CN111725052A - Method for recycling silicon carbide wafer after corrosion - Google Patents
Method for recycling silicon carbide wafer after corrosion Download PDFInfo
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- CN111725052A CN111725052A CN202010620360.7A CN202010620360A CN111725052A CN 111725052 A CN111725052 A CN 111725052A CN 202010620360 A CN202010620360 A CN 202010620360A CN 111725052 A CN111725052 A CN 111725052A
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 184
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 184
- 238000005260 corrosion Methods 0.000 title claims abstract description 108
- 230000007797 corrosion Effects 0.000 title claims abstract description 108
- 238000000034 method Methods 0.000 title claims abstract description 58
- 238000004064 recycling Methods 0.000 title claims abstract description 13
- 239000010410 layer Substances 0.000 claims abstract description 150
- 239000011241 protective layer Substances 0.000 claims abstract description 34
- 230000007547 defect Effects 0.000 claims abstract description 20
- 238000007747 plating Methods 0.000 claims abstract description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 74
- 229910052759 nickel Inorganic materials 0.000 claims description 37
- 229920002120 photoresistant polymer Polymers 0.000 claims description 18
- 239000004642 Polyimide Substances 0.000 claims description 14
- 229920001721 polyimide Polymers 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 238000005530 etching Methods 0.000 claims description 7
- 239000003292 glue Substances 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 238000005498 polishing Methods 0.000 description 133
- 235000012431 wafers Nutrition 0.000 description 123
- 239000000758 substrate Substances 0.000 description 56
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 54
- 239000002245 particle Substances 0.000 description 36
- 239000000243 solution Substances 0.000 description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 24
- 229910003460 diamond Inorganic materials 0.000 description 24
- 239000010432 diamond Substances 0.000 description 24
- 238000004140 cleaning Methods 0.000 description 20
- 229910052580 B4C Inorganic materials 0.000 description 18
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 18
- 239000007800 oxidant agent Substances 0.000 description 16
- 238000000227 grinding Methods 0.000 description 15
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 12
- 238000001035 drying Methods 0.000 description 11
- 239000004814 polyurethane Substances 0.000 description 10
- 229920002635 polyurethane Polymers 0.000 description 10
- 239000002270 dispersing agent Substances 0.000 description 9
- 230000001590 oxidative effect Effects 0.000 description 9
- 239000012670 alkaline solution Substances 0.000 description 8
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 8
- 239000000908 ammonium hydroxide Substances 0.000 description 7
- 229910052681 coesite Inorganic materials 0.000 description 7
- 229910052906 cristobalite Inorganic materials 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 229910052682 stishovite Inorganic materials 0.000 description 7
- 229910052905 tridymite Inorganic materials 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 229910052717 sulfur Inorganic materials 0.000 description 6
- 239000011593 sulfur Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 5
- 238000004026 adhesive bonding Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 235000019253 formic acid Nutrition 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 238000011109 contamination Methods 0.000 description 4
- 238000007781 pre-processing Methods 0.000 description 4
- 125000001453 quaternary ammonium group Chemical group 0.000 description 4
- 238000006748 scratching Methods 0.000 description 4
- 230000002393 scratching effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000009713 electroplating Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
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- 239000003921 oil Substances 0.000 description 3
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- 239000007789 gas Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
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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
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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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- 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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- 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
- H01L21/02032—Preparing bulk and homogeneous wafers by reclaiming or re-processing
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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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/0445—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising crystalline silicon carbide
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Abstract
The invention provides a method for recycling a silicon carbide wafer after corrosion, which comprises the following steps: 1) covering a protective layer on the surface to be corroded of the silicon carbide wafer; 2) plating corrosion-resistant layers on the other surfaces of the silicon carbide wafer treated in the step 1); 3) removing the protective layer; 4) corroding the silicon carbide wafer treated in the step 3); 5) observing the defect condition of the silicon carbide wafer; 6) removing the corrosion-resistant layer of the silicon carbide wafer; 7) and removing the corrosion layer on the surface to be corroded of the silicon carbide wafer to obtain the recyclable silicon carbide wafer. Compared with the prior art, the silicon carbide wafer processed by the method still has a certain thickness, and the side surface integrity is good, so that the requirement of recycling can be met, and the cost is reduced.
Description
Technical Field
The invention relates to the field of semiconductor manufacturing, in particular to a method for recycling a silicon carbide wafer after corrosion.
Background
At present, silicon carbide attracts great attention because of high forbidden bandwidth. The method can be applied to the fields of high temperature, high frequency, high power and the like, and has huge market.
At present, the biggest bottleneck in the field of silicon carbide manufacturing is the preparation of basic crystal materials, and only a few companies in a few countries master key core preparation methods all over the world, so that the cost for obtaining silicon carbide wafers is very high, and the saving of wafer resources and the reduction of corresponding cost are very important.
The existing silicon carbide wafer has limited defect research means, and in order to carry out deep research on the defects of the silicon carbide wafer, the defect analysis needs to be carried out by corroding the silicon carbide wafer, and the corroded thick silicon carbide wafer has uneven front and back surfaces and edges, obvious etching pits and a large number of corrosion pits, so that the silicon carbide wafer cannot be reused.
