CN102817083A - Annealing method for SiC wafer - Google Patents
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- CN102817083A CN102817083A CN2012103526908A CN201210352690A CN102817083A CN 102817083 A CN102817083 A CN 102817083A CN 2012103526908 A CN2012103526908 A CN 2012103526908A CN 201210352690 A CN201210352690 A CN 201210352690A CN 102817083 A CN102817083 A CN 102817083A
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Abstract
The invention relates to an annealing method for an SiC wafer. The method comprises the following steps of: firstly, putting the SiC wafer into a ceramic tool; putting the ceramic tool into a ceramic crucible; filling SiC powder into the middle part of the ceramic tool and the ceramic crucible; directly raising the temperature to be between 200 and 400 DEG C in a low temperature area; keeping the temperature for 3-6 hours; keeping the temperature raising time to be more than or equal to 1.5 hours in the step; raising the temperature to between 500 and 700 DEG C in a middle temperature area after the temperature is preserved; keeping the temperature for 5-10 hours; keeping the temperature raising time to be more than or equal to 2.5 hours in the step; raising the temperature to be between 800 and 1,900 DEG C in a high temperature area after the intermeidate temperature is preserved; keeping the temperature for 10-20 hours; keeping the temperature raising time to be more than or equal to 10 hours in the step; reducing the temperature to be room temperature in a mode of 10-15 DEG C every hour after the high temperature preservation is finished; and enabling the product to be out of furnace. By the wafer which is annealed by adopting the method, the processing stress is substantially eliminated, the whole wafer is uniformly annealed, and the wrapping and the bending of the wafer caused by the processing stress generated by the processing of the wafer are reduced.
Description
Technical field
The present invention relates to a kind of annealing process of SiC wafer.
Background technology
The SiC crystal is a ultra-high brightness LED luminescent material GaN substrate material commonly used; And GaN brilliant crystal mass and employed SiC substrate (substrate) suface processing quality of heap of stone is closely related; Especially being used for surface topography and warpage and the degree of crook of SiC substrate and wafer of photoetching gets in touch closely; The warpage and the degree of crook of wafer are excessive, are difficult to during photoetching focus on, and cause yield to descend; If it is of heap of stone brilliant directly to be GaN with plain film, plain film and epitaxial film very easily come off, and influence the extension quality.Grind at the cutting of SiC substrate, twin grinding and single face, in the polishing process; Although the machining stress of part can discharge in following one manufacturing procedure; But this stress relief is unordered release, and the machining stress that does not discharge simultaneously can be gathered in wafer surface, influences the warpage and the degree of crook of SiC wafer; Serious warpage can produce fragmentation in road, the back course of processing with crooked, influences whole machining process round-robin wafer quality.
Summary of the invention
One of the object of the invention is the method for annealing that is to provide a kind of high-quality SiC wafer, is applicable to SiC cutting blade, twin grinding sheet, monolithic abrasive sheet and polished section.
Two of the object of the invention is to make the machining stress of the SiC wafer of processing eliminate even, abundant; Reduce because chip warpage and the degree of crook that the machining stress that crystal processing produces causes; Improve the yield of photoetching, alleviate the degree that comes off of substrate wafer and epitaxial film.
To achieve these goals, technical scheme of the present invention is: a kind of method for annealing of SiC wafer, and concrete steps are:
(1) the SiC wafer is packed in the ceramic frock, the potter is installed in the ceramic crucible, fills up with the SiC powder in the middle of ceramic frock and the ceramic crucible;
(2) directly be warming up to 200 ℃ ~ 400 ℃ in low temperature zone, be incubated 3 ~ 6 hours, this stage TRT >=1.5 hour;
(3) through after low temperature insulation for some time, temperature area is 500 ℃ ~ 700 ℃ in being warming up to, and is incubated 5 ~ 10 hours, this stage TRT >=2.5 hour;
(4) through in after temperature insulation for some time, be warming up to 800 ℃ ~ 1900 ℃ of high-temperature areas, be incubated 10 ~ 20 hours, this stage TRT >=10 hour;
(5) after soak finishes, be cooled to room temperature with per hour 10 ℃ ~ 15 ℃, come out of the stove.
The SiC wafer is any in cutting blade, twin grinding sheet, single face abrasive sheet, polished section and the substrate slice.The SiC polished section is any in single-sided polishing sheet and the twin polishing sheet.The SiC wafer is conductivity type or semi-insulating type.SiC wafer crystal formation is any among 4H, 6H, 3C and the 15R.
