CN113611593A - Method for controlling warping morphology of ultrathin germanium sheet - Google Patents
Method for controlling warping morphology of ultrathin germanium sheet Download PDFInfo
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- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 title claims abstract description 164
- 229910052732 germanium Inorganic materials 0.000 title claims abstract description 163
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000000227 grinding Methods 0.000 claims abstract description 112
- 230000007797 corrosion Effects 0.000 claims abstract description 47
- 238000005260 corrosion Methods 0.000 claims abstract description 47
- 239000002253 acid Substances 0.000 claims abstract description 28
- 238000005520 cutting process Methods 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 239000002585 base Substances 0.000 claims abstract description 4
- 239000012530 fluid Substances 0.000 claims description 24
- 238000005530 etching Methods 0.000 claims description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- 239000012752 auxiliary agent Substances 0.000 claims description 8
- 230000005587 bubbling Effects 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000012634 fragment Substances 0.000 abstract description 2
- 238000003754 machining Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000587240 Cynanchum Species 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- JGJLWPGRMCADHB-UHFFFAOYSA-N hypobromite Inorganic materials Br[O-] JGJLWPGRMCADHB-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000013585 weight reducing agent Substances 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
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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
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- H—ELECTRICITY
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- 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
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- 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
- H01L21/02035—Shaping
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- H01L31/1804—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof comprising only elements of Group IV of the Periodic Table
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Abstract
The invention provides a control method of the warpage appearance of an ultrathin germanium sheet, which comprises the following steps of firstly, mechanically grinding a germanium cutting sheet, and preliminarily controlling the warpage direction of the germanium sheet while removing cutting damage through germanium sheet grinding processing; secondly, performing acid corrosion on the germanium grinding sheet by using an acid corrosion machine, removing grinding damage of the germanium sheet in an acid corrosion process, and optimizing the warping appearance of the germanium sheet; thirdly, single-side removal is carried out on the back surface of the germanium sheet by a grinding machine, and the warping appearance of the germanium sheet is further controlled by the single-side grinding with small removal amount; and fourthly, carrying out weak base corrosion on the germanium grinding sheet by adopting an alkaline corrosion solution, and finally removing stress through weak corrosion of the germanium sheet alkali liquor to improve the surface quality and the mechanical strength of the germanium sheet. The method realizes the control of the warping appearance in the thinning processing process of the ultrathin germanium sheet, has high processing efficiency and can well control the warping appearance of the germanium sheet. The ultrathin germanium sheet prepared by the method has low fragment rate in the subsequent epitaxial process.
Description
Technical Field
The invention belongs to the technical field of ultrathin germanium sheet preparation, and particularly relates to a method for controlling the warping morphology of an ultrathin germanium sheet.
Background
In the preparation of the three-junction gallium arsenide solar cell for the space power supply, the germanium single crystal polished wafer not only plays a role of supporting a substrate, but also plays a role of a bottom cell. The quality of the germanium single crystal polished wafer directly determines the quality of the triple-junction gallium arsenide solar cell. With the continuous weight reduction requirement of the battery system, the required thickness of the germanium sheet is gradually reduced. The reduction of the thickness leads the germanium sheet to show more elastic characteristics in a plurality of machining steps such as slicing, chamfering, grinding, corroding, polishing and the like, the mechanical strength is easy to reduce due to improper control, and finally the epitaxial yield in the battery manufacturing process is greatly reduced. The warping appearance is simple and easy to measure, and the internal stress of the germanium sheet can be intuitively reflected.
The patent CN103862354B by zhao et al discloses that the germanium sheet is polished by using a frozen fixed abrasive as a polishing disk, but the properties of the polished germanium sheet are not characterized.
Wangshenkei in patent CN102569027B, the size of the nano microstructure on the surface of the germanium sheet is controlled by a thermal oxidation method, and the patent does not relate to the content of a machining part.
The patent CN109352430B discloses that how far east et al adopt different grinding methods to grind the front and back surfaces of a germanium sheet respectively, and adopt a corrosive liquid composed of sulfuric acid, hydrogen peroxide and deionized water to carry out weak corrosion cleaning on the germanium grinding sheet, thereby realizing the reduction of the curvature value.
