CN102607916A - Preparation method of silicon chip metallographic specimen - Google Patents
Preparation method of silicon chip metallographic specimen Download PDFInfo
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- CN102607916A CN102607916A CN201210064168XA CN201210064168A CN102607916A CN 102607916 A CN102607916 A CN 102607916A CN 201210064168X A CN201210064168X A CN 201210064168XA CN 201210064168 A CN201210064168 A CN 201210064168A CN 102607916 A CN102607916 A CN 102607916A
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Abstract
The invention discloses a preparation method of a silicon chip metallographic specimen. The preparation method comprises the following steps: (1) proportioning and mixing acrylic resin powder and a liquid curing agent uniformly according to instructions, adding an organic solvent with the weight of 5-25% of the total weight of the acrylic resin powder and the liquid curing agent, and mixing uniformly to prepare a cold inserted agent; (2) placing a silicon chip on the bottom of a silicon gel cold inserted mold, pouring the cold inserted agent prepared in the step (1), and curing; and (3) carrying out polishing and corrosion treatment on the cured metallographic specimen, wherein the organic solvent is ethanol, glycol or isopropanol. The preparation method of the silicon chip metallographic specimen disclosed by the invention has the advantages that the metallographic specimen of the ultra-thin and fragile silicon chip can be prepared, structure morphologies such as dislocation with clear materials are obtained, the phenomena of wrapping, crashing and the like of the ultra-thin silicon chip in specimen insertion and polishing processes are avoided, the problem that the micro scratch of the ultra-thin silicon chip is difficult to remove is solved, and the metallographic specimen of the ultra-thin silicon chip is prepared successfully.
Description
Technical field
The invention belongs to the preparing technical field of metallographic specimen; Be specifically related to semiconductor and photovoltaic production technology and research field; Relate in particular to a kind of preparation method of silicon chip metallographic specimen; Be mainly used in the metallographic specimen of preparation ultra thin silicon wafers, be applicable to the observation of microstructures such as ultra thin silicon wafers dislocation and crystal boundary.
Background technology
Solar energy-level silicon wafer thickness is generally below the 250 μ m; In the process that is used for metallographic observation, scanning electron microscopic observation specimen preparation; Because the silicon chip thin and fragile, the heating and pressurizing process when adopting heat edge quadrat method is prone to cause silicon chip broken, can't meet the demands; And cold edge method has the advantage of the heating and pressurizing of need not, and can be used for the encapsulation of silicon chip sample.Simultaneously; Silicon chip surface is prone to form dark cut when using traditional glossing to polish; Sometimes even cause the local broken of silicon chip; And polishing has had a strong impact on the observation of silicon chip surface microscopic defect after the sample of test under microscope no marking is handled the back silicon chip surface in erosion and a large amount of little cuts occurred.Therefore, the preparation of ultra thin silicon wafers metallographic specimen and glossing are difficult point and the key points that its specimen preparation and tissue show.
In cold edge method, cold edge agent mainly can be divided into two big types, acrylic resene and epoxy resin.The cold edge agent of acrylic resene has the fast advantage of setting rate; Be solidifiable in the 0.5h at ambient temperature generally; But there is the problem that differential contraction stress is big, thermal discharge is high; In sample making course, make the bigger stress of the inner generation of thin silicon sheet, in follow-up grinding and polishing process, cause sample warpage, fragmentation, polishing process can't be accomplished; It is little that the cold edge agent of epoxy resin has shrinkage factor, the advantage that stress is less, and made sample has effect preferably, but setting rate is slow, generally needs more than the 12h, and efficient is low, also can't satisfy a large amount of demands of sample preparation fast.