The SiC wafer is the 4H-SiC wafer of 2 inches conductivity types, and above-mentioned second to the 5th step is: be warming up to 200 ℃ with 2 ℃/minute temperature rise rates from room temperature; Temperature keep 200 ℃ 6 hours; After the low temperature insulation finishes, be warming up to 500 ℃ from 200 ℃ with 2 ℃/minute temperature rise rates; Temperature keep 500 ℃ 10 hours; After middle temperature insulation finishes, be warming up to 800 ℃ from 500 ℃ with 0.5 ℃/minute temperature rise rate; Temperature keep 800 ℃ 20 hours; Soak is cooled to room temperature with 10 ℃/hour rate of temperature fall after finishing, and opens burner hearth, takes out wafer.
The SiC wafer is 2 inches conductivity type 6H-SiC wafers, and above-mentioned second to the 5th step is: be warming up to 400 ℃ with 2 ℃/minute temperature rise rates from room temperature; Temperature keep 400 ℃ 3 hours; After the low temperature insulation finishes, be warming up to 700 ℃ from 400 ℃ with 2 ℃/minute temperature rise rates; Temperature keep 700 ℃ 5 hours; After middle temperature insulation finishes, be warming up to 1900 ℃ from 700 ℃ with 1 ℃/minute temperature rise rate; Temperature keep 1900 ℃ 10 hours; Soak is cooled to room temperature with 15 ℃/hour rate of temperature fall after finishing, and opens burner hearth, takes out wafer.
The SiC wafer is 2 inches semi-insulating type 4H-SiC wafers, and above-mentioned second to the 5th step is: be warming up to 300 ℃ with 2 ℃/minute temperature rise rates from room temperature; Temperature keep 300 ℃ 4 hours; After the low temperature insulation finishes, be warming up to 600 ℃ from 300 ℃ with 2 ℃/minute temperature rise rates; Temperature keep 600 ℃ 9 hours; After middle temperature insulation finishes, be warming up to 1200 ℃ from 600 ℃ with 0.5 ℃/minute temperature rise rate; Temperature keep 1000 ℃ 16 hours; Soak is cooled to room temperature with 10 ℃/hour rate of temperature fall after finishing, and opens burner hearth, takes out wafer.
The SiC wafer is 2 inches semi-insulating type 6H-SiC wafers, and above-mentioned second to the 5th step is: be warming up to 380 ℃ with 2 ℃/minute temperature rise rates from room temperature; Temperature keep 300 ℃ 3 hours; After the low temperature insulation finishes, be warming up to 700 ℃ from 300 ℃ with 2 ℃/minute temperature rise rates; Temperature keep 700 ℃ 6 hours; After middle temperature insulation finishes, be warming up to 1000 ℃ from 700 ℃ with 0.5 ℃/minute temperature rise rate; Temperature keep 1000 ℃ 11 hours; Soak is cooled to room temperature with 10 ℃/hour rate of temperature fall after finishing, and opens burner hearth, takes out wafer.
Beneficial effect of the present invention:
Without annealing, directly be used for photoetching or extension to the SiC wafer of present processing, machining stress is fully discharged, and causes the yield of photoetching wafer extremely low, the defective that epitaxial film and substrate wafer very easily come off.Implementation of the present invention is in annealing process, heats up stage by stage, is incubated, and the machining stress that this method makes the SiC wafer in cutting, grinding and polishing process, produce discharges even, abundant.When this method has overcome the direct extension of SiC wafer and the photoetching of existing processing, be difficult to during photoetching focus on, yield is extremely low, the caducous many shortcomings of epitaxial film and substrate wafer; Can be so that the machining stress that the SiC wafer produces in cutting, grinding and polishing process discharges even, abundant.Reduced the machining stress that processing produces with wafer annealed method, reduced chip warpage and degree of crook that machining stress causes significantly, the quality of photoetching yield and extension all is improved.
Description of drawings
Fig. 1 is the annealing curve synoptic diagram of the method for annealing of SiC wafer;
Fig. 2 is the annealing device synoptic diagram of the method for annealing of SiC wafer.
Embodiment
Through embodiment the present invention is further set forth below, but do not limit the present invention.