The cynanchum wangchensis adopts a double-sided grinding machine to grind the germanium sheet in the patent CN103240666B, overcomes the defect of manual grinding, promotes the surface quality of the germanium sheet, but only explains a single grinding procedure and does not relate to the influence of subsequent processing procedures on the surface quality and the geometric morphology of the germanium sheet.
The radix cynanchi wangtii electrophoresis puts the germanium sheet into HF solution, glacial acetic acid, bromine water and nitric acid solution in the patent CN103233228A in sequence, so that the mechanical strength of the germanium sheet is improved, and the change condition of the surface morphology of the corroded germanium sheet is not mentioned.
In summary, in the related patents, although there are studies on processing of the germanium sheet, no study is made on controlling the warpage morphology of the germanium sheet.
Disclosure of Invention
In view of the conditions of the prior art, the invention integrates the mechanical thinning and chemical thinning effects, innovatively optimizes the grinding process, and provides a control method for the warping morphology of the ultrathin germanium sheet.
The technical scheme adopted by the invention is as follows: a method for controlling the warping morphology of an ultrathin germanium sheet is characterized by comprising the following steps:
firstly, thickness grading is carried out on a germanium sheet before grinding, a planetary wheel is placed on a lower disc of a grinding machine, a germanium cutting sheet is placed in the planetary wheel, the grinding machine is started to carry out mechanical grinding on the germanium cutting sheet, cutting damage is removed, and meanwhile, the warping direction of the germanium sheet is preliminarily controlled by optimizing and adjusting the rotating speed ratio of the upper disc to the lower disc;
secondly, acid etching is carried out on the germanium grinding sheet by adopting an acid etching machine, the removal of grinding damage of the germanium sheet is realized by optimizing the arrangement mode of the germanium sheet and the etching process parameters, and the warping appearance of the germanium sheet is optimized;
attaching UV films with the same size to the front surface of the germanium sheet, downwards adsorbing the front surface of the germanium sheet on a vacuum chuck, grinding the back surface of the germanium sheet by using a grinding machine, and further controlling the warping appearance of the germanium sheet by controlling the grinding removal amount of the back surface;
and fourthly, removing the UV film on the back surface of the germanium sheet under the irradiation of an ultraviolet lamp, carrying out weak base corrosion on the germanium grinding sheet by adopting an alkaline corrosion solution, and finally removing stress through weak corrosion of the germanium sheet alkali liquor to improve the surface quality and the mechanical strength of the germanium sheet.
The invention has the beneficial effects that:
according to the method, according to the characteristics of the ultrathin germanium sheet in the machining process, the influence of physical action and chemical action in the germanium sheet machining process is comprehensively considered, the warpage morphology control in the ultrathin germanium sheet thinning machining process is realized by adopting a method combining the working procedures of grinding, acid corrosion, grinding, alkali corrosion and the like, the machining efficiency is high, the warpage value of the prepared germanium sheet can be controlled below 10 micrometers, and the warpage morphology is bent towards a single direction. The fragment rate of the ultrathin germanium sheet prepared by the method in the subsequent epitaxial process is 10% higher than that of the ultrathin germanium sheet prepared by the conventional processing method.
