JP3275022B2 - Photoluminescence measurement device in crystal - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for measuring photoluminescence of an object crystal made of silicon or another crystal.

[0002]

2. Description of the Related Art Conventionally, as a method for measuring the distribution of defects in a crystal to be inspected, photoluminescence (photoluminescence) has been used.
minescence) There is a measurement method. In the case of silicon (Si) crystal,
Argon Ar (488.514 nm) or Helium Lion He
A photoluminescence method using a -Ne laser (633 nm) is known. FIG. 1 shows such an Ar or He-
1 shows a photoluminescence measuring instrument according to a conventional technique for projecting a Ne laser beam A onto an object crystal B from above and spectrally measuring generated fluorescence under a microscope. In FIG. 1, an Ar or He-Ne laser beam A projected from a horizontal direction is changed in direction by 90 degrees by a half mirror C, and is condensed on an object crystal B by an objective lens D. Fluorescence emitted by the light emission center excited by the laser beam A projected on the specimen crystal B passes through the half mirror C and forms an image on the pinhole or slit F provided in the spectroscope E by the imaging lens G. Then, the fluorescence diffracted by the diffraction grating H provided in the spectroscope E is guided to the light receiving element I through the pinhole or the slit N, and is distributed on the element according to the frequency distribution. The control computer J analyzes the light-receiving image of the light-receiving element I, controls the stage controller K, and displays the distribution of the fluorescence generated by moving the subject crystal B two-dimensionally on the image display device L. M is a stage. As other prior arts relating to the photoluminescence method, Japanese Patent Application Laid-Open No. 54-109488 and Japanese Patent Application Laid-Open No.
There are 2-119446 publications. Japanese Patent Application Laid-Open No. 61-21365 discloses a technique for obtaining a scattered image of a defect in a silicon crystal using a YAG laser. Related technologies include K. Moriya and T. ogawa, Jpn.J. Appl. Phy.
s., 22 (1983) L207, JP-A-1-182739, JP-A-2-203254, JP-A-1-314953.
JP, JP-A-61-76939, JP-A-63-76939
JP-A-221234, JP-A-3-269347,
JP-A-3-29336, JP-A-53-12037
No. 0 and JP-A-63-18250.

[0003]

The above-described photoluminescence measurement method for silicon is performed by irradiating an Ar / He-Ne laser A onto a test crystal B from above. Is relatively short and cannot sufficiently reach the inside of the crystal, so that only the vicinity of the crystal surface (about 1 to 2 μm) can be measured. The surface recombination level (Surface Recombination Cente)
r) has occurred and is in a state different from the original crystal internal structure. Therefore, accurate measurement of physical properties inside a crystal cannot be expected with the conventional technique which can only measure near the surface. When the specimen crystal B is a silicon crystal, IG (I
Since the process has been performed, defects are distributed in the depth direction of the wafer. Even when the crystal is cleaved and the cross-sectional shape is observed, the distribution of defects in the depth direction is also affected by the cross-section, and accurate measurement cannot be performed. Therefore, the present invention provides a photoluminescence measuring device capable of measuring up to the inside of a crystal. In the photoluminescence measurement method, it is important to measure the radiative lifetime ((Life Time)) of the luminescent particles, which is usually measured by using a pulsed laser as the projection light as shown in FIG. Alternatively, the measurement is generally performed by using a pulsed light source and evaluating the attenuation state of the received pulsed light.In addition, as another method of measuring the radiation life, a semiconductor laser beam is injected as excitation energy and a There is also a method of observing the exciton attenuation by a wave, but the measurement system using a pulsed laser is complicated and expensive, and the fluorescence generated by excitation light with low absorption reaching the inside of the crystal is extremely high. In order to obtain fluorescent light of measurable intensity, a pulse laser with a high peak value (energy intensity) must be used, and the crystal itself is dark. Therefore, an object of the present invention is to provide an apparatus capable of measuring the lifetime of fluorescence without using a pulse laser source.In the conventional example shown in FIG. Although the system uses a wavelength dispersion type spectroscope E, the spectrometer E is dark and unsuitable for measuring weak fluorescence, and the optical system is expensive and large in scale. It is an object of the present invention to provide a photoluminescence measuring instrument that can measure with a simple optical system without using a spectroscope E.

