CN104550133A - Method for removing organic pollutants in hollow micro-defect and on surface of wafer of silicon carbide single crystal - Google Patents
Method for removing organic pollutants in hollow micro-defect and on surface of wafer of silicon carbide single crystal Download PDFInfo
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- CN104550133A CN104550133A CN201410764416.0A CN201410764416A CN104550133A CN 104550133 A CN104550133 A CN 104550133A CN 201410764416 A CN201410764416 A CN 201410764416A CN 104550133 A CN104550133 A CN 104550133A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
- B08B7/0064—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes
- B08B7/0071—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by heating
- B08B7/0085—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by heating by pyrolysis
Abstract
The invention provides a method for removing organic pollutants in a hollow micro-defect and on a surface of a wafer of a silicon carbide single crystal. According to the method, the decomposition of organic wax at high temperature is realized in a vacuum reaction chamber and in the atmosphere of high temperature and reducing gas, and meanwhile, inorganic carbon generated by the decomposition of the organic wax performs chemical reaction with the reducing gas, and a new inorganic gas phase matter is generated, so that the purpose of thoroughly removing organic waxes in defects in a micro-pipe, a micro-pipeline, a hexagonal pot hole, a wafer surface, and the like is achieved. The method is excellent in repeatability and low in processing cost; under an effect of high temperature, atoms in the silicon carbide single crystal are reconstructed, so that the stress of a single crystal can be reduced; the method provided by the invention can be utilized to remove the organic pollutants and assist in promoting the quality of the crystal surface and an epitaxial layer.
Description
Technical field
The present invention relates to single-crystal silicon carbide preparing technical field, be specifically related to a kind of method removing single-crystal silicon carbide hollow microdefect inside and wafer surface organic pollution.
Background technology
Single-crystal silicon carbide has application space widely at field of power electronics, optoelectronic areas, the application of silicon carbide-based wafer is need in the certain thickness extension functional layer of silicon carbide substrate wafer (Bare-wafer) surface deposition in advance, and carry out structural manufacturing process process, to realize its design function.
For realizing the control externally delaying the technical indicators such as silicon carbide wafer electrical property uniformity, must avoid introduced contaminants in epitaxial layer, introduce doped energy-band, affecting epitaxial layer and even device performance.Based on this, must the strict impurity content controlling silicon carbide substrate wafer surface.
Silicon carbide wafer has the feature of, i.e. the defect such as microtubule, microchannel, six Fang Keng holes of residual some in crystal, and such defect belongs to and runs through type or partly run through type defect.Meanwhile, in the polishing process carrying out silicon carbide substrate wafer, need to adopt the consumptive materials such as organic wax, such consumptive material in use can pass microtubule, microchannel, six Fang Keng holes etc., and remains in silicon carbide substrate wafer inside.Because the flaw sizes such as microtubule, microchannel, six Fang Keng holes are distributed as from nanoscale in tens micrometer ranges, size is very little, adopts the normal wet cleaning that traditional ultrasonic and million sound are auxiliary, is difficult to ensure such impurity thoroughly to dispose.
Summary of the invention
The present invention is intended to the technological deficiency for prior art, there is provided a kind of method removing single-crystal silicon carbide hollow microdefect inside and wafer surface organic pollution, to solve the technical problem that the organic wax that is inner and wafer surface existence of single-crystal silicon carbide hollow microdefect in prior art is difficult to remove.
For realizing above technical purpose, the present invention by the following technical solutions:
Remove a method for single-crystal silicon carbide hollow microdefect inside and wafer surface organic pollution, comprise the following steps:
1) pending carborundum crystals is placed in confined space, be (1E-2) ~ (1E-5) Pa to this evacuate space to vacuum, keep 5 ~ 15min, and in this space backward, pass into carrier gas to 40 ~ 120Kpa, keep 2 ~ 10min;
2) be then (1E-2) ~ (1E-5) Pa to above-mentioned evacuate space to vacuum, keep 5 ~ 15min, get reducibility gas and carrier gas is mixed to get the first gaseous mixture, in this first gaseous mixture, the content of reducibility gas is 5 ~ 100% (v/v), then in above-mentioned space, pass into this first gaseous mixture to 20 ~ 100Kpa, keep 1 ~ 10min;
3) be then (1E-2) ~ (1E-5) Pa to above-mentioned evacuate space to vacuum, then be heated to 1000 ~ 1200 DEG C, keep 10 ~ 30min;
4) reducibility gas is got and carrier gas is mixed to get the second gaseous mixture, in this second gaseous mixture, the content of reducibility gas is 5 ~ 100% (v/v), then in above-mentioned space, pass into this second gaseous mixture to 10 ~ 150Kpa, be heated to 1200 ~ 1900 DEG C again, keep 5 ~ 30min, then vacuumize;
5) in above-mentioned space, pour carrier gas to 20 ~ 80Kpa, maintain the cooling of this pressure.