Drawings
FIG. 1 is a schematic diagram of a germanium wafer polishing process according to the present invention;
FIG. 2 is a schematic view of the placement of germanium sheets in the roller of the acid etching machine of the present invention;
FIG. 3 is a graph showing the results of mechanical strength tests of the germanium sheet in example 1 of the present invention;
fig. 4 is a graph of the mechanical strength test result of the germanium sheet in embodiment 2 of the present invention.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings:
as shown in fig. 1 and fig. 2, a method for controlling the warpage morphology of an ultra-thin germanium sheet includes the following steps:
firstly, placing a planetary gear on a lower disc of a grinding machine, placing a germanium cutting piece into the planetary gear, starting the grinding machine to mechanically grind the germanium cutting piece to remove cutting damage, and simultaneously, primarily controlling the warping direction of the germanium piece by optimally adjusting the rotating speed ratio of the upper disc to the lower disc;
before grinding, the thickness of the germanium sheets is graded, and the difference between the thickness sheets of the same germanium sheet is less than or equal to 3 mu m; repairing the equipment before grinding of each germanium sheet; set up during the grinding and grind quick-witted lower wall anticlockwise rotation, hanging wall clockwise rotation, the germanium piece openly is placed downwards uniformly, and the grinding fluid ratio is water: grinding sand: and (3) auxiliary agent A: auxiliary agent B = (1-4): (0.5-3): (0.01-0.1): (0.01-0.1), and grinding according to the following process:
1) the pressure is 40-60 Kg, the rotating speed of the lower disc is 1-3 rpm, the flow of the grinding fluid is 1400-1800 ml/min, and the time is 1 min;
2) the pressure is 60-90 Kg, the rotating speed of the lower disc is 3-5 rpm, the flow of the grinding fluid is 1400-1800 ml/min, and the time is 1 min;
3) the pressure is 90-120 Kg, the rotating speed of the lower disc is 5-7 rpm, the flow of the grinding fluid is 1400-1800 ml/min, and the time is 1 min;
4, the pressure is 120-140 Kg, the rotating speed of the lower disc is 7-9 rpm, the flow of the grinding fluid is 1400-1800 ml/min, and the time is 1 min;
5) the pressure is 140-160 Kg, the rotating speed of the lower disc is 9-10 rpm, the flow of the grinding fluid is 1400-1800 ml/min, and the time is 15-20 min;
the setting range of the rotating speed ratio of the upper disc and the lower disc of the grinding machine is 1: 3-1: and 5, grinding and removing the back surface by 5-10 microns, and grinding and removing the front surface by 15-20 microns.
Secondly, acid etching is carried out on the germanium grinding sheet by adopting an acid etching machine, the removal of grinding damage of the germanium sheet is realized by optimizing the arrangement mode of the germanium sheet and the etching process parameters, and the warping appearance of the germanium sheet is optimized;
the germanium sheets are placed in an interval mode, the roller bears the germanium sheets to rotate clockwise, the front surfaces of all the germanium sheets face to the same side, the germanium sheets in the area A and the germanium sheets in the area C of the roller are symmetrically placed in number, and the placing number is larger than that of the germanium sheets placed in the area B; the corrosion is carried out in an acid liquid tank, the flushing is carried out in a pure water tank, the flushing adopts a mode of soaking and spraying, the spraying time is not less than 2 times of the corrosion time, and the mixed acid used in the corrosion process is HNO3、HF、CH3COOH, wherein the volume ratio of the three components is (2-5): (2-3): (0.5 to 2); the corrosion temperature is 21-23 ℃; the uniformity of germanium sheet corrosion is improved by blowing nitrogen in the reaction process, and the bubbling amount is set to be 160-200L/minThe bubbling time = corrosion time-12 s, the rotating speed of the roller is 10-35 rpm, and the acid corrosion removal amount is 30-40 μm.
Attaching UV films with the same size to the front surface of the germanium sheet, downwards adsorbing the front surface of the germanium sheet on a vacuum chuck, grinding the back surface of the germanium sheet by using a grinding machine, and further controlling the warping appearance of the germanium sheet by controlling the grinding removal amount of the back surface;
and removing the back surface of the germanium sheet by adopting a single-side grinding mode, wherein the model of a grinding wheel is 4000-6000 # grinding wheel, the rotating speed of the grinding wheel is 3500-5000 rpm, the grinding is carried out in three steps, the feeding rate of the first step is 0.6-0.9 mu m/s, the feeding rate of the second step is 0.1-0.3 mu m/s, the feeding rate of the third step is 0.05-0.2 mu m/s, and the back surface removal amount is controlled to be 7-10 mu m.
Fourthly, removing the UV film on the back surface of the germanium sheet under the irradiation of an ultraviolet lamp, carrying out weak base corrosion on the germanium grinding sheet by adopting an alkaline corrosion solution, and finally removing stress through weak corrosion of the germanium sheet alkali liquor to improve the surface quality and the mechanical strength of the germanium sheet;
the adopted alkaline corrosive liquid is KOH solution, the temperature is 50-70 ℃, the concentration is 48%, the weak corrosion removal amount is controlled below 10 mu m, and the corrosion time is not more than 25 s.
The thickness of the germanium sheet is 120-500 microns.
Example 1:
the germanium sheet has a diameter of 100 + -0.2 mm, a resistivity of 0.01-0.03 omega-cm, a thickness of 295 + -15 μm, and a crystal orientation P <100> 9 DEG (111), as shown in FIG. 1 and FIG. 2.
