CN1796968A - Method for detecting defect of single crystal structure of gallium arsenide in large size - Google Patents
Method for detecting defect of single crystal structure of gallium arsenide in large size Download PDFInfo
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Abstract
The invention is a defect detecting method for a large-size GaAs monocrystalline structure, comprising: grinding and polishing, i.e. mechanically or chemically polishing, where the formula of the adopted polishing solution is that the ratio of sulphuric acid to oxydol to water is 3 : 1 : 1; dislocation corroding, i.e. placing potassium hydroxide in a silver pot and heating to melt potassium hydroxide into a clear state and immediately placing the clear-state potassium hydroxide in a wafer sample for corroding, then taking out the sample and cooling, and then washing with water and blow-dry; selecting measuring direction, measuring point position and number of measuring points, observing visual field area, where the first measuring point is D/10mm apart from the wafer edge and the others are selected at 10 mm intervals, each of which is a measuring visual field; calculating for the selected measuring points. The invention enlarges the range of dislocation density detection, convenient and simple to operate and saving time.
Description
Affiliated field
The present invention relates to be applied to the single crystal structure of gallium arsenide defect inspection method of semiconductor applications, the particularly detection method of gallium arsenide in large size monocrystalline dislocation desity.
Background technology
Adopting according to qualifications, the chemical corrosion technology shows dislocation.Lattice in the crystal around the dislocation line distorts, and the place of appearing on plane of crystal is preferentially corroded some chemical mordant.Therefore the defective place of appearing forms easily and forms etch pit with given shape or the hillock of being with corner angle by some low index face on a certain crystal face of crystal.
At present, the detection method step of existing arsenide gallium monocrystal dislocation desity is: the gallium arsenide single-crystal wafer that cuts is ground, polishing, corrosion, detect and calculate, when the corrosion wafer, need treat just can put into when potassium hydroxide is heated to 400 ° ± 5 ℃ temperature the sample corrosion, need thermometer to measure like this, control etching time for the gallium arsenide in large size single-chip by existing method like this, the effect of corrosion is unintelligible, undesirable not even not denumerable meeting brings very big detection error, directly influence measuring accuracy, increased the complicacy of Measuring Time length and measuring operation in addition; When after corrosion, detecting, the mode of choosing of the measurement point of existing method is D/10mm, wherein D is the diameter of gallium arsenide single-crystal wafer, promptly choose a measurement point every D/10mm, when the diameter of gallium arsenide single-crystal wafer hour, choosing method is still all right like this, but when the increasing diameter added-time of gallium arsenide single-crystal wafer, this kind choosing method causes choosing of measurement point too wide, and measurement point reduces, and accuracy of detection does not reach requirement.In order to reduce measuring error, need set up the detection method of 150mm and above arsenide gallium monocrystal dislocation desity thereof, with the accuracy of guaranteeing to detect.
Summary of the invention
Technology of the present invention is dealt with problems and is: overcome the deficiencies in the prior art, a kind of defect inspection method of single crystal structure of gallium arsenide in large size is provided, being applicable to the detection of the above arsenide gallium monocrystal dislocation desity of 150mm, and this kind method to detect error little, the accuracy height.
Technical scheme of the present invention is: the defect inspection method of single crystal structure of gallium arsenide in large size, its characteristics are to comprise the following steps:
(1) grinds, the gallium arsenide single-crystal wafer that cuts is ground with emery, make surfacing, bright and clean, no marking, clean;
(2) polishing: mechanical buffing or chemical polishing, adopting the chemical polishing formula of liquid is sulfuric acid: hydrogen peroxide: water=3: 1: 1, be placed near room temperature after when polishing＜511〉crystal orientation monocrystalline, the polishing fluid for preparing need being stirred, again＜511〉the crystal orientation monocrystalline soaks in the polishing fluid, until＜511〉crystal orientation monocrystalline are polished, the polishing fluid temperature need not room temperature when polishing other crystal orientation monocrystalline;
(3) dislocation corrosion, potassium hydroxide is placed in silver crucible or the nickel crucible heats, putting into sample wafer when making the potassium hydroxide fusing be heated to clear state corrodes, for＜100 〉,＜111〉crystal orientation single-chips are 5～10 minutes, for＜511〉the crystal orientation single-chip is 7～13 minutes, take out sample then, flushing with clean water is used in the cooling back, dries up;
(4) carry out choosing of direction of measurement, measurement point position, number and measurement visual field, observation visual field area.Choose different measuring direction,＜100 according to the gallium arsenide single-crystal wafer of different crystal orientations 〉,＜511〉crystal orientation single-chips choose [110], [010] direction, and＜111〉crystal orientation single-chips are chosen [110], [112] direction is measured; First measurement point is chosen at the D/10mm place apart from Waffer edge, the every interval 10mm-12mm of other measurement point is one and measures the visual field, wherein D is the diameter of gallium arsenide wafer, the selection of measurement point i.e. (measurement point is oversize too many detection time) too much, measurement point can not reflect the distribution of whole gallium arsenide single-crystal wafer dislocation corrosion defective very little, and of the present invention choosing is to determine through a large amount of analysis of experimentss; Each measures visual field area 1mm
2, will the good at first macroscopic view observation of test piece of corrosion, according to the test piece dislocation etch pit what, choose different measuring visual field area, make different masks according to the arsenide gallium monocrystal of different size, different crystal orientations to detect, for dislocation desity less than 10000/cm
2, the visual field area is chosen 1mm
2, dislocation desity is greater than 10000/cm
2, the visual field area is chosen 1mm
2Can carry out full wafer to gallium arsenide single-crystal wafer and detect, also can choose 1/4 disk and detect.