Disclosure of Invention
The invention aims to provide a method for recycling a silicon carbide wafer after corrosion.
The specific technical scheme of the invention is as follows:
the invention provides a method for recycling a silicon carbide wafer after corrosion, which comprises the following steps:
1) covering a protective layer on the surface to be corroded of the silicon carbide wafer;
2) plating corrosion-resistant layers on the other surfaces of the silicon carbide wafer treated in the step 1);
3) removing the protective layer;
4) corroding the silicon carbide wafer treated in the step 3);
5) observing the defect condition of the silicon carbide wafer;
6) removing the corrosion-resistant layer of the silicon carbide wafer;
7) and removing the corrosion layer on the surface to be corroded of the silicon carbide wafer to obtain the recyclable silicon carbide wafer.
Further, the silicon carbide wafer is pretreated and then covered with the protective layer, and the specific pretreatment method comprises the following steps: firstly, ultrasonically cleaning a silicon carbide wafer by using acetone to remove impurities such as oil stains on the surface; then, ultrasonically cleaning the silicon carbide wafer by using absolute ethyl alcohol to remove acetone possibly remaining on the surface of the substrate; and finally, ultrasonically cleaning the silicon carbide wafer by using deionized water to remove ethanol remained on the surface of the substrate. In order to achieve the best cleaning effect, the growth surface of the silicon carbide wafer is downward when the silicon carbide wafer is subjected to ultrasonic cleaning, and the time for each ultrasonic cleaning is 5-10 minutes. And after all the cleaning steps are carried out, completely blowing the surface of the silicon carbide substrate by using high-purity argon to prevent the surface of the silicon carbide substrate from leaving water marks after natural drying.
The protective layer in the step 1) is polyimide or photoresist; covering photoresist, and adding a developing process; polyimide does not need to be developed; in the invention, a protective layer is covered on the surface to be corroded, a small amount of corrosion-resistant substances are plated on the protective layer covered on the surface to be corroded when the corrosion-resistant layer is plated on the side surface, the protective layer is easy to remove, the silicon carbide wafer is corroded after the protective layer is removed, and the side surface and the other surface of the silicon carbide wafer are protected from corrosion by the corrosion-resistant layer. Therefore, the protective layer is covered firstly, so that the removal process can be simplified, the surface to be corroded does not need to be electroplated with the corrosion-resistant layer, and the process for plating the corrosion-resistant layer on the surface to be corroded and the process for removing the corrosion-resistant layer are omitted; meanwhile, the corrosion resistance protection of the side face and the other face is not influenced, and the reutilization of the silicon carbide wafer is not influenced.
In the step 1), the specific method for covering the photoresist protective layer comprises the following steps: selecting AZ5206E photoresist, and coating with a coating thickness of 50nm-5 μm at a rotation speed of 500rpm-5000 rpm.
In the step 1), after covering the photoresist, baking for 60-120sec at the temperature of 90-120 ℃; finally, exposure to PLA 501F (Proximaty) intensity 189mJ/cm2。
The method for covering the polyimide protective layer in the step 1) comprises the following steps: selecting PW1500s polyimide, selecting a rotating speed of 500rpm-5000rpm for gluing, wherein the gluing thickness is 50nm-15 mu m; the curing conditions after gluing are as follows: 110 ℃ and 130 ℃ for 60-300 sec.
The step 2) is specifically as follows: plating a corrosion-resistant layer on the side surface and the other surface opposite to the surface to be corroded of the SiC wafer processed in the step 1). Preferably, the corrosion-resistant layer is an inert metal protective layer. More preferably, the corrosion-resistant layer in step 2) is a nickel layer.
Further, the method for plating the corrosion-resistant layer in the step 2) comprises the following steps: firstly, a seed layer is grown and then a nickel layer is electroplated or a nickel layer is directly electroplated.
The method for growing the seed layer in the step 2) comprises the following steps: under the condition of room temperature, the pressure of 0.1Pa-0.2Pa rotates the wafer at the growth speed of 1nm/min and the speed of more than 20rpm, firstly the nickel seed layer 1 with the thickness of 0.5nm-30nm grows, and then the nickel seed layer 2 with the thickness of 30nm-300nm grows at the growth speed of 1.5 nm-2 nm/min under the pressure of 0.2Pa-0.4 Pa. The method realizes that the nickel seed layer grows on the side surface of the silicon carbide wafer and the other surface opposite to the surface to be etched. The seed layer 1 mainly has the function of forming a uniform nucleation center; the seed layer 2 mainly has the function of forming a compact seed layer, so that the adhesiveness and the surface electrical property of the nickel layer and the silicon carbide material are ensured; preparing for the next step of rapid electroplating and surface roughness control.
The electroplated nickel layer in the step 2) is specifically as follows: electroplating double-layer nickel or three-layer nickel.