(1) The germanium sheet carries out thickness stepping according to 2 mu m, places the germanium sheet openly down in the wandering star wheel of double side grinder, puts 16 germanium sheets in every wandering star wheel, sets up the mill lower wall anticlockwise rotation during the grinding, hanging wall clockwise rotation, and upper and lower wall speed ratio sets up to 1: 4, the grinding fluid is prepared from the following components in percentage by weight: grinding sand: and (3) auxiliary agent A: auxiliary agent B = 4: 2: 0.1: 0.1.
the grinding was carried out as follows:
1) the pressure is 50Kg, the rotating speed of the lower disc is 2rpm, the flow of the grinding fluid is 1400ml/min, and the time is 1 min;
2) the pressure is 70Kg, the rotating speed of the lower disc is 5rpm, the flow of the grinding fluid is 1400ml/min, and the time is 1 min;
3) the pressure is 100Kg, the rotating speed of the lower disc is 7rpm, the flow of the grinding fluid is 1400ml/min, and the time is 1 min;
4, the pressure is 130Kg, the rotating speed of the lower disc is 9rpm, the flow of the grinding fluid is 1400ml/min, and the time is 1 min;
5) the pressure is 150Kg, the rotating speed of the lower disc is 10rpm, the flow of the grinding fluid is 1400ml/min, and the time is 18 min;
controlling the back surface removal amount to be 10 mu m, the front surface removal amount to be 20 mu m, and the thickness of the ground germanium sheet to be 265 +/-5 mu m;
(2) acid etching is carried out on the germanium grinding sheet by adopting an acid etching machine, during acid etching, the number of the germanium sheets placed in the area A, the area B and the area C in the figure 2 is respectively 13 sheets, 12 sheets and 13 sheets, the front surfaces of the germanium sheets are uniformly placed towards the right hand side direction of an operator, the germanium sheets are etched in an acid mixing tank, and the mixed acid is etched by HNO3、HF、CH3COOH, and the volume ratio of the three components is 3: 2: 1; the corrosion temperature is 21 ℃, the corrosion time is 39s, the rotating speed of the roller is 35rpm, the bubbling amount is 200L/min, and the bubbling time is 27 s; the corroded germanium sheet is driven by a mechanical arm to be transferred into a pure water tank for spraying, soaking and cleaning, the spraying time is 78s, and the thickness of the germanium sheet after acid corrosion is 230 +/-5 microns;
(3) and (4) carrying out single-side removal on the back surface of the germanium sheet by using a grinding machine. The grinding wheel is 4000#, the rotating speed of the main shaft is set to be 4000rpm, grinding is carried out in three steps, the feeding rate of the first step is 0.7 mu m/s, the feeding rate of the second step is 0.1 mu m/s, the feeding rate of the third step is 0.05 mu m/s, and the thickness of the germanium sheet after back surface grinding is 220 +/-5 mu m;
(4) weakly corroding the germanium grinding sheet by using a KOH solution with the concentration of 48%, wherein the corrosion temperature is 60 ℃, the corrosion time is 16s, and the thickness of the germanium sheet after alkali corrosion is 212 +/-5 mu m;
(5) and after corrosion, a flatness measuring instrument is adopted to test the geometric morphology of the germanium sheet, the result shows that the ratio of the morphology of the germanium sheet warping towards a single direction is more than 90%, and after polishing, a mechanical strength tester is adopted to test the mechanical strength of the germanium sheet to be 10.425 lbf, which is shown in figure 3, so that the use requirement is met.
Example 2:
the germanium sheet has a diameter of 100 + -0.2 mm, a resistivity of 0.03-0.05 omega-cm, a thickness of 310 + -15 μm, and a crystal orientation P <100> 9 DEG (111), as shown in FIG. 1 and FIG. 2.
