CN104966683A - Method of using section cutting corrosion technology to detect microdefect in silicon wafer body - Google Patents
Method of using section cutting corrosion technology to detect microdefect in silicon wafer body Download PDFInfo
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- CN104966683A CN104966683A CN201510417761.1A CN201510417761A CN104966683A CN 104966683 A CN104966683 A CN 104966683A CN 201510417761 A CN201510417761 A CN 201510417761A CN 104966683 A CN104966683 A CN 104966683A
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- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/10—Measuring as part of the manufacturing process
- H01L22/12—Measuring as part of the manufacturing process for structural parameters, e.g. thickness, line width, refractive index, temperature, warp, bond strength, defects, optical inspection, electrical measurement of structural dimensions, metallurgic measurement of diffusions
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Abstract
A method of using a section cutting corrosion technology to detect a microdefect in a silicon wafer body is suitable for carrying out detection and control of a defect in the silicon wafer body by a semiconductor silicon substrate slice manufacturing plant. Badness of the substrate slice is discovered timely and failure of a finished product device is reduced. The invention adopts a three-times-circulation wet-oxidation high-temperature thermal oxidation technology and a section cutting technology. An internal defect which can not be detected by a conventional detection method is fully decorated and grown up, and then different positions of an oxidated silicon wafer selection surface are cut into a silicon wafer strip (1) with a 1.5-2.0cm width. After preferred etching, a double faced adhesive tape is used to bond a back side of the silicon wafer strip (1) to a four fluorine cushion block (2). An optical microscope is used to observe section (3) morphology. And a continuous scanning method is used to count defect density under a microscopic state. The detection method of the invention is suitable for large scale and batch production usage of a factory.
Description
Technical field
The invention belongs to crystal defect detection technique field in semiconductor silicon material, relate generally to a kind of method adopting section to cut microdefect in corrosion technology detection silicon wafer body.
Background technology
Bulk silicon substrate sheet usually will through multiple tracks high-temperature heat treatment operations such as peroxidating, diffusion, ion implantation, extensions in device fabrication process.In heat treatment process, due to the room in silicon wafer body, interstitial atom and foreign atom motion and rearrange combination, luring that the microdefect in silicon materials lamellar body assembles nucleation into, forming the defect such as dislocation or fault and by displaying after preferential etch.The existence of defect, can cause the inefficacy of the increase of the leakage current of circuit devcie product, power consumption penalty and finished device.In order to ensure the quality of bulk silicon substrate sheet, usual manufacture of materials factory can carry out Corrosion monitoring to the grown-in defect of crystals.But the method for this kind of Corrosion monitoring cannot determine the defect change of silicon chip in device fabrication factory after multiple tracks thermal technology sequence.
At present the concrete grammar that the detection of microdefect in wafer bulk is conventional is had:
Method 1, grown-in defects etch:
Due to a large amount of point defects, fault and dislocation etc. can be produced in crystal growth process; these defects can extend in epitaxial loayer; have a strong impact on the quality of substrate slice; so substrate slice producer can adopt the method for silicon chip being carried out preferential etch again after chemical polishing usually, defect in protobiont is controlled.This kind of method can show the primary latent defect of crystal, but cannot determine that the defect of substrate slice in device producer after the thermal process that multiple tracks is indispensable shows and quality condition.
Method 2: scanning electron microscopy SEM observation:
Utilize secondary electron signal imaging to observe the configuration of surface of sample.Scanning electron microscope magnification is high, and the depth of field and visual field are all very large, carry out imaging, to determine that whether each Rotating fields is identical to the deck structure of silicon chip different depth.The drawback of this kind of method needs special sample preparation, complex operation; Only can observe the structure of different depth layer, but cannot qualitative defect type; Be limited to sample size, only can observe silicon chip local, silicon chip overall picture cannot be evaluated; ESEM input cost is higher.
Method 3: transmission electron microscope tem observation method:
Transmission electron microscope makes light source with electron beam, makes lens with electromagnetic field, by e-beam projection on very thin sample, and the atomic collision in electronics and sample and change direction, thus produce solid angle scattering, form the different image of light and shade thus.Transmission electron microscope resolution is very high, but owing to only can observe the ultra-thin section that thickness is about about 50nm, needs to configure ultramicrotome, only can be used to experimental study, cannot be applied to batch production at semicon industry.