The double-layer nickel: the bottom layer semi-bright nickel layer is 15-60 μm thick, and the outer layer sulfur-containing bright nickel layer is 15-60 μm thick;
the three layers of nickel: the bottom layer is a semi-bright nickel layer with the thickness of 15-30 mu m, the middle layer is a high-sulfur nickel layer with the thickness of 1-2 mu m, the sulfur content is 0.12-0.25%, and the outer layer is a sulfur-containing bright nickel layer with the thickness of 15-30 mu m;
further, in step 3), when the protective layer is a photoresist, step 2) plating the corrosion-resistant layer and then developing the photoresist to remove the protective layer. The development specifically comprises the following steps: AZ 300MIF (2.38%), 23 deg.C, 60 sec.
When the protective layer is polyimide, removing PW1500s polyimide glue after plating the corrosion-resistant layer in the step 2), wherein the removing method comprises the following steps: exposure,1.0J/cm2(ii) a 2 times for 1min, 2.38% TMAH solution (tetramethylammonium hydroxide solution) was used.
The corrosion in the step 4) is specifically as follows: corroding the silicon carbide wafer treated in the step 3) by using high-temperature alkaline molten liquid. Preferably, the method for etching the silicon carbide wafer processed in the step 3) comprises the following steps: corroding the silicon carbide wafer for 5-30 minutes by using the high-temperature alkaline solution at 350-550 ℃, taking out, cleaning, drying and spin-drying; the alkaline melt is NaOH and/or KOH mixed melt; in the case of a mixed melt of NaOH and KOH, the ratio can be adjusted, and preferably, the mass ratio of both is 1: 1.
Step 5): the OM microscope observes the defect condition of the silicon carbide wafer after corrosion and carries out defect analysis;
and step 6) comprises chamfering and removing the corrosion-resistant layer on the side surface of the silicon carbide wafer and CMP (chemical mechanical polishing) removing the corrosion-resistant layer on the other surface opposite to the surface to be corroded. The chamfering removal of the corrosion-resistant layer on the side surface of the silicon carbide wafer refers to the direct chamfering removal by using a diamond chamfering grinding wheel.
The step 6) of removing the corrosion-resistant layer on the other surface opposite to the surface to be corroded by CMP specifically comprises the following steps: placing the other surface opposite to the surface to be corroded upwards, selecting an abrasion-resistant polyurethane polishing pad, polishing by using polishing liquid, and controlling the polishing pressure to be 1g/cm2-10g/cm2The rotation speed of the polishing machine is 10-50rpm, the polishing temperature is controlled at 25-40 ℃, and the polishing is carried out according to the method until the surface corrosion-resistant layer is removed.
Step 2) the polishing solution is an acidic polishing solution or an alkaline polishing solution;
the alkaline polishing solution contains: colloidal SiO2Quaternary ammonium hydroxide, abrasive, polishing oxidizing agent and glycerol. The pH value of the quaternary ammonium base adjusting polishing solution is more than 8; the grinding material is boron carbide and diamond particles with the particle size of less than or equal to 135nm, and the mass ratio of the boron carbide to the diamond particles is 1:1, the addition amount of the grinding material is less than or equal to 20 wt%; the polishing oxidant is H2O2The content is 1 to 3 volume percent; the glycerol is used as a dispersant, and the content of the glycerol is 1-3% by volume.
The acidic polishing solution contains: colloidal SiO2Organic acid, abrasive, polishing oxidizer and glycerol. The organic acid is used for adjusting the pH value of the polishing solution to be less than or equal to 6; the organic acid is preferably formic acid. The grinding material is boron carbide and diamond particles with the particle size of less than or equal to 135nm, and the mass ratio of the boron carbide to the diamond particles is 1:1, the addition amount of the grinding material is less than or equal to 20 wt%; the polishing oxidant is H2O2The content is 1 to 3 volume percent; the glycerol is used as a dispersant, and the content of the glycerol is 1-3% by volume.
The step 7) is specifically as follows: and removing the corrosion layer on the surface to be corroded of the silicon carbide wafer by CMP.
Preferably, step 7) is specifically:
placing the surface of the corrosion layer of the surface to be corroded of the silicon carbide wafer upwards, selecting a wear-resistant polyurethane polishing pad, polishing by using polishing liquid, and controlling the polishing pressure to be 50g/cm2-150g/cm2The rotating speed of the polishing machine is 10-50rpm, the polishing temperature is 25-40 ℃, and the corrosion layer is removed; adding polishing solution to continue polishing, and controlling the polishing pressure to be 10g/cm2-50g/cm2The rotating speed of the polishing machine is 10-50rpm, the temperature of the polishing machine is controlled to be 25-40 ℃, and the polishing is carried out until the corrosion layer and the damage layer are removed; wherein the thickness of the corrosion layer is 1-3 μm, and the thickness of the damage layer is 0.5-1 μm.
Indexes of the polishing solution used for 2 times of polishing in the step 7) are within the range of the polishing solution in the step 6).
The silicon carbide wafer comprises a silicon carbide substrate or an epitaxial wafer, wherein the epitaxial wafer is a wafer on which an epitaxial layer with a certain thickness is grown by an epitaxial method on the basis of the silicon carbide substrate, the epitaxial layer grown by the epitaxial method needs to be removed by means of CMP (chemical mechanical polishing) and the like, and the removal method is the same as the step 6). After the epitaxial layer is removed, the epitaxial layer can be reused after being treated by the method disclosed by the application.
