without creationary, all should protection scope of the present invention be belonged to.
Claims (9)
1. measure the method that monocrystalline silicon subrogates carbon and interstitial oxygen content, the steps include:
(A), twin polishing and the surperficial no marking of parallel reference silicon chip and sample silicon chip, removing Surface Oxygen SiClx;
(B), reference silicon chip and sample silicon chip are placed on the sample holder of the multiple transmission-reflection measuring attachement of infrared spectrometer respectively;
(C) p linear polarization infrared beam, is used, projecting light path is as follows: light beam is with brewster angle incidence and all through silicon chip → metallic mirror surface reflection → brewster angle incidence and all through silicon chip → metallic mirror surface reflection, light repeats above-mentioned transmission and reflection process for N time in silicon chip;
(D), after above-mentioned N transmission and reflection process, N is integer, p linear polarization infrared beam arrives infrared detector, when obtaining taking air as reference in monocrystalline silicon impurity subrogate carbon and interstitial oxygen concentration absorption peak strengthen after infared spectrum, the infared spectrum of sample silicon chip finds the absorbance of the absorption peak position of subrogating carbon and interstitial oxygen concentration, the infrared light collection of illustrative plates of reference silicon chip finds the absorbance of the absorption peak position of subrogating carbon and interstitial oxygen concentration, the absorbance using sample silicon chip to subrogate the absorption peak position of carbon and interstitial oxygen concentration deducts the absorbance of subrogating the absorption peak position of carbon and interstitial oxygen concentration of reference silicon chip, namely the absorbance of subrogating carbon and interstitial oxygen concentration in sample silicon chip is obtained,
(E), according to single Brewster infrared transmission equation and Lambert-Beer law, obtain final transmissivity and the proportionate relationship of subrogating carbon or interstitial oxygen content, converse the concentration of subrogating carbon or interstitial oxygen concentration according to the transmissivity obtained thus;
Wherein, single Brewster infrared transmission equation:
R
s: polarized light reflectivity; α: absorption coefficient; ψ: the phase transformation caused during light transmission sample one time; T
b: the transmittance during transmission of single Brewster angle, %; b
b: the light path passing silicon chip when representing single brewster angle incidence;
Lambert-Beer law:
Infrared absorbance and the content of element proportional, be expressed as follows:
A＝α·b·c,
Wherein A represents absorbance; α represents absorptivity, and unit is cm
-1; B representative sample thickness, unit is cm; C represents impurity concentration, and unit is at/cm
3.
2. a kind of method measured monocrystalline silicon and subrogate carbon and interstitial oxygen content according to claim 1, is characterized in that, in described step (A), the physical dimension of reference silicon chip and sample silicon chip, i.e. length × wide × thick the same, length × wide >=2cm × 1cm, thickness 0.1mm ~ 2.0mm.
3. a kind of method measured monocrystalline silicon and subrogate carbon and interstitial oxygen content according to claim 2, it is characterized in that, the length of reference silicon chip and sample silicon chip should make the incidence point at p linear polarization infrared beam center and eye point all at silicon chip surface instead of bounding edge, and forms integer time transmission.
4. a kind of method measured monocrystalline silicon and subrogate carbon and interstitial oxygen content according to claim 2, is characterized in that, in described step (A), and the surface flatness <1 μm of reference silicon chip and sample silicon chip.
5. a kind of method measured monocrystalline silicon and subrogate carbon and interstitial oxygen content according to claim 3, is characterized in that, free from foreign meterly in described reference silicon chip subrogates carbon and interstitial oxygen concentration.
6. a kind of method measured monocrystalline silicon and subrogate carbon and interstitial oxygen content according to claim 3, it is characterized in that, during measurement, the temperature of spectrometer sample chamber should control at 25 ± 5 DEG C.
7. a kind of method measured monocrystalline silicon and subrogate carbon and interstitial oxygen content according to claim 1, it is characterized in that, the thickness difference of reference silicon chip and sample silicon chip is within ± 0.5%, sample surfaces flatness is less than 1/4 of the wavelength of incident infrared light, to avoid the impact of silicon crystal lattice vibration in carbon absorption band, the transmissivity at absorption peak place is not less than 20%.
8. a kind of method measured monocrystalline silicon and subrogate carbon and interstitial oxygen content according to claim 4, it is characterized in that, described reference silicon chip and sample silicon chip are p-type silicon chip or n-type silicon chip, the resistivity > 0.5 Ω .cm of described p-type silicon chip, the resistivity > 0.1 Ω .cm of described n-type silicon chip.
9. a kind of method measured monocrystalline silicon and subrogate carbon and interstitial oxygen content according to claim 4, it is characterized in that, when adopting said method measured resistivity lower than n-type silicon chip lower than 1 Ω .cm of the p-type silicon chip of 3 Ω .cm or resistivity, the resistivity of reference silicon chip is equal with the resistivity of sample silicon chip.
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| CN112882145A (en) * | 2021-02-22 | 2021-06-01 | 长春长光辰英生物科学仪器有限公司 | Reflective light filtering module and light filtering method thereof |
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