Like Fig. 1, shown in 2, the method for annealing of SiC wafer of the present invention, concrete steps are:
(1) SiC wafer 4 is packed in the ceramic frock 3, ceramic frock 3 places in the ceramic crucible 1, fills up with SiC powder 2 in the middle of ceramic frock 3 and the ceramic crucible 1;
(2) directly be warming up to 200 ℃ ~ 400 ℃ in low temperature zone, be incubated 3 ~ 6 hours, this stage TRT >=1.5 hour;
(3) through after low temperature insulation for some time, temperature area is 500 ℃ ~ 700 ℃ in being warming up to, and is incubated 5 ~ 10 hours, this stage TRT >=2.5 hour;
(4) through in after temperature insulation for some time, be warming up to 800 ℃ ~ 1900 ℃ of high-temperature areas, be incubated 10 ~ 20 hours, this stage TRT >=10 hour;
(5) after soak finishes, be cooled to room temperature with per hour 10 ℃ ~ 15 ℃, come out of the stove.
The SiC wafer is any in cutting blade, twin grinding sheet, single face abrasive sheet, polished section and the substrate slice.The SiC polished section is any in single-sided polishing sheet and the twin polishing sheet.The SiC wafer is conductivity type or semi-insulating type.SiC wafer crystal formation is any among 4H, 6H, 3C and the 15R.
One of embodiment
(1) during the 4H-SiC wafer of 2 inches conductivity types after will cutting is packed ceramic frock into, again the potter is installed in the ceramic crucible, fills up with the SiC powder in the middle of ceramic frock and the ceramic crucible;
(2) cold zone heats up: be warming up to 200 ℃ with 2 ℃/minute temperature rise rates from room temperature;
(3) cold zone insulation: temperature keep 200 ℃ 6 hours;
(4) warm area heats up in: after the low temperature insulation finishes, be warming up to 500 ℃ with 2 ℃/minute temperature rise rates from 200 ℃;
(5) warm area insulation in: temperature keep 500 ℃ 10 hours;
(6) heat up in the high-temperature zone: after middle temperature insulation finishes, be warming up to 800 ℃ with 0.5 ℃/minute temperature rise rate from 500 ℃;
(7) high-temperature zone insulation: temperature keep 800 ℃ 20 hours;
(8) cooling: soak is cooled to room temperature with 10 ℃/hour rate of temperature fall after finishing, and opens burner hearth, takes out wafer;
Using the angularity of the SiC wafer before the FM200 WAFER SYSTEM test annealing of Corning company is-12.83 microns, the SiC wafer whole angularity-2.24 after the annealing micron, machining stress basically eliminate.
Two of embodiment
(1) 2 inches conductivity type 6H-SiC wafers after the twin grinding is packed in the ceramic frock, again the potter is installed in the ceramic crucible, fills up with the SiC powder in the middle of ceramic frock and the ceramic crucible;
(2) cold zone heats up: be warming up to 400 ℃ with 2 ℃/minute temperature rise rates from room temperature;
(3) cold zone insulation: temperature keep 400 ℃ 3 hours;
(4) warm area heats up in: after the low temperature insulation finishes, be warming up to 700 ℃ with 2 ℃/minute temperature rise rates from 400 ℃;
(5) warm area insulation in: temperature keep 700 ℃ 5 hours;
(6) heat up in the high-temperature zone: after middle temperature insulation finishes, be warming up to 1900 ℃ with 1 ℃/minute temperature rise rate from 700 ℃;
(7) high-temperature zone insulation: temperature keep 1900 ℃ 10 hours;
(8) cooling: soak is cooled to room temperature with 15 ℃/hour rate of temperature fall after finishing, and opens burner hearth, takes out wafer;
Using the angularity of the SiC wafer before the FM200 WAFER SYSTEM test annealing of Corning company is-9.38 microns, the SiC wafer whole angularity-1.12 after the annealing micron, machining stress basically eliminate.
Three of embodiment
(1) during 2 inches semi-insulating type 4H-SiC wafers after single face is ground are packed ceramic frock into, the potter is installed in the ceramic crucible, ceramic frock is filled up with the SiC powder with the ceramic crucible centre again;
(2) cold zone heats up: be warming up to 300 ℃ with 2 ℃/minute temperature rise rates from room temperature;
(3) cold zone insulation: temperature keep 300 ℃ 4 hours;
(4) warm area heats up in: after the low temperature insulation finishes, be warming up to 600 ℃ with 2 ℃/minute temperature rise rates from 300 ℃;
(5) warm area insulation in: temperature keep 600 ℃ 9 hours;
(6) heat up in the high-temperature zone: after middle temperature insulation finishes, be warming up to 1200 ℃ with 0.5 ℃/minute temperature rise rate from 600 ℃;
(7) high-temperature zone insulation: temperature keep 1000 ℃ 16 hours;
(8) cooling: soak is cooled to room temperature with 10 ℃/hour rate of temperature fall after finishing, and opens burner hearth, takes out wafer;
Using the angularity of the SiC wafer before the FM200 WAFER SYSTEM test annealing of Corning company is-11.98 microns, the SiC wafer whole angularity-2.36 after the annealing micron, machining stress basically eliminate.