Summary of the invention
Technical matters to be solved by this invention provides a kind of preparation method of silicon chip metallographic specimen; Can effectively avoid the problem of ultra thin silicon wafers warpage, fragmentation in metallographic specimen preparation and grinding and polishing process, be specially adapted to the preparation of ultra thin silicon wafers (thickness＜250 μ m) metallographic specimen.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is following:
A kind of preparation method of silicon chip metallographic specimen, it comprises the steps:
(1) acrylic resin-oatmeal and LCM are pressed operation instruction proportioning mixing, add 5～25% organic solvents of both general assembly (TW)s, mixing is processed cold edge agent;
(2) silicon chip is placed on the cold edge mold bottom of silica gel, the cold edge agent that its top casting step (1) makes is solidified;
(3) to the metallographic specimen after solidifying polish, corrosion treatment;
Wherein, described organic solvent is ethanol, monoethylene glycol or isopropyl alcohol.
Wherein, described silicon wafer thickness is below the 250 μ m.
The present invention does not have specific (special) requirements to the acrylic resin-oatmeal of use and supporting LCM thereof, and commercially available metallographic all can use with acrylic resin-oatmeal and supporting reagent thereof.
In the step (2), solidification temperature is 20～30 ℃, and be 0.5～2h set time.
In the step (2), described cold embedding die is the silica gel material.
In the step (3), described polishing, corrosion treatment are that second polishing and anticaustic are handled.
In the step (3), to the metallographic specimen after solidifying polish, the corrosion treatment concrete steps are following:
(3a) on the buffing machine metallographic specimen after solidifying is tentatively being polished, polishing fluid is followed successively by the diamond suspension of particle diameter 9 μ m, 3 μ m, uses the SiO of particle diameter 0.05～0.1 μ m then
2Suspending liquid polishes;
(3b) sample after step (3a) polishing is cleaned up and dries up with pure water;
(3c) use the specimen surface after acid corrosion liquid or caustic corrosion liquid are handled step (3b) to carry out shallow corrosion, the time is 2～5min;
(3d) sample after step (3c) processing is carried out second polishing, polishing cloth is selected soft short flannel cloth for use, and it is the SiO of 0.05～0.1 μ m that polishing fluid is selected particle diameter
2Suspending liquid, the time is 1～2min;
(3e) specimen surface after with pure water step (3d) being handled cleans up, and removes all kinds of organic or the soda acid thing is residual;
(3f) sample after with preferential etch liquid step (3e) being handled carries out preferential etch, and the time is 3～15min;
(3g) use the sample after pure water is handled step (3f) to clean up and dry up.
The acid corrosion liquid that uses in the step (3b) is the nitric acid of 68%mol/L, hydrofluorite and the H of 40%mol/L
23: 1: 5 by volume～3: 1: 20 potpourri of O; Described caustic corrosion liquid is NaOH and H
2O was by weight 1: 5～1: 20 potpourri.The preferential etch liquid that uses in the step (3f) is hydrofluorite and the 0.15M K of 49%mol/L
2Cr
2O
72: 1 by volume potpourri of the WS.
Beneficial effect:
The present invention realizes quick sample preparation through organic solvents such as a certain proportion of ethanol of adding in the cold edge agent of acrylic resene, and not warpage, the nothing fragmentation in the grinding and polishing process of the thin silicon sheet sample of preparation, and performance is stablized.The cold edge agent of sample preparation efficiency ratio epoxy resin of this method is fast more than 6～10 times, has shortened the sample preparation time of ultra thin silicon wafers metallographic specimen greatly, has improved stability and the reliability of sample in the grinding and polishing process; Through in polishing process, adopting etchant to show the treatment process of the little cut of silicon chip surface, finally obtained the high-quality clear picture of silicon chip metallographic microstructure.
Description of drawings
Fig. 1 is prepared sample outward appearance picture.
Fig. 2 is the optical microscope picture (50x) of prepared sample metallographic.
Fig. 3 is the optical microscope picture (200x) of prepared sample metallographic.
Embodiment
According to following embodiment, can understand the present invention better.Yet, those skilled in the art will readily understand that the described content of embodiment only is used to explain the present invention, and the present invention that should also can not limit in claims to be described in detail.
