CN110277307B - Process method for preparing single-side high-brightness sour bean curd slices - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 41
- 230000008569 process Effects 0.000 title claims abstract description 28
- 235000013527 bean curd Nutrition 0.000 title claims description 6
- 239000002253 acid Substances 0.000 claims abstract description 90
- 238000000227 grinding Methods 0.000 claims abstract description 78
- 230000007797 corrosion Effects 0.000 claims abstract description 71
- 238000005260 corrosion Methods 0.000 claims abstract description 71
- 238000010008 shearing Methods 0.000 claims abstract description 25
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 37
- 229910052710 silicon Inorganic materials 0.000 claims description 37
- 239000010703 silicon Substances 0.000 claims description 37
- 238000004519 manufacturing process Methods 0.000 claims description 17
- 238000012545 processing Methods 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 5
- 125000000896 monocarboxylic acid group Chemical group 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 2
- 238000005530 etching Methods 0.000 abstract description 18
- 238000005498 polishing Methods 0.000 abstract description 11
- 238000002310 reflectometry Methods 0.000 abstract description 10
- 235000012431 wafers Nutrition 0.000 description 38
- 238000012360 testing method Methods 0.000 description 11
- 239000010410 layer Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012935 Averaging Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000004857 zone melting Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02008—Multistep processes
- H01L21/0201—Specific process step
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02008—Multistep processes
- H01L21/0201—Specific process step
- H01L21/02013—Grinding, lapping
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02008—Multistep processes
- H01L21/0201—Specific process step
- H01L21/02019—Chemical etching
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02008—Multistep processes
- H01L21/0201—Specific process step
- H01L21/02024—Mirror polishing
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/06—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions
Abstract
The invention provides a process method for preparing single-side high-brightness acid etching slices, which comprises the following steps: (1) single-side shearing grinding: shearing and grinding one surface of the double-sided grinding sheet by using a grinding wheel, wherein the grinding removal amount is 10-20 mu m, and obtaining a single-sided grinding sheet; (2) acid corrosion: and (3) performing acid corrosion on the single-side grinding sheet obtained in the step (1) by using an acid corrosion solution to obtain a single-side high-brightness acid corrosion sheet. Compared with the traditional process route, the single-side shearing and grinding process is added, the single-side shearing and grinding process realizes the difference of the brightness of the front side and the back side of the acid corrosion sheet, the acid corrosion sheet with the single-side glossiness of more than 360Gs, the reflectivity of more than 98 percent and the smaller roughness is prepared after acid corrosion, the use requirement is ensured, the polishing sheet is replaced, and the cost is saved.
Description
Technical Field
The invention belongs to the technical field of processing of semiconductor material silicon single crystal and silicon wafer and other production wafers, and particularly relates to a process method for preparing a silicon single crystal single-side high-brightness corrosion wafer.
Background
Currently, silicon polishing sheets are mainly used in high-end applications of silicon-based semiconductor materials, and the preparation of the polishing sheets mainly comprises the following steps: single crystal bar, cut, round, slice, chamfer, grind, corrode, polish and clean, package, etc. The polished surface of the silicon wafer has high flatness and cleanness, and the crystal lattice is complete, so that the silicon wafer can be applied to various high and new technology industries, and the requirements of different types of semiconductor materials and devices are met. However, the polishing process has higher process requirements on the precision of equipment, the processing environment, polishing solution, polishing cloth, a chemical purity packaging box, a packaging bag and the like, and has the characteristics of high manufacturing cost and long production period, and the polishing processing cost is about 6 to 10 times of the chemical corrosion cost generally.
The corrosion plate, an intermediate product of the grinding plate and the polishing plate, is more and more widely applied due to the characteristics of better performance than the grinding plate, lower cost than the polishing plate, short processing industry chain and the like. In the fields of thyristors, silicon controlled rectifiers and the like, in order to realize automatic production or reduce energy consumption during photoetching focusing, special requirements are required on the surface brightness (reflectivity) and roughness (note: roughness refers to roughness Ra) of the silicon wafer, but the requirements on other parameters of the surface of the silicon wafer are not high, the cost is high if a polished wafer is used, and the use requirements are difficult to meet when a common silicon wafer is used.
With the progress of silicon single wafer processing technology, a few companies in the industry can realize stable mass production of acid etching wafers with the surface gloss of more than 320 GS. However, the silicon single crystal etched wafer used in the field of thyristors can meet the automatic production requirements only when the glossiness reaches more than 360GS (reflectivity 98%), and the surface glossiness which stably reaches more than 360GS (reflectivity more than 98%) by means of the traditional grinding and etching process is still difficult, and the traditional process method can hardly realize stable mass production. In addition, in the field of thyristors, only strict requirements are generally required on the front surface (working surface) of a silicon wafer, and no special requirements are generally required on the back surface of the silicon wafer, but the traditional acid etching processing mode is mostly double-sided etching.
