Epitaxial silicon wafer
10020203 ยท 2018-07-10
Assignee
Inventors
Cpc classification
H01L21/3225
ELECTRICITY
H01L29/16
ELECTRICITY
H01L29/365
ELECTRICITY
C30B15/203
CHEMISTRY; METALLURGY
H01L21/0262
ELECTRICITY
International classification
H01L23/58
ELECTRICITY
H01L21/02
ELECTRICITY
H01L29/36
ELECTRICITY
H01L21/322
ELECTRICITY
H01L29/16
ELECTRICITY
Abstract
An epitaxial silicon wafer includes a silicon wafer consisting of a COP region in which a nitrogen concentration is 110.sup.12110.sup.13 atoms/cm.sup.3, and an epitaxial silicon film formed on the silicon wafer. When heat treatment for evaluation is applied, a density of BMD formed inside the silicon wafer is 110.sup.8310.sup.9 atoms/cm.sup.3 over the entire radial direction of the silicon wafer. An average density of the BMD formed in an outer peripheral region of the silicon wafer which is a 1-10 mm range separated inward from an outermost periphery thereof is lower than the average density of the BMD formed in a center region. A variation in the BMD density in the outer peripheral region is 3 or less, and a residual oxygen concentration in the outer peripheral region is 810.sup.17 atoms/cm.sup.3 or more.
Claims
1. An epitaxial silicon wafer comprising: a silicon wafer consisting of a crystal oriented particle region in which a nitrogen concentration is from 110.sup.12 atoms/cm.sup.3 to 110.sup.13 atoms/cm.sup.3; and an epitaxial silicon film formed on a surface of the silicon wafer, wherein when treatment for evaluating oxygen precipitates is applied to the epitaxial silicon wafer, a density of oxygen precipitates formed inside the silicon wafer is from 110.sup.8 atoms/cm.sup.3 to 310.sup.9 atoms/cm.sup.3 over the entire radial direction of the silicon wafer, an average density of the oxygen precipitates formed in an outer peripheral region of the silicon wafer within 1-10 mm separated inward from an outermost periphery thereof is lower than an average density of the oxygen precipitates formed in a center region of the silicon wafer which is the region of the silicon wafer other than the outer peripheral region, a value obtained by dividing a difference between a maximum value and a minimum value of the density of the oxygen precipitates in the outer peripheral region by an average value of the density of the oxygen precipitates in the outer peripheral region is 3 or less, and a residual oxygen concentration in the outer peripheral region is 810.sup.17 atoms/cm.sup.3 or more as measured by Old-ASTM_F121, 1979.
2. The epitaxial silicon wafer as claimed in claim 1, wherein the maximum value of the density of the oxygen precipitates exists in a region separated inward from the outermost periphery from 6 mm to 10 mm, and the minimum value of the density of the oxygen precipitates exists in a region separated inward from the outermost periphery from 0 to less than 6 mm.
3. The epitaxial silicon wafer as claimed in claim 2, wherein the density of the oxygen precipitates in the outer peripheral region is gradually reduced toward the outermost periphery of the silicon wafer.
4. The epitaxial silicon wafer as claimed in claim 1, wherein when heat treatment for evaluating oxidation-induced stacking fault is applied, the density of oxidation-induced stacking fault observed on the back surface of the epitaxial silicon wafer is 100/cm.sup.2 or less.
5. The epitaxial silicon wafer as claimed in claim 1, wherein the silicon wafer is cut out from a silicon single crystal ingot whose oxygen concentration is adjusted in a range of from 810.sup.17 atoms/cm.sup.3 to 1410.sup.17 atoms/cm.sup.3 or less, as measured by Old-ASTM_F121, 1979.
6. The epitaxial silicon wafer as claimed in claim 1, wherein a diameter of the epitaxial silicon wafer is 300 mm or more.
7. The epitaxial silicon wafer as claimed in claim 1, wherein the silicon wafer is cut out from a straight body section of a silicon single crystal ingot having a diameter 1.02 to 1.07 times larger than a target diameter and processed into the target diameter.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
(1) The above features and advantages of the present invention will be more apparent from the following description of certain preferred embodiments taken in conjunction with the accompanying drawings, in which:
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DETAILED DESCRIPTION OF THE EMBODIMENTS
(11) Preferred embodiments of the present invention will be described hereinafter in detail with reference to the accompanying drawings.
(12)
(13) As illustrated in
(14)
(15) As illustrated in
(16) When the silicon single crystal 10 is grown by the CZ method, the type and distribution of the defect contained in the single crystal depend upon a ratio V/G between a single crystal pull-up speed V and a temperature gradient G in a single crystal growing direction.
