CN102456549A - Indium phosphide wafer and surface cleaning method thereof - Google Patents
Indium phosphide wafer and surface cleaning method thereof Download PDFInfo
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- CN102456549A CN102456549A CN2011103520019A CN201110352001A CN102456549A CN 102456549 A CN102456549 A CN 102456549A CN 2011103520019 A CN2011103520019 A CN 2011103520019A CN 201110352001 A CN201110352001 A CN 201110352001A CN 102456549 A CN102456549 A CN 102456549A
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Abstract
The invention requires to protect a method for cleaning an indium phosphide wafer, wherein the method comprises the following steps: (1) processing a wafer at minus 10-25 DEG C by use of an ammonia solution containing H2O2; (2) cleaning the wafer with deionized water; (3) processing the wafer at minus 10-55 DEG C by use of a concentrated acid; (4) cleaning the wafer with deionized water; (5) processing the wafer at minus 10-35 DEG C by use of an organic acid; (6) cleaning the wafer with deionized water; and (7) drying the wafer. The method provided by the invention not only can be used for effectively reducing the particles and metal residue on the surface of the indiumn phosphide wafer, especially an indium phosphide special crystal orientation angle wafer, but also can be used for improving the corrosion uniformity of the surface of the wafer and reducing the white mist value. The indium phosphide wafer obtained by the method can well meet the epitaxial growth requirement of 'ready to use after a box is open'.
Description
Technical field
The present invention relates to a kind of inp wafer and method for cleaning surface thereof.
Background technology
Indium phosphide (InP) wafer is important compound semiconductor materials, and (GaAs) compares with GaAs, and its superiority mainly is high saturated electric field drift velocity, the capability of resistance to radiation that thermal conductivity is good and stronger etc.At the current optical-fibre communications field that develops rapidly, inp wafer is first-selected backing material.
Along with the extensive use of inp wafer, people also have higher requirement to the surface quality of wafer.The cleaning method of silicon (Si) and gallium arsenide wafer has obtained better solution, described in Chinese patent CN101661869.Yet because indium phosphide special physicochemical characteristic, same method often is applied to the cleaning of indium phosphide unsatisfactorily.Indium phosphide belongs to binary compound, and the chemical characteristic of different crystal orientations has very big-difference.For example special crystal orientation angle wafers such as (111) B and (311) B wait and compare with general crystal orientation (110), (100), and P elements is rich on the surface, and phosphorus/indium compares greater than 1.Because the difference of surperficial proportioning adopts conventional method for cleaning surface can cause the corrosion aggravation to its cleaning, the rough surface after causing cleaning is inhomogeneous, and the oxidation bed thickness.Under major light, detect, " white mist " appears in visible surface unevenly, can't satisfy the epitaxial growth needs of " opening box promptly uses ".
In addition, method of the prior art also is difficult to remove simultaneously preferably the particle and the metal residue on above-mentioned inp wafer surface.
Summary of the invention
Make the present invention for solving one or more the problems referred to above that exist in the prior art.
The present invention provides a kind of method of cleaning inp wafer, and this method may further comprise the steps:
(1) at-10 to 25 ℃ with a kind of H that contains
2O
2The ammonia spirit processing wafers;
(2) use the deionized water wash wafer;
(3) at-10 to 55 ℃ with a kind of concentrated acid processing wafers;
(4) use the deionized water wash wafer;
(3) at-10 to 35 ℃ with a kind of organic acid soln processing wafers;
(5) use the deionized water wash wafer; And
(6) dry gained wafer.
Unexpectedly, method of the present invention not only can reduce the particle and the metal residual of the special crystal orientation of inp wafer, particularly indium phosphide angle wafer surface effectively, and can also improve its surperficial corrosion uniformity and reduce white mist value.Thus obtained inp wafer can satisfy the epitaxial growth requirement of " opening box promptly uses " well.
Therefore, the present invention also provides the special crystal orientation of a kind of inp wafer, particularly indium phosphide angle wafer, in its every square centimeter wafer surface sectional area greater than 0.11 μ m
2Particle≤3.3/cm
2Wafer surface (by the mean value of granule number in the wafer surface sectional area), metal residual Cu≤10 * 10 of wafer surface
10Atom/cm
2And Zn≤10 * 10
10Atom/cm
2, the average white mist value≤1.0ppm in surface.
Embodiment
The present invention provides a kind of method of cleaning inp wafer, may further comprise the steps:
(1) at-10 to 25 ℃ with a kind of H that contains
2O
2The ammonia spirit processing wafers;
(2) use the deionized water wash wafer;
(3) at-10 to 55 ℃ with a kind of concentrated acid processing wafers;
(4) use the deionized water wash wafer;
(5) at-10 to 35 ℃ with a kind of organic acid soln processing wafers;
(6) use the deionized water wash wafer; And
(7) dry gained wafer.
Unexpectedly, method of the present invention not only can be cleaned the inp wafer surface effectively, reduces the wafer surface particle and reduces the residual quantity of metal, particularly copper and zinc, and can also guarantee the uniformity of corroding to make white mist value lower.Therefore, the wafer that uses the inventive method to obtain can satisfy the epitaxial growth requirement of " opening box promptly uses " well.