(1) The germanium sheet carries out thickness stepping according to 3 mu m, places the germanium sheet openly down in the wandering star wheel of double side grinder, puts 16 germanium sheets in every wandering star wheel, sets up the mill lower wall anticlockwise rotation during the grinding, hanging wall clockwise rotation, and upper and lower wall speed ratio sets up to 1: 5, the grinding fluid is prepared from the following components in percentage by weight: grinding sand: and (3) auxiliary agent A: auxiliary agent B = 4: 2: 0.1: 0.1.
the grinding was carried out as follows:
1) the pressure is 60Kg, the rotating speed of the lower disc is 3rpm, the flow of the grinding fluid is 1600ml/min, and the time is 1 min;
2) the pressure is 80Kg, the rotating speed of the lower disc is 5rpm, the flow of the grinding fluid is 1600ml/min, and the time is 1 min;
3) the pressure is 110Kg, the rotating speed of the lower disc is 7rpm, the flow of the grinding fluid is 1600ml/min, and the time is 1 min;
4, the pressure is 140Kg, the rotating speed of the lower disc is 9rpm, the flow of the grinding fluid is 1600ml/min, and the time is 1 min;
5) the pressure is 160Kg, the rotating speed of the lower disc is 10rpm, the flow of the grinding fluid is 1600ml/min, and the time is 16 min;
controlling the removal amount of the back surface to be 7 microns, the removal amount of the front surface to be 18 microns, and the thickness of the ground germanium sheet to be 285 +/-5 microns;
(2) acid etching is carried out on the germanium grinding sheet by adopting an acid etching machine, during acid etching, the number of the germanium sheets placed in the area A, the area B and the area C in the figure 2 is respectively 11, 10 and 11, the front surfaces of the germanium sheets are uniformly placed towards the right hand side direction of an operator, the germanium sheets are etched in an acid mixing tank, and the mixed acid is etched by HNO3、HF、CH3COOH, and the volume ratio of the three components is 3: 2: 1; the corrosion temperature is 22 ℃, the corrosion time is set to be 42s, the rotating speed of the roller is set to be 35rpm, the bubbling amount is set to be 180L/min, and the bubbling time is 30 s; the corroded germanium sheet is driven by a mechanical arm to be transferred into a pure water tank for spraying, soaking and cleaning, the spraying time is 90s, and the thickness of the acid-corroded germanium sheet is 245 +/-5 microns;
(3) and (4) carrying out single-side removal on the back surface of the germanium sheet by using a grinding machine. The grinding wheel is 5000#, the rotating speed of the main shaft is set to be 4000rpm, grinding is carried out in three steps, the feeding speed of the first step is 0.8 mu m/s, the feeding speed of the second step is 0.2 mu m/s, the feeding speed of the third step is 0.1 mu m/s, and the thickness of the germanium sheet after back surface grinding is 237 +/-5 mu m;
(4) weakly corroding the germanium grinding sheet by using a KOH solution with the concentration of 48%, wherein the corrosion temperature is 60 ℃, the corrosion time is 20s, and the thickness of the germanium sheet after alkali corrosion is 227 +/-5 mu m;
(5) and after corrosion, a flatness measuring instrument is adopted to test the geometric morphology of the germanium sheet, the result shows that the ratio of the morphology of the germanium sheet warping towards a single direction is more than 90%, and after polishing, a mechanical strength tester is adopted to test the mechanical strength of the germanium sheet to be 8.333 lbf, which is shown in figure 4, so that the use requirement is met.
Claims (5)
1. A method for controlling the warping morphology of an ultrathin germanium sheet is characterized by comprising the following steps:
firstly, thickness grading is carried out on a germanium sheet before grinding, a planetary wheel is placed on a lower disc of a grinding machine, a germanium cutting sheet is placed in the planetary wheel, the grinding machine is started to carry out mechanical grinding on the germanium cutting sheet, cutting damage is removed, and meanwhile, the warping direction of the germanium sheet is preliminarily controlled by optimizing and adjusting the rotating speed ratio of the upper disc to the lower disc;
secondly, acid etching is carried out on the germanium grinding sheet by adopting an acid etching machine, the removal of grinding damage of the germanium sheet is realized by optimizing the arrangement mode of the germanium sheet and the etching process parameters, and the warping appearance of the germanium sheet is optimized;
attaching UV films with the same size to the front surface of the germanium sheet, downwards adsorbing the front surface of the germanium sheet on a vacuum chuck, grinding the back surface of the germanium sheet by using a grinding machine, and further controlling the warping appearance of the germanium sheet by controlling the grinding removal amount of the back surface;
and fourthly, removing the UV film on the back surface of the germanium sheet under the irradiation of an ultraviolet lamp, carrying out weak base corrosion on the germanium grinding sheet by adopting an alkaline corrosion solution, and finally removing stress through weak corrosion of the germanium sheet alkali liquor to improve the surface quality and the mechanical strength of the germanium sheet.