[0004]

Accordingly, the present invention provides a method for manufacturing a crystal surface 3
a and a crystal 3 having an incident side surface 3b in a direction intersecting with the crystal surface 3a, and incident on the crystal 3 from the incident side 3b into the crystal 3 or the crystal surface 3a. Incident on the sample crystal 3 at an oblique angle from the crystal surface 3a to be able to pass through the sample crystal 3 and excite carriers in the sample crystal 3
A laser projection optical system 1 for generating a laser beam 2 of the energy intensity possible with the laser beam 2 a diaphragm that condensing lens 4 in a predetermined diameter, said laser beam 2 in the subject within the crystal 3
The carrier is excited by
Objective lens 5 for receiving fluorescence light generated in body crystal 3
And a light receiving optical system 9 composed of an imaging lens 7 and an image sensor 8
Provided between the objective lens 5 and the imaging lens 7.
Scattered light only the fluorescence generated by the excited carriers
A narrow band pass filter 6 having a narrow-band transmission characteristic of transmitting selected from, excited from the imaging element 8 key
This is a device for measuring photoluminescence in a crystal, comprising an image processing device 10 for processing image information including the spread of fluorescence generated by carriers and a computer 11 for controlling necessary information. Further, the laser projection optical system 1
Laser stage 13 equipped with a crystal and the object crystal
The object movement stage 14 on which the laser beam 3 is mounted, and the laser movement stage 14
Movement of the moving stage 13 and the object moving stage 14
In a crystal provided with a stage controller 12 for controlling
Of the present invention. Further, a photoluminescence measuring device is provided in which a polarizing element 15 is provided in the laser projection optical system 1 and a polarizing element 16 is provided in the light receiving optical system 9.

[0005]

FIG. 3 shows a first embodiment of the present invention. In FIG. 3, reference numeral 1 denotes a laser projection optical system that irradiates the laser beam 2 horizontally, and includes a polarizing element 15 and a condenser lens 4 described later. Reference numeral 3 denotes an object crystal, 3a denotes a crystal surface of the object crystal 3, and 3b denotes an incident side surface orthogonal thereto. An objective lens 5 is provided on the crystal surface 3a of the sample crystal 3, and an imaging lens 7 is provided at an interval, and a narrow band transmission filter 6 having a band transmission characteristic between the objective lens 5 and the imaging lens 7 is provided. A polarizing element 16 is provided, and an imaging element 8 is provided at a position where an image is formed by the imaging lens 7. Reference numeral 9 denotes a light receiving optical system, 10 denotes an image processing device that processes image information picked up by the image pickup device 8, and 11 denotes a computer that controls necessary information. The laser projection optical system 1 includes a laser moving stage 1
The sample crystal 3 is mounted on a sample crystal moving stage 14, and the laser moving stage 13 and the sample crystal moving stage 14 are mounted on a stage controller 1.
2 is controlled.

FIG. 4 shows a second embodiment of the present invention, in which a condenser lens 4, an objective lens 5, an imaging lens 7, a narrow-band transmission filter 6, an image pickup device 8, an image processing device 10, and a computer 1.
1, laser movement stage 13, object crystal movement stage 14, stage controller 12, polarizing elements 15, 16
Is the same as FIG. 3, but the laser projection optical system 1 and the subject crystal 3 are different. That is, the laser projection optical system 1 is an example in the case of observing the sample crystal 3 from the crystal surface 3a.
The light is incident at an incident angle of 60 to 77 degrees (θ = 13 to 30 degrees), refracted downward on the crystal surface 3a, and enters the crystal at a refraction angle (α) of about 16 degrees. Since a part of the component of the incident laser beam 2 is reflected on the crystal surface, the observation is performed from a direction (β = 10 to 35 degrees) such that the reflected beam does not enter the image sensor 8.

The condensing lens 4 shown in FIGS. 3 and 4 condenses the laser beam 2 with a diameter of 3 to 20 μm. The narrow-band transmission filter 6 has a gorge band characteristic that allows only the fluorescence generated by the carrier excited by the projection laser light 2 in the subject crystal 3 to be selected and transmitted from the scattered light. In the case of silicon, since the wavelength of the generated fluorescence is 0.9 to 2 microns, the narrow band transmission filter 6 only needs to have transmission characteristics in this band.

Reference numeral 12 denotes a stage controller for controlling a laser moving stage 13 for changing the projection position of the projection laser or a crystal moving stage 14 for moving the crystal 3, and two-dimensionally controlling the state of fluorescence emission. The stage controller 12 two-dimensionally controls the positions of the laser light source 2 and the test object crystal 3 for two-dimensional observation, and analyzes two-dimensional imaging information from the obtained image information.