When the silicon carbide wafer is a silicon carbide substrate, the silicon carbide wafer can be directly processed by the method described in the application.
Compared with the prior art, the invention covers the protective layer on the surface to be corroded of the silicon carbide wafer before corrosion, then plates the corrosion-resistant layer on the side surface of the silicon carbide wafer and the other surface opposite to the surface to be corroded, and removes the corrosion-resistant layer and the corrosion-resistant layer after corrosion, so that the silicon carbide wafer still has a certain thickness and good side surface integrity, can meet the requirement of recycling, and reduces the cost.
Drawings
FIG. 1 is a surface of a silicon carbide wafer prior to treatment in example 1; scratch in the figure: scratching; pit of Pit; bump: salient points; stain: surface contamination; particle: surface particles;
FIG. 2 is a surface of a silicon carbide wafer after treatment according to example 1; scratch in the figure: scratching; pit of Pit; bump: salient points; stain: surface contamination; particle: surface particles;
FIG. 3 is a schematic view of a SiC wafer of the present invention showing 1-the surface to be etched, 2-the other surface opposite the surface to be etched, 3-the side surface;
FIG. 4 is a surface of a silicon carbide wafer before treatment in example 3; scratch in the figure: scratching; pit of Pit; bump: salient points; stain: surface contamination; particle: surface particles;
FIG. 5 is a surface of a silicon carbide wafer before treatment in example 3; scratch in the figure: scratching; pit of Pit; bump: salient points; stain: surface contamination; particle: surface particles.
Detailed Description
Example 1
A method for recycling a silicon carbide wafer after corrosion comprises the following steps:
1) firstly, preprocessing a silicon carbide wafer (substrate), and then covering a photoresist on a surface to be etched for protection;
the method for pretreating the silicon carbide wafer comprises the following steps: firstly, ultrasonically cleaning a SiC substrate by using acetone to remove impurities such as oil stains on the surface; then, ultrasonically cleaning the SiC substrate by using absolute ethyl alcohol to remove acetone possibly remaining on the surface of the substrate; and finally, ultrasonically cleaning the SiC substrate by using deionized water to remove ethanol remained on the surface of the substrate. For the best cleaning effect, the growth surface of the SiC substrate should be faced down when the substrate is ultrasonically cleaned, and the time for each ultrasonic cleaning should be 5 to 10 minutes. After all the cleaning steps are carried out, the surface of the silicon carbide substrate is completely blown dry by high-purity argon gas so as to prevent water marks from being left on the surface of the silicon carbide substrate after the silicon carbide substrate is naturally dried.
Then, coating a photoresist on the surface 1 of the silicon carbide wafer to be corroded: using AZ5206E photoresist, and coating the photoresist to a thickness of 3.2 μm at a rotating speed of 3000 rpm; pre-baking at 110 deg.C for 70 sec; finally, exposure is carried out, PLA 501F (proximitity) 189mJ/cm2；
2) Plating a corrosion-resistant layer on the other surfaces of the SiC wafer treated in the step 1): the seed layer and the nickel layer are uniformly plated on the side surface 3 of the SiC wafer processed in the step 1) and the other surface 2 opposite to the surface to be corroded, and the method comprises the following steps: under the condition of room temperature, the pressure of 0.15Pa, the growth speed of 1nm/min, the speed of more than 20rpm and the growth of 30nm of nickel seed layer 1, and then the pressure of 0.3Pa, the growth speed of 2nm/min and the growth of 300nm of nickel seed layer 2. The method is used for growing the nickel seed layer on the side surface 3 of the silicon carbide wafer and the other surface 2 opposite to the surface to be corroded, and then growing the nickel seed layer electroplated nickel layer on the side surface 3 of the silicon carbide wafer and the other surface 2 opposite to the surface to be corroded, and specifically comprises the following steps: double-layer nickel: the bottom layer of the semi-bright nickel layer is 40 μm thick, and the outer layer of the sulfur-containing bright nickel layer is 50 μm thick.
3) Developing the positive photoresist of the silicon carbide wafer: AZ 300MIF (2.38%), 23 ℃,60 sec; removing the protective layer on the surface to be corroded;
4) etching the silicon carbide wafer treated in the step 3): putting the silicon carbide wafer treated in the step 3) into a high-temperature alkaline solution at 450 ℃ to corrode the silicon carbide wafer for 10min, taking out, cleaning, drying and spin-drying; the high-temperature alkaline solution is a mixed solution of NaOH and KOH, and the mass ratio of the NaOH to the KOH is 1: 1.