Therefore, in view of production cost, processing process flow and the like, the development of the corrosion piece with the single-side glossiness of more than 360Gs (the reflectivity is more than 98%) becomes a key problem of applying the corrosion piece to the field of automatic production of thyristors instead of a polishing piece.
Disclosure of Invention
In view of the above, the present invention aims to provide a process for preparing a single-sided high-brightness sour rot sheet, and provides a novel process route: compared with the traditional process route, the process route is added with the process of single-side shearing and grinding, the single-side shearing and grinding realizes the different brightness of the front side and the back side of the acid corrosion sheet, the acid corrosion sheet with single-side glossiness more than 360Gs, reflectivity more than 98 percent and smaller roughness is prepared after acid corrosion, the use requirement is ensured, the polishing sheet is replaced, and the cost is saved.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a process method for preparing single-side high-brightness sour bean curd slices comprises the following steps:
(1) single-side shearing grinding: shearing and grinding one surface of the double-sided grinding sheet by using a grinding wheel, wherein the grinding removal amount is 10-20 mu m, and obtaining a single-sided grinding sheet;
(2) acid corrosion: and (3) performing acid corrosion on the single-side grinding sheet obtained in the step (1) by using an acid corrosion solution to obtain a single-side high-brightness acid corrosion sheet.
Specifically, the shearing grinding refers to the rotation of a grinding wheel, a workbench for fixedly placing a grinding sheet drives the grinding sheet to rotate, and the rotation directions of the grinding wheel and the workbench are opposite to each other for grinding. After one surface of the grinding sheet is subjected to single-side mechanical thinning by adding single-side shearing grinding, the surface state of the grinding sheet is changed, the product appearance is originally silicon gray, the surface glossiness is less than 10Gs, and the roughness is between 0.25 and 0.35 mu m. After the process of single-side shearing and grinding, one surface of the grinding sheet becomes bright, the glossiness can reach 370Gs, and the roughness is 0.05-0.1 μm. After the single-side shearing and grinding is finished, acid corrosion is carried out, and the acid corrosion tablets with different surface states of the front side and the back side can be prepared by the method. By adjusting the technological parameters of single-side shearing and grinding and the technological parameters of acid corrosion, the high-reflectivity acid corrosion sheet with single-side glossiness of 360Gs and roughness of less than 0.1 mu m can be stably prepared, and the trace of single-side shearing and grinding can be removed and is basically invisible under a fluorescent lamp.
Further, the mesh number of the grinding wheel in the step (1) is 2000# -8000#, the rotation speed of the grinding sheet is 150-.
Further, the grinding removal amount in the step (1) is 13-17 μm.
Further, the acid etching solution in the step (2) is a mixed acid solution, and the mixed acid solution is composed of an HF solution and HNO3Solution, CH3COOH solution with concentration of 40-50 wt%, HNO3The concentration of the solution is 65-70 wt%, CH3The concentration of COOH solution is 95-99.5 wt%, HF solution and HNO3Solution, CH3The volume ratio of the COOH solution is (1-1.2): (3.6-4): (1.8-2).
Further, the service life of the acid etching solution in the step (2) is 5 ten thousand single-sided grinding sheets processed at the maximum.
Further, the temperature of the acid corrosion in the step (2) is 28-32 ℃, the time is 60-80s, and the removal amount of the acid corrosion is 40-60 mu m per double surfaces.
Furthermore, the glossiness of the acid corrosion piece obtained in the step (2) is more than 360Gs, and the roughness is 0.02-0.1 μm.
Further, the silicon single crystal is sliced and ground in sequence before the step (1).
By adopting the technical scheme, the silicon single crystal is cut and then ground to obtain the grinding sheet. And then, carrying out single-side shearing grinding on the silicon wafer, cleaning after the single-side shearing grinding, and then carrying out acid corrosion, wherein the acid corrosion pieces with different front and back surface states can be prepared by the method.
Furthermore, after each step of processing, cleaning and drying procedures are added.
The main action principle of the invention is as follows:
the method has the advantages that the better surface glossiness of the acid corrosion wafer is obtained, in addition to higher requirements on corrosion process parameters, the surface state parameters of the silicon wafer before acid corrosion, such as surface roughness, a damaged layer, glossiness and the like, have direct influence on the surface state of the silicon wafer after acid corrosion, and therefore how to obtain the silicon wafer surface with better surface roughness, a damaged layer and glossiness than a grinding wafer is the key for stably producing products with the surface glossiness of more than 360Gs (the reflectivity is more than 98%).