Summary of the invention
For detecting and evaluate the problem of silicon wafer in the defect change of device fabrication factory after the multiple tracks high-temperature heat treatment process such as necessary extension, oxidation, diffusion, injection in domestic and international prior art, the present invention propose a kind of be applicable to large-scale production, can three road oxidation technologies of defect and section cutting detection method in accurate evaluation silicon substrate lamellar body.
Detection method of the present invention is based on following theoretical foundation: in silicon wafer, topmost impurity oxygen can form precipitation in high thermal process, point defect in silicon wafer, metal impurities can find new complex centre, room, electronics and various atom also can rearrange and find balance in repeatedly thermal process, at atom, molecule, in the motion process of point defect, nuclearing centre new in a large number can be produced, these nuclearing centre agglomerations, induced by high temperature wet-oxygen oxidation, can with the morphologic appearance of the raw defect of the heat of oxidation out, and different temperature, different oxidization times, different hot number of times, different impacts can be produced to the raw defect of heat.Pass through a large amount of engineer testings simultaneously, adopt three circulation wet-oxygen oxidation techniques, make the abundant decoration of defect in silicon wafer body and grow up, then surperficial diverse location place is selected to cut the silicon wafer after oxidation, differential interference microscope continuous sweep is utilized to observe its pattern, to evaluate the microdefect density of crystals, can detect the radial variations of the inner microdefect in silicon wafer diverse location place simultaneously.
For achieving the above object, the present invention take a kind of adopt section cut corrosion technology detect the step of the method for microdefect in silicon wafer body and concrete technology scheme as follows:
Step 1:
The spacing of the silicon chip of cleaning by 5mm is evenly placed on quartz boat, oxidation furnace or diffusion furnace are warming up to 800 degree with the speed of 10 ± 2 degree/point and constant, quartz boat are sent in oxidation furnace or diffusion furnace with the speed of about 200mm/min and starts to carry out high-temperature thermal oxidation; High-temperature thermal oxidation technological temperature is 1100 ~ 1150 degree, and heating rate is 5 ± 1 degree/point, and oxidization time is 100 ~ 150 minutes;
Step 2:
Pass into high purity oxygen gas and 18,000,000 pure water water vapours that flow is 3 ± 0.5L/min in oxidizing process, after oxidization time terminates, furnace temperature is slowly down to 800 degree with the speed of 3 degree/point by controlled oxidization stove or diffusion furnace;
Step 3:
Slowly pull out completing the silicon wafer after high-temperature oxydation from oxidation furnace or diffusion furnace with the speed of about 200mm/min;
Step 4:
Silicon wafer naturally cools to room temperature under being placed on more than 100 grades clean laminar flow environment;
Step 5:
According to the method described in step 1 to step 4, three high-temperature thermal oxidation process are repeated to silicon chip;
Step 6:
Lain on smooth, clean tetrafluoro flat board by silicon chip after completing high-temperature thermal oxidation process, determine the silicon wafer position needing to observe, along silicon chip diametric(al), silicon chip being cut into width with all steel slate pencil is the rectangular of 1.5 to 2.0cm;
Step 7:
Be placed in tetrafluoro flower hurdle by rectangular for the silicon chip after cutting, with the rectangular residual silica flour of pure water rinsing silicon chip, then rectangular to silicon chip in chromic acid corrosion solution cutting section corrosion totally also dried up with High Purity Nitrogen air gun by pure water rinsing after 3 ~ 4 minutes;
Step 8:
Section detects, with double faced adhesive tape, the back side rectangular for silicon chip is bonded on tetrafluoro cushion block, the rectangular section of silicon chip will exceed tetrafluoro cushion block, under 200 times, the rectangular cross-section morphology of silicon chip is observed with light microscope, and the section defect concentration under using metallomicroscope to adopt continuous sweep method counting microstate.
