CN105140111A - Method for removing punch-through defects on silicon carbide epitaxial surface - Google Patents
Method for removing punch-through defects on silicon carbide epitaxial surface Download PDFInfo
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- CN105140111A CN105140111A CN201510489191.7A CN201510489191A CN105140111A CN 105140111 A CN105140111 A CN 105140111A CN 201510489191 A CN201510489191 A CN 201510489191A CN 105140111 A CN105140111 A CN 105140111A
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- H—ELECTRICITY
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/20—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy
- H01L21/208—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy using liquid deposition
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- C—CHEMISTRY; METALLURGY
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B19/00—Liquid-phase epitaxial-layer growth
- C30B19/12—Liquid-phase epitaxial-layer growth characterised by the substrate
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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Abstract
The invention discloses a method for removing punch-through defects on a silicon carbide epitaxial surface. The method comprises the steps as follows: (1) a silicon carbide substrate is taken and cleaned; (2) the surface of the substrate is etched until a defect pit is exposed; (3) a silicon layer is fabricated on the substrate; (4) the silicon layer is molten by raising the temperature, so that the defect pit is fully filled with the silicon layer and the external surface is smooth; (5) a carbon source is introduced, so that the molten silicon layer is partially transformed into a first silicon carbide layer; (6) the carbon source is introduced, so that the residual silicon carbide layer is partially transformed into a second silicon carbide layer; and (7) the residual silicon layer is etched away; and the intact first silicon carbide layer and second silicon carbide layer are left to finish preparation. According to the method, the defects on the epitaxial surface of the silicon carbide substrate are removed to prevent the defects from punching through the epitaxial layer.
Description
Technical field
The present invention relates to technical field of semiconductors, particularly relate to a kind of carborundum isoepitaxial growth method, can be used for eliminating silicon carbide epitaxy face break-through defect, improve epitaxial material crystal mass.
Background technology
Carborundum (4H-SiC, 6H-SiC) be a kind of semiconductor material with wide forbidden band, its band gap length can reach 3.0-3.2eV, it is 3 times of Si, therefore, it has high critical breakdown electric field (10 times of Si), the features such as high carrier saturated concentration (2 times of Si), in addition, it also has the feature of high heat conductance (3 times of Si), therefore, it is at military and high temperature that is space industry, high frequency, high-power electric and electronic, photoelectric device aspect has superior using value, and be expected to be applied to the inefficient occasion of existing silica-based high power device, one of key foundation material becoming power electronic semiconductor of future generation.
Although the commercialization of single-crystal silicon carbide material, but still there are many defects in wafer, as microtubule (MP), cardinal plane dislocation (BPD), helical dislocation (TSD) etc., during isoepitaxial growth, these defects along interface break-through in epitaxial loayer, can reduce the quality of epitaxial material.As shown in Figure 1, have defect in silicon carbide substrates, outer time delay, defect, along aufwuchsplate break-through in epitaxial loayer, finally causes having the defect through with substrate in epitaxial loayer.There is limited evidence currently of has people to study how to eliminate above-mentioned defect break-through, and general way improves carborundum crystals crystalline quality further, reduces defect concentration.
Summary of the invention
In order to solve the problem, the invention provides a kind of method eliminating silicon carbide epitaxy face break-through defect, by the defect expressivity of silicon carbide substrates epitaxial surface, and then reach and prevent defect break-through to the object in epitaxial loayer.
The invention provides a kind of method eliminating silicon carbide epitaxy face break-through defect, comprise the steps:
Step 1: get a silicon carbide substrates, and clean up;
Step 2: corrode the surface of substrate, until appear defect hole;
Step 3: make silicon layer on substrate;
Step 4: raised temperature makes silicon layer melt, makes it to fill up defect hole, and makes outer surface smooth;
Step 5: pass into carbon source, makes melted silicon layer segment be transformed into the first silicon carbide layer;
Step 6: pass into carbon source, makes remaining melted silicon layer segment be transformed into the second silicon carbide layer;
Step 7: corrosion, erodes remaining silicon layer, leave first, second complete silicon carbide layer, complete preparation.