In the present invention, said inp wafer is preferably the special crystal orientation of a kind of indium phosphide angle wafer.With regard to the present invention, the special crystal orientation of indium phosphide angle wafer is meant the inp wafer of all angles except that indium phosphide (100) and (110), preferred indium phosphide (111) B or indium phosphide (311) B crystal orientation angle wafer.
In the methods of the invention; The wafer (i.e. the wafer of (1) step use) that uses as raw wafers is a wafer (promptly having accomplished meticulous bright finished wafer) of having accomplished chemical mechanical polishing and chemical meticulous polishing; The wafer behind the single-sided polishing normally; Its burnishing surface surface microroughness Ra≤0.5nm (with AFM (AFM) test), preferred Ra≤0.3nm.If require polishing both surfaces, then above-mentioned parameter is the mean value on two sides.
In the step (1) of the inventive method (at-10 to 25 ℃ with a kind of H that contains
2O
2The ammonia spirit processing wafers) in, the said H that contains
2O
2Ammonia spirit be meant NH
3, H
2O
2Mixture with water.With the said H that contains
2O
2The total weight of ammonia spirit be benchmark, NH
3Concentration be generally 2-25 weight %, preferred 4-20 weight %, more preferably 5-15 weight %; H
2O
2Concentration be generally 0.5-15 weight %, preferred 1-10 weight %, more preferably 2-6 weight %.Processing procedure is advantageously being carried out below 23 ℃, preferably carries out-5 to 20 ℃ temperature, more preferably carries out 0-15 ℃ temperature.The processing time of this step is generally 5-300 second, preferred 30-240 second, more preferably 60-120 second.Said processing comprises, but is not limited to, and flushing or immerse is handled, and preferred the immersion handled.
In a particularly preferred embodiment of the present invention, the concentration of ammoniacal liquor (is NH in the step (1)
3Concentration) C
1, step (1) treatment temperature T
1With processing time P
1Relation below satisfying:
30≤C
1×P
1×(T
1+273.15)/1000≤1,100
Preferably,
50≤C
1×P
1×(T
1+273.15)/1000≤500
Further preferably,
80≤C
1×P
1×(T
1+273.15)/1000≤200
Above-mentioned various in, the concentration unit concentration that is weight percentage, treatment temperature is degree centigrade, the processing time is second.
In the present invention, employed term " deionized water " has implication as known in the art.Usually, it is meant 25 ℃ resistivity and preferably is not less than 15 megaohms centimetres (1.5 * 10
7Ω cm), more preferably be not less than the water of 17 megaohms centimetre.
In the step (2) of the inventive method, (4) and (6) (using the deionized water wash wafer), each step is preferably carried out at lower temperature, and for example preferred 0-30 ℃, more preferably 5-25 ℃, most preferably at 8-20 ℃.Washing time is generally 5-100 second, preferred 20-80 second, more preferably 40-60 second.
In the step (3) of the inventive method (at-10 to 55 ℃ with a kind of concentrated acid processing wafers), preferably, said concentrated acid is an inorganic acid, and preferred inorganic acid includes, but not limited to sulfuric acid, hydrochloric acid, phosphoric acid and nitric acid etc., preferably sulfuric acid or nitric acid.Because at a certain temperature, the dissolubilities of different acid are different, so adopt differently when sour, all adopt its concentrated acid under operating temperature, for example when its concentration C
3For 60% when above of the saturated concentration under the relevant temperature, think that then it is " concentrated acid ".Preferably, when adopting sulfuric acid, its concentration is not less than 65 weight % usually.Usually, used sulfuric acid concentration is 65-98 weight %, preferred 70-97 weight %, more preferably 85-95 weight %.Treatment temperature T
3Be preferably 15-50 ℃, more preferably 25-45 ℃, most preferably 35-40 ℃.The processing time P of this step
3Be generally 1-20 second, be preferably 2-15 second, more preferably 3-10 second.Said processing comprises, but is not limited to, and flushing or immerse is handled, and preferred the immersion handled.In processing procedure, preferably adopt mega sonic wave or ultrasonic wave auxiliary processing.
Preferably, the concentration C of the acid of step (3)
3, treatment temperature T
3With processing time P
3Relation below satisfying:
30≤C
3×P
3×(T
3+273.15)/1000≤1,000；
Further preferred again:
80≤C
3×P
3×(T
3+273.15)/1000≤500；
Further preferred:
100≤C
3×P
3×(T
3+273.15)/1000≤300。
More than various in, the concentration unit concentration that is weight percentage, treatment temperature is degree centigrade, the processing time is second.
In a preferred embodiment, method of the present invention step (3) afterwards, step (4) before, also comprise a step (3A): at-10 to 30 ℃ with a kind of concentrated acid processing wafers.
In the step (3A) of the inventive method (at-10 to 30 ℃ with a kind of concentrated acid processing wafers), preferably, said concentrated acid is an inorganic acid, and preferred inorganic acid includes, but not limited to sulfuric acid, hydrochloric acid, phosphoric acid and nitric acid etc., preferably sulfuric acid or nitric acid.Because at a certain temperature, the dissolubilities of different acid are different, so adopt differently when sour, all adopt its concentrated acid under operating temperature, for example when its concentration C
3AFor 60% when above of the saturated concentration under the relevant temperature, think that then it is " concentrated acid ".Preferably, when adopting sulfuric acid, its concentration is not less than 65 weight % usually.Usually, used sulfuric acid concentration is 65-98 weight %, preferred 70-97 weight %.Treatment temperature T
3ABe preferably 5-30 ℃, more preferably 10-28 ℃, most preferably 20-25 ℃.The processing time P of this step
3ABe generally 0.5-15 second, preferred 1-10 second, more preferably 2-6 second.Said processing comprises, but is not limited to, and flushing or immerse is handled, and preferred the immersion handled.In processing procedure, preferably adopt mega sonic wave or ultrasonic wave auxiliary processing.