5) OM optical microscope observation: the OM microscope observes the defect condition of the corrosion surface of the silicon carbide wafer and analyzes the defect condition;
6) removing the corrosion-resistant layer of the silicon carbide wafer: the diamond chamfering grinding wheel removes the corrosion-resistant layer on the side surface of the silicon carbide wafer by chamfering, and the CMP removes the corrosion-resistant layer on the other surface opposite to the surface to be corroded, and specifically comprises the following steps: placing the other surface opposite to the surface to be corroded upwards, selecting an abrasion-resistant polyurethane polishing pad, polishing by using polishing liquid, and controlling the polishing pressure to be 5g/cm2The rotation speed of the polishing machine is 20rpm, the polishing temperature is controlled at 30 ℃, and the polishing is carried out until the corrosion-resistant layer on the surface is removed. The polishing liquid contains: colloidal SiO2Quaternary ammonium hydroxide, abrasive, polishing oxidizing agent and glycerol. The pH value of the polishing solution is adjusted to 10 by the quaternary ammonium hydroxide; the grinding material is boron carbide and diamond particles with the particle size of 100nm, and the mass ratio of the boron carbide to the diamond particles is 1:1, 15 wt% of abrasive addition; the polishing oxidant is H2O2The content is 1.5 percent by volume; glycerol was used as a dispersant in an amount of 1.5% by volume.
7) Removing the corrosion layer on the surface to be corroded of the silicon carbide wafer: placing the surface of the corrosion layer of the surface to be corroded of the silicon carbide wafer upwards, selecting a wear-resistant polyurethane polishing pad, polishing by using polishing liquid, and controlling the polishing pressure to be 100g/cm2The rotating speed of the polishing machine is 30rpm, the polishing temperature is controlled at 30 ℃, and the thickness of a corrosion layer is 3 mu m; then adding polishing solution to polish the mixture, wherein the polishing pressure is controlled to be 25g/cm2The rotating speed of the polishing machine is 20rpm, the polishing temperature is controlled at 30 ℃, and the polishing is carried out until the damaged layer is removed by 0.5 mu m; finally, obtaining the recyclable silicon carbide wafer. Two used polishing solutions simultaneously 6).
The silicon carbide wafer processed in the embodiment 1 is a silicon carbide substrate which is 350um thick, and a 3-micron corrosion layer and a 0.5-micron damage layer are removed after single corrosion of the silicon carbide substrate processed by the method; the removal of the protective layer and the corrosion-resistant layer does not lose the thickness of the silicon carbide substrate, so the silicon carbide substrate processed by the method is 346.5 mu m thick, the thickness of the general silicon carbide wafer substrate can be reused within the range of 330-.
The surface of the silicon carbide substrate before the treatment of the embodiment 1 is shown in figure 1, and the surface of the silicon carbide substrate after the treatment of the embodiment 1 is shown in figure 2, and the comparison of the figure 1 and the figure 2 shows that the surface defects of the silicon carbide wafer after the treatment of the invention are not increased, even fewer defects are generated, and the silicon carbide wafer can be recycled.
Example 2
A method for recycling a silicon carbide wafer after corrosion comprises the following steps:
1) firstly, preprocessing a silicon carbide wafer (substrate), and then covering a polyimide layer on a surface to be corroded to be used as a protective layer; pretreatment of the silicon carbide wafer: firstly, ultrasonically cleaning a SiC substrate by using acetone to remove impurities such as oil stains on the surface; then, ultrasonically cleaning the SiC substrate by using absolute ethyl alcohol to remove acetone possibly remaining on the surface of the substrate; and finally, ultrasonically cleaning the SiC substrate by using deionized water to remove ethanol remained on the surface of the substrate. For the best cleaning effect, the growth surface of the SiC substrate should be faced down when the substrate is ultrasonically cleaned, and the time for each ultrasonic cleaning should be 5 to 10 minutes. After all the cleaning steps are carried out, the surface of the silicon carbide substrate is completely blown dry by high-purity argon gas so as to prevent water marks from being left on the surface of the silicon carbide substrate after the silicon carbide substrate is naturally dried.
Then, the polyimide on the surface to be corroded of the silicon carbide wafer is subjected to gluing treatment, and the specific process comprises the following steps: PW1500s polyimide, coating with a thickness of 4 μm at 3500rpm, and curing at 120 deg.C for 180 sec;
2) and 1) plating a seed layer and a nickel layer on the side surface of the SiC wafer treated in the step 1) and the other surface opposite to the surface to be corroded, wherein the specific process comprises the following steps: under the condition of room temperature, the pressure of 0.15Pa, the growth speed of 1nm/min, the speed of more than 20rpm and the growth of 30nm of nickel seed layer 1, and then the pressure of 0.3Pa, the growth speed of 1.5nm/min and the growth of 300nm of nickel seed layer 2. The method realizes that the nickel seed layer grows on the side surface of the silicon carbide wafer and the other surface opposite to the surface to be etched. Then electroplating nickel layers on the side surface of the silicon carbide wafer and the other surface opposite to the surface to be corroded, specifically comprising the following steps: double-layer nickel: the bottom layer of the semi-bright nickel layer is 30 μm thick, and the outer layer of the sulfur-containing bright nickel layer is 50 μm thick.
3) Removing the PW1500s polyimide glue protective layer on the surface to be corroded, wherein the removing conditions are as follows: 1.0J/cm2(ii) a The treatment was performed 2 times for 1min using 2.38% TMAH solution (tetramethylammonium hydroxide solution) to remove the protective layer.
