SILICON CARBIDE SEED CRYSTAL AND METHOD OF MANUFACTURING THE SAME, AND METHOD OF MANUFACTURING SILICON CARBIDE INGOT
20220025543 · 2022-01-27
Assignee
Inventors
Cpc classification
H01L29/30
ELECTRICITY
International classification
Abstract
A silicon carbide seed crystal and method of manufacturing the same, and method of manufacturing silicon carbide ingot are provided. The silicon carbide seed crystal has a silicon surface and a carbon surface opposite to the silicon surface. A difference D between a basal plane dislocation density BPD1 of the silicon surface BPD1 and a basal plane dislocation density BPD2 of the carbon surface satisfies the following formula (1):
D=(BPD1−BPD2)/BPD1≤25% (1).
Claims
1. A silicon carbide seed crystal, wherein the silicon carbide seed crystal comprises a silicon surface and a carbon surface opposite to the silicon surface, wherein a difference D between a basal plane dislocation density BPD1 of the silicon surface and a basal plane dislocation density BPD2 of the carbon surface satisfies a formula (1) as follows:
D=(BPD1−BPD2)/BPD1≤25% (1).
2. The silicon carbide seed crystal of claim 1, wherein the difference A BPD of the basal plane dislocation density between the silicon surface and the carbon surface is 20% or less.
3. The silicon carbide seed crystal of claim 1, wherein the difference A BPD of the basal plane dislocation density between the silicon surface and the carbon surface is 15% or less.
4. A method of manufacturing a silicon carbide seed crystal, comprising: disposing a silicon carbide based raw material in a crucible; disposing a silicon carbide seed crystal on a top of the crucible; heating the silicon carbide based raw material to form a thermal field in the crucible so that the silicon carbide based raw material is sublimated in the thermal field of the crucible, wherein a radial temperature gradient of the thermal field in the crucible is greater than or equal to 5° C./cm and less than or equal to 50° C./cm; growing a silicon carbide single crystal from the sublimed silicon carbide after being in contact with the seed crystal disposed on the top of the crucible; growing the silicon carbide single crystal on the seed crystal continuously to obtain silicon carbide ingots; and processing the obtained silicon carbide ingots to form a plurality of silicon carbide seed crystals, wherein the plurality of silicon carbide seed crystals comprise the silicon carbide seed crystals of claim 1.
5. A method of manufacturing silicon carbide seed crystals, comprising: disposing a silicon carbide based raw material in a crucible; disposing a silicon carbide seed crystal on a top of the crucible; heating the silicon carbide based raw material to form a thermal field in the crucible so that the silicon carbide based raw material is sublimated in the thermal field of the crucible, wherein a radial temperature gradient of the thermal field in the crucible is greater than or equal to 5° C./cm and less than or equal to 50° C./cm; growing a silicon carbide single crystal from the sublimed silicon carbide after being in contact with the seed crystal disposed on the top of the crucible; and growing the silicon carbide single crystal on the seed crystal continuously to obtain silicon carbide ingots; wherein the silicon carbide seed crystal located on the top of the crucible is a first crystal, the silicon carbide ingot obtained by the growth of the first seed crystal and processed to satisfy D≤25% is a second seed crystal, and a method of manufacturing the second seed crystal further comprises: disposing the second seed crystal on a top of a crucible to grow a silicon carbide single crystal on the second seed crystal to grow an Nth silicon carbide ingot; and reusing the second seed crystal to grow an N+1th silicon carbide ingot on the second seed crystal.
6. A method of manufacturing a silicon carbide ingot, comprising: disposing the second seed crystal of claim 5 on a top of a crucible; disposing a silicon carbide based raw material in the crucible; heating the silicon carbide based raw material so that the silicon carbide based raw material is sublimed in a thermal field of the crucible, wherein a radial temperature gradient of the thermal field in the crucible is greater than or equal to 5° C./cm and less than or equal to 50° C./cm; growing a silicon carbide single crystal from the sublimed silicon carbide after being in contact with the silicon carbide seed crystal; and growing the silicon carbide single crystal continuously on the silicon carbide seed crystal to obtain an N+1th silicon carbide ingot.
7. The method of manufacturing the silicon carbide ingot of claim 6, further comprising: processing the obtained silicon carbide ingot to form a reusable silicon carbide seed crystal and a plurality of silicon carbide wafers.
