CN104502351A - GaN-based epitaxial material dislocation defect determination method - Google Patents
GaN-based epitaxial material dislocation defect determination method Download PDFInfo
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- CN104502351A CN104502351A CN201410548619.6A CN201410548619A CN104502351A CN 104502351 A CN104502351 A CN 104502351A CN 201410548619 A CN201410548619 A CN 201410548619A CN 104502351 A CN104502351 A CN 104502351A
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Abstract
The invention discloses a GaN-based epitaxial material dislocation defect determination method. The GaN-based epitaxial material dislocation defect determination method comprises the following steps of heating a phosphoric acid solution or a mixed solution of phosphoric acid and sulfuric acid until the solution is boiling, putting a gallium nitride sample into the boiling acid for corrosion lasting for 20-30min, taking out the sample, carrying out chemical cleaning on the sample, carrying out drying, observing the sample by a fluorescence microscope, switching a light source of the fluorescence microscope into a powerful light source, setting a dark field mode, wherein the material surface observed by an eyepiece has a black color, inclined planes and bottoms of pits formed by dislocation and having different sizes reflect incident light so that light spots with different sizes are formed, calculating the number of the light spots on the sample to obtain the total numbers of different dislocations, and calculating corresponding dislocation density by dividing the corresponding total number of dislocation by the observation area at the amplification multiple. The method utilizes combination of boiling acid chemical etching and a dark field fluorescent microscope technology, and utilizes powerful light source-produced light spots with different sizes at different dislocation defect positions under the dark field condition to determine the dislocation.
Description
Technical field
The invention belongs to the observation of semiconductor material dislocation and representational field, particularly relate to the observation of dislocation defects type and the assay method of density thereof of a kind of gallium nitride (GaN) base epitaxial grown material.
Background technology
Owing to lacking the homogeneity substrate being applicable to large-scale production, nitride semiconductor light-emitting epitaxial loayer generally uses heterogeneousization substrate, as sapphire (Al
2o
3), SiC or Si etc.Due to the mismatch of grating constant and thermal expansivity, can cause there is 107 ~ 109/cm in nitride epitaxial layer
2dislocation run through whole epitaxial loayer.Because dislocation size is much smaller than visible wavelength, usually directly can observe and run through dislocation and judge that the detection method of its type only has transmission electronic microscope technology (TEM), but the limitation of this technology is expensive TEM equipment and safeguards to drop into, complicated TEM film sample technology of preparing and limited observation area scope, be unsuitable for quick detection feedback mechanism required in producing.
The method of indirect inspection dislocation desity conventional at present by x-ray diffractive technology (XRD), sample surfaces is carried out to the scanning of very zonule, by measuring the half-peak breadth of particular crystal plane (as 102 or 002 crystal face), to estimating corresponding dislocation desity than empirical data in the past.But the limitation of this technology is that surveyed area is little, estimation degree of accuracy is low, cannot detect the line dislocation with particular characteristics, as caused the tubular wire defect of leakage current.
Publication number is the gallium nitride method for measuring dislocation density that the Chinese invention patent application of CN103487453A discloses a kind of heteroepitaxial growth, utilize high-temperature fusion potassium hydroxide to etch gallium nitride epitaxial film, be aided with scanning electron microscope and atomic force microscope technology research gallium nitride epitaxial film surface dislocation type and distribution and mensuration dislocation desity.But the method has the following disadvantages: first, need epitaxial material to be heated in strong alkaline liquid high temperature (400 ~ 600 degree), operation exists potential safety hazard, and general heating arrangement is more difficult reaches temperature required; Secondly, the observation area of scanning electron microscope and atomic force microscope is less, is difficult to carry out defect distribution analysis to large scale material in industry, and scope costly, needs professional to operate.
Summary of the invention
The object of this invention is to provide a kind of assay method of GaN base epitaxial material dislocation defects, can Simple visual observation gallium nitride epitaxial film surface dislocation Type and distribution and calculate dislocation desity.