Employed acrylic resin-oatmeal of following examples and LCM are available from Zhong Ze Instr Ltd. in Suzhou, model C M1.
Embodiment 1:
Silicon chip is ultra-thin polysilicon chip, and silicon wafer thickness is 180 μ m, and the preparation of its metallographic specimen and the step display of microstructure are:
1) inlaying of sample: acrylic resin-oatmeal and LCM are mixed by operation instruction proportioning (weight ratio 1: 1), and slow stir about 1min, in the solution that has mixed, add the ethanol of 10% (w/w) and be stirred to evenly, process cold edge agent;
The silicon chip that 2) will be of a size of 15*20mm is placed on the cold edge mold bottom of silica gel that internal diameter is 40mm, and the cold edge agent of the above-mentioned prescription of casting, at 25 ℃ of following heat preservation solidification 1h.
3) on buffing machine, metallographic specimen is tentatively polished, polishing fluid is followed successively by the diamond suspension of particle diameter 9 μ m, 3 μ m, and the time is respectively 4min, and polishing process uses single-point to load, and pressure is 15～20N; Adopting particle diameter then is the SiO of 0.05 μ m
2Suspending liquid carries out finishing polish, and the time is 3～5min, and polishing process uses single-point to load, and pressure is 20～25N.
4) use pure water that sample is cleaned up and dries up.
5) use acid corrosion liquid (nitric acid of 68%mol/L, the hydrofluorite of 40%mol/L and H
2O 3: 1: 10 by volume) sample is carried out shallow corrosion, the time is 3min.
6) sample is carried out second polishing, polishing cloth is selecting soft short flannel cloth, and it is the SiO of 0.05 μ m that polishing fluid is selected particle diameter
2Suspending liquid, the time is 1min.
7) it is clean with pure water silicon chip surface to be carried out clean, removes all kinds of organic or the soda acid thing is residual.
8) use preferential etch liquid (hydrofluorite of 49%mol/L and 0.15M K
2Cr
2O
72: 1 by volume potpourri of the WS) sample is carried out preferential etch, the time is 7min.
9) use pure water that sample is cleaned up and dries up.
10) use microscopic examination silicon chip metallographic specimen surface texture, the result sees Fig. 2 and Fig. 3.
Embodiment 2:
With the preparation method of embodiment 1, different is, in the step 1), in the solution that has mixed, adds the ethanol of 5% (w/w) and is stirred to evenly, processes cold edge agent.
Embodiment 3:
With the preparation method of embodiment 1, different is, in the step 1), in the solution that has mixed, adds the ethanol of 25% (w/w) and is stirred to evenly, processes cold edge agent.
Embodiment 4:
With the preparation method of embodiment 1, different is that in the step 1), the spent glycol instead of ethanol is processed cold edge agent.
Embodiment 5:
With the preparation method of embodiment 1, different is in the step 1), to process cold edge agent with the isopropyl alcohol instead of ethanol.
Embodiment 6:
With the preparation method of embodiment 1, different is step 2) in, at 20 ℃ of following heat preservation solidification 2h.
Embodiment 7:
With the preparation method of embodiment 1, different is step 2) in, at 30 ℃ of following heat preservation solidification 0.5h.
Embodiment 8:
With the preparation method of embodiment 1, different is that in the step 3), adopting particle diameter is the SiO of 0.1 μ m
2Suspending liquid carries out finishing polish.
Embodiment 9:
With the preparation method of embodiment 1, different is in the step 5), to use acid corrosion liquid (nitric acid of 68%mol/L, the hydrofluorite of 40%mol/L and H
2O 3: 1: 5 by volume) sample is carried out shallow corrosion, the time is 3min.