The invention has the beneficial effects as follows, utilize the method that silicon carbide substrates epitaxial surface corrodes by melting alkali lye, defect can be appeared, form etch pit, fill out hole with liquid silicon thereupon, adopt liquid-phase epitaxial growth process to carry out the isoepitaxial growth of carborundum, can prevent substrate defects break-through from entering epitaxial loayer.Compared with existing carborundum homoepitaxy, this method can eliminate silicon carbide epitaxy face break-through defect, and improve epitaxial loayer quality, tool has great advantage.In addition, this beneficial effect also may be used for the epitaxial growth of other compound semiconductor, as the homoepitaxy of semiconducting nitride aluminium (AlN), gallium nitride (GaN), zinc oxide (ZnO) etc.
The present invention is easy and simple to handle, is easy to promote, and obtains good result.
Accompanying drawing explanation
For further illustrating technology contents of the present invention, be described in detail as follows below in conjunction with embodiment and accompanying drawing, wherein:
Fig. 1 is break-through defect schematic diagram in prior art;
Fig. 2 is preparation flow figure of the present invention;
Fig. 3 is the structural representation of preparation flow of the present invention;
Fig. 4 is the defect optical microscope photograph manifested after substrate etching in the present invention;
Fig. 5 is silicon carbide epitaxy face optical microscope photograph in the present invention;
Fig. 6 is the Raman collection of illustrative plates of silicon carbide epitaxial layers provided by the invention.
Embodiment
Refer to shown in Fig. 2-Fig. 3, the invention provides a kind of method eliminating silicon carbide epitaxy face break-through defect, comprise the steps:
Step 1: get a silicon carbide substrates 1, be 4H-SiC or 6H-SiC, and clean up.
Step 2: the surface of substrate 1 is corroded, until appear defect hole 1.Wherein said surface corrosion adopts melting alkali lye, and this melting alkali lye is KOH or NaOH, or KOH and Na
2o
2mixture, or NaOH and Na
2o
2mixture, corrosion temperature is 500 DEG C-700 DEG C, and the time of corrosion is 1-30 minute.
Step 3: make silicon layer 2 on substrate 1.The manufacture craft of silicon layer 2 is: the silicon source SiH passing into 800 DEG C-1350 DEG C
4, SiH
4hydrogen is adopted to be carrier gas and diluent gas, wherein SiH
4flow is 1-10sccm, and hydrogen flowing quantity is 1-10slm, and the extension duration is 1-15 minute, and growth pressure is 1-40Torr.
Step 4: raised temperature makes silicon layer 2 melt, makes it to fill up defect hole 1, and makes outer surface smooth.The technique that wherein said silicon layer 2 melts is: temperature is elevated to 1450 DEG C-1550 DEG C, and be incubated 10-30 minute under an argon, argon flow amount used is 1-5slm, and pressure used is 500-760Torr, and silicon carbide substrates 1 is rotated, and rotating speed is 1-10 rev/min.
Step 5: pass into carbon source, makes fusing silicon layer 2 be partially converted to the first silicon carbide layer 3.Growth technique is: keep substrate 1 to rotate, rotating speed is 1-10 rev/min, passes into hydrogen, and the flow of hydrogen is 1-5slm, and pressure used is 10-760Torr, and temperature is 1550 DEG C-1850 DEG C, passes into carbon source C2H4 or C
3h
8, flow is 100-500sccm, and pass into the dopant of identical type of adulterating with substrate, flow is 10-50sccm, and the duration is 10-30 minute simultaneously.
Step 6: pass into carbon source, makes remaining fusing silicon layer 2 be partially converted to the second silicon carbide layer 4.Growth technique is: keep substrate 1 to rotate, rotating speed is 1-10 rev/min, passes into hydrogen, and the flow of hydrogen is 1-5slm, and pressure used is 10-760Torr, and temperature is 1550 DEG C-1850 DEG C, passes into carbon source C
2h
4or C
3h
8, flow is 100-500sccm, and the duration is 10-100 minute.
Step 7: corrosion, erodes remaining silicon layer 2, leave first, second complete silicon carbide layer 3,4, complete preparation.The etching process wherein remaining silicon layer 2 is: keep silicon carbide substrates 1 to rotate, rotating speed is 1-10 rev/min, and hydrogen flowing quantity used is 1-5slm, pressure used is 10-760Torr, and temperature is 1550 DEG C-1850 DEG C, passes into HCl gas, flow is 100-500sccm, and the duration is 10-100 minute.The etching process of residue silicon layer 2 also can be: silicon carbide substrates 1 is immersed in HF and HNO that volume ratio is 1: 1
3mixed solution in 5-30 minute.