4) Etching the silicon carbide wafer treated in the step 2): placing the silicon carbide wafer treated in the step 3) in a high-temperature alkaline solution within the range of 450 ℃ to corrode the silicon carbide wafer for 12min, taking out, cleaning, drying and spin-drying;
5) the OM microscope is used for observing the defect condition of the corrosion surface of the silicon carbide and analyzing the defects;
6) the side surface and the other surface opposite to the surface to be corroded of the silicon carbide wafer are provided with a corrosion-resistant layer: firstly, removing the corrosion-resistant layer on the side surface of the silicon carbide wafer by chamfering with a diamond chamfering grinding wheel, and then removing the corrosion-resistant layer on the other surface opposite to the surface to be corroded by CMP (chemical mechanical polishing), wherein the method specifically comprises the following steps: the other surface opposite to the surface to be corroded was placed upward, and an abrasion-resistant polyurethane polishing pad was selected and polished with the same polishing liquid as in example 1 under a polishing pressure of 3g/cm2The rotation speed of the polishing machine is 20rpm, the polishing temperature is controlled at 30 ℃, and the polishing is carried out according to the method until the corrosion-resistant layer on the surface is removed.
7) The CMP removes the corrosion layer of the surface to be corroded of the silicon carbide wafer, and specifically comprises the following steps: placing the surface of the corrosion layer of the surface to be corroded of the silicon carbide wafer upwards, selecting a wear-resistant polyurethane polishing pad, and controlling the polishing pressure to be 110g/cm2The rotating speed of the polishing machine is 30rpm, the polishing temperature is controlled at 35 ℃, and a 3-micron corrosion layer is removed; then adding polishing solution to continue polishing, and controlling the polishing pressure to be 30g/cm2The rotating speed of the polishing machine is 30rpm, the polishing temperature is controlled at 35 ℃, a 0.6 mu m damage layer is removed, and finally, the recyclable silicon carbide wafer is obtained. The polishing solution used in the first step contains: colloidal SiO2Quaternary ammonium hydroxide, abrasive, polishing oxidizing agent and glycerol. The pH value of the polishing solution is adjusted to 10 by the quaternary ammonium hydroxide; the abrasiveThe diamond particles are boron carbide and diamond particles with the particle size of 110nm, and the mass ratio of the boron carbide to the diamond particles is 1:1, 15 wt% of abrasive addition; the polishing oxidant is H2O2The content is 1.5 percent by volume; glycerol was used as a dispersant in an amount of 1.5% by volume. The polishing solution used in the second step contains: colloidal SiO2Quaternary ammonium hydroxide, abrasive, polishing oxidizing agent and glycerol. The pH value of the polishing solution is adjusted to 10 by the quaternary ammonium hydroxide; the grinding material is boron carbide and diamond particles with the particle size of 40nm, and the mass ratio of the boron carbide to the diamond particles is 1:1, 15 wt% of abrasive addition; the polishing oxidant is H2O2The content is 1.5 percent by volume; glycerol was used as a dispersant in an amount of 1.5% by volume.
The silicon carbide wafer processed in the embodiment 2 is a silicon carbide substrate which is 350um thick, and a 3-micron corrosion layer and a 0.6-micron damage layer are removed after single corrosion of the silicon carbide substrate processed by the method; the removal of the protective layer and the corrosion-resistant layer does not lose the thickness of the silicon carbide substrate, so the silicon carbide substrate processed by the method is 346.4 mu m thick, the thickness of the general silicon carbide wafer substrate can be reused within the range of 330-.
Example 3
A method for recycling a silicon carbide wafer after corrosion comprises the following steps:
1) firstly, preprocessing a silicon carbide wafer (substrate), and then covering a photoresist on a surface to be etched for protection; the concrete steps are the same as the step 1) in the embodiment 1;
2) plating a corrosion-resistant layer on the other surfaces of the SiC wafer treated in the step 1): the concrete steps are the same as the step 2) of the embodiment 1;
3) developing the positive photoresist of the silicon carbide wafer: the concrete steps are the same as the step 3) in the embodiment 1;
4) etching the silicon carbide wafer treated in the step 3): placing the silicon carbide wafer treated in the step 3) in a high-temperature alkaline solution at 450 ℃ to corrode the silicon carbide wafer for 16min, taking out, cleaning, drying and spin-drying; the high-temperature alkaline solution is a mixed solution of NaOH and KOH, and the mass ratio of the NaOH to the KOH is 1: 1.
5) OM optical microscope observation: the OM microscope observes the defect condition of the corrosion surface of the silicon carbide wafer and analyzes the defect condition;
6) removing the corrosion-resistant layer of the silicon carbide wafer: the diamond chamfering grinding wheel removes the corrosion-resistant layer on the side surface of the silicon carbide wafer by chamfering, and the CMP removes the corrosion-resistant layer on the other surface opposite to the surface to be corroded, and specifically comprises the following steps: placing the other surface opposite to the surface to be corroded upwards, selecting an abrasion-resistant polyurethane polishing pad, polishing by using polishing liquid, and controlling the polishing pressure to be 3g/cm2The rotation speed of the polishing machine is 20rpm, the polishing temperature is controlled at 30 ℃, and the polishing is carried out until the corrosion-resistant layer on the surface is removed. The polishing liquid contains: colloidal SiO2Formic acid, abrasives, polishing oxidizing agents and glycerol. The pH value of the formic acid adjusting polishing solution is 4; the grinding material is boron carbide and diamond particles with the particle size of 90nm, and the mass ratio of the boron carbide to the diamond particles is 1:1, adding 10 wt% of abrasive; the polishing oxidant is H2O2The content is 1 percent by volume; glycerol was used as a dispersant in an amount of 1% by volume.