Four of embodiment
(1) 2 inches behind single grinding and polishing light semi-insulating type 6H-SiC wafers is packed in the ceramic frock, again the potter is installed in the ceramic crucible, fills up with the SiC powder in the middle of ceramic frock and the ceramic crucible;
(2) cold zone heats up: be warming up to 380 ℃ with 2 ℃/minute temperature rise rates from room temperature;
(3) cold zone insulation: temperature keep 300 ℃ 3 hours;
(4) warm area heats up in: after the low temperature insulation finishes, be warming up to 700 ℃ with 2 ℃/minute temperature rise rates from 300 ℃;
(5) warm area insulation in: temperature keep 700 ℃ 6 hours;
(6) heat up in the high-temperature zone: after middle temperature insulation finishes, be warming up to 1000 ℃ with 0.5 ℃/minute temperature rise rate from 700 ℃;
(7) high-temperature zone insulation: temperature keep 1000 ℃ 11 hours;
(8) cooling: soak is cooled to room temperature with 10 ℃/hour rate of temperature fall after finishing, and opens burner hearth, takes out wafer;
Using the angularity of the SiC wafer before the FM200 WAFER SYSTEM test annealing of Corning company is-10.96 microns, the SiC wafer whole angularity-2.13 after the annealing micron, machining stress basically eliminate.
Claims (9)
1. the method for annealing of a SiC wafer is characterized in that, concrete steps are:
(1) the SiC wafer is packed in the ceramic frock, the potter is installed in the ceramic crucible, fills up with the SiC powder in the middle of ceramic frock and the ceramic crucible;
(2) directly be warming up to 200 ℃ ~ 400 ℃ in low temperature zone, be incubated 3 ~ 6 hours, this stage TRT >=1.5 hour;
(3) through after low temperature insulation for some time, temperature area is 500 ℃ ~ 700 ℃ in being warming up to, and is incubated 5 ~ 10 hours, this stage TRT >=2.5 hour;
(4) through in after temperature insulation for some time, be warming up to 800 ℃ ~ 1900 ℃ of high-temperature areas, be incubated 10 ~ 20 hours, this stage TRT >=10 hour;
(5) after soak finishes, be cooled to room temperature with per hour 10 ℃ ~ 15 ℃, come out of the stove.
2. the method for annealing of SiC wafer according to claim 1 is characterized in that: described SiC wafer is any in cutting blade, twin grinding sheet, single face abrasive sheet, polished section and the substrate slice.
3. the method for annealing of SiC wafer according to claim 1 is characterized in that: described SiC wafer is conductivity type or semi-insulating type.
4. the method for annealing of SiC wafer according to claim 1 is characterized in that: described SiC wafer crystal formation is any among 4H, 6H, 3C and the 15R.
5. the method for annealing of SiC wafer according to claim 1 is characterized in that: the 4H-SiC wafer that described SiC wafer is 2 inches conductivity types, and above-mentioned second to the 5th step is: be warming up to 200 ℃ with 2 ℃/minute temperature rise rates from room temperature; Temperature keep 200 ℃ 6 hours; After the low temperature insulation finishes, be warming up to 500 ℃ from 200 ℃ with 2 ℃/minute temperature rise rates; Temperature keep 500 ℃ 10 hours; After middle temperature insulation finishes, be warming up to 800 ℃ from 500 ℃ with 0.5 ℃/minute temperature rise rate; Temperature keep 800 ℃ 20 hours; Soak is cooled to room temperature with 10 ℃/hour rate of temperature fall after finishing, and opens burner hearth, takes out wafer.
6. the method for annealing of SiC wafer according to claim 1 is characterized in that: described SiC wafer is 2 inches conductivity type 6H-SiC wafers, and above-mentioned second to the 5th step is: be warming up to 400 ℃ with 2 ℃/minute temperature rise rates from room temperature; Temperature keep 400 ℃ 3 hours; After the low temperature insulation finishes, be warming up to 700 ℃ from 400 ℃ with 2 ℃/minute temperature rise rates; Temperature keep 700 ℃ 5 hours; After middle temperature insulation finishes, be warming up to 1900 ℃ from 700 ℃ with 1 ℃/minute temperature rise rate; Temperature keep 1900 ℃ 10 hours; Soak is cooled to room temperature with 15 ℃/hour rate of temperature fall after finishing, and opens burner hearth, takes out wafer.