Below in conjunction with accompanying drawing, exemplary embodiments of the present invention are described.For clarity and brevity, actual embodiment is not limited to these technical characteristics described in specification.It should be understood, however, that in the process improving practical embodiments described in any one, the decision of multiple specific embodiment must be the specific objective that can realize improvement personnel, such as, defer to industry and to be correlated with the restriction relevant with business, described restriction changes along with the difference of embodiment.And even it should be understood that the effect of aforementioned improved is very complicated and consuming time, but this remains routine techniques means for the those skilled in the art knowing benefit of the present invention.
Fig. 3 shows the schematic diagram of an embodiment of elimination silicon carbide epitaxy face break-through defect provided by the invention.As shown in Figure 3, adopt 4 inches of N-shaped 4H-SiC substrates, substrate epitaxial crystal face is silicon face (0001), and has the drift angle of 4 degree towards <11-20> direction.Adopt KOH and Na
2o
2the mixture of (mass ratio 2: 1) is corrosive agent, it is heated to 550 DEG C, makes it fusing.4H-SiC substrate to be fully immersed in melting alkali lye and to be incubated, took out every 1 minute and check, until appear defect hole, in order to check the eradicating efficacy to variety classes defect, need the hole appearing hexagonal hole and shell-like, wherein, being that micropipe defects causes in large hexagonal hole, is that helical dislocation defect causes in little hexagonal hole, hole in shell-like is that basal plane dislocation defect causes, as shown in Figure 4, now, corrosion is stopped.4H-SiC standard RCA clean technique is cleaned up, and dries up with hot nitrogen, load in epitaxial furnace.Now, carry out silicon layer epitaxial growth, its two skill is: furnace temperature rises to 860 DEG C, is incubated 30 minutes, and 4H-SiC substrate is rotated with holder, and rotating speed is 8 revs/min.Pass into H
2gas, flow is 10slm, keeps 30 minutes, further cleaning 4H-SiC surface.Then silicon source SiH is passed into
4, flow is 5sccm, and the extension duration is 10 minutes, keeps growth room's pressure to be 1Torr.Can growth thickness be the epitaxial silicon of 6 microns.After this, melted by silicon layer, its technique is: make temperature be elevated to 1550 DEG C, is incubated 10 minutes under an argon, argon flow amount used is 5slm, and pressure used is 760Torr, and adjustment silicon carbide substrates rotating speed is 10 revs/min, silicon layer is melted, fills up defect hole, and make outer surface smooth.After this, carry out the growth of carborundum, during extension the first silicon carbide layer, its technique is: argon gas is switched to hydrogen, close argon gas, open hydrogen, flow is 5slm, and pressure is 200Torr, temperature is 1750 DEG C, passes into carbon source C2H4, and flow is 200sccm, passes into n-type dopant NH simultaneously
3, flow is 20sccm, and the duration is 60 minutes.The thin layer carborundum of 1 micron can be about by growth thickness.Then, extension second silicon carbide layer, technique with the first silicon carbide layer epitaxy technique, but does not pass into n-type dopant NH
3.Finally, unreacted excess silicon removed by corrosion, its technique is: hydrogen flowing quantity is 3slm, and pressure is 300Torr, and temperature is 1550 DEG C, passes into HCl gas, and flow is 200sccm, and the duration is 30 minutes.The carbofrax material that final acquisition does not have silicon residual, as shown in Figure 5.Through Raman test, result as shown in Figure 6, shows that epitaxial loayer crystal formation is all 4H carborundum, does not have other polytype to be mingled with.
Although based on some preferred embodiments, invention has been described, and those skilled in the art should know, and scope of the present invention is not limited to those embodiments.Without departing from the spirit and substance in the present invention, those of ordinary skill in the art can carry out variations and modifications to embodiment on understanding basis of the present invention, and therefore falls into the protection range of claims of the present invention restriction.
Claims (9)
1. eliminate a method for silicon carbide epitaxy face break-through defect, comprise the steps:
Step 1: get a silicon carbide substrates, and clean up;
Step 2: corrode the surface of substrate, until appear defect hole;
Step 3: make silicon layer on substrate;
Step 4: raised temperature makes silicon layer melt, makes it to fill up defect hole, and makes outer surface smooth;
Step 5: pass into carbon source, makes melted silicon layer segment be transformed into the first silicon carbide layer;
Step 6: pass into carbon source, makes remaining melted silicon layer segment be transformed into the second silicon carbide layer;
Step 7: corrosion, erodes remaining silicon layer, leave first, second complete silicon carbide layer, complete preparation.