8. The method of manufacturing the silicon carbide ingot of claim 7, the processing comprises cutting, grinding or polishing, and a difference D of a basal plane dislocation density between the silicon surface and the carbon surface of the processed silicon carbide reusable seed crystal is 25% or less.
9. The method of manufacturing the silicon carbide ingot of claim 6, a basal plane dislocation density BPD of the unprocessed silicon carbide ingot is 300 EA/cm.sup.2 or less, a stacking fault (SF) density is 10 EA/cm.sup.2 or less, and a threading screw dislocation (TSD) density is 35 EA/cm.sup.2 or less.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
[0016]
[0017]
[0018]
[0019]
[0020]
DESCRIPTION OF THE EMBODIMENTS
[0021] The exemplary embodiments of the disclosure will be fully described below with reference to the drawings, but the disclosure may also be implemented in many different forms and should not be construed as being limited to the embodiments described herein. In the drawings, for clarity, a relative size, a thickness, and a location of each region, portion, and/or layer may not be necessarily drawn to scale.
[0022] <Silicon Carbide Seed Crystal>
[0023]
D=(BPD1−BPD2)/BPD1≤25% (1).
[0024] The silicon carbide seed crystal 10 has the silicon surface 10Si and the carbon surface 10C opposite to the silicon surface 10Si. With the silicon carbide seed crystal 10 satisfying the formula (1) of the disclosure, the basal plane dislocation density difference D between the growth surface and the surface opposite to the growth surface is controlled within a specific range, and accordingly the ingots grown based on that are ensured to have low defects. Moreover, each of the multiple silicon carbide seed crystals 10 obtained from processing the ingots can be reused in the crystal growth process and serve as seed crystals in another silicon carbide ingot manufacturing process for growing new silicon carbide ingots in the subsequent process. The growth surface of the silicon carbide seed crystal of the disclosure can be the silicon surface 10Si or the carbon surface 10C; the processing process can include cutting, grinding, and polishing; the silicon carbide seed crystal 10 can be 6H silicon carbide or 4H silicon carbide; and the disclosure is not limited thereto.
[0025] Taking the carbon surface 10C as the growth surface as an example, in the disclosure, the relationship between the basal plane dislocation density BPD2 of the carbon surface 10C as the growth surface in the silicon carbide seed crystal 10 and the basal plane dislocation density BPD1 of the silicon surface 10Si which is the other side of the silicon carbide seed crystal 10 satisfies formula (1), so in ingot growth process, this can solve the defect problem resulting from the ingots growing in different directions due to the poor quality of the seed crystal during the crystal growth process, especially the problem of a higher density of defects around the seed crystal of the ingots obtained in the example. If there are many defects in the silicon carbide ingots, the silicon carbide wafers cut from the silicon carbide ingots may also have the defects and cannot be used as silicon carbide seed crystals 10. Taking the basal plane dislocation density as an example, the basal plane dislocation density of the obtained silicon carbide ingot may extend to the epitaxial layer, causing shockley-type stacking faults in various layers of the epitaxial layer, resulting in increased leakage current of the element, reducing the performance of the electronic element, and reducing the number of the yield of elements available. When the growth surface is the silicon surface 10Si, the growth mechanism and trend are the same as the above, which is not iterated herein. In the embodiment, for example, the thickness of the silicon carbide seed crystal 10 ranges from 8 mm to 50 mm, preferably 17 mm to 20 mm.
[0026] In the embodiment, for example, the detection of the basal plane dislocation density (BPD) can be analyzed with the following methods. The silicon carbide ingot is etched with KOH at 500° C., and then a measuring instrument such as automated optical inspection (AOI) instrument is used to calculate the number of BPD per unit area. The AOI instrument is a high-speed and high-precision optical image inspection system including applications such as measurement lens technology, optical lighting technology, positioning measurement technology, electronic circuit testing technology, image processing technology, automation technology, and the like. The AOI instrument uses machine vision as the testing standard technology. The measuring instrument uses optical instruments to obtain the surface condition of a finished product, and then computer image processing technology is used to detect defects such as foreign objects or abnormal patterns.