(17)
(18) As illustrated in
(19) Normally, when the V/G is large, the OSF is generated in a ring shape around the center axis of a silicon single crystal, so that it is also called R-OSF region. The range of the V/G where the R-OSF region appears is very narrow, so that it is necessary to strictly manage the pull-up speed V in the manufacturing process of the silicon single crystal 10 containing the R-OSF region. That is, control needs to be performed so that the V/G falls within an adequate range in both the diameter direction and length direction of the crystal. For the diameter direction of the single crystal, the pull-up speed V is constant at any position in the diameter direction, so that the structure of a hot zone in a CZ furnace should be designed so that the temperature gradient G falls within a predetermined range. For the length direction, the temperature gradient G depends upon a pull-up distance, so that the V should be changed in the crystal length direction in order to keep the V/G within a predetermined range.
(20) Then, a pull-up speed profile is set so that the R-OSF region is contained in the silicon single crystal, and Cu (copper) decoration and heat treatment for OSF evaluation are applied to a wafer sample cut out from the pulled-up silicon single crystal to evaluate the width or position of the OSF region. Then, based on the width or position, subsequent pull-up speed profile is adjusted. That is, a wider R-OSF region means an excessively large V/G (V is excessively large), so that the V is set relatively low as the subsequent pull-up profile; conversely, a narrower R-OSF region means an excessively small V/G (V is excessively small), so that the V is set relatively high as the subsequent pull-up profile.
(21) As described above, by adjusting the subsequent pull-up speed profile using the width or position of the R-OSF region as an index, the silicon single crystal 10 containing the R-OSF region in the outer peripheral grinding region 11 can be stably pulled up. Crystal heat hysteresis at this time is preferably as follows: a temperature range of 1080 C. to 1150 C. for 40 minutes or less; a temperature range of 980 C. to 1020 C. for 30 minutes or less; and a temperature range of 650 C. to 750 C. for 150 minutes or less.
(22) The silicon single crystal 10 is doped with nitrogen of 110.sup.12 atoms/cm.sup.3 or more and 110.sup.13 atoms/cm.sup.3 or less. The doping of nitrogen can increase the BMD density in the wafer surface, thereby enhancing the gettering capability of the epitaxial silicon wafer.
(23) The nitrogen doping amount is preferably 110.sup.13 atoms/cm.sup.3 or less. By increasing the doping amount, the BMD density on the entire wafer surface can be increased, and thus required gettering capability can be easily ensured; on the other hand, however, the BMD density is further increased in the wafer outer peripheral region 21 illustrated in
(24)
(25) As illustrated in
(26) Thus, in the present embodiment, in order to position the R-OSF region within the outer peripheral grinding region 11 outside the silicon wafer 20, the nitrogen doping amount is reduced as much as possible to reduce the BMD density of the wafer outer peripheral region 21 to a low value, and the width of the R-OSF region is narrowed as much as possible. Further, as described later, by positioning a part of the R-OSF region near the outer peripheral region 21 at the boundary portion thereof, the BMD density of the outer peripheral region 21 can be reduced, so that it is possible to enhance the strength of the outer peripheral region 21 to thereby suppressing occurrence of the slip dislocation.
(27) Subsequently, the silicon single crystal is processed to obtain a silicon wafer (polished wafer) (step S12 of
(28) The COP region means a region where the COP is detected by observation/evaluation to be described below. First, SC-1 cleaning (cleaning using a liquid mixture obtained by mixing ammonia water, hydrogen peroxide water, and ultrapure water in a ratio of 1:1:15) is applied to the silicon wafer. Then, the surface of the silicon wafer after the cleaning is observed/evaluated using a surface defect inspection apparatus (e.g., KLA-Tencor: Surfscan SP-2) to specify a LPD (Light Point Defect) estimated as surface pits. At this time, an observation is set to an Oblique mode (oblique incidence mode), and estimation of the surface pits is made based on a detection size ratio between wide and narrow channels. Then, whether the thus specified LPD is the COP is evaluated using an AFM (Atomic Force Microscope). Through this observation/evaluation, a region having the COP is defined as the COP region.
(29) Whether the entire surface of the obtained silicon wafer is the COP region can be confirmed by applying heat treatment for evaluation (heat treatment for evaluation of oxidation-induced stacking fault) to a wafer sample (step S13 of
(30) Subsequently, annealing treatment (pre-annealing) for growing BMD nuclei is performed (step S14 of
(31) Further, in the present embodiment, the BMD density in the wafer outer peripheral region 21 can be reduced by positioning the R-OSF region within the outer peripheral grinding region 11.