2. the method for elimination silicon carbide epitaxy face break-through defect according to claim 1, the material of wherein said substrate is 4H-SiC or 6H-SiC.
3. the method for elimination silicon carbide epitaxy face break-through defect according to claim 1, wherein said surface corrosion adopts melting alkali lye, and this melting alkali lye is KOH or NaOH, or KOH and Na
2o
2mixture, or NaOH and Na
2o
2mixture, corrosion temperature is 500 DEG C-700 DEG C, and the time of corrosion is 1-30 minute.
4. the method for elimination silicon carbide epitaxy face break-through defect according to claim 1, the manufacture craft of wherein said silicon layer is: the silicon source SiH passing into 800 DEG C-1350 DEG C
4, SiH
4hydrogen is adopted to be carrier gas and diluent gas, wherein SiH
4flow is 1-10sccm, and hydrogen flowing quantity is 1-10slm, and the extension duration is 1-15 minute, and growth pressure is 1-40Torr.
5. the method for elimination silicon carbide epitaxy face break-through defect according to claim 4, the technique of wherein said silicon layer fusing is: temperature is elevated to 1450 DEG C-1550 DEG C, be incubated 10-30 minute under an argon, argon flow amount used is 1-5slm, pressure used is 500-760Torr, and silicon carbide substrates is rotated, rotating speed is 1-10 rev/min.
6. the method for elimination silicon carbide epitaxy face break-through defect according to claim 1, the technique of wherein said growth first silicon carbide layer is: keep substrate to rotate, rotating speed is 1-10 rev/min, pass into hydrogen, the flow of hydrogen is 1-5slm, pressure used is 10-760Torr, and temperature is 1550 DEG C-1850 DEG C, passes into carbon source C2H4 or C
3h
8, flow is 100-500sccm, and pass into the dopant of identical type of adulterating with substrate, flow is 10-50sccm, and the duration is 10-30 minute simultaneously.
7. the method for elimination silicon carbide epitaxy face break-through defect according to claim 1, the technique of wherein said growth second silicon carbide layer is: keep substrate to rotate, rotating speed is 1-10 rev/min, pass into hydrogen, the flow of hydrogen is 1-5slm, pressure used is 10-760Torr, and temperature is 1550 DEG C-1850 DEG C, passes into carbon source C
2h
4or C
3h
8, flow is 100-500sccm, and the duration is 10-100 minute.
8. the method for elimination silicon carbide epitaxy face break-through defect according to claim 1, the etching process of wherein said residue silicon layer is: keep silicon carbide substrates to rotate, rotating speed is 1-10 rev/min, hydrogen flowing quantity used is 1-5slm, pressure used is 10-760Torr, and temperature is 1550 DEG C-1850 DEG C, passes into HCl gas, flow is 100-500sccm, and the duration is 10-100 minute.
9. the method for elimination silicon carbide epitaxy face break-through defect according to claim 1, the etching process of wherein said residue silicon layer is: silicon carbide substrates is immersed in HF and HNO that volume ratio is 1: 1
3mixed solution in 5-30 minute.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110112057A (en) * | 2019-04-28 | 2019-08-09 | 台州市一能科技有限公司 | A kind of silicon carbide epitaxial wafer and production method and the chip with silicon carbide epitaxial wafer |
| CN111584349A (en) * | 2020-05-25 | 2020-08-25 | 芜湖启迪半导体有限公司 | Filling method of SiC epitaxial deep groove |
| CN112048769A (en) * | 2020-07-24 | 2020-12-08 | 山东天岳先进材料科技有限公司 | Device for healing silicon carbide crystal micropipe and application |
| CN113122922A (en) * | 2020-06-09 | 2021-07-16 | 北京世纪金光半导体有限公司 | Seed crystal for growth of large-size silicon carbide crystal |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110112057A (en) * | 2019-04-28 | 2019-08-09 | 台州市一能科技有限公司 | A kind of silicon carbide epitaxial wafer and production method and the chip with silicon carbide epitaxial wafer |
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| CN113122922A (en) * | 2020-06-09 | 2021-07-16 | 北京世纪金光半导体有限公司 | Seed crystal for growth of large-size silicon carbide crystal |
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Application publication date: 20151209 |