Embodiment 10:
With the preparation method of embodiment 1, different is in the step 5), to use acid corrosion liquid (nitric acid of 68%mol/L, the hydrofluorite of 40%mol/L and H
2O 3: 1: 20 by volume) sample is carried out shallow corrosion, the time is 2min.
Embodiment 11:
With the preparation method of embodiment 1, different is in the step 5), to use caustic corrosion liquid (NaOH and H
2O was by weight 1: 5) sample is carried out shallow corrosion, the time is 3min.
Embodiment 12:
With the preparation method of embodiment 1, different is in the step 5), to use caustic corrosion liquid (NaOH and H
2O was by weight 1: 20) sample is carried out shallow corrosion, the time is 5min.
Embodiment 13:
With the preparation method of embodiment 1, different is that in the step 6), it is the SiO of 0.1 μ m that polishing fluid is selected particle diameter
2Suspending liquid, the time is 2min.
Embodiment 14:
With the preparation method of embodiment 1, different is that in the step 8), the preferential etch time is 3min.
Embodiment 15:
With the preparation method of embodiment 1, different is that in the step 8), the preferential etch time is 15min.
Comparative Examples 1:
With the preparation method of embodiment 1, different is, does not carry out second polishing, does not promptly carry out step 6).
Comparative Examples 2:
With the preparation method of embodiment 1, different is, in the step 1), does not add organic solvents such as ethanol, and be 0.5 hour set time.
Comparative Examples 3:
With the preparation method of embodiment 1, different is, in the step 1), adds the ethanol of 30% (w/w), and be 5h set time.
The testing result of embodiment 1～15, Comparative Examples 1～3 is seen table 1.
Table 1
Optical microscope picture through Fig. 2 and Fig. 3 silicon chip metallographic can clear observation print the distribution details of defective such as crystal boundary, dislocation, explain that this method is practicable.
Claims (7)
1. the preparation method of a silicon chip metallographic specimen is characterized in that, it comprises the steps:
(1) acrylic resin-oatmeal and LCM are pressed operation instruction proportioning mixing, add 5～25% organic solvents of both general assembly (TW)s, mixing is processed cold edge agent;
(2) silicon chip is placed on the cold edge mold bottom of silica gel, the cold edge agent that its top casting step (1) makes is solidified;
(3) to the metallographic specimen after solidifying polish, corrosion treatment;
Wherein, described organic solvent is ethanol, monoethylene glycol or isopropyl alcohol.
2. the preparation method of silicon chip metallographic specimen according to claim 1 is characterized in that, described silicon wafer thickness is below the 250 μ m.
3. the preparation method of silicon chip metallographic specimen according to claim 1 is characterized in that, in the step (2), solidification temperature is 20～30 ℃, and be 0.5～2h set time.
4. the preparation method of silicon chip metallographic specimen according to claim 1 is characterized in that, in the step (3), described polishing, corrosion treatment are that second polishing and anticaustic are handled.
5. the preparation method of silicon chip metallographic specimen according to claim 4 is characterized in that, in the step (3), to the metallographic specimen after solidifying polish, the corrosion treatment concrete steps are following:
(3a) on the buffing machine metallographic specimen after solidifying is tentatively being polished, polishing fluid is followed successively by the diamond suspension of particle diameter 9 μ m, 3 μ m, uses the SiO of particle diameter 0.05～0.1 μ m then
2Suspending liquid polishes;
(3b) sample after step (3a) polishing is cleaned up and dries up with pure water;
(3c) use the specimen surface after acid corrosion liquid or caustic corrosion liquid are handled step (3b) to carry out shallow corrosion, the time is 2～5min;
(3d) sample after step (3c) processing is carried out second polishing, polishing cloth is selected soft short flannel cloth for use, and it is the SiO of 0.05～0.1 μ m that polishing fluid is selected particle diameter
2Suspending liquid, the time is 1～2min;
(3e) specimen surface after with pure water step (3d) being handled cleans up;
(3f) sample after with preferential etch liquid step (3e) being handled carries out preferential etch, and the time is 3～15min;
(3g) use the sample after pure water is handled step (3f) to clean up and dry up.