The polarizing element 15 for polarizing the scattered light of the projection laser light 2 or the polarizing element 16 for polarizing the received scattered light is rotated to obtain a required polarization state. Can be investigated. If the polarization elements 15 and 16 are adjusted to the azimuth at which the scattering intensity is minimized, weak fluorescence can be easily detected. In the example of FIG. 3, when the polarization direction (electric field direction) is parallel to the paper surface, the minute precipitate (diameter <
λ / 10) becomes smaller. The scattered light and the fluorescence have different polarization dependences. Generally, scattered light is strongly direction-dependent, while fluorescence tends to be direction-dependent or low. Therefore, when observing the fluorescent light, the polarization direction is set so that the scattered light becomes weak, and when observing the scattered light, the polarization direction is set to be strong, so that appropriate measurement can be performed.

In general, an interference film is applied to the surface of the band-pass narrow band-pass filter 6, and if the narrow band-pass filter 6 is rotated appropriately, the apparent interference film thickness changes and the transmission center wavelength Can be made variable. Therefore,
If the angle between the surface of the narrow-band transmission filter 6 and the optical axis is changed, the transmission center wavelength can be changed, so that the wavelength dependence of the state of generation of fluorescence can be examined. If an infinity-corrected lens is used as the objective lens 5, a parallel beam is formed between the objective lens 5 and the imaging lens 7 (omitted in FIG. 4), which is convenient for inserting the interference narrow-band transmission filter 6. Also, even if the interference narrow band transmission filter 6 is tilted,
No lateral displacement of the image occurs. FIG. 7 is a diagram showing a change in the center wavelength of transmitted light when the narrow-band interference transmission filter 6 is inclined with respect to the optical axis, and FIG. 8 is a graph showing changes in the peak transmittance and the half-value width when the center wavelength is changed. It is a figure showing a situation. In addition,
It is natural that the wavelength dependence of fluorescence can be easily measured by using a wavelength tunable laser.

FIG. 5 is a diagram schematically showing a state of generation of fluorescent light when the sample crystal 3 is irradiated with an excitation laser. FIG. 6 shows the spread of generated fluorescence (L) and the intensity of fluorescence (I).
Is a graph showing the penetration depth of laser light from the surface of the test object on the horizontal axis. By calculating L and I as a function of the depth from the crystal surface, the life of excited carriers (L
ife Time) can be evaluated as a function of depth.
Here, the spread (L) of the fluorescent image is calculated based on the position where the fluorescent intensity becomes 1 / e.

Generally, the diffusion coefficient of excited carriers is expressed as follows from Einstein's relational expression. _{D n = μ e k B T} / e, D p = μ p k B T / ek B is the Boltzmann constant, T is the temperature, e is the charge, mu _e is the electron mobility, mu _p is the hole mobility It is. The recombination lifetime (τ) of the minority carrier is given by the following equation. τ ⁻¹ = Nr · S · v _th where Nr is the density of recombination centers, S is the capture cross section, v
_th is the thermal velocity of the minority carrier. In conclusion, when the excited minority carrier travels the distance R, its existence probability becomes EXP (−R / M). Here, since there is a relationship of M = √ (D _n τ) between the diffusion length (M) of the carrier and the recombination lifetime (τ), if the spread (L) of the fluorescence intensity distribution can be measured, the carrier diffusion The distance (M) is obtained. That is, the position where the fluorescence intensity becomes 1 / e corresponds to M.

[0013]

According to the present invention, the crystal surface 3a and the crystal surface 3
the subject crystalline 3 having an incident side surface 3b of the intersecting direction with respect to a, the from the incidence side surface 3b with respect to the analyte crystals 3
Enters into the subject crystalline 3 from the crystal surface 3a relative or the crystal surface 3a is incident on the inside sample crystal 3 at an oblique angle cutlet a permeable to the subject crystalline 3
Wherein the laser projection optical system 1 for generating a laser beam 2 of excitable energy intensity carriers in the subject crystalline 3, a diaphragm that condensing lens 4 the laser beam 2 to the predetermined diameter, the
The key excited by the laser beam 2 in the specimen crystal 3
Carrier in the crystal 3
Objective lens 5 and imaging lens 7 for receiving fluorescence as light
And a light receiving optical system 9 consisting of the image pickup device 8, is provided et Re said excitation between said objective lens 5 of the image forming lens 7
A narrow-band transmission filter 6 having a narrow-band transmission characteristic for transmitting only fluorescence generated by carriers from scattered light.
And excited carriers are generated from the image sensor 8.
Since the photoluminescence measuring device in the crystal includes the image processing device 10 for processing the image information including the spread of the fluorescence and the computer 11 for controlling the necessary information, the crystal surface 3a and the incident side surface 3b orthogonal to the crystal surface 3a. the crystal surface 3a is incident to the inside at an oblique angle from, and subject the crystal 3 can transmit an a in and subject the crystal to 3 against or the crystal surface 3a is incident on the interior horizontally from
Laser beam 2 with energy intensity that can excite carriers in
, So both transmission into the crystal and carrier excitation are compatible
As a result, the internal fluorescence observation can be performed satisfactorily. Further, the excitation light is applied between the objective lens 5 and the imaging lens 7 which receive the generated light.
Since the narrow-band transmission filter 6 having the narrow-band transmission characteristic for transmitting only the fluorescence generated by the generated carrier from the scattered light is provided, the fluorescence can be observed well. In addition,
Akira describes a laser moving slider to which the laser projection optical system 1 is attached.
Movement of the test object to which the stage 13 and the test crystal 3 are attached
Moving stage 14, the laser moving stage 13 and the
Stage control for controlling the movement of the inspection object movement stage 14
Photoluminescence in crystals with trawler 12
Since the measuring device is used, the laser projection optical system 1 and the subject crystal 3 can be observed two-dimensionally by moving them two-dimensionally. Further, according to the present invention , since the polarizing element 15 is provided in the laser projection optical system 1 and the polarizing element 16 is provided in the light receiving optical system 9, it is possible to rotate the polarizing elements 15 and 16 to obtain a required polarization state. The polarization dependence of the fluorescence generated can be examined.