Preferably, the concentration C of the acid of step (3A)
3A, treatment temperature T
3AWith processing time P
3ABetween satisfy below relation:
10≤C
3A×P
3A×(T
3A+273.15)/1000≤400；
Further preferred again:
30≤C
3A×P
3A×(T
3A+273.15)/1000≤200；
Further preferred:
40≤C
3A×P
3A×(T
3A+273.15)/1000≤120。
More than various in, the concentration unit concentration that is weight percentage, treatment temperature is degree centigrade, the processing time is second.
Preferably, the treatment temperature of step (3) is higher than the treatment temperature of step (3A).In addition, step (3) can preferably adopt identical acid to handle with (3A).At this moment, can adopt with a concentrated acid, handle continuously according to different temperature, for example at completing steps (3) afterwards, the treatment temperature that is cooled to step (3A) rapidly continues to handle; In this embodiment, C
3AConcentration when beginning for step (3A).If used sour different of the used acid of step (3A) and step (3), then in step (3) afterwards, preferably, wafer carries out step (3A) again with deionized water wash 5-30 after second.
In a particularly preferred embodiment of the present invention, the concentration C of the acid of step (3)
3, treatment temperature T
3With processing time P
3Concentration C with the acid of step (3A)
3A, treatment temperature T
3AWith processing time P
3ABetween satisfy below relation:
2×C
3A×P
3A×(T
3A+273.15)≤C
3×P
3×(T
3+273.15)
≤3×C
3A×P
3A×(T
3A+273.15)，
In the following formula, the concentration unit concentration that is weight percentage, treatment temperature is degree centigrade, and the processing time is second.
In the step (5) of the inventive method (at-10 to 35 ℃ with a kind of organic acid soln processing wafers), used organic acid can be a kind of organic multicomponent acid commonly used, preferred C
3-C
12Organic dibasic acid or ternary acid, more preferably C
3-C
10Organic dibasic acid or ternary acid.Said acid includes, but not limited to citric acid, tartaric acid, maleic acid, fumaric acid, malic acid, gluconic acid and glucoheptonic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, azelaic acid, decanedioic acid etc., most preferably citric acid.Said organic acid concentration C
6Be generally 1-10 weight %, preferred 2-8 weight %, more preferably 3-6 weight %.Temperature T when handling with organic acid
5Be generally 5-30 ℃, preferred 15-28 ℃, more preferably 20-25 ℃.The processing time P of this step
5Be generally 15-50 second, preferred 20-40 second, more preferably 25-30 second.Said processing comprises, but is not limited to, and flushing or immerse is handled, and preferred the immersion handled.
Further preferably, the concentration C of acid in the step (5)
5, treatment temperature T
5With processing time P
6Relation below satisfying:
5≤C
5×P
5×(T
5+273.15)/1000≤150。
Further preferably,
10≤C
5×P
5×(T
5+273.15)/1000≤60。
More than various in, the concentration unit concentration that is weight percentage, treatment temperature is degree centigrade, the processing time is second.
In a particularly preferred embodiment according to the invention, the concentration C of acid in concentration, treatment temperature, processing time and the step (5) of acid in step (3), the step (3A)
5, treatment temperature T
5With processing time P
5Relation below satisfying:
1/12[C
3×P
3×(T
3+273.15)+C
3A×P
3A×(T
3A+273.15)]
≤C
5×P
5×(T
5+273.15)
≤1/4[C
3×P
3×(T
3+273.15)+C
3A×P
3A×(T
3A+273.15)]，
More than various in, the concentration unit concentration that is weight percentage, treatment temperature is degree centigrade, the processing time is second.
In the step (7) of the inventive method, for example can select drying crystal wafer in air, nitrogen or other inert gas (for example argon gas etc.), or select vacuumize, the preferred 20-120 of baking temperature ℃, preferred 40-90 ℃, more preferably 50-70 ℃; Preferred 0.5-20 minute drying time, more preferably 1-10 minute.
The inventive method is suitable for cleaning inp wafer, the inp wafer of preferred special angle, more preferably indium phosphide (111) B or indium phosphide (311) B crystal orientation angle wafer.The diameter of said wafer is for example 2.50-15.0 centimetre, like 5.0 centimetres, 7.5 centimetres, 10.0 centimetres, 12.5 centimetres or 15.0 centimetres (wafer process for example allows ± 0.05 cm size tolerance).The inp wafer of gained, in every square centimeter of wafer surface sectional area greater than 0.11 μ m
2Particle≤3.3/cm
2Wafer surface, preferred≤2.2/cm
2Wafer surface; Metal residual Cu≤10 * 10 of wafer surface
10Atom/cm
2, preferred Cu≤5 * 10
10Atom/cm
2, more preferably Cu≤2 * 10
10Atom/cm
2, the residual Cu of most preferred metal≤1 * 10
10Atom/cm
2, and metal residual Zn≤10 * 10 of wafer surface
10Atom/cm
2, preferred Zn≤6 * 10
10Atom/cm
2, more preferably Zn≤3 * 10
10Atom/cm
2, Zn≤1 * 10 most preferably
10Atom/cm
2The average white mist value≤1.0ppm in surface, the average white mist value≤0.8ppm of preferred surface, more preferably≤0.5ppm; Its surface microroughness Ra≤0.5nm (with AFM (AFM) test), preferred Ra≤0.3nm.Usually, wafer single-sided polishing; If require polishing both surfaces, then above-mentioned parameter is the mean value on two sides.