7) Removing the corrosion layer on the surface to be corroded of the silicon carbide wafer: placing the surface of the corrosion layer of the surface to be corroded of the silicon carbide wafer upwards, selecting a wear-resistant polyurethane polishing pad, polishing by using polishing liquid, and controlling the polishing pressure to be 100g/cm2The rotating speed of the polishing machine is 30rpm, the polishing temperature is controlled at 30 ℃, and the thickness of a corrosion layer is 3 mu m; then adding polishing solution to polish the mixture, wherein the polishing pressure is controlled to be 10g/cm2The rotating speed of the polishing machine is 20rpm, the polishing temperature is controlled at 30 ℃, and the polishing is carried out until the damaged layer is removed by 0.5 mu m; finally, obtaining the recyclable silicon carbide wafer. Two polishing solutions were used: adjusting the pH value of the polishing solution to be 4 by formic acid; the grinding material is boron carbide and diamond particles with the particle size of 100nm, and the mass ratio of the boron carbide to the diamond particles is 1:1, adding 10 wt% of abrasive; the polishing oxidant is H2O2The content is 1 percent by volume; glycerol was used as a dispersant in an amount of 1% by volume.
The silicon carbide wafer processed in the embodiment 3 is a silicon carbide substrate which is 350um thick, and a 3-micron corrosion layer and a 0.5-micron damage layer are removed after single corrosion of the silicon carbide substrate processed by the method; the removal of the protective layer and the corrosion-resistant layer does not lose the thickness of the silicon carbide substrate, so the silicon carbide substrate processed by the method is 346.5 mu m thick, the thickness of the general silicon carbide wafer substrate can be reused within the range of 330-.
The surface of the silicon carbide substrate before the treatment of the embodiment 3 is shown in fig. 4, and the surface of the silicon carbide substrate after the treatment of the embodiment 1 is shown in fig. 5, and the comparison of fig. 4 and fig. 5 shows that the surface defects of the silicon carbide wafer after the treatment of the invention are not increased, the defects are obviously fewer, and the silicon carbide wafer can be recycled.
Example 4
A method for recycling a silicon carbide wafer after corrosion comprises the following steps:
1) firstly, preprocessing a silicon carbide wafer (substrate), and then gluing polyimide; the concrete steps are the same as the step 1) of the embodiment 2;
2) plating a corrosion-resistant layer on the other surfaces of the SiC wafer treated in the step 1): the concrete steps are the same as the step 2) of the embodiment 2;
3) removing the PW1500s polyimide glue protective layer on the surface to be corroded, and performing the same step 3) as the step 2);
4) etching the silicon carbide wafer treated in the step 3): placing the silicon carbide wafer treated in the step 3) in a high-temperature alkaline solution at 500 ℃ to corrode the silicon carbide wafer for 20min, taking out, cleaning, drying and spin-drying; the high-temperature alkaline solution is a mixed solution of NaOH and KOH, and the mass ratio of the NaOH to the KOH is 1: 1.
5) OM optical microscope observation: the OM microscope observes the defect condition of the corrosion surface of the silicon carbide wafer and analyzes the defect condition;
6) removing the corrosion-resistant layer of the silicon carbide wafer: the diamond chamfering grinding wheel removes the corrosion-resistant layer on the side surface of the silicon carbide wafer by chamfering, and the CMP removes the corrosion-resistant layer on the other surface opposite to the surface to be corroded, and specifically comprises the following steps: placing the other surface opposite to the surface to be corroded upwards, selecting an abrasion-resistant polyurethane polishing pad, polishing by using polishing liquid, and controlling the polishing pressure to be 5g/cm2The rotation speed of the polishing machine is 30rpm, the polishing temperature is controlled at 35 ℃, and the polishing is carried out until the corrosion-resistant layer on the surface is removedCan be prepared. The polishing liquid contains: colloidal SiO2Formic acid, abrasives, polishing oxidizing agents and glycerol. The pH value of the formic acid adjusting polishing solution is 4; the grinding material is boron carbide and diamond particles with the particle size of 100nm, and the mass ratio of the boron carbide to the diamond particles is 1:1, 15 wt% of abrasive addition; the polishing oxidant is H2O2The content is 1 percent by volume; glycerol was used as a dispersant in an amount of 1% by volume.