[0027] In the embodiment, the difference D between the basal plane dislocation density of the silicon surface 10Si and the basal plane dislocation density of the carbon surface 10C is 25% or less, preferably 20% or less, more preferably 15% or less, 10% or less, and most preferably 5% or less. In other embodiments, it may be 3% to 5%, 3% to 10%, 3% to 25%, 5% to 10%, 5% to 25%, and 10% to 25%. The basal plane dislocation density BPD1 of the silicon surface 10Si in the silicon carbide seed crystal 10 can range from 70 to 300 EA/cm.sup.2, preferably 70 to 200 EA/cm.sup.2. In other embodiments, it can range from 70 to 130 EA/cm.sup.2, or 70 to 90 EA/cm.sup.2. The basal plane dislocation density BPD2 of the carbon surface 10C in the silicon carbide seed crystal 10 can range from 70 to 300 EA/cm.sup.2, preferably 70 to 170 EA/cm.sup.2. In other embodiments, it may be 70 to 120 EA/cm.sup.2, or 70 to 90 EA/cm.sup.2, but the disclosure is not limited thereto.
[0028] In the embodiment, the processing process of the silicon carbide seed crystal 10 may include cutting, grinding, polishing, etching, and/or the like, and the disclosure is not limited thereto.
[0029] The manufacturing method for forming the silicon carbide seed crystal is illustrated in the following paragraphs.
[0030] <The Manufacturing Method for Forming the Silicon Carbide Seed Crystal of a Silicon Carbide Ingot>
[0031]
[0032] Referring to
[0033] More specifically, referring to
[0034] Next, in step S240, the obtained silicon carbide ingot is processed to form multiple silicon carbide seed crystals 10 as shown in
[0035] Therefore, according to the method of manufacturing the silicon carbide seed crystal of the disclosure, by controlling the radial temperature gradient of the thermal field in the crucible to be less than or equal to 50° C./cm, the difference between the basal plane dislocation density of the two opposing surfaces of the seed crystal obtained by cutting the silicon carbide ingot grown by the method can be 25% or less, that is, the difference between the basal plane dislocation density of the carbon surface and the silicon surface of the seed crystal.
[0036]
[0037] Referring to
[0038] Generally, the PVT device has a furnace 100 including a graphite crucible 102 and a crystal carrier 104. A silicon carbide based raw material 106 is disposed at the bottom of the graphite crucible 102. Moreover, in the embodiment, in the implementation in which silicon carbide ingots are grown by reusable silicon carbide seed crystals, the silicon carbide seed crystals 10 are disposed on the crystal carrier 104. In the embodiment, the surface of the carbon surface 10C of the silicon carbide seed crystal 10 facing the silicon carbide based raw material 106 is served as a growth surface 112. In the implementation of manufacturing silicon carbide seed crystals in other embodiments, the silicon carbide seed crystal 10 can also be redisposed by an original seed crystal 2, and the disclosure is not limited thereto. An induction coil 114 is further disposed outside the graphite crucible 102 for heating the silicon carbide based raw material 106 in the graphite crucible 102.
[0039] In
[0040] Note that in the manufacturing method of the silicon carbide seed crystal 10 of the disclosure, as shown in
[0041] <The Method of Manufacturing Silicon Carbide Ingots by Using the Reusable Silicon Carbide Seed Crystals>
[0042]
[0043] Referring to
[0044] More specifically, referring to
[0045] Moreover, as shown in
[0046] <Re-Use of the Silicon Carbide Seed Crystal 10>
[0047]
[0048] Referring to
[0049] Next, referring to
[0050] Moreover, as shown in
[0051] Based on the above, the silicon carbide seed crystal 10 of the disclosure can control the basal plane dislocation density difference between the silicon surface 10Si and the carbon surface 10C, so that the crystal growth direction can be consistent, and high-quality silicon carbide ingots with fewer defects can be produced. Moreover, by using the manufacturing method of silicon carbide seed crystal 10 of the disclosure, high-quality silicon carbide ingots with fewer defects can be manufactured, and the obtained silicon carbide seed crystal 10 after being processed can be reused to reduce the cost of silicon carbide growth.
[0052] Several experiments are illustrated below to verify the efficacy of the disclosure, but the experimental content is not intended to limit the scope of the disclosure.
Preparation Example 1-9
[0053] In the device shown in
[0054] <Analysis of Seed Crystal Defects>
[0055] Basal Plane Dislocation (BPD) density analysis: the silicon carbide ingot is cut into multiple wafers, the wafers are etched with KOH at 500° C., and then a measuring instrument such as automated optical inspection (AOI) instrument is used to calculate the BPD density of the silicon surface 10Si and the carbon surface 10C of the silicon carbide seed crystal 10 per unit area. The results are shown in Table 1.