Therefore, the present invention also provides a kind of inp wafer, special angle inp wafer particularly, preferred indium phosphide (111) B or indium phosphide (311) B crystal orientation angle wafer, in its every square centimeter wafer surface sectional area greater than 0.11 μ m
2Particle≤3.3/cm
2Wafer surface, preferred≤2.2/cm
2Wafer surface; Metal residual Cu≤10 * 10 of wafer surface
10Atom/cm
2And Zn≤10 * 10
10Atom/cm
2, the residual Cu of preferable alloy≤5 * 10
10Atom/cm
2And Zn≤6 * 10
10Atom/cm
2, more preferably metal residual Cu≤2 * 10
10Atom/cm
2And Zn≤3 * 10
10Atom/cm
2, the residual Cu of most preferred metal≤1 * 10
10Atom/cm
2And Zn≤1 * 10
10Atom/cm
2The average white mist value≤1.0ppm in surface, the average white mist value≤0.8ppm of preferred surface, more preferably≤0.5ppm; Its surface microroughness Ra≤0.5nm (with AFM (AFM) test), preferred Ra≤0.3nm.Usually, wafer single-sided polishing; If require polishing both surfaces, then above-mentioned parameter is the mean value on two sides.
In the present invention, as do not have other explanation, then all percentage or umber are all by weight.As do not have other explanation, then all concentration are all calculated based on the pure material of said material.As do not have other explanation, and temperature is room temperature, and pressure is atmospheric pressure.In context of the present invention, can make up each other between General Definition and the preferred definition at different levels, form new technical scheme, also be regarded as disclosed by this specification.
Embodiment:
Instrument and device:
Wet-cleaned platform (comprising the groove and rinsing bowl and draining and the exhaust system that soak wafer);
Wafer rotary drier (the 101 type SRD of U.S. Semitool company, rotating speed adjustable).The wafer quality testing instrument:
(light intensity is greater than 500,000Lux) for the Yamada major light;
Wafer surface analyzer (U.S. KLA-TENCOR company 6220 types);
AFM (AFM) (U.S. NanoScopeIIIa of Digital Instrument company type) (vertical resolution 0.03nm, analyzed area 5 μ m * 5 μ m);
With reflection x-ray fluorescence analyzer (TREX 610 types, OSAKA Japan Technos company) testing wafer surface-element.
Test wafers:
As do not have other explanation, then all adopt 5.08 centimetres of diameters (2 inches), wherein one side is through rough polishing and meticulous bright finished inp wafer, thickness is 350 μ m, burnishing surface surface microroughness Ra=0.3nm.All detections are all carried out to burnishing surface.
Embodiment 1
Clean inp wafer with following step, said wafer is indium phosphide (a 311) B crystal orientation angle wafer:
(1) 1 wafer immersion to be washed is contained H
2O
2Ammonia spirit in, handled 60 seconds at about 20 ℃, the concentration of ammoniacal liquor is 5 weight % in the said solution, H
2O
2Concentration be 2 weight %;
(2) above-mentioned wafer is taken out, puts into flushed channel, about 16 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 60 seconds;
(3) wafer after will washing immerses in the concentrated sulfuric acid of 90 weight %, handles 5 seconds at about 40 ℃;
(4) above-mentioned wafer is taken out, puts into flushed channel, about 16 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 60 seconds;
(5) wafer after will washing immerses in the 2 weight % citric acids and handled 30 seconds at about 25 ℃;
(6) above-mentioned wafer is taken out, puts into flushed channel, about 16 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 60 seconds;
(7) wafer after will washing takes out, and puts into the wafer rotary drier with hot nitrogen (70 ℃) drying 1 minute.
Dried wafer detects wafer surface with major light, wafer surface analyzer, AFM and reflection x-ray fluorescence analyzer.