7) Removing the corrosion layer on the surface to be corroded of the silicon carbide wafer: placing the surface of the corrosion layer of the surface to be corroded of the silicon carbide wafer upwards, selecting a wear-resistant polyurethane polishing pad, polishing by using a polishing solution, and controlling the polishing pressure to be 120g/cm2The rotating speed of the polishing machine is 35rpm, the polishing temperature is controlled at 30 ℃, and the thickness of a corrosion layer is 3 mu m; then adding polishing solution for polishing, and controlling the polishing pressure to be 8g/cm2The rotating speed of the polishing machine is 25rpm, the polishing temperature is controlled at 30 ℃, and the polishing is carried out until the damaged layer is removed by 0.8 mu m; finally, obtaining the recyclable silicon carbide wafer. Two polishing solutions were used: adjusting the pH value of the polishing solution to be 4 by formic acid; the grinding material is boron carbide and diamond particles with the particle size of 90nm, and the mass ratio of the boron carbide to the diamond particles is 1:1, adding 10 wt% of abrasive; the polishing oxidant is H2O2The content is 1 percent by volume; glycerol was used as a dispersant in an amount of 1% by volume.
The silicon carbide wafer processed in the embodiment 4 is a silicon carbide substrate which is 350um thick, and a 3 μm corrosion layer and a 0.8 μm damage layer are removed after single corrosion of the silicon carbide substrate processed by the method; the removal of the protective layer and the corrosion-resistant layer does not lose the thickness of the silicon carbide substrate, so the silicon carbide substrate processed by the method is 346.2 mu m thick, the thickness of the silicon carbide wafer substrate can be reused within the range of 330-370 mu m, the thickness of the silicon carbide wafer processed by the embodiment meets the use requirement, and the side surface of the silicon carbide substrate processed by the method is flat without unevenness and can be reused for many times.
Claims (10)
1. A method for recycling a silicon carbide wafer after etching, the method comprising the steps of:
1) covering a protective layer on the surface to be corroded of the silicon carbide wafer;
2) plating corrosion-resistant layers on the other surfaces of the silicon carbide wafer treated in the step 1);
3) removing the protective layer;
4) corroding the silicon carbide wafer treated in the step 3);
5) observing the defect condition of the silicon carbide wafer;
6) removing the corrosion-resistant layer of the silicon carbide wafer;
7) and removing the corrosion layer on the surface to be corroded of the silicon carbide wafer to obtain the recyclable silicon carbide wafer.
2. The protection method according to claim 1, wherein the protective layer in step 1) is polyimide or photoresist.
3. The protection method according to claim 1 or 2, characterized in that step 2) is specifically: plating a corrosion-resistant layer on the side surface and the other surface opposite to the surface to be corroded of the SiC wafer processed in the step 1).
4. The protection method according to claim 1, wherein the corrosion-resistant layer is an inert metal protective layer.
5. The protection method according to claim 1 or 4, characterized in that the corrosion-resistant layer in step 2) is a nickel layer.
6. The protection method according to claim 1, wherein the method of plating the corrosion-resistant layer in step 2) is: firstly, a seed layer is grown and then a nickel layer is electroplated or a nickel layer is directly electroplated.
7. The protection method according to claim 2, wherein in step 3), when the protective layer is a photoresist, the photoresist development is performed after plating the corrosion-resistant layer in step 2) to remove the protective layer; or, when the protective layer is photoresist, removing the polyimide glue after plating the corrosion-resistant layer in the step 2).
8. The protection method according to claim 1, characterized in that the corrosion in step 4) is in particular: corroding the silicon carbide wafer treated in the step 3) by using high-temperature alkaline molten liquid.
9. The protection method according to claim 1, wherein step 6) includes chamfering to remove the corrosion-resistant layer of the side face of the silicon carbide wafer and CMP to remove the corrosion-resistant layer of the other surface opposite to the face to be corroded.
10. The protection method according to claim 1, wherein step 7) is specifically: and removing the corrosion layer on the surface to be corroded of the silicon carbide wafer by CMP.
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| US6406923B1 (en) * | 2000-07-31 | 2002-06-18 | Kobe Precision Inc. | Process for reclaiming wafer substrates |
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| US20040112866A1 (en) * | 2002-12-06 | 2004-06-17 | Christophe Maleville | Method for recycling a substrate |
| CN102044428A (en) * | 2009-10-13 | 2011-05-04 | 中芯国际集成电路制造(上海)有限公司 | Method for thinning wafer |
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| CN111261496A (en) * | 2018-11-30 | 2020-06-09 | 有研半导体材料有限公司 | Acid corrosion processing method of large-diameter substrate wafer suitable for single-side polishing |
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| US6406923B1 (en) * | 2000-07-31 | 2002-06-18 | Kobe Precision Inc. | Process for reclaiming wafer substrates |
| EP1427001A1 (en) * | 2002-12-06 | 2004-06-09 | S.O.I. Tec Silicon on Insulator Technologies S.A. | A method for recycling a surface of a substrate using local thinning |
| US20040112866A1 (en) * | 2002-12-06 | 2004-06-17 | Christophe Maleville | Method for recycling a substrate |
| CN102044428A (en) * | 2009-10-13 | 2011-05-04 | 中芯国际集成电路制造(上海)有限公司 | Method for thinning wafer |
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