(32)
(33) As illustrated in
(34) With attention paid to such a phenomenon that the BMD density is reduced, the present embodiment aims at reducing the BMD density in the wafer outer peripheral region 21 by positioning the R-OSF region within the outer peripheral grinding region 11 of the silicon single crystal and positioning the region in the vicinity of the boundary between the R-OSF region and the COP region where the BMD density is reduced within the wafer outer peripheral region 21.
(35) Subsequently, an epitaxial process for forming a silicon epitaxial film on the surface of the silicon wafer is performed (step S15 of
(36) The BMD density distribution of the thus produced epitaxial silicon wafer can be confirmed by performing heat treatment for evaluation (heat treatment for evaluation of oxygen precipitates) simulating the device process to grow the BMD nuclei (step S16). The BMD density is defined as follows. The heat treatment for evaluation of oxygen precipitates is applied to the epitaxial silicon wafer at 900 C. to 1100 C. for 16 hours in an oxygen gas atmosphere. Then, the epitaxial silicon wafer is cleaved in the thickness direction thereof, and selecting etching is performed to etch the cleaved cross section thereof by a depth of 2 m using a Wright etching liquid. Thereafter, the cleaved cross section in the thickness direction center of the silicon wafer is observed using an optical microscope, and an etch pit density in a 100 m100 m square area is defined as the BMD density. The epitaxial silicon wafer according to the present embodiment has the following features in terms of the BMD density.
(37) First, the BMD density on the entire wafer surface is 110.sup.8/cm.sup.3 or more. This makes it possible to enhance the gettering capability of the epitaxial silicon wafer. Preferably, the BMD density on the entire wafer surface is 310.sup.9/cm.sup.3 or less. When the BMD density of the wafer is excessively high, the residual oxygen concentration in the wafer is reduced to decrease wafer strength, with the result that slip dislocation easily occurs especially in the wafer outer peripheral region 21.
(38) The BMD density in the wafer outer peripheral region 21 which is the 1 mm to 10 mm range separated inward from the outermost periphery (outermost peripheral edge) of the wafer is lower than the BMD density in the center region inside the wafer outer peripheral region 21. With this configuration, the residual oxygen concentration in the wafer outer peripheral region 21 can be increased to thereby suppress occurrence of the slip dislocation.
(39) Further, the BMD density in the wafer outer peripheral region 21 which is the 1-10 mm range separated inward from the outermost periphery is gradually reduced toward the wafer outermost periphery, and a value ((MaxMin/Ave): variation in the BMD density) obtained by dividing a difference between the maximum value (Max) and the minimum value (Min) of the BMD density in the wafer outer peripheral region 21 by an average value (Ave) of the BMD density in the wafer outer peripheral region 21 is 3 or less. Further, the maximum value of the BMD density exists in a 6-10 mm range separated inward from the wafer outermost periphery, and the minimum value of the BMD density exists in a 0-less than 6 mm range separated inward from the wafer outermost periphery. Such a reduction in the BMD density in the wafer outer peripheral region 21 can increase the residual oxygen concentration to thereby enhance the strength of the wafer outer peripheral region 21. The reason that the wafer outer peripheral region 21 is separated inward from the outermost periphery by 1 mm or more is not only that the wafer edge is chamfered, but also that it is impossible to measure the BMD density at the outermost periphery (0 mm position from the outermost periphery).
(40) The residual oxygen concentration in the wafer outer peripheral region 21 is 810.sup.17 atoms/cm.sup.3 or more. With this configuration, it is possible to suppress occurrence of the slip dislocation. The residual oxygen concentration in the wafer is higher in a region where the BMD density is lower and lower in a region where the BMD density is higher. This is considered because oxygen in the wafer is consumed for BMD formation, and the residual oxygen is reduced as the oxygen precipitates increase. In the present invention, the BMD density in the wafer outer peripheral region 21 is low, so that the residual oxygen concentration in the wafer outer peripheral region 21 can be increased to thereby enhance the wafer strength in the wafer outer peripheral region 21.
(41) As described above, in the epitaxial silicon wafer according to the present embodiment, the BMD density in the wafer outer peripheral region 21 is low, so that the strength of the wafer outer peripheral region 21 can be enhanced to thereby suppress occurrence of the slip dislocation. Thus, during heat treatment of the wafer in a vertical furnace, it is possible to prevent occurrence of a minute flaw at a support position for the wafer housed in a vertical boat, which thereby prevents the slip dislocation from occurring with the flaw as a starting point and spreading.