Learn that by the major light detection wafer surface does not have visible particle, do not have white mist.Detect by the wafer surface analyzer and to learn, in the wafer surface sectional area greater than 0.11 μ m
2Particle be 1.50/cm
2Wafer surface, white mist value (Haze value)=0.29ppm.Detect tenor by the reflection x-ray fluorescence analyzer and learn the Cu=0.62 of wafer surface * 10
10Atom/cm
2, Zn=1.03 * 10
10Atom/cm
2
Embodiment 2
Clean inp wafer with following step, said wafer is indium phosphide (a 311) B crystal orientation angle wafer:
(1) 1 wafer immersion to be washed is contained H
2O
2Ammonia spirit in, handled 60 seconds at about 20 ℃, the concentration of ammoniacal liquor is 5 weight % in the said solution, H
2O
2Concentration be 2 weight %;
(2) above-mentioned wafer is taken out, puts into flushed channel, about 16 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 60 seconds;
(3) wafer after will washing immerses in the concentrated sulfuric acid of 90 weight %, handles 5 seconds at about 40 ℃;
(3A) above-mentioned wafer is taken out, immerse in the concentrated sulfuric acid of 90 weight %, handled 2 seconds at about 25 ℃;
(4) above-mentioned wafer is taken out, puts into flushed channel, about 16 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 60 seconds;
(5) wafer after will washing immerses in the 2 weight % citric acids and handled 30 seconds at about 25 ℃;
(6) above-mentioned wafer is taken out, puts into flushed channel, about 16 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 60 seconds;
(7) wafer after will washing takes out, and puts into the wafer rotary drier with hot nitrogen (70 ℃) drying 1 minute.
Dried wafer detects wafer surface with major light, wafer surface analyzer, AFM and reflection x-ray fluorescence analyzer.
Learn that by the major light detection wafer surface does not have visible particle, do not have white mist.Detect by the wafer surface analyzer and to learn, in the wafer surface sectional area greater than 0.11 μ m
2Particle be 1.42/cm
2Wafer surface, white mist value (Haze value)=0.21ppm.Detect tenor by the reflection x-ray fluorescence analyzer and learn the Cu=0.5 of wafer surface * 10
10Atom/cm
2, Zn=0.8 * 10
10Atom/cm
2
Embodiment 3
Clean inp wafer with following step, said wafer is indium phosphide (a 111) B crystal orientation angle wafer:
(1) 1 wafer immersion to be washed is contained H
2O
2Ammonia spirit in, handled 60 seconds at about 20 ℃, the concentration of ammoniacal liquor is 5 weight % in the said solution, H
2O
2Concentration be 2 weight %;
(2) above-mentioned wafer is taken out, puts into flushed channel, about 16 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 60 seconds;
(3) wafer after will washing immerses in the concentrated sulfuric acid of 90 weight %, handles 5 seconds at about 40 ℃;
(3A) above-mentioned wafer is taken out, immerse in the concentrated sulfuric acid of 90 weight %, handled 2 seconds at about 25 ℃;
(4) above-mentioned wafer is taken out, puts into flushed channel, about 16 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 60 seconds;
(5) wafer after will washing immerses in the 2 weight % citric acids and handled 30 seconds at about 25 ℃;
(6) above-mentioned wafer is taken out, puts into flushed channel, about 16 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 60 seconds;
(7) wafer after will washing takes out, and puts into the wafer rotary drier with hot nitrogen (70 ℃) drying 1 minute.
Dried wafer detects wafer surface with major light, wafer surface analyzer, AFM and reflection x-ray fluorescence analyzer.
Learn that by the major light detection wafer surface does not have visible particle, do not have white mist.Detect by the wafer surface analyzer and to learn, in the wafer surface sectional area greater than 0.11 μ m
2Particle be 1.36/cm
2Wafer surface, white mist value (Haze value)=0.22ppm.Detect tenor by the reflection x-ray fluorescence analyzer and learn the Cu=0.4 of wafer surface * 10
10Atom/cm
2, Zn=0.7 * 10
10Atom/cm
2
Embodiment 4
Clean inp wafer with following step, said wafer is the conventional crystal orientation of indium phosphide (a 100) angle wafer:
(1) 1 wafer immersion to be washed is contained H
2O
2Ammonia spirit in, handled 60 seconds at about 20 ℃, the concentration of ammoniacal liquor is 5 weight % in the said solution, H
2O
2Concentration be 2 weight %;
(2) above-mentioned wafer is taken out, puts into flushed channel, about 16 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 60 seconds;
(3) wafer after will washing immerses in the concentrated sulfuric acid of 90 weight %, handles 5 seconds at about 40 ℃;
(3A) above-mentioned wafer is taken out, immerse in the concentrated sulfuric acid of 90 weight %, handled 2 seconds at about 25 ℃;
(4) above-mentioned wafer is taken out, puts into flushed channel, about 16 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 60 seconds;
(5) wafer after will washing immerses in the 2 weight % citric acids and handled 30 seconds at about 25 ℃;
(6) above-mentioned wafer is taken out, puts into flushed channel, about 16 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 60 seconds;
(7) wafer after will washing takes out, and puts into the wafer rotary drier with hot nitrogen (70 ℃) drying 2 minutes.
Dried wafer detects wafer surface with major light, wafer surface analyzer, AFM and reflection x-ray fluorescence analyzer.