[Brief description of the drawings]

FIG. 1 shows a known fluorescence observation device.

FIG. 2 is an explanatory diagram showing the emission lifetime of fluorescence generated by a pulse laser.

FIG. 3 is a system diagram of a first embodiment of the present invention.

FIG. 4 is a system diagram of a second embodiment of the present invention.

FIG. 5 is a schematic diagram showing a state of generation of fluorescence.

FIG. 6 is a correlation diagram between the spread of a fluorescent image and the intensity.

FIG. 7 is a diagram showing a change in a transmission center wavelength when a filter is inclined.

FIG. 8 is a diagram illustrating a correlation between a center wavelength, a peak transmittance, and a half width with respect to a rotation angle of a filter.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... Laser projection optical system, 2 ... Laser light, 3 ... Test object crystal, 3a ... Crystal surface of test object crystal 3, 3b ... Side, 4 ...
Condensing lens, 5: objective lens, 6: narrow band transmission filter, 7: imaging lens, 8: imaging element, 9: light receiving optical system,
DESCRIPTION OF SYMBOLS 10 ... Image processing apparatus, 11 ... Computer, 12 ... Stage controller, 13 ... Laser moving stage, 14 ...
Object crystal moving stage, 15, 16 ... Polarizing element.

──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int.Cl. ⁷ , DB name) G01N 21/62-21/74 G01N 21/00-21/01 G01N 21/17-21/61 G01N 21 / 88 G01N 21/94 Practical file (PATOLIS) Patent file (PATOLIS)

Claims (3)

(57) [Claims] 1. A crystal surface 3a and the crystals between the subject crystalline 3 having an incident side surface 3b of the intersecting direction with respect to the surface 3a, analyte crystal 3 subject crystalline 3 from the incident side surface 3b with respect to
Or the crystal surface 3a the crystal surface 3a enters into the subject crystalline 3 at an oblique angle from the subject crystalline 3 in transmission possible even with and the subject against entering the interior
A laser projection optical system 1 for generating a laser beam 2 of excitable energy intensity carriers in the crystal 3, a diaphragm that condensing lens 4 the laser beam 2 to the predetermined diameter, the subject crystalline
In FIG. 3, carriers excited by the laser beam 2 are emitted.
The fluorescent light which is generated in the specimen crystal 3 by being generated
A light receiving optical system 9 consisting of the objective lens 5 and the imaging lens 7 and the imaging device 8 for receiving light, the objective lens 5 and is provided et Re said excited carriers between the imaging lens 7
A narrow-band transmission filter 6 having a narrow-band transmission characteristic for selectively transmitting only the generated fluorescence from the scattered light, and an increase in the width of the fluorescence generated by the excited carriers from the image sensor 8;
An apparatus for measuring photoluminescence in a crystal, comprising: an image processing apparatus 10 for processing image information including a laser beam; and a computer 11 for controlling necessary information. 2. The laser projection optical system according to claim 1, wherein
Laser moving stage 13 to which system 1 is attached and the object
A test object moving stage 14 on which the crystal 3 is mounted;
Of the moving stage 13 and the object moving stage 14
A connection provided with a stage controller 12 for controlling movement
Photoluminescence measurement device in the crystal. 3. A photoluminescence measuring apparatus according to claim 1 , wherein a polarizing element is provided in the laser projection optical system, and a polarizing element is provided in the light receiving optical system.