Preferably, step 5) speed of described cooling is 5 ~ 10 DEG C/min.
Preferably, described reducibility gas be selected from hydrogen, ammonia or hydrogen chloride wherein one or more.
Preferably, described carrier gas is selected from nitrogen, inert gas or its mixture; Can also carry out preferably following on this basis: described inert gas is argon gas.
Preferably, step 1) repeat 2 ~ 5 implementation steps 2 again).
Preferably, step 2) repeat 2 ~ 5 implementation steps 3 again).
Preferably, step 4) repeat 2 ~ 8 implementation steps 5 again).
In technical solution of the present invention, organic wax chemical constituent is the mixture of multiple alkane, belongs to hydrocarbon solid mixture, short according to organic wax hydrocarbon company commander, chemical composition is different, and its decomposition temperature is 200 ~ 500 DEG C.Described carrier gas refer to not with material generation chemical reaction in system, be mainly used in as system provides pressure or takes up space gas.Described reducibility gas, by the random motion of gas molecule, to be oxidized with the carbon be decomposed to form, reduction reaction under certain conditions, generates gas, drains with vacuum, thus obtains the residual wafer surface of free from admixture.For ensureing concentration, the purity of reducing gas, therefore technical solution of the present invention is repeatedly filled with as the carrier gas such as high-purity argon gas, nitrogen to reaction cavity, the oxygen for diluting, in displacement reaction chamber, thus ensures the concentration of the reducing gas in course of reaction.Above vacuum pumping utilizes molecular pump to complete.
Technical solution of the present invention is in vacuum reaction chamber, in the atmosphere of high temperature and reducing gas, realize the decomposition at high temperature of organic wax, simultaneously, the DIC that organic wax decomposition produces and reducing gas produce chemical reaction, and generate new inorganic gaseous substance eliminating, thus realize the object thoroughly removing organic wax of the defect inside such as microtubule, microchannel, six Fang Keng holes.
Meanwhile, technical solution of the present invention has following advantage:
The first, this process repeatability is high, and processing cost is low;
The second, in this process, there is pyroprocess, under the effect of high temperature, the atom in single-crystal silicon carbide can reconstruct, and can reduce monocrystal stress;
3rd, the C atom on reducing gas and silicon carbide wafer surface reacts, and has the volatilization of Si atom simultaneously, thus can remove machining damage, contributes to improving plane of crystal quality;
4th, by Controlling Technology condition, comprise reducing gas, technological temperature, operation pressure etc., can the atomic steps pattern (highly, width) on silicon carbide wafer surface crossed of control treatment, suitable atomic steps pattern is highly beneficial for the two-dimentional forming core in epitaxial process, contributes to improving epitaxial layer quality.
Detailed description of the invention
Below will be described in detail the specific embodiment of the present invention.In order to avoid too much unnecessary details, in the examples below to belonging to known structure or function will not be described in detail.
The approximating language used in following examples can be used for quantitative expression, shows to allow quantity to have certain variation when not changing basic function.Therefore, this exact value itself is not limited to the numerical value that the language such as " approximately ", " left and right " is revised.In certain embodiments, " approximately " represents and allows its numerical value revised to change in the positive and negative scope of 10 (10%), such as, and any numerical value that what " about 100 " represented can be between 90 to 110.In addition, in the statement of " about first numerical value is to second value ", revise the first and second numerical value two numerical value approximately simultaneously.In some cases, approximating language may be relevant with the precision of measuring instrument.
Apart from outside definition, technology used in following examples and scientific terminology have the identical meanings generally understood with those skilled in the art of the invention.