To achieve these goals, the present invention takes following technical solution:
An assay method for GaN base epitaxial material dislocation defects, comprises the following steps:
Step one, the mixed solution of phosphoric acid solution or phosphoric acid and sulfuric acid is heated to solution boiling;
Step 2, gallium nitride sample is put into boiling acid corrosion 20 ~ 30 minutes;
Step 3, taking-up sample, carry out chemical cleaning and drying by sample;
Step 4, employing fluorescence microscope sample, the light source of fluorescent microscope is transformed into intense light source, and be set to dark field mode, the material surface observed in eyepiece presents black, due to inclined-plane and the bottom reflection incident light of the pit of the different sizes of dislocation formation, forms the hot spot varied in size, the quantity of hot spot on statistics sample, obtain different dislocation sum, by corresponding dislocation sum divided by the viewing area under this enlargement factor, obtain corresponding dislocation desity.
The further technical scheme of the present invention is: in step one, the heating-up temperature of solution is 160 ~ 200 DEG C.
The further technical scheme of the present invention is: when adopting the mixed solution of phosphoric acid and sulfuric acid in step one, and the percent by volume of phosphoric acid is 50% ~ 99%, remaining as sulfuric acid.
The further technical scheme of the present invention is: in step 4 fluorescence microscope to picture in, larger is hollow dislocation, and less is helical dislocation, and minimum is edge dislocation.
The further technical scheme of the present invention is: the light source of described fluorescent microscope is the laser that Halogen lamp LED or wavelength are less than 405nm.
The further technical scheme of the present invention is: the multiple of the object lens of described fluorescent microscope is 5 times.
The further technical scheme of the present invention is: in step 4, is derived by image by fluorescence CCD, artificial or adopt the dislocation number of software statistics sample on the picture of deriving.
The further technical scheme of the present invention is: the time that in step 2, gallium nitride sample etches in the acid of boiling is 30 minutes.
From above technical scheme, the inventive method utilizes the acids chemicals etching of boiling in conjunction with details in a play not acted out on stage, but told through dialogues fluorescence microscopy, utilize the hot spot of intense light source different sizes that light presents in different dislocation defects position under dark fieid conditions, can measure dislocation, this method requires lower to dislocation etching condition, handling safety is easy to get guarantee, but also general pattern process software can be utilized to carry out Auto-counting, be convenient to comparatively large regions and area carry out detection statistics, operating personnel are required low, can Simple visual observation gallium nitride epitaxial film surface dislocation Type and distribution and calculate dislocation desity.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention, simple introduction is done below by the accompanying drawing used required in embodiment or description of the prior art, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the dislocation schematic side view of sample after embodiment of the present invention employing acid liquid corrosion;
Fig. 2 is the spot size of dislocation under microscope dark field pattern different after the embodiment of the present invention adopts acid liquid corrosion;
Fig. 3 is leakage current yield and hollow defect concentration corresponding relation figure.
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in more detail.
Embodiment
The present invention adopts the acids chemicals etch nitride gallium sample of boiling, adopt the dislocation situation of fluorescence microscopy sample, Types of Dislocations judgement and analysis can be carried out, such as: sapphire, SiC, Si, LiAlO2, LiGaO2, magnesium aluminate spinel etc. to the gallium nitride film that many various substrates prepare.
The step of the inventive method is as follows:
The mixed solution of phosphoric acid solution or phosphoric acid and sulfuric acid is placed in acid corrosion-resistant plastic containers, is heated to 160 ~ 200 DEG C, solution is seethed with excitement; When adopting the mixed solution of phosphoric acid and sulfuric acid, the percent by volume of phosphoric acid is 50% ~ 99%, and remaining as sulfuric acid, preferably, the percent by volume of phosphoric acid is 80% ~ 99%;
The acid of gallium nitride sample being put into boiling is corroded 20 ~ 30 minutes;
Take out sample, sample is carried out chemical cleaning and drying;
Adopt fluorescence microscope sample, the light source of fluorescent microscope is transformed into intense light source, as Halogen lamp LED or wavelength are less than the laser of 405nm, and be dark field mode by patten transformation, under this kind of operator scheme, the material surface observed in eyepiece presents black, and the inclined-plane of the pit of the different sizes formed by dislocation and bottom are owing to reflecting the incident light, form the hot spot varied in size, corrosion rear surface pit is larger, and hot spot is larger;
The number of dislocations (hot spot number) of statistics sample unit area, computer software can manually or be utilized to carry out dislocation counting to the image under specific enlargement factor, obtain different dislocation sum, namely obtain dislocation desity divided by the viewing area under this enlargement factor.