(5) calculate, after selected point in the step (4) and visual field area determined, the applied optics microscopic examination is measured each and is observed visual field number, or application image gathers computation processing method and measure each visual field number, for＜100 〉,＜511〉crystal orientation single-chip average dislocation densities
Calculate by formula (1); For＜111〉crystal orientation single-chip average dislocation density
Calculate by formula (2).General single-chip dislocation etch pit central point quantity is many, only calculates once when calculating.
In the formula: i=1,2,3......n, the number of measurement point
N
iThe dislocation etch pit number of i measurement point
The microscopical design factor of C, C=l/s, cm
-2
S visual field area, cm
2
N
oCenter measurement point dislocation etch pit number
Principle of the present invention is: according to the characteristics of arsenide gallium monocrystal, at first solve demonstration dislocation defects technology, make its dislocation defects clear display, and then detect and calculate.Therefore of the present inventionly at first to grind, polish and corrosion makes its dislocation defects clear display, and then the rule that distributes according to 150mm arsenide gallium monocrystal dislocation desity, select limited measured zone, reflect whole according to 150mm single crystal structure of gallium arsenide defect situation, comprise: choosing, measure visual field number, measurement point position and observing determining of visual field area of direction of measurement reaches and detects purpose accurately.The present invention is the fault of construction that detects arsenide gallium monocrystal, general defect distribution entire wafer diverse location, after a large amount of tests, according to the gallium arsenide single-crystal wafer dislocation etch pit regularity of distribution, science, objectively calculate the entire wafer average dislocation density.The present invention not only can detect the gallium arsenide single-crystal wafer of the above size of 150mm, and simultaneous adaptation is less than the detection of the gallium arsenide single-crystal wafer dislocation desity of 150mm size.
In addition, the present invention if will detect accurately and reliably＜511〉dislocation desity, at first to solve＜pattern of 511〉crystal orientation monocrystalline corrosion dislocation defects, because,＜511〉crystal orientation monocrystalline dislocation defects pattern and＜111 〉,＜100〉crystal orientation monocrystalline dislocation defects patterns are different fully, though the same in whole technological process,, to solve especially＜511〉crystal orientation monocrystalline dislocation defects pattern appearing technique problems, just can make＜511〉crystal orientation monocrystalline dislocation defects manifest complete display.So, at first solve the polishing problem of＜511〉crystal orientation monocrystalline, the configuration of polishing fluid and the same (water: hydrogen peroxide: sulfuric acid=1: 1: 3) of other crystal orientation monocrystalline configuration, but, be placed into room temperature after when polishing＜511〉crystal orientation monocrystalline, the polishing fluid for preparing need being stirred, again＜511〉the crystal orientation monocrystalline soaks in the polishing fluid, until with＜511〉crystal orientation monocrystalline polished (the polishing fluid temperature need not room temperature when polishing other crystal orientation monocrystalline), improve polishing effect so greatly, when corrosion＜511〉crystal orientation monocrystalline dislocation defects, etching time is grown 2～3 minutes than other crystal orientation monocrystalline etching time, and this also is to corrode＜511〉crystal orientation monocrystalline dislocation defects pattern key points.Otherwise, be can not corrode dislocation defects or corrosive effect is bad.