In the process of grinding the silicon wafer, grinding sand grains vertically act on the surface of the silicon wafer by means of the pressure of a grinding disc, and the surface damage layer of a grinding disc is 10-15 mu m per single surface and is equivalent to the grain size of the grinding sand grains; the surface layer of the grinding sheet becomes a broken crystalline layer under the vertical action, the surface glossiness is less than 10Gs, the surface roughness is between 0.25 and 0.4 mu m, and the damaged layer and the roughness are both high.
The single-side shearing grinding process is to grind the surface of a silicon wafer by using a 2000# grinding wheel rotating at a high speed, and the force acting on the surface of the grinding sheet is a transverse shearing force. After one surface of the grinding sheet is sheared and ground by 13-17 microns, a surface damage layer formed in the silicon wafer grinding process is removed, the surface of the silicon wafer becomes bright, the glossiness reaches 370Gs, the roughness is in the range of 0.02-0.1 micron, and the surface damage layer of the silicon wafer after shearing and grinding is 1-2 microns per single surface; the surface parameters of the silicon wafer after shearing and grinding are obviously superior to those of the grinding sheet, and the production of products with the surface glossiness of more than 360Gs (the reflectivity is more than 98%) is facilitated.
Compared with the prior art, the process method for preparing the single-side high-brightness acid corrosion slices has the following advantages:
1. according to the invention, the single-side high-brightness acid corrosion piece is prepared by single-side shearing grinding and acid corrosion, the brightness difference of the front side and the back side of the acid corrosion piece is realized, the process is simple, the steps of polishing and subsequent cleaning are omitted, the quality surplus of the double-side high brightness is avoided, the cost and the working hour are saved, the product processing performance is ensured, and the stable mass production can be realized.
2. The acid corrosion sheet obtained by the invention achieves a high-brightness mirror surface state, the glossiness is greater than 360Gs (the reflectivity is greater than 98 percent), the roughness is 0.02-0.1 mu m, and the glossiness and the roughness index are superior to those of the traditional high-brightness acid corrosion sheet.
3. The invention adopts single-side shearing grinding, reduces the thickness of the damaged layer on the surface of the silicon wafer, and the acid corrosion removal amount is 40-60 mu m per double side, while the acid corrosion removal amount of the traditional high-brightness product is 90 mu m per double side.
Drawings
FIG. 1 is a graph showing the relationship between the glossiness of an acid corrosion tablet and the service life of an acid corrosion solution;
FIG. 2 is a graph showing the relationship between the roughness of the acid corrosion wafer and the lifetime of the acid corrosion solution.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional chemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to examples.
Examples
Preparation of the process:
1. preparation of an experimental piece: 6 cun zone-melting double-sided lapping plate, diameter 150 +/-0.2 mm, thickness: 550. + -.5 μm, resistivity: 60-80 Ω · cm, number: 300 pieces, 300 double-sided lapping pieces were divided into 5 groups of 60 pieces each.
2. Testing equipment: a gloss meter, a dial gauge, a fluorescent lamp, a microscope;
3. main processing equipment and frock: a grinding machine, a 2000# grinding wheel, an acid etching machine and a cleaning machine;
4. acid corrosion solution: hydrofluoric acid solution: nitric acid solution: acetic acid solution ═ 1: 4: 1.8 (volume ratio); wherein the HF content in the hydrofluoric acid solution is 49 wt%, and the HNO content in the nitric acid solution is370 wt% of CH in acetic acid solution3The COOH content was 99.5% wt.
5. Acid corrosion temperature: 30 +/-2 ℃;
the process method for preparing the single-side high-brightness sour bean curd sheet comprises the following steps:
1) single-side shearing grinding, wherein the grinding removal amount is 13-17 mu m, the rotating speed of a grinding sheet is 150rpm, and the rotating speed of a grinding wheel is 1800 rpm;
2) and respectively carrying out acid corrosion on five groups of silicon wafers under the service life conditions of 5 acid corrosion solutions, wherein the acid corrosion removal amount is 40 mu m per double surface, and the time is 60s, so as to prepare the acid corrosion wafer.
The service lives of the five acid corrosive liquids are respectively as follows: the number of processed silicon wafers is less than 1000, and is marked as acid 1; the number of processed silicon wafers is 10000 +/-500, and is marked as acid 2; the number of processed silicon wafers is 30000 +/-500, and is marked as acid 3; the number of processed silicon wafers is 50000 +/-500, and is marked as acid 4; the number of processed silicon wafers is 70000 +/-500 wafers, and is marked as acid 5.