Learn that by the major light detection wafer surface does not have visible particle, do not have white mist.Detect by the wafer surface analyzer and to learn, in the wafer surface sectional area greater than 0.11 μ m
2Particle be 1.06/cm
2Wafer surface, white mist value (Haze value)=0.18ppm.Detect tenor by the reflection x-ray fluorescence analyzer and learn the Cu=0.2 of wafer surface * 10
10Atom/cm
2, Zn=0.4 * 10
10Atom/cm
2
Embodiment 5
Clean inp wafer with following step, said wafer is indium phosphide (a 311) B crystal orientation angle wafer:
(1) 1 wafer immersion to be washed is contained H
2O
2Ammonia spirit in, handled 25 seconds at about 8 ℃, the concentration of ammoniacal liquor is 15 weight % in the said solution, H
2O
2Concentration be 1 weight %;
(2) above-mentioned wafer is taken out, puts into flushed channel, about 20 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 75 seconds;
(3) wafer after will washing immerses in the concentrated sulfuric acid of 98 weight %, handles 10 seconds at about 30 ℃;
(3A) above-mentioned wafer is taken out, immerse in the concentrated sulfuric acid of 98 weight %, handled 4 seconds at about 22 ℃;
(4) above-mentioned wafer is taken out, puts into flushed channel, about 20 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 75 seconds;
(5) wafer after will washing immerses in the 6 weight % citric acids and handled 40 seconds at about 20 ℃;
(6) above-mentioned wafer is taken out, puts into flushed channel, about 20 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 75 seconds;
(7) wafer after will washing takes out, and puts into the wafer rotary drier with hot nitrogen (70 ℃) drying 0.5 minute.
Dried wafer detects wafer surface with major light, wafer surface analyzer, AFM and reflection x-ray fluorescence analyzer.
Learn that by the major light detection wafer surface does not have visible particle, do not have white mist.Detect by the wafer surface analyzer and to learn, in the wafer surface sectional area greater than 0.11 μ m
2Particle be 1.56/cm
2Wafer surface, white mist value (Haze value)=0.38ppm.Detect tenor by the reflection x-ray fluorescence analyzer and learn the Cu=2.0 of wafer surface * 10
10Atom/cm
2, Zn=3.5 * 10
10Atom/cm
2
Embodiment 6
Clean inp wafer with following step, said wafer is indium phosphide (a 311) B crystal orientation angle wafer:
(1) 1 wafer immersion to be washed is contained H
2O
2Ammonia spirit in, handled 100 seconds at about 3 ℃, the concentration of ammoniacal liquor is 3 weight % in the said solution, H
2O
2Concentration be 6 weight %;
(2) above-mentioned wafer is taken out, puts into flushed channel, about 25 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 30 seconds;
(3) wafer after will washing immerses in the red fuming nitric acid (RFNA) of 65 weight %, handles 15 seconds at about 50 ℃;
(3A) above-mentioned wafer is taken out, immerse in the red fuming nitric acid (RFNA) of 65 weight %, handled 6 seconds at about 20 ℃;
(4) above-mentioned wafer is taken out, puts into flushed channel, about 25 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 30 seconds;
(5) wafer after will washing immerses in the 8 weight % malic acid and handled 20 seconds at about 15 ℃;
(6) above-mentioned wafer is taken out, puts into flushed channel, about 25 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 30 seconds;
(7) wafer after will washing takes out, and puts into the wafer rotary drier with hot nitrogen (70 ℃) drying 10 minutes.
Dried wafer detects wafer surface with major light, wafer surface analyzer, AFM and reflection x-ray fluorescence analyzer.
Learn that by the major light detection wafer surface does not have visible particle, do not have white mist.Detect by the wafer surface analyzer and to learn, in the wafer surface sectional area greater than 0.11 μ m
2Particle be 2.2/cm
2Wafer surface, white mist value (Haze value)=0.53ppm.Detect tenor by the reflection x-ray fluorescence analyzer and learn the Cu=5.5 of wafer surface * 10
10Atom/cm
2, Zn=4.2 * 10
10Atom/cm
2
Embodiment 7
Clean inp wafer with following step, said wafer is indium phosphide (a 111) B crystal orientation angle wafer:
(1) 1 wafer immersion to be washed is contained H
2O
2Ammonia spirit in, approximately-3 ℃ handled 200 seconds, the concentration of ammoniacal liquor is 20 weight % in the said solution, H
2O
2Concentration be 10 weight %;
(2) above-mentioned wafer is taken out, puts into flushed channel, about 30 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 10 seconds;
(3) wafer after will washing immerses in the concentrated hydrochloric acid of 36 weight %, approximately-5 ℃ handled 3 seconds;
(3A) above-mentioned wafer is taken out, immerse in the concentrated hydrochloric acid of 30 weight %, handled 10 seconds at about-10 ℃;
(4) above-mentioned wafer is taken out, puts into flushed channel, about 30 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 10 seconds;
(5) wafer after will washing immerses in the 10 weight % citric acids and handled 17 seconds at about 30 ℃;
(6) above-mentioned wafer is taken out, puts into flushed channel, about 30 ℃ with resistivity greater than the deionized water rinsing of 17 megaohms centimetre 10 seconds;
(7) wafer after will washing takes out, and puts into the wafer rotary drier with hot nitrogen (70 ℃) drying 1 minute.
Dried wafer detects wafer surface with major light, wafer surface analyzer, AFM and reflection x-ray fluorescence analyzer.