The present invention's advantage compared with prior art is as follows:
(1) conventional detection is for the explanation of not testing of large-sized arsenide gallium monocrystal detection architecture defective, therefore use conventional detection, the selection of its field positions can not be satisfied large size single crystal and detect requirement, the present invention then to direction of measurement choose, measure visual field number, measurement point position and observe the visual field area determine carried out strict regulation, reached and detected purpose accurately.
(2) conventional detection, dislocation desity are applicable to 0～100000/cm
2, the dislocation desity scope of application of the present invention is 0～150000/cm
2, high to the arsenide gallium monocrystal dislocation desity, be connected on the computing machine with video camera by microscope, appliance computer software carries out the image acquisition computing, has enlarged the dislocation desity sensing range.
(3) conventional detection, the detection of arsenide gallium monocrystal dislocation desity is only right＜and 100 〉,＜111〉crystal orientation detect, and the present invention has improved detection method, make and detect the crystal orientation expanded range, not only can be to arsenide gallium monocrystal＜100 〉,＜111〉crystal orientation detect, can also right＜511 crystal orientation detects.
(4) the present invention is that potassium hydroxide is heated to clear state at dislocation corrosion, promptly puts into wafer, need not be heated to more than the 400C, therefore, does not need thermometer, and heat time heating time is short, easy and simple to handle, saves time.
(5) the present invention is in order accurately to detect the wafer dislocation desity, can save wafer material again, detect and 1/4 wafer dislocation desity detection contrast and a large amount of evidence through carrying out full wafer monocrystalline dislocation desity, can detect, especially large size single crystal is more had practical application with 1/4 wafer.
In a word, the present invention can detect 150mm and above arsenide gallium monocrystal dislocation desity thereof accurately and reliably.
Description of drawings
Fig. 1 among the present invention＜100,＜511〉crystal orientation disk monocrystalline measurement point position and sequence number figure;
Fig. 2 among the present invention＜100,＜511〉crystal orientation 1/4 disk monocrystalline measurement point position and sequence number figure;
Fig. 3 among the present invention＜111〉crystal orientation disk monocrystalline measurement point position and sequence number figure;
Fig. 4 among the present invention＜111〉crystal orientation 1/4 disk monocrystalline measurement point position and sequence number figure;
Fig. 5 among the present invention＜511〉crystal orientation monocrystalline dislocation defects shape appearance figures.
Embodiment
Embodiment 1, and it is as follows that the dislocation defects of 150mm gallium arsenide detects step:
(1) grinds, the 150mm gallium arsenide single-crystal wafer that cuts is ground with emery, make surfacing, bright and clean, no marking, clean;
(2) polishing: adopt chemical polishing, the polishing fluid prescription is a sulfuric acid: hydrogen peroxide: water=3: 1: 1, be placed into room temperature after when polishing＜511〉crystal orientation monocrystalline, the polishing fluid for preparing need being stirred, again＜511〉the crystal orientation monocrystalline soaks in the polishing fluid, until＜511〉crystal orientation monocrystalline are polished, the polishing fluid temperature need not room temperature when polishing other crystal orientation monocrystalline;
(3) dislocation corrosion, potassium hydroxide is placed in the silver crucible heats, putting into sample wafer when making the potassium hydroxide fusing be heated to clear state corrodes, for＜100 〉,＜111〉crystal orientation single-chips are 5-10 minute, for＜511〉the crystal orientation single-chip is 7-13 minute, takes out sample then, cooling back flushing with clean water, dry up, for＜511 crystal orientation single-chip dislocation defects shape appearance figure as shown in Figure 5;
(4) carry out choosing of direction of measurement, measurement point position, number and measurement visual field, observation visual field area, choose the different measuring direction according to the gallium arsenide single-crystal wafer of different crystal orientations, main reference plane, secondary reference surface＜100 according to gallium arsenide single-crystal wafer 〉,＜511〉crystal orientation single-chips choose [110], [010] direction, and＜111〉crystal orientation single-chips are chosen [110], [112] direction is measured; First measurement point is chosen at the 150/10mm place apart from Waffer edge, i.e. 15mm place, and the every interval 10mm of later measurement point is one and measures the visual field that each measures visual field area 1mm
2, dislocation desity is less than 10000/cm
2, the visual field area is chosen 1mm
2, dislocation desity is greater than 10000/cm
2, the visual field area is chosen 1mm
2Can select the arsenide gallium monocrystal full wafer to choose and detect, also can only choose 1/4 disk and choose and detect, shown in Fig. 1,2,3,4;
(5) calculate, to selected point in the step (4) and visual field area, the applied optics microscopic examination is measured each and is observed the visual field number, or application image collection computation processing method measures each visual field number, dislocation desity is calculated in through type (1), (2), for＜100 〉,＜511〉crystal orientation single-chip average dislocation densities
Calculate by formula (1): for＜111 crystal orientation single-chip average dislocation density
Calculate by formula (2).