As depicted in figs. 1 and 2, after adopting acid liquid corrosion sample, under fluorescent microscope, usually can observe hot spot sample having three kinds of sizes, wherein, larger is hollow dislocation, and less is helical dislocation, and minimum is edge dislocation.After observing hot spot, the number of spots on statistical observation area, can calculate the dislocation number of unit area, i.e. dislocation desity.Also by fluorescence CCD, image is derived simultaneously, use PaintShop, software carries out observe and the mensuration of dislocation desity.
Below by a specific embodiment, method of the present invention is described in detail.
Step one, in the descaling bath that can heat, add industrial phosphoric acid, phosphoric acid is heated to boiling, temperature is approximately 180 ~ 200 DEG C;
Step 2, gallium nitride epitaxial slice to be corroded to be loaded in the gaily decorated basket, cover semi-open top cover, to prevent epitaxial wafer from floating in acid solution, landing is in descaling bath, and the gaily decorated basket that gallium nitride epitaxial slice is housed is put into the sour descaling bath seethed with excitement and corrode, etching time is 30 minutes;
Step 3, by the gaily decorated basket take out, to corrosion after epitaxial wafer carry out conventional chemical cleaning, use acetone, ethanol and deionized water rinsing successively 10 minutes, finally dry up with high pure nitrogen, to remove the contamination of sample surfaces;
Step 4, epitaxial wafer is placed on fluorescent microscope objective table, use high-intensity light source, and pattern is set to dark field mode, the white hot spot of different size in observation area can be seen, naked eyes are utilized to count the number of large spot, then divided by the observation area under enlargement factor, the density of this defect is drawn.Object lens multiple is lower, and observation area is larger, and the defect concentration obtained is more accurate, can arrange the object lens of minimum multiple, normally 5X.
Or light signal is switched to fluorescence ccd video camera to receive, is derived by observed image, open image processing software, adjustment contrast, and preserve photo, observe picture, what in photo, spot diameter was maximum is hollow dislocation.
The hollow defect concentration of sample is carried out contrast with the leakage current yield of corresponding extension batch products map, as shown in Figure 3, as seen from Figure 3, the hollow defect concentration of product is larger, the leakage current yield that corresponding extension batch makes chip product is lower, and whether the extension utilizing the method can monitor different batches there will be the low problem of leakage current yield.
Etching condition of the present invention is lower, and security is high; Checkout equipment is comparatively simple, equipment purchasing and maintenance cost lower, simple to operate, software can be utilized to replace personnel to count, be applicable to the monitoring in gallium nitride semiconductor manufacturing enterprise and feedback, to filter out the bad extension that can cause device performance hidden danger in time, improve product yield.
Above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit, although with reference to above-described embodiment to invention has been detailed description, those of ordinary skill in the field are to be understood that, still can modify to the specific embodiment of the present invention or equivalent replacement, and not departing from any amendment of spirit and scope of the invention or equivalent replacement, it all should be encompassed among right of the present invention.