6. the preparation method of silicon chip metallographic specimen according to claim 5 is characterized in that, the acid corrosion liquid that uses in the step (3b) is the nitric acid of 68%mol/L, hydrofluorite and the H of 40%mol/L
23: 1: 5 by volume～3: 1: 20 potpourri of O; Described caustic corrosion liquid is NaOH and H
2O was by weight 1: 5～1: 20 potpourri.
7. the preparation method of silicon chip metallographic specimen according to claim 5 is characterized in that, the preferential etch liquid that uses in the step (3f) is hydrofluorite and the 0.15M K of 49%mol/L
2Cr
2O
72: 1 by volume potpourri of the WS.
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| CN102944457A (en) * | 2012-11-15 | 2013-02-27 | 苏州华碧微科检测技术有限公司 | Paint physical evidence separation technology |
| CN103236406A (en) * | 2013-04-15 | 2013-08-07 | 阿特斯(中国)投资有限公司 | Method for detecting polycrystalline silicon wafer dislocation density |
| CN103900880A (en) * | 2014-03-28 | 2014-07-02 | 中国科学院上海技术物理研究所 | Sample preparation method for observing invert-welding interconnection situation |
| CN104458517A (en) * | 2014-12-12 | 2015-03-25 | 株洲硬质合金集团有限公司 | Method for measuring radius-thickness ratio of flaky metal powder |
| CN104535393A (en) * | 2015-01-16 | 2015-04-22 | 山东泰山钢铁集团有限公司 | Method for manufacturing metallographic specimen by using denture base resin |
| 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 |
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| CN108760451A (en) * | 2018-05-25 | 2018-11-06 | 河南科技大学 | The preparation method of magnesium alloy metallographic specimen after a kind of creep |
| CN108896339A (en) * | 2018-04-04 | 2018-11-27 | 江苏科泰检测技术服务有限公司 | The preparation method of metallographic specimen |
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| CN103236406A (en) * | 2013-04-15 | 2013-08-07 | 阿特斯(中国)投资有限公司 | Method for detecting polycrystalline silicon wafer dislocation density |
| CN103236406B (en) * | 2013-04-15 | 2016-01-20 | 阿特斯(中国)投资有限公司 | A kind of method detecting polycrystalline silicon wafer dislocation density |
| CN103900880A (en) * | 2014-03-28 | 2014-07-02 | 中国科学院上海技术物理研究所 | Sample preparation method for observing invert-welding interconnection situation |
| CN104458517B (en) * | 2014-12-12 | 2017-06-20 | 株洲硬质合金集团有限公司 | The method for measuring flake metal powder radius-thickness ratio |
| CN104458517A (en) * | 2014-12-12 | 2015-03-25 | 株洲硬质合金集团有限公司 | Method for measuring radius-thickness ratio of flaky metal powder |
| CN104535393A (en) * | 2015-01-16 | 2015-04-22 | 山东泰山钢铁集团有限公司 | Method for manufacturing metallographic specimen by using denture base resin |
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| CN107462451B (en) * | 2017-08-25 | 2024-01-19 | 中国科学院金属研究所 | Stress corrosion tensile sample simulating neutron irradiation by ion irradiation and preparation method thereof |
| CN108896339A (en) * | 2018-04-04 | 2018-11-27 | 江苏科泰检测技术服务有限公司 | The preparation method of metallographic specimen |
| CN108760451A (en) * | 2018-05-25 | 2018-11-06 | 河南科技大学 | The preparation method of magnesium alloy metallographic specimen after a kind of creep |
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| CN115728194A (en) * | 2022-11-21 | 2023-03-03 | 山东大学 | Method for detecting crystal grain morphology of copper foil section |
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Application publication date: 20120725 |