7. the method for annealing of SiC wafer according to claim 1 is characterized in that: described SiC wafer is 2 inches semi-insulating type 4H-SiC wafers, and above-mentioned second to the 5th step is: be warming up to 300 ℃ with 2 ℃/minute temperature rise rates from room temperature; Temperature keep 300 ℃ 4 hours; After the low temperature insulation finishes, be warming up to 600 ℃ from 300 ℃ with 2 ℃/minute temperature rise rates; Temperature keep 600 ℃ 9 hours; After middle temperature insulation finishes, be warming up to 1200 ℃ from 600 ℃ with 0.5 ℃/minute temperature rise rate; Temperature keep 1000 ℃ 16 hours; Soak is cooled to room temperature with 10 ℃/hour rate of temperature fall after finishing, and opens burner hearth, takes out wafer.
8. the method for annealing of SiC wafer according to claim 1 is characterized in that: described SiC wafer is 2 inches semi-insulating type 6H-SiC wafers, and above-mentioned second to the 5th step is: be warming up to 380 ℃ with 2 ℃/minute temperature rise rates from room temperature; Temperature keep 300 ℃ 3 hours; After the low temperature insulation finishes, be warming up to 700 ℃ from 300 ℃ with 2 ℃/minute temperature rise rates; Temperature keep 700 ℃ 6 hours; After middle temperature insulation finishes, be warming up to 1000 ℃ from 700 ℃ with 0.5 ℃/minute temperature rise rate; Temperature keep 1000 ℃ 11 hours; Soak is cooled to room temperature with 10 ℃/hour rate of temperature fall after finishing, and opens burner hearth, takes out wafer.
9. the method for annealing of SiC wafer according to claim 2 is characterized in that: described SiC polished section is single-sided polishing sheet or twin polishing sheet.
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| CN103114336A (en) * | 2013-03-12 | 2013-05-22 | 中国科学院上海硅酸盐研究所 | Method for annealing silicon carbide wafer |
| CN105200526A (en) * | 2015-10-14 | 2015-12-30 | 盐城工学院 | Gallium oxide wafer stress relieving annealing method |
| CN105332060A (en) * | 2015-10-30 | 2016-02-17 | 江苏吉星新材料有限公司 | Secondary sapphire wafer annealing method |
| CN105734673A (en) * | 2016-04-26 | 2016-07-06 | 北京世纪金光半导体有限公司 | Method for obtaining high machining precision of large silicon carbide single crystal wafer |
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| CN103114336A (en) * | 2013-03-12 | 2013-05-22 | 中国科学院上海硅酸盐研究所 | Method for annealing silicon carbide wafer |
| CN105200526B (en) * | 2015-10-14 | 2017-11-28 | 盐城工学院 | A kind of gallium oxide wafer stress relief annealing method |
| CN105200526A (en) * | 2015-10-14 | 2015-12-30 | 盐城工学院 | Gallium oxide wafer stress relieving annealing method |
| CN105332060A (en) * | 2015-10-30 | 2016-02-17 | 江苏吉星新材料有限公司 | Secondary sapphire wafer annealing method |
| CN105734673A (en) * | 2016-04-26 | 2016-07-06 | 北京世纪金光半导体有限公司 | Method for obtaining high machining precision of large silicon carbide single crystal wafer |
| CN106784189B (en) * | 2016-12-26 | 2018-09-21 | 盐城工学院 | The preparation method of monocrystalline gallium oxide substrate base surface atom grade step structure |
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| CN111394795A (en) * | 2020-04-10 | 2020-07-10 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Annealing device and annealing method for removing residual stress of seed crystal |
| CN111394795B (en) * | 2020-04-10 | 2021-10-15 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Annealing device and annealing method for removing residual stress of seed crystal |
| CN113174638A (en) * | 2021-04-27 | 2021-07-27 | 云南鑫耀半导体材料有限公司 | High-temperature secondary annealing method of silicon carbide crystals |
| CN113174638B (en) * | 2021-04-27 | 2022-06-03 | 云南鑫耀半导体材料有限公司 | High-temperature secondary annealing method of silicon carbide crystals |
| TWI771049B (en) * | 2021-06-08 | 2022-07-11 | 環球晶圓股份有限公司 | Wafer fixture structure and processing apparatus for causing high-temperature creep deformation |
| CN113564719A (en) * | 2021-07-26 | 2021-10-29 | 河北天达晶阳半导体技术股份有限公司 | Secondary annealing method of silicon carbide crystals |
| CN117166055A (en) * | 2022-06-02 | 2023-12-05 | 株式会社力森诺科 | SiC single crystal substrate |
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