(42) While the preferred embodiment of the present invention has been described, the present invention is not limited to the above embodiment, but various modifications may be made without departing from the scope of the invention, and such modifications may be included within the scope of the present invention.
(43) For example, although the wafer has a diameter of 300 mm in the above embodiment, the wafer diameter only needs to be 300 mm or more and, for example, may be 450 mm.
EXAMPLES
(44) First, the characteristics of the epitaxial silicon wafers were evaluated with nitrogen concentration, oxygen concentration, and presence/absence of pre-annealing as parameters.
(45) In this characteristic evaluation, a nitrogen-doped silicon single crystal having a diameter of 310 mm was grown by the CZ method, followed by outer periphery grinding to reduce the diameter of the silicon single crystal to 300 mm to show a round shape, and then by wafer processing. Then, before epitaxial process, heat treatment was applied, as pre-annealing, to some wafer samples at 890 C. for 20 minutes. In the epitaxial process, an epitaxial silicon film of 4 m thickness was formed at 1100 C.
(46) In BMD density measurement, after heat treatment for evaluation was performed at 1000 C. for 16 hours in an oxygen gas atmosphere, the epitaxial silicon wafer was cleaved in the thickness direction thereof, and then selecting etching was performed to etch the cleaved cross section thereof by a depth of 2 m using a Wright etching liquid. Thereafter, the cleaved cross section in the thickness direction center of the silicon wafer was observed using an optical microscope to measure the BMD density. The BMD density was measured at a 10 mm pitch radially from the wafer center. In particular, in the wafer outer peripheral region (1-10 mm range separated inward from the outermost periphery), the measurement was performed at a 1 mm pitch.
(47) The residual oxygen concentration in the epitaxial silicon wafer was measured at a 1 mm pitch in the radial direction from the wafer center, and the average value was calculated.
(48) In slip-resistance test, additional heat treatment was performed for evaluation of thermal stress loading in a boat-shaped vertical furnace supporting the outer peripheral region of the wafer. Conditions of the evaluation heat treatment were: feeding temperature of 700 C.; temperature rising rate of 8 C./min; holding temperature and holding time of 1100 C. and 30 minutes, respectively; temperature falling rate of 3 C./min; and take-out temperature of 700 C. Then, a wafer after the heat treatment was observed by X-ray topography. Evaluation was made in terms of the length of the slip dislocation: o, 2 mm or less; , 2 mm to 5 mm; and x, exceeding 5 mm.
(49) In gettering capability evaluation, Ni was applied onto the surface of the epitaxial silicon wafer after evaluation heat treatment by 110.sup.12 atoms/cm.sup.2, followed by heat treatment at 900 C. for 30 minutes, and then, the wafer surface was Wright-etched by 2 m. Then, the Wright-etched wafer surface was observed through an optical microscope. Evaluation was made in terms of the present/absence of Ni silicide pits: o, absence; and x, presence.
(50) The results of the above evaluation test are shown in
(51) As is clear from.
(52) On the other hand, Comparative Example 1 has a low nitrogen concentration and has not been subjected to pre-annealing, resulting in low BMD density and poor gettering capability.
(53) Comparative Example 2 has not been subjected to pre-annealing, but it shows a high nitrogen concentration of 510.sup.13 atoms/cm.sup.3, so that the BMD density exhibiting sufficient gettering capability is obtained, while the minimum residual oxygen concentration in the wafer outer peripheral region is as low as 7.810.sup.17 atoms/cm.sup.3. Further, a variation ((Max/Min)/Ave) in the BMD density in the wafer outer peripheral region is as large as 3.8, resulting in an increase in slip dislocation length. This is considered because the excessively large variation in BMD density in the wafer outer peripheral region changes heat transfer at the wafer support position, causing increase in thermal stress.
(54) Comparative Example 3 is similar to Comparative Example 2, but the residual oxygen concentration thereof in the wafer outer peripheral region is 7.510.sup.17 atoms/cm.sup.3, which is as low as lower than 810.sup.17 atoms/cm.sup.3, and a variation ((Max/Min)/Ave) in the BMD density is as large as 5.7, resulting in a further increase in the slip dislocation length.
(55) Comparative Examples 4 and 5 show results obtained when using a wafer having a nitrogen concentration higher than 110.sup.13 atoms/cm.sup.3 and applying pre-annealing to the wafer. The BMD density exceeding 310.sup.9/cm.sup.3 is observed in the wafer. Excessive BMD formation is undesirable since it induces an epitaxial defect due to the BMD. In addition, the BMD density in the water outer peripheral region is high, and residual oxygen concentration in the wafer outer peripheral region is low, resulting in poor slip resistance.