3) And (3) carrying out acid etching on each component for 2 times, etching 30 sheets each time, and respectively selecting the 1 st acid etching sheet, the 15 th acid etching sheet and the 30 th acid etching sheet to carry out the test of glossiness and roughness. The data of 6 acid corrosion slices to be tested in each group are recorded as 1#, 2#, 3#, 4#, 5#, 6 #.
Test examples
And (3) testing the glossiness: testing the glossiness of the high-brightness side of the acid corrosion sheet by using an MN-60 glossiness instrument, wherein the test points are a central point and 4 points 10mm away from the edge respectively, and then taking an average value of 5 points;
and (3) roughness testing: testing the roughness of the high-brightness side of the acid corrosion sheet by using a VK-9700 microscope under a condition of 20 times, wherein the test points are respectively a central point, 4 points are 10mm away from the edge, and the average value of 5 points is taken;
and (3) testing results:
the gloss data of the acid corrosion tablets prepared by five groups of double-sided grinding tablets under 5 acid corrosion process conditions are shown in table 1.
TABLE 1 data table of glossiness of acid etching sheet and life of acid etching solution
The gloss data of the acid corrosion tablets prepared by five groups of double-sided grinding tablets under 5 acid corrosion process conditions are shown in table 1.
TABLE 2 data table of roughness of acid corrosion wafer and service life of acid corrosion solution
And averaging the glossiness and roughness data of the 6 acid corrosion pieces in each group, wherein the relationship between the glossiness and the service life of the acid corrosion liquid is shown in figure 1, and the relationship between the roughness and the service life of the acid corrosion liquid is shown in figure 2. As can be seen from FIGS. 1 and 2, the gloss gradually decreased from 369.83Gs to 352.33Gs as the lifetime of the acid etching solution increased, and the roughness increased from 0.030 μm to 0.069 μm, that is, the quality of the acid etching sheet gradually decreased as the lifetime of the acid etching solution became longer.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. A process method for preparing single-sided high-brightness sour bean curd slices is characterized by comprising the following steps: the method comprises the following steps:
(1) single-side shearing grinding: shearing and grinding one surface of the double-sided grinding sheet by using a grinding wheel to obtain a single-sided grinding sheet;
(2) acid corrosion: performing acid corrosion on the single-side grinding sheet obtained in the step (1) by using an acid corrosion solution to obtain a single-side high-brightness acid corrosion sheet;
the grinding removal amount in the step (1) is 13-17 mu m;
in the step (1), the mesh number of the grinding wheel is 2000# -8000#, the rotation speed of the grinding sheet is 150-;
the temperature of the acid corrosion in the step (2) is 28-32 ℃, the time is 60-80s, and the acid corrosion removal amount is 40-60 mu m per double surface.
2. The process for preparing a single-sided high brightness sour flakes according to claim 1, wherein: the acid corrosion solution in the step (2) is a mixed acid solution, and the mixed acid solution is composed of an HF solution and HNO3Solution, CH3COOH solution with concentration of 40-50 wt%, HNO3The concentration of the solution is 65-70 wt%, CH3The concentration of COOH solution is 95-99.5 wt%, HF solution and HNO3Solution, CH3The volume ratio of the COOH solution is (1-1.2): (3.6-4): (1.8-2).
3. The process for preparing a single-sided high brightness sour flakes according to claim 1, wherein: the service life of the acid corrosion solution in the step (2) is 5 ten thousand of single-sided grinding sheets processed at the maximum.
4. The process for preparing a single-sided high brightness sour flakes according to claim 1, wherein: the glossiness of the acid corrosion piece obtained in the step (2) reaches more than 360Gs, and the roughness is 0.02-0.1 μm.
5. The process for preparing a single-sided high brightness sour flakes according to claim 1, wherein: and (2) sequentially carrying out slicing and grinding on the silicon single crystal before the step (1).
6. The process for preparing a single-sided high brightness sour bean curd sheet according to any one of claims 1 to 5, wherein: after each step of processing, cleaning and drying procedures are added.
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| CN102528597B (en) * | 2010-12-08 | 2015-06-24 | 有研新材料股份有限公司 | Manufacturing process of large-diameter silicon wafer |
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| CN101656193A (en) * | 2008-08-21 | 2010-02-24 | 北京有色金属研究总院 | Technique for processing silicon chip |
| CN102517584A (en) * | 2011-12-15 | 2012-06-27 | 天津中环领先材料技术有限公司 | Processing method for high reflectivity acid corrosion chip |
| CN103014877A (en) * | 2012-12-03 | 2013-04-03 | 天津中环领先材料技术有限公司 | Processing method of monocrystalline silicon wafer etched sheet with different glossiness at two sides |
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