A kind of method adopting section to cut microdefect in corrosion technology detection silicon wafer body of the present invention, by carrying out three high-temperature thermal oxidation process to silicon chip, make microdefect in wafer bulk fully grow up and induce to manifest, then section cutting is carried out, observe the radial distribution situation of diverse location place latent defect in silicon wafer body, the thoroughly evaluating to microdefect in silicon wafer body can be realized.The present invention detects microdefect in substrate lamellar body to substrate slice factory and provides novel feasible method, provides simple and effective method for evaluating the quality condition of substrate slice in device fabrication process after multiple tracks thermal process.The oxidation furnace used in detection method of the present invention, diffusion furnace, microscope etc. are the existing equipment of factory, additionally need not drop into increase cost, and detection method of the present invention is applicable to detection when extensive and batch production.
Accompanying drawing explanation
Fig. 1 is the rectangular schematic diagram be bonded on tetrafluoro cushion block of silicon wafer in the present invention.
In figure: 1, silicon wafer is rectangular; 2, tetrafluoro cushion block; 3, section.
Embodiment
A kind of embodiment adopting section to cut the method for microdefect in corrosion technology detection silicon wafer body of the present invention is provided below in conjunction with accompanying drawing:
As shown in Figure 1, a kind of concrete steps adopting section to cut microdefect method in corrosion technology detection silicon wafer body of the present invention are:
Step 1: the silicon wafer of cleaning is evenly placed on quartz boat with the spacing of 5mm, oxidation furnace or diffusion furnace are warming up to 800 degree with the speed of 10 ± 2 degree/point and constant, then with the speed of about 200mm/min quartz boat are sent in oxidation furnace or diffusion furnace and carry out thermal oxidation process.Setting oxidation technology is as follows: target temperature is 1150 degree, and heating rate is 5 degree/point, and oxidization time is 100 minutes.
Step 2: for ensureing the effect of oxidation induced between the heat of oxidation, high purity oxygen gas and 18,000,000 pure water water vapours that flow is 3 ± 0.5L/min can be passed into.After oxidization time completes, controlled oxidization stove or diffusion furnace are spent with the speed slow cooling to 800 of 3 degree/point.
Step 3: the silicon chip after adopting the speed of 200mm/min to make oxidation slowly pulls out in stove.The silicon chip brought for reducing huge temperature difference shrinks deformation, and the speed of coming out of the stove must be slow.
Step 4: wait for about 30 minutes, treats that silicon chip naturally cools to room temperature under clean laminar flow environment.
Step 5: according to the method for step 1 ~ step 4, repeats to carry out three high temperature oxidation process to silicon wafer.
Step 6: lie in completing the silicon wafer after oxidation on smooth, clean tetrafluoro plate, determine the wafer position needing to observe, diametrically carefully cutting into width with diamond pen is the rectangular of 1.5 ~ 2.0cm.
Step 7: be placed on by the silicon wafer rectangular 1 after cutting in tetrafluoro flower hurdle (slice, thin piece is less, will note during placement), with the silica flour that a large amount of pure water rinsing cutting is residual.Then use good chromic acid corrosion solution (wright or the schimmel) corrosion of preferentially property after 3 ~ 4 minutes, clean by pure water rinsing, and dry up with High Purity Nitrogen air gun.
Step 8: carefully the back side of rectangular for silicon wafer 1 is bonded in (wafer profiles 1 outline is higher than cushion block) on tetrafluoro cushion block 2 with double faced adhesive tape, observes section 3 pattern with light microscope under 200 times, and the defect concentration under adopting continuous sweep method to count microcosmic.