(56)
(57) As illustrated in
(58) In Comparative Example 2, the BMD density is increased toward the wafer outer periphery, and the BMD density in the outer peripheral region is as high as 110.sup.1/cm.sup.3 or more. Thus, the residual oxygen concentration is reduced due to high BMD density, resulting in poor slip resistance.
(59) The above results show that the BMD density is desirably 110.sup.8/cm.sup.3 or more (and 110.sup.9/cm.sup.3 or less) in the wafer surface and has a surface distribution in which it is gradually reduced in the wafer outer peripheral region.
(60)
(61) Secondly, the characteristics of the epitaxial silicon wafers produced using a plurality of silicon single crystals having different nitrogen concentrations and diameters were evaluated.
(62) In this characteristic evaluation, a plurality of silicon single crystals having different nitrogen concentrations were grown by the CZ method, followed by outer periphery grinding to reduce the diameter of each silicon single crystal to 300 mm, and then by wafer processing. In the growing process of the silicon single crystal, a portion having a wide outer periphery grinding region and a portion having a narrow outer periphery grinding region were made to be included in one silicon single crystal ingot by changing the crystal diameter.
(63) Then, the maximum value of the OSF density of the processed wafer (polished wafer) was measured. In the OSF density measurement, heat treatment for evaluation was performed at 1140 C. for two hours, followed by 2 m Wright etching. After that, the OSF density on the wafer surface was measured using an optical microscope.
(64) Then, before epitaxial process, heat treatment was applied, as pre-annealing, to the silicon wafer at 890 C. for 20 minutes. In the epitaxial process, an epitaxial silicon film of 4 m thickness was formed at 1100 C.
(65) In BMD density measurement, after heat treatment for evaluation was performed at 1000 C. for 16 hours in an oxygen gas atmosphere, the epitaxial silicon wafer was cleaved in the thickness direction thereof, and then selecting etching was performed to etch the cleaved cross section thereof by a depth of 2 m using a Wright etching liquid. Thereafter, the cleaved cross section in the thickness direction center of the silicon wafer was observed using an optical microscope to measure the BMD density. The BMD density was measured at a 10 mm pitch radially from the wafer center. In particular, in the wafer outer peripheral region (1-10 mm range separated inward from the outermost periphery), the measurement was performed at a 1 mm pitch.
(66) In slip-resistance test, additional heat treatment was performed for evaluation of thermal stress loading in a boat-shaped vertical furnace supporting the outer peripheral region of the wafer. Conditions of the evaluation heat treatment were: feeding temperature of 700 C.; temperature rising rate of 8 C./min; holding temperature and holding time of 1100 C. and 30 minutes, respectively; temperature falling rate of 3 C./min; and take-out temperature of 700 C. Then, a wafer after the heat treatment was observed by X-ray topography. Evaluation was made in terms of the length of the slip dislocation: o, 2 mm or less; , 2 mm to 5 mm; and x: exceeding 5 mm.
(67) The results of the above evaluation test are shown in
(68) As is clear from
(69) On the other hand, in the Comparative Examples 1 to 3, the diameter ratio of the silicon single crystal is as low as 1.01, and the maximum value of the OSF density is as large as 109 to 163/cm.sup.2. Thus, it can be understood that the R-OSF region exists not only in the outer periphery grinding region of the silicon single crystal, but also inside the silicon wafer, with the result that an epitaxial defect is induced to degrade epitaxial quality.
(70) In Comparative Examples 4 to 6, the nitrogen concentration is as high as 1.910.sup.13 to 9.510.sup.13 atoms/cm.sup.3, so that the width of the OSF ring is increased. Thus, even when a silicon single crystal having the diameter ratio of 1.05 is subjected to rounding processing, the R-OSF region cannot be removed, resulting in very high OSF density, which in turn induces an epitaxial defect. Further, the BMD density in the wafer outer peripheral region is high, and its variation is 3 or more, resulting in poor slip resistance.
(71) In Comparative Examples 7 to 9 as well, the nitrogen concentration is as high as 1.910.sup.13 to 9.510.sup.13 atoms/cm.sup.3, while the diameter ratio of the silicon single crystal is as large as 1.08, so that the R-OSF region can be removed by rounding processing. However, the BMD density in the wafer outer peripheral region is high, and the residual oxygen concentration in the wafer outer peripheral region is low, resulting in poor slip resistance. Further, the diameter of the silicon single crystal needs to be 324 mm. Accordingly, more silicon raw material is required for wafer manufacturing, resulting in poor productivity and thus in low suitability for mass production.