In the formula: i=1,2,3......n, the number of measurement point
N
iThe dislocation etch pit number of i measurement point
The microscopical design factor of C, C=l/s, cm
-2
S visual field area, cm
2
No center measurement point dislocation etch pit number
Example:
| Sample number into spectrum | GYM 20407 tail | The crystal orientation | <100> | The visual field area | 0.22mm 2 | Etching time | 7 minutes | ||||||||||||
| Measurement point and etch pit number | |||||||||||||||||||
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | 13 | |||||||
| < 110> | 169 | 66 | 89 | 157 | 144 | 128 | 169 | 134 | 105 | 65 | 116 | 127 | 137 | ||||||
| <0 10> | 136 | 128 | 145 | 143 | 129 | 109 | - | 135 | 101 | 112 | 88 | 132 | 145 | ||||||
| Average dislocation density is (individual/cm 2) | 5.6×10 4 | ||||||||||||||||||
By formula calculate (1), on show the 7th of data and be the center wafer point, other each point write down from left to right from wafer successively each observe the number of visual field.
2 couples of size 180mm of embodiment are directly through the detection of gallium arsenide single-crystal wafer dislocation desity
Whole implementation step is identical with 150mm diameter gallium arsenide single-crystal wafer, just the difference of choosing in the field of detection position is that the mask preparation is different, first measurement point is chosen at the D/10mm place apart from Waffer edge, be 18mm, the every interval 12mm of later measurement point is one and measures the visual field, selected directions is identical, chooses identically with 150mm diameter monocrystalline measurement point number like this, and the position of choosing is different.Other grinding-polishing-corrosion-observation-calculating is all identical.
Claims (3)
1, the defect inspection method of single crystal structure of gallium arsenide in large size is characterized in that comprising the following steps:
(1) grinds, the gallium arsenide single-crystal wafer that cuts is ground with emery, make surfacing, bright and clean, no marking, clean;
(2) polishing: mechanical buffing or chemical polishing, adopting the chemical polishing formula of liquid is sulfuric acid: hydrogen peroxide: water=3: 1: 1, be placed into room temperature after when polishing＜511〉crystal orientation monocrystalline, the polishing fluid for preparing need being stirred, again＜511〉the crystal orientation monocrystalline soaks in the polishing fluid, until＜511〉crystal orientation monocrystalline are polished, the polishing fluid temperature need not room temperature when polishing other crystal orientation monocrystalline;
(3) dislocation corrosion, potassium hydroxide is placed in the silver crucible heats, putting into sample wafer when making the potassium hydroxide fusing be heated to clear state corrodes, for＜100 〉,＜111〉crystal orientation single-chips are 5～10 minutes, for＜511〉the crystal orientation single-chip is 7～13 minutes, take out sample then, flushing with clean water is used in the cooling back, dries up;
(4) carry out choosing of direction of measurement, measurement point position and measurement visual field, first measurement point is chosen at the D/10mm place apart from Waffer edge, and the every interval 10-12mm of other measurement point is one and measures the visual field that each measures visual field area 1mm
2, wherein D is the diameter of gallium arsenide wafer.
(5) calculate, selected point in the step (4) and visual field area application image are gathered computation processing method, for＜100,＜511〉crystal orientation single-chip average dislocation densities
Calculate by formula (1); For＜111〉crystal orientation single-chip average dislocation density
Calculate by formula (2).
In the formula: i=1,2,3......n, the number of measurement point;
N
i, the dislocation etch pit number of i measurement point
C, microscopical design factor, C=I/s, cm
-2
S, visual field area, cm
2
No, center measurement point dislocation etch pit number
2, the defect inspection method of single crystal structure of gallium arsenide in large size according to claim 1 is characterized in that: dislocation desity is less than 10000/cm
2, the visual field area is chosen 1mm
2Dislocation desity is greater than 10000/cm
2, the visual field area is chosen 1mm
2
3, the defect inspection method of single crystal structure of gallium arsenide in large size according to claim 1 is characterized in that: described step (4), and can select the arsenide gallium monocrystal full wafer to choose and detect, also can only choose 1/4 disk and choose and detect.