Claims (1)
1. adopt section to cut a method for microdefect in corrosion technology detection silicon wafer body, it is characterized in that: in described silicon wafer body, the step of microdefect and section detection method is as follows:
Step 1:
Be placed on quartz boat by the silicon wafer of cleaning with a determining deviation, operation oxidation furnace or diffusion furnace are warming up to 800 degree with the speed of 10 ± 2 degree/point, constant; At this moment sent in oxidation furnace or diffusion furnace with the speed of about 200mm/min by quartz boat and start to carry out high-temperature thermal oxidation, high-temperature thermal oxidation technological temperature is 1150 degree, and heating rate is 5 degree/point, and oxidization time is 100 minutes;
Step 2:
In high-temperature oxidation process, pass into high purity oxygen gas and 18,000,000 pure water water vapours that flow is 3 ± 0.5L/min, after oxidization time terminates, controlled oxidization stove or diffusion furnace are spent with the speed slow cooling to 800 of 3 degree/point;
Step 3:
With the speed of 200mm/min, the silicon wafer after high-temperature oxydation is slowly pulled out from oxidation furnace or diffusion furnace, and allow silicon wafer naturally cool to room temperature under clean laminar flow environment;
Step 4:
According to step 1 to the process approach of step 3, three high-temperature thermal oxidation process are repeated to silicon wafer;
Step 5:
Silicon wafer after high-temperature thermal oxidation process is lain on clean tetrafluoro flat board, determines to observe silicon wafer surface position, adopt diamond pen diametrically silicon wafer to be cut into the silicon wafer rectangular (1) that width dimensions is 1.5 ~ 2.0cm;
Step 6:
Rectangular for silicon wafer (1) is positioned in tetrafluoro flower hurdle, with the residual silica flour on pure water rinsing silicon wafer rectangular (1), then use chromic acid corrosion solution to corrode 3 minutes the cutting section (3) of silicon wafer rectangular (1), totally also dry up with High Purity Nitrogen air gun by pure water rinsing;
Step 7: carry out section detection, with double faced adhesive tape, the back side of rectangular for silicon wafer (1) is bonded on tetrafluoro cushion block (2), the section (3) of silicon wafer rectangular (1) will exceed tetrafluoro cushion block (2), under 200 times, observe upper section (3) pattern of silicon wafer rectangular (1) with light microscope, and adopt continuous sweep method to count the defect concentration of section (3) under microstate.
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Cited By (6)
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| CN109580635A (en) * | 2018-12-03 | 2019-04-05 | 高佳太阳能股份有限公司 | A kind of diamond cut silicon wafer piece thickness ununiformity reason fast determination method |
| CN110618132A (en) * | 2019-09-26 | 2019-12-27 | 天津中环领先材料技术有限公司 | Method for detecting soft damage density of back surface of silicon wafer |
| CN110993483A (en) * | 2019-11-19 | 2020-04-10 | 江苏英锐半导体有限公司 | Oxygen content selection method of bipolar IC silicon wafer |
| CN114280072A (en) * | 2021-12-23 | 2022-04-05 | 宁夏中欣晶圆半导体科技有限公司 | Method for detecting BMD in monocrystalline silicon body |
| CN116337875A (en) * | 2023-03-31 | 2023-06-27 | 宁夏中欣晶圆半导体科技有限公司 | Method for detecting silicon wafer oxidation induced stacking fault defect |
| CN116642914A (en) * | 2023-05-29 | 2023-08-25 | 山东有研半导体材料有限公司 | Detection method for micro defects of heavily arsenic-doped low-resistivity silicon single crystal |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109580635A (en) * | 2018-12-03 | 2019-04-05 | 高佳太阳能股份有限公司 | A kind of diamond cut silicon wafer piece thickness ununiformity reason fast determination method |
| CN110618132A (en) * | 2019-09-26 | 2019-12-27 | 天津中环领先材料技术有限公司 | Method for detecting soft damage density of back surface of silicon wafer |
| CN110993483A (en) * | 2019-11-19 | 2020-04-10 | 江苏英锐半导体有限公司 | Oxygen content selection method of bipolar IC silicon wafer |
| CN114280072A (en) * | 2021-12-23 | 2022-04-05 | 宁夏中欣晶圆半导体科技有限公司 | Method for detecting BMD in monocrystalline silicon body |
| CN116337875A (en) * | 2023-03-31 | 2023-06-27 | 宁夏中欣晶圆半导体科技有限公司 | Method for detecting silicon wafer oxidation induced stacking fault defect |
| CN116642914A (en) * | 2023-05-29 | 2023-08-25 | 山东有研半导体材料有限公司 | Detection method for micro defects of heavily arsenic-doped low-resistivity silicon single crystal |
| CN116642914B (en) * | 2023-05-29 | 2024-02-13 | 山东有研半导体材料有限公司 | Detection method for micro defects of heavily arsenic-doped low-resistivity silicon single crystal |
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Address after: 471000 No. 99 Binhe North Road, Luoyang hi tech Industrial Development Zone, Henan Patentee after: Mesk Electronic Materials Co., Ltd Address before: 471000 No. 99 Binhe North Road, Luoyang hi tech Industrial Development Zone, Henan Patentee before: MCL ELECTRONIC MATERIALS Ltd. |