Learn that by the major light detection wafer surface does not have visible particle, do not have white mist.Detect by the wafer surface analyzer and to learn, in the wafer surface sectional area greater than 0.11 μ m
2Particle be 2.8/cm
2Wafer surface, white mist value (Haze value)=0.86ppm.Detect tenor by the reflection x-ray fluorescence analyzer and learn the Cu=7.8 of wafer surface * 10
10Atom/cm
2, Zn=6.3 * 10
10Atom/cm
2
Comparative Examples 1
Clean inp wafer with following step, said wafer is indium phosphide (a 311) B crystal orientation angle wafer:
(1) wafer to be washed is immersed in the concentrated sulfuric acid of 92 weight % handled 4 seconds in 65 ℃;
(2) above-mentioned wafer taking-up is immersed in the 98 weight % concentrated sulfuric acids in 25 ℃ of processing 2 seconds then;
(3) then in 20 ℃, wafer is put into flushed channel, with resistivity greater than the deionized water rinsing wafer surface of 17.5 megohms 55 seconds;
The wafer that (4) will wash immerses in the citric acid solution of 8 weight % to be handled 30 seconds in 25 ℃;
(5) then wafer is put into flushed channel, in 20 ℃, with resistivity greater than the deionized water rinsing wafer surface of 17.5 megohms 20 seconds;
The wafer that (6) will wash immerses NH
4OH-H
2O
2Solution (H
2O
2: NH
4OH: H
2The weight ratio of O is 1: 2: 7) in handled 5 seconds in 25 ℃;
(7) then in 20 ℃, wafer is put into flushed channel, with resistivity greater than the deionized water rinsing wafer surface of 17.5 megohms 30 seconds;
(8) wafer after will washing is put into the wafer rotary drier with dry 15 minutes of hot nitrogen (70 ℃).
Dried wafer detects wafer surface with major light, wafer surface analyzer, AFM and reflection x-ray fluorescence analyzer.
Learn that by the major light detection wafer surface does not have visible particle, do not have white mist.Detect by the wafer surface analyzer and to learn, in the wafer surface sectional area greater than 0.11 μ m
2Particle be 3.55/cm
2Wafer surface, white mist value (Haze value)=1.30ppm.Detect tenor by the reflection x-ray fluorescence analyzer and learn the Cu=11.5 of wafer surface * 10
10Atom/cm
2, Zn=14.2 * 10
10Atom/cm
2
Comparative Examples 2
Clean inp wafer with following step, said wafer is indium phosphide (a 111) B crystal orientation angle wafer:
(1) 1 wafer to be washed is put into mega sonic wave cleaning machine (H63-132/ZM; Available from Beijing Co., Ltd of Sevenstar Huachuang Electronic) in the rinse bath that fills mega sonic wave cleaning fluid (the clear DZ-4B series that is used for production process of semiconductor rosin and paraffin) in, cleaned 6-15 minute;
(2) with flushing in wafer taking-up immersion deionized water 4-10 minute;
(3) above-mentioned wafer is taken out, immerse 70-100 ℃ the middle 30-40 of cleaning of hot concentrated sulfuric acid (98 weight %) second;
(4) wafer is taken out, immerse 25 ℃ the middle 5-10 of cleaning of the concentrated sulfuric acid (98 weight %) second;
(5) with deionized water rinsing wafer 1-5 minute;
(6) wafer after will washing takes out, and immerses NH
4OH-H
2O
2The aqueous solution in clean 3-10 second, the NH in the said aqueous solution at 0-5 ℃
4OH: H
2O
2: H
2The volume ratio of O is 1-5: 1-5: 6-12;
(7) wafer is taken out, with deionized water rinsing 1-5 minute;
(8) wafer after will washing is put into the wafer rotary drier with dry 15 minutes of hot nitrogen (70 ℃).
Dried wafer detects wafer surface with major light, wafer surface analyzer, AFM and reflection x-ray fluorescence analyzer.
Learn that by the major light detection wafer surface does not have visible particle, do not have white mist.Detect by the wafer surface analyzer and to learn, in the wafer surface sectional area greater than 0.11 μ m
2Particle be 15.6/cm
2Wafer surface, white mist value (Haze value)=4.80ppm.Detect tenor by the reflection x-ray fluorescence analyzer and learn the Cu=10.2 of wafer surface * 10
10Atom/cm
2, Zn=17.8 * 10
10Atom/cm
2
The foregoing description is the preferred embodiment of the present invention; But execution mode of the present invention is not restricted to the described embodiments; Other any do not deviate from the change done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. method of cleaning inp wafer may further comprise the steps:
(1) at-10 to 25 ℃ with a kind of H that contains
2O
2The ammonia spirit processing wafers;
(2) use the deionized water wash wafer;
(3) at-10 to 55 ℃ with a kind of concentrated acid processing wafers;
(4) use the deionized water wash wafer;
(5) at-10 to 35 ℃ with a kind of organic acid soln processing wafers;
(6) use the deionized water wash wafer; And
(7) dry gained wafer.
2. the process of claim 1 wherein that the wafer that step (1) is used is a wafer of having accomplished chemical mechanical polishing and chemical meticulous polishing, its burnishing surface surface microroughness Ra≤0.5nm.
3. the process of claim 1 wherein the concentration C of ammoniacal liquor in the step (1)
1, treatment temperature T
1With processing time P
1Relation below satisfying:
30≤C
1×P
1×(T
1+273.15)/1000≤1,100
In the following formula, the concentration unit concentration that is weight percentage, treatment temperature is degree centigrade, and the processing time is second.
4. the process of claim 1 wherein step (3) afterwards, step (4) before, also comprise a step (3A): at-10 to 30 ℃ with a kind of concentrated acid processing wafers.