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| CN102445373A (en) * | 2011-11-19 | 2012-05-09 | 元亮科技有限公司 | Detection method of sapphire monocrystal dislocation density |
| CN101655427B (en) * | 2009-09-04 | 2012-08-01 | 中国电子科技集团公司第四十六研究所 | Dislocation corrosion detecting method of single germanium wafer |
| CN103487453A (en) * | 2013-08-20 | 2014-01-01 | 南京信息工程大学 | Measuring method for dislocation density of heteroepitaxially grown gallium nitride |
| CN103698339A (en) * | 2013-12-29 | 2014-04-02 | 云南北方驰宏光电有限公司 | Crystal dislocation corrosion detection method |
| CN104297667A (en) * | 2014-09-19 | 2015-01-21 | 上海华虹宏力半导体制造有限公司 | Crystal lattice dislocation detecting method |
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| CN110205681A (en) * | 2019-06-03 | 2019-09-06 | 中国科学院半导体研究所 | Indium arsenide single-chip dislocation corrosion liquid and dislocation corrosion detecting method |
| CN111406130A (en) * | 2018-02-23 | 2020-07-10 | 住友电气工业株式会社 | Gallium arsenide crystal substrate |
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| CN101655427B (en) * | 2009-09-04 | 2012-08-01 | 中国电子科技集团公司第四十六研究所 | Dislocation corrosion detecting method of single germanium wafer |
| CN102445373A (en) * | 2011-11-19 | 2012-05-09 | 元亮科技有限公司 | Detection method of sapphire monocrystal dislocation density |
| CN103487453A (en) * | 2013-08-20 | 2014-01-01 | 南京信息工程大学 | Measuring method for dislocation density of heteroepitaxially grown gallium nitride |
| CN103698339B (en) * | 2013-12-29 | 2015-12-09 | 云南北方驰宏光电有限公司 | A kind of crystal dislocation corrosion detection method |
| CN103698339A (en) * | 2013-12-29 | 2014-04-02 | 云南北方驰宏光电有限公司 | Crystal dislocation corrosion detection method |
| CN104297667B (en) * | 2014-09-19 | 2017-06-06 | 上海华虹宏力半导体制造有限公司 | The method for detecting lattice dislocation |
| CN104297667A (en) * | 2014-09-19 | 2015-01-21 | 上海华虹宏力半导体制造有限公司 | Crystal lattice dislocation detecting method |
| CN104900758A (en) * | 2015-05-25 | 2015-09-09 | 连云港市产品质量监督检验中心 | Method for detecting microdefects of quasi monocrystalline silicon sheets |
| CN104900758B (en) * | 2015-05-25 | 2017-03-15 | 连云港市产品质量监督检验中心 | A kind of detection method of quasi-monocrystalline silicon microdefect |
| CN108169228A (en) * | 2017-11-28 | 2018-06-15 | 中国工程物理研究院电子工程研究所 | A kind of method of accurate discrimination single-crystal silicon carbide Types of Dislocations |
| CN111406130A (en) * | 2018-02-23 | 2020-07-10 | 住友电气工业株式会社 | Gallium arsenide crystal substrate |
| CN111406130B (en) * | 2018-02-23 | 2021-10-15 | 住友电气工业株式会社 | Gallium arsenide crystal substrate |
| US11408091B2 (en) | 2018-02-23 | 2022-08-09 | Sumitomo Electric Industries, Ltd. | Gallium arsenide crystal substrate |
| CN110018279A (en) * | 2019-04-26 | 2019-07-16 | 西安奕斯伟硅片技术有限公司 | A kind of detection method and device of Defect |
| CN110205681A (en) * | 2019-06-03 | 2019-09-06 | 中国科学院半导体研究所 | Indium arsenide single-chip dislocation corrosion liquid and dislocation corrosion detecting method |
| CN111781243A (en) * | 2020-06-16 | 2020-10-16 | 天津中环领先材料技术有限公司 | Silicon wafer micro-defect testing method |
| CN112964710A (en) * | 2021-01-22 | 2021-06-15 | 威科赛乐微电子股份有限公司 | Dislocation measuring method of gallium arsenide wafer |
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