Embodiment 1
Remove a method for single-crystal silicon carbide hollow microdefect inside and wafer surface organic pollution, comprise the following steps:
1) take out system vacuum to 1E-3 handkerchief with molecular pump, keep 10 minutes, then pass into argon gas to 80Kpa, keep 5 minutes, this action repeats 2 times;
2) take out system vacuum to 1E-2 handkerchief with molecular pump, keep 10 minutes, then pass into concentration be the mist of 20% (hydrogen 20%, argon gas 80%) to 50Kpa, keep 3 minutes, this action repeats 2 times;
3) take out system vacuum to 1E-2 handkerchief with molecular pump, and be heated to 1000-1200 DEG C, keep 20 minutes;
4) being filled with concentration is 20% (hydrogen 20%, argon gas 80%) mist to 70Kpa, and to set heating-up temperature be about 1700 DEG C, and by the infrared radiation thermometer calibrated, this temperature is tested, guarantee that temperature is 1700 ± 10 DEG C, under this vacuum and temperature, maintain 15 minutes, and then vacuumize; Repeat this action 3 times;
5) after 4 process curves more than are complete, pass into argon gas, and to maintain pressure be 50Kpa, the cooling rate of control is 5-10 DEG C and cools, to room temperature.
Embodiment 2
Remove a method for single-crystal silicon carbide hollow microdefect inside and wafer surface organic pollution, comprise the following steps:
1) take out system vacuum to 1E-3 handkerchief with molecular pump, keep 10 minutes, then pass into argon gas to 80Kpa, keep 5 minutes, this action repeats 2 times;
2) take out system vacuum to 1E-2 handkerchief with molecular pump, keep 10 minutes, then pass into concentration be the mist of 20% (hydrogen 20%, argon gas 80%) to 50Kpa, keep 3 minutes, this action repeats 2 times;
3) take out system vacuum to 1E-2 handkerchief with molecular pump, and be heated to 1000-1200 DEG C, keep 20 minutes;
4) being filled with concentration is 10% (hydrogen 10%, argon gas 90%) mist to 60Kpa, and to set heating-up temperature be 1800 DEG C, and by the infrared radiation thermometer calibrated, this temperature is tested, guarantee that temperature is 1800 ± 10 DEG C, under this vacuum and temperature, maintain 15 minutes, and then vacuumize; Repeat this action 5 times;
5) after 4 process curves more than are complete, pass into argon gas, and to maintain pressure be 50Kpa, the cooling rate of control is 5-10 DEG C and cools, to room temperature.
Embodiment 3
Remove a method for single-crystal silicon carbide hollow microdefect inside and wafer surface organic pollution, comprise the following steps:
1) pending carborundum crystals being placed in confined space, is 1E-2Pa to this evacuate space to vacuum, keeps 5min, and passes into carrier gas in this space backward to 40Kpa, keeps 2min;
2) be then 1E-3Pa to above-mentioned evacuate space to vacuum, keep 5min, get reducibility gas and carrier gas is mixed to get the first gaseous mixture, in this first gaseous mixture, the content of reducibility gas is 5% (v/v), in above-mentioned space, then pass into this first gaseous mixture to 20Kpa, keep 1min;
3) be then 1E-3Pa to above-mentioned evacuate space to vacuum, then be heated to about 1100 DEG C, keep 10min;
4) reducibility gas is got and carrier gas is mixed to get the second gaseous mixture, in this second gaseous mixture, the content of reducibility gas is 90% (v/v), in above-mentioned space, then passes into this second gaseous mixture to 10Kpa, then is heated to 1300 DEG C, keep 5min, then vacuumize;
5) in above-mentioned space, pour carrier gas to 20Kpa, maintain the cooling of this pressure.
In above technical scheme, step 5) speed of described cooling is approximately 7 DEG C/min.
Described reducibility gas is selected from the mixture of ammonia and hydrogen chloride.
Described carrier gas is nitrogen.
Step 1) repeat 3 implementation steps 2 again).
Step 2) repeat 4 implementation steps 3 again).
Step 4) repeat 7 implementation steps 5 again).
Embodiment 4
Remove a method for single-crystal silicon carbide hollow microdefect inside and wafer surface organic pollution, comprise the following steps:
1) pending carborundum crystals being placed in confined space, is 1E-4Pa to this evacuate space to vacuum, keeps 15min, and passes into carrier gas in this space backward to 120Kpa, keeps 10min;
2) be then 1E-4Pa to above-mentioned evacuate space to vacuum, keep 15min, get reducibility gas and carrier gas is mixed to get the first gaseous mixture, in this first gaseous mixture, the content of reducibility gas is 50% (v/v), in above-mentioned space, then pass into this first gaseous mixture to 100Kpa, keep 10min;
3) be then 1E-4Pa to above-mentioned evacuate space to vacuum, then be heated to 1150 DEG C, keep 25min;
4) reducibility gas is got and carrier gas is mixed to get the second gaseous mixture, in this second gaseous mixture, the content of reducibility gas is 40% (v/v), in above-mentioned space, then passes into this second gaseous mixture to 150Kpa, then is heated to about 1500 DEG C, keep 30min, then vacuumize;
5) in above-mentioned space, pour carrier gas to 80Kpa, maintain the cooling of this pressure.