2. The method for controlling the warping morphology of the ultrathin germanium sheet as claimed in claim 1, wherein in the first step, the germanium sheet is graded in thickness before grinding, and the difference between the germanium sheet thickness of the same disc is less than or equal to 3 μm; repairing the equipment before grinding of each germanium sheet; set up during the grinding and grind quick-witted lower wall anticlockwise rotation, hanging wall clockwise rotation, the germanium piece openly is placed downwards uniformly, and the grinding fluid ratio is water: grinding sand: and (3) auxiliary agent A: auxiliary agent B = (1-4): (0.5-3): (0.01-0.1): (0.01-0.1), and grinding according to the following process:
1) the pressure is 40-60 Kg, the rotating speed of the lower disc is 1-3 rpm, the flow of the grinding fluid is 1400-1800 ml/min, and the time is 1 min;
2) the pressure is 60-90 Kg, the rotating speed of the lower disc is 3-5 rpm, the flow of the grinding fluid is 1400-1800 ml/min, and the time is 1 min;
3) the pressure is 90-120 Kg, the rotating speed of the lower disc is 5-7 rpm, the flow of the grinding fluid is 1400-1800 ml/min, and the time is 1 min;
4, the pressure is 120-140 Kg, the rotating speed of the lower disc is 7-9 rpm, the flow of the grinding fluid is 1400-1800 ml/min, and the time is 1 min;
5) the pressure is 140-160 Kg, the rotating speed of the lower disc is 9-10 rpm, the flow of the grinding fluid is 1400-1800 ml/min, and the time is 15-20 min;
the setting range of the rotating speed ratio of the upper disc and the lower disc of the grinding machine is 1: 3-1: and 5, grinding and removing the back surface by 5-10 microns, and grinding and removing the front surface by 15-20 microns.
3. The method for controlling the warping morphology of the ultrathin germanium sheets as claimed in claim 1, wherein in the second step, the germanium sheets are placed in an interval manner such that the roller bears the germanium sheets to rotate clockwise, the front surfaces of all the germanium sheets are placed towards the same side, the germanium sheets in the areas A and C of the roller are placed in a symmetrical manner, and the number of the germanium sheets placed in the areas A and C is greater than that of the germanium sheets placed in the area B; the corrosion is carried out in an acid liquid tank, the flushing is carried out in a pure water tank, the flushing adopts a mode of soaking and spraying, the spraying time is not less than 2 times of the corrosion time, and the mixed acid used in the corrosion process is HNO3、HF、CH3COOH, wherein the volume ratio of the three components is (2-5): (2-3): (0.5 to 2); the corrosion temperature is 21-23 ℃; in the reaction process, the uniformity of germanium sheet corrosion is improved by blowing nitrogen, the bubbling amount is set to be 160-200L/min, the bubbling time = corrosion time-12 s, the rotating speed of the roller is 10-35 rpm, and the acid corrosion removal amount is 30-40 μm.
4. The method for controlling the warping morphology of the ultrathin germanium sheet as claimed in claim 1, wherein in the third step, the back surface of the germanium sheet is removed by single-side grinding, the type of the grinding wheel is 4000-6000 # grinding wheel, the rotating speed of the grinding wheel is 3500-5000 rpm, the grinding is carried out in three steps, the feeding rate of the first step is 0.6-0.9 μm/s, the feeding rate of the second step is 0.1-0.3 μm/s, the feeding rate of the third step is 0.05-0.2 μm/s, and the back surface removal amount is controlled to be 7-10 μm;
the method for controlling the warpage morphology of the ultrathin germanium sheet as claimed in claim 1, wherein in the fourth step, the adopted alkaline etching solution is a KOH solution, the temperature is 50-70 ℃, the concentration is 48%, the weak etching removal amount is controlled below 10 μm, and the etching time is not more than 25 s.
5. The method as claimed in claim 1, wherein the thickness of the germanium sheet is 120-500 μm.
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