5. the process of claim 1 wherein that step (3) and the said concentrated acid that (3A) uses are inorganic acid, its concentration is more than 60% of saturated concentration of its operating temperature.
6. the method for claim 4, the wherein concentration C of the acid of step (3)
3, treatment temperature T
3With processing time P
3Concentration C with the acid of step (3A)
3A, treatment temperature T
3AWith processing time P
3ABetween satisfy below relation:
2×C
3A×P
3A×(T
3A+273.15)≤C
3×P
3×(T
3+273.15)
≤3×C
3A×P
3A×(T
3A+273.15)
In the following formula, the concentration unit concentration that is weight percentage, treatment temperature is degree centigrade, and the processing time is second.
7. the process of claim 1 wherein that the acid of step (5) is citric acid.
8. the method for claim 4, the wherein concentration C of the acid of step (3)
3, treatment temperature T
3With processing time P
3Concentration C with the acid of step (3A)
3A, treatment temperature T
3AWith processing time P
3AAnd with step (5) in acid concentration C
5, treatment temperature T
5With processing time P
5Relation below satisfying:
1/12[C
3×P
3×(T
3+273.15)+C
3A×P
3A×(T
3A+273.15)]
≤C
5×P
5×(T
5+273.15)
≤1/4[C
3×P
3×(T
3+273.15)+C
3A×P
3A×(T
3A+273.15)]，
In the following formula, the concentration unit concentration that is weight percentage, treatment temperature is degree centigrade, and the processing time is second.
9. inp wafer, wherein in every square centimeter of wafer surface sectional area greater than 0.11 μ m
2Particle≤3.3/cm
2, metal residual Cu≤10 * 10 of wafer surface
10Atom/cm
2, Zn≤10 * 10
10Atom/cm
2, the average white mist value≤1.0ppm in surface.
10. the inp wafer of claim 9, it is indium phosphide (111) B or indium phosphide (311) B crystal orientation angle wafer.
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| CN104181026A (en) * | 2014-08-27 | 2014-12-03 | 中国电子科技集团公司第十三研究所 | Chemical polishing solution and dislocation measurement method for indium phosphide slice |
| CN105225988A (en) * | 2015-09-25 | 2016-01-06 | 江苏中科晶元信息材料有限公司 | Wafer cleaning checks all-in-one |
| CN107338481A (en) * | 2017-06-27 | 2017-11-10 | 台山市华兴光电科技有限公司 | A kind of cleaning method of indium phosphide polycrystal material |
| CN112382555A (en) * | 2020-11-12 | 2021-02-19 | 广东先导先进材料股份有限公司 | Method for cleaning indium phosphide substrate |
| US10964786B2 (en) | 2017-05-26 | 2021-03-30 | Sumitomo Electric Industries, Ltd. | Group III-V compound semiconductor substrate and group III-V compound semiconductor substrate with epitaxial layer |
| CN113035690A (en) * | 2021-02-26 | 2021-06-25 | 中锗科技有限公司 | Method for cleaning indium phosphide wafer |
| CN113690128A (en) * | 2021-08-27 | 2021-11-23 | 珠海鼎泰芯源晶体有限公司 | Method for cleaning indium phosphide wafer |
| CN113793801A (en) * | 2021-09-07 | 2021-12-14 | 广东先导微电子科技有限公司 | Method for cleaning indium phosphide substrate wafer |
| CN113894112A (en) * | 2021-09-14 | 2022-01-07 | 先导薄膜材料有限公司 | Indium foil surface treatment method |
| CN114042684A (en) * | 2022-01-12 | 2022-02-15 | 北京通美晶体技术股份有限公司 | Indium phosphide wafer and mixed cleaning process thereof |
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| CN107338481A (en) * | 2017-06-27 | 2017-11-10 | 台山市华兴光电科技有限公司 | A kind of cleaning method of indium phosphide polycrystal material |
| CN112382555A (en) * | 2020-11-12 | 2021-02-19 | 广东先导先进材料股份有限公司 | Method for cleaning indium phosphide substrate |
| CN113035690B (en) * | 2021-02-26 | 2023-09-22 | 中锗科技有限公司 | Method for cleaning indium phosphide wafer |
| CN113035690A (en) * | 2021-02-26 | 2021-06-25 | 中锗科技有限公司 | Method for cleaning indium phosphide wafer |
| CN113690128A (en) * | 2021-08-27 | 2021-11-23 | 珠海鼎泰芯源晶体有限公司 | Method for cleaning indium phosphide wafer |
| CN113793801A (en) * | 2021-09-07 | 2021-12-14 | 广东先导微电子科技有限公司 | Method for cleaning indium phosphide substrate wafer |
| CN113894112A (en) * | 2021-09-14 | 2022-01-07 | 先导薄膜材料有限公司 | Indium foil surface treatment method |
| CN114335239A (en) * | 2021-12-06 | 2022-04-12 | 浙江光特科技有限公司 | InP substrate cleaning method |
| CN114042684A (en) * | 2022-01-12 | 2022-02-15 | 北京通美晶体技术股份有限公司 | Indium phosphide wafer and mixed cleaning process thereof |
| CN114042684B (en) * | 2022-01-12 | 2022-03-22 | 北京通美晶体技术股份有限公司 | Indium phosphide wafer and mixed cleaning process thereof |
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