Claims (8)
1. an assay method for GaN base epitaxial material dislocation defects, is characterized in that, comprises the following steps:
Step one, the mixed solution of phosphoric acid solution or phosphoric acid and sulfuric acid is heated to solution boiling;
Step 2, gallium nitride sample is put into boiling acid corrosion 20 ~ 30 minutes;
Step 3, taking-up sample, carry out chemical cleaning and drying by sample;
Step 4, employing fluorescence microscope sample, the light source of fluorescent microscope is transformed into intense light source, and be set to dark field mode, the material surface observed in eyepiece presents black, due to inclined-plane and the bottom reflection incident light of the pit of the different sizes of dislocation formation, forms the hot spot varied in size, the quantity of hot spot on statistics sample, obtain different dislocation sum, by corresponding dislocation sum divided by the viewing area under this enlargement factor, obtain corresponding dislocation desity.
2. the assay method of GaN base epitaxial material dislocation defects as claimed in claim 1, is characterized in that: in step one, the heating-up temperature of solution is 160 ~ 200 DEG C.
3. the assay method of GaN base epitaxial material dislocation defects as claimed in claim 1 or 2, it is characterized in that: when adopting the mixed solution of phosphoric acid and sulfuric acid in step one, the percent by volume of phosphoric acid is 50% ~ 99%, remaining as sulfuric acid.
4. the assay method of GaN base epitaxial material dislocation defects as claimed in claim 1, is characterized in that: in step 4 fluorescence microscope to picture in, larger is hollow dislocation, and less is helical dislocation, and minimum is edge dislocation.
5. the assay method of GaN base epitaxial material dislocation defects as claimed in claim 1, is characterized in that: the light source of described fluorescent microscope is the laser that Halogen lamp LED or wavelength are less than 405nm.
6. the assay method of GaN base epitaxial material dislocation defects as claimed in claim 1, is characterized in that: the multiple of the object lens of described fluorescent microscope is 5 times.
7. the assay method of GaN base epitaxial material dislocation defects as claimed in claim 1, be is characterized in that: in step 4, is derived by image by fluorescence CCD, artificial or adopt the dislocation number of software statistics sample on the picture of deriving.
8. the assay method of GaN base epitaxial material dislocation defects as claimed in claim 1, is characterized in that: the time that in step 2, gallium nitride sample etches in the acid of boiling is 30 minutes.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109738469A (en) * | 2018-12-29 | 2019-05-10 | 赛纳生物科技(北京)有限公司 | A kind of compactness detection method of FOP surface micro-pit plated film |
| CN113295616A (en) * | 2021-03-30 | 2021-08-24 | 浙江大学杭州国际科创中心 | Comprehensive test method for SiC wafer and epitaxial layer structure thereof |
| CN114486926A (en) * | 2021-12-30 | 2022-05-13 | 深圳瑞波光电子有限公司 | Semiconductor laser chip failure analysis method |
| CN114594119A (en) * | 2022-01-24 | 2022-06-07 | 中国电子产品可靠性与环境试验研究所（（工业和信息化部电子第五研究所）（中国赛宝实验室）） | Method for detecting dislocation condition of gallium nitride crystal |
| CN116577340A (en) * | 2023-05-28 | 2023-08-11 | 兰州大学 | Method for distinguishing threading screw dislocation and threading edge dislocation in silicon carbide |
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| CN109738469A (en) * | 2018-12-29 | 2019-05-10 | 赛纳生物科技(北京)有限公司 | A kind of compactness detection method of FOP surface micro-pit plated film |
| CN113295616A (en) * | 2021-03-30 | 2021-08-24 | 浙江大学杭州国际科创中心 | Comprehensive test method for SiC wafer and epitaxial layer structure thereof |
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| CN114594119B (en) * | 2022-01-24 | 2024-10-11 | 中国电子产品可靠性与环境试验研究所（（工业和信息化部电子第五研究所）（中国赛宝实验室）） | Method for detecting dislocation condition of gallium nitride crystal |
| CN116577340A (en) * | 2023-05-28 | 2023-08-11 | 兰州大学 | Method for distinguishing threading screw dislocation and threading edge dislocation in silicon carbide |
| CN116577340B (en) * | 2023-05-28 | 2024-01-05 | 兰州大学 | Method for distinguishing threading screw dislocation and threading edge dislocation in silicon carbide |
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Application publication date: 20150408 |