In above technical scheme, step 5) speed of described cooling is 6 DEG C/min.
Described reducibility gas is hydrogen chloride.
Described carrier gas is the mixture of helium and neon.
Step 1) repeat 5 implementation steps 2 again).
Step 2) repeat 5 implementation steps 3 again).
Step 4) repeat 8 implementation steps 5 again).
Embodiment 5
Remove a method for single-crystal silicon carbide hollow microdefect inside and wafer surface organic pollution, comprise the following steps:
1) pending carborundum crystals being placed in confined space, is 1E-5Pa to this evacuate space to vacuum, keeps 8min, and passes into carrier gas in this space backward to 60Kpa, keeps 12min;
2) be then 1E-5Pa to above-mentioned evacuate space to vacuum, keep 11min, get reducibility gas and carrier gas is mixed to get the first gaseous mixture, in this first gaseous mixture, the content of reducibility gas is 10% (v/v), in above-mentioned space, then pass into this first gaseous mixture to 80Kpa, keep 2min;
3) be then 1E-5Pa to above-mentioned evacuate space to vacuum, then be heated to 1050 DEG C, keep 30min;
4) reducibility gas is got and carrier gas is mixed to get the second gaseous mixture, in this second gaseous mixture, the content of reducibility gas is 50% (v/v), in above-mentioned space, then passes into this second gaseous mixture to 100Kpa, then is heated to about 1200 DEG C, keep 25min, then vacuumize;
5) in above-mentioned space, pour carrier gas to 30Kpa, maintain the cooling of this pressure.
In above technical scheme, step 5) speed of described cooling is 9 DEG C/min.
Described reducibility gas is ammonia.
Described carrier gas is the mixture of Krypton and nitrogen.
Above embodiments of the invention have been described in detail, but described content is only preferred embodiment of the present invention, not in order to limit the present invention.All make in application range of the present invention any amendment, equivalent to replace and improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. remove a method for single-crystal silicon carbide hollow microdefect inside and wafer surface organic pollution, it is characterized in that comprising the following steps:
1) pending carborundum crystals is placed in confined space, be (1E-2) ~ (1E-5) Pa to this evacuate space to vacuum, keep 5 ~ 15min, and in this space backward, pass into carrier gas to 40 ~ 120Kpa, keep 2 ~ 10min;
2) be then (1E-2) ~ (1E-5) Pa to above-mentioned evacuate space to vacuum, keep 5 ~ 15min, get reducibility gas and carrier gas is mixed to get the first gaseous mixture, in this first gaseous mixture, the content of reducibility gas is 5 ~ 100% (v/v), then in above-mentioned space, pass into this first gaseous mixture to 20 ~ 100Kpa, keep 1 ~ 10min;
3) be then (1E-2) ~ (1E-5) Pa to above-mentioned evacuate space to vacuum, then be heated to 1000 ~ 1200 DEG C, keep 10 ~ 30min;
4) reducibility gas is got and carrier gas is mixed to get the second gaseous mixture, in this second gaseous mixture, the content of reducibility gas is 5 ~ 100% (v/v), then in above-mentioned space, pass into this second gaseous mixture to 10 ~ 150Kpa, be heated to 1200 ~ 1900 DEG C again, keep 5 ~ 30min, then vacuumize;
5) in above-mentioned space, pour carrier gas to 20 ~ 100Kpa, maintain the cooling of this pressure.
2. method according to claim 1, is characterized in that step 5) speed of described cooling is 5 ~ 10 DEG C/min.
3. method according to claim 1, it is characterized in that described reducibility gas be selected from hydrogen, ammonia or hydrogen chloride wherein one or more.
4. method according to claim 1, is characterized in that described carrier gas is selected from nitrogen, inert gas or its mixture.
5. method according to claim 4, is characterized in that described inert gas is argon gas.
6. method according to claim 1, is characterized in that step 1) repeat 2 ~ 5 implementation steps 2 again).
7. method according to claim 1, is characterized in that step 2) repeat 2 ~ 5 implementation steps 3 again).
8. method according to claim 1, is characterized in that step 4) repeat 2 ~ 8 implementation steps 5 again).
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| CN107699955A (en) * | 2017-08-30 | 2018-02-16 | 昆明理工大学 | It is a kind of using microwave heat remove single-crystal silicon carbide defect in and surface organic impurities method |
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