[0056] <Polishing Conditions>
[0057] The silicon carbide wafer is processed by chemical mechanical polishing (CMP) to form the silicon carbide seed crystal 10. The pressure during CMP is greater than 15 g/cm.sup.2, the polishing speed is not less than 15 rpm, and the time is about 0.5 hour.
[0058] <The Base Dislocation Density (BPD) of the Seed Crystal>
[0059] The basal plane dislocation density is measured for the grown silicon carbide ingot, and the measured results are shown in Table 1 below. The basal plane dislocation density BPD evaluation of the seed crystal is as follows:
[0060] The basal plane dislocation density BPD of the seed crystal measured to be greater than 300 EA/cm.sup.2 is evaluated as NG, which represents poor quality, and the value less than or equal to 300 EA/cm.sup.2 is evaluated as G, which represents good quality.
TABLE-US-00001 TABLE 1 Preparation Comparative examples Embodiments Examples 1 2 3 1 2 3 4 5 6 Seed 1403 1353 1295 118 285 213 158 86 79 Crystal BPD 1 (EA/cm.sup.2) Seed 1105 976 998 109 229 172 141 82 76 Crystal BPD 2 (EA/cm.sup.2) D 26.97% 38.63% 29.76% 8.26% 24.45% 23.84% 12.06% 4.88% 3.95% temperature 65 85 70 15 25 30 50 5 10 gradient (50° C./cm) ingot SF 25 22 23 6 8 10 9 3 5 density (EA/cm.sup.2) Ingot BPD 1451 1958 1898 95 203 156 102 76 71 density (EA/cm.sup.2) Ingot TSD 198 153 185 30 25 31 30 23 26 density (EA/cm.sup.2) Evaluation NG NG NG G G G G G G
[0061] As the silicon carbide seed crystals shown in comparative examples 1 to 3 in Table 1, when the seed crystal with the basal plane dislocation density difference D between the silicon surface and the carbon surface greater than 25% is used to grow silicon carbide ingots, the quality of the silicon carbide ingots processed is not good, which cannot be used to grow silicon carbide seed crystals that can be reused in the next batch. In contrast, as the silicon carbide seed crystals shown in Examples 1 to 6 in Table 1, when the seed crystal with the basal plane dislocation density difference D between the silicon surface and the carbon surface less than or equal to 25% is used to grow silicon carbide ingots, the quality of the silicon carbide ingots is good, and silicon carbide seed crystals processed from the silicon carbide ingots can be reused, thereby reducing the cost of silicon carbide growth. Moreover, according to the comparison between the quality of silicon carbide ingots grown from the silicon carbide seed crystals of Examples 1 to 6 and that of silicon carbide ingots grown from the silicon carbide seed crystals of Comparative Examples 1 to 3, when the temperature gradient is less than or equal to 50° C./cm, the seed crystal growth process is more stable and there are fewer defects. However, if the temperature gradient is less than 5° C./cm, seed crystals cannot be grown. Moreover, if the temperature gradient is too low, it takes long time to process crystals, and the temperature gradient may preferably be greater than or equal to 5° C./cm. On the contrary, if the temperature gradient is too high, the crystal growth may be fast, which may cause more defects in the grown silicon carbide ingots, which may affect the crystal quality and the yield of the subsequent processing process. Therefore, the temperature gradient should preferably be less than or equal to 50° C./cm.
[0062] In summary, since the silicon carbide seed crystal of the disclosure has the basal plane dislocation density difference D between the growth surface and the opposite surface less than or equal to 25%, the silicon carbide ingot grown from the silicon carbide seed crystal has a basal dislocation density BPD less than 300/cm.sup.2, or preferably a basal dislocation density BPD less than 900/cm.sup.2, and thus the quality of the film layer formed by subsequent epitaxy is ensured. Moreover, by using the silicon carbide seed crystals of the disclosure to grow seed crystals, the grown silicon carbide ingots can be used again as silicon carbide seed crystals due to their low defect characteristics after processing, thereby reducing the cost of crystal growth.
[0063] Although the disclosure has been described with reference to the above embodiments, they are not intended to limit the disclosure. It will be apparent to one of ordinary skill in the art that modifications and changes to the described embodiments may be made without departing from the spirit and the scope of the disclosure. Accordingly, the scope of the disclosure will be defined by the attached claims and their equivalents and not by the above detailed descriptions.