CN114350366B - Silicon nitride and P-type polycrystalline silicon constant-speed etching solution - Google Patents
Silicon nitride and P-type polycrystalline silicon constant-speed etching solution Download PDFInfo
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- 238000005530 etching Methods 0.000 title claims abstract description 74
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 36
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 33
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 31
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims abstract description 9
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 claims abstract description 8
- 239000003381 stabilizer Substances 0.000 claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229920005591 polysilicon Polymers 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 5
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 4
- AFBPFSWMIHJQDM-UHFFFAOYSA-N N-methylaniline Chemical compound CNC1=CC=CC=C1 AFBPFSWMIHJQDM-UHFFFAOYSA-N 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 229910021645 metal ion Inorganic materials 0.000 claims description 4
- -1 perfluoroalkyl carboxylic acid Chemical class 0.000 claims description 4
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 claims description 3
- ADCBKYIHQQCFHE-UHFFFAOYSA-N 1,3-dimethyl-1,3-diphenylurea Chemical compound C=1C=CC=CC=1N(C)C(=O)N(C)C1=CC=CC=C1 ADCBKYIHQQCFHE-UHFFFAOYSA-N 0.000 claims description 2
- YZEUHQHUFTYLPH-UHFFFAOYSA-N 2-nitroimidazole Chemical compound [O-][N+](=O)C1=NC=CN1 YZEUHQHUFTYLPH-UHFFFAOYSA-N 0.000 claims description 2
- XLAXIIXNAXMBRK-UHFFFAOYSA-N 3-nitrobutan-1-ol Chemical compound [O-][N+](=O)C(C)CCO XLAXIIXNAXMBRK-UHFFFAOYSA-N 0.000 claims description 2
- YISPKQZWSIMXMX-UHFFFAOYSA-N 3-nitropropan-1-ol Chemical compound OCCC[N+]([O-])=O YISPKQZWSIMXMX-UHFFFAOYSA-N 0.000 claims description 2
- QLILRKBRWXALIE-UHFFFAOYSA-N 3-nitropyridine Chemical compound [O-][N+](=O)C1=CC=CN=C1 QLILRKBRWXALIE-UHFFFAOYSA-N 0.000 claims description 2
- LQSJUQMCZHVKES-UHFFFAOYSA-N 6-iodopyrimidin-4-amine Chemical compound NC1=CC(I)=NC=N1 LQSJUQMCZHVKES-UHFFFAOYSA-N 0.000 claims description 2
- ZHZPKMZKYBQGKG-UHFFFAOYSA-N 6-methyl-2,4,6-tris(trifluoromethyl)oxane-2,4-diol Chemical compound FC(F)(F)C1(C)CC(O)(C(F)(F)F)CC(O)(C(F)(F)F)O1 ZHZPKMZKYBQGKG-UHFFFAOYSA-N 0.000 claims description 2
- YPJUNDFVDDCYIH-UHFFFAOYSA-N perfluorobutyric acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)F YPJUNDFVDDCYIH-UHFFFAOYSA-N 0.000 claims description 2
- ZWBAMYVPMDSJGQ-UHFFFAOYSA-N perfluoroheptanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F ZWBAMYVPMDSJGQ-UHFFFAOYSA-N 0.000 claims description 2
- UZUFPBIDKMEQEQ-UHFFFAOYSA-N perfluorononanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F UZUFPBIDKMEQEQ-UHFFFAOYSA-N 0.000 claims description 2
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 claims description 2
- SIDINRCMMRKXGQ-UHFFFAOYSA-N perfluoroundecanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SIDINRCMMRKXGQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 6
- 150000002828 nitro derivatives Chemical class 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000012431 wafers Nutrition 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The invention discloses a constant-speed etching solution for silicon nitride and P-type polycrystalline silicon, which mainly comprises phosphoric acid, a mononitro compound, a nitro stabilizer, a surfactant and water, and can realize that the etching rate ratio of a silicon nitride layer and a P-type polycrystalline silicon layer is stabilized at 1.0 +/-0.1 by controlling the process temperature and adjusting the addition of each component.
Description
Technical Field
The invention belongs to the field of electronic chemicals, and particularly relates to a constant-speed etching solution for silicon nitride and P-type polycrystalline silicon and a preparation method thereof
Background
In the integrated circuit manufacturing process, when a specific grid MOSFET device is prepared, two hard masks of silicon nitride and silicon dioxide need to be respectively deposited on P-type polycrystalline silicon, and after a through hole is etched by a dry method, the P-type polycrystalline silicon and the upper layer of silicon nitride hard mask need to be synchronously etched inwards for a certain depth.
The commonly used silicon nitride etching solution at present is high-temperature phosphoric acid, the etching rate of the high-temperature phosphoric acid to silicon nitride is about 65A/min, and the etching rate to P-type polycrystalline silicon is less than 1A/min; the etching rate of the general etching solution for the polysilicon to the polysilicon is 1000A/s, the etching selection ratio to the silicon nitride is more than 100.
Disclosure of Invention
The invention provides a constant-speed etching solution for silicon nitride and P-type polycrystalline silicon, which solves the problems that the etching appearance is difficult to control and the etching end point is difficult to judge when the silicon nitride and the P-type polycrystalline silicon layer are etched step by step.
In order to realize the purpose of the invention, the technical scheme adopted by the invention is as follows:
the constant-speed etching solution for silicon nitride and P-type polycrystalline silicon is characterized in that the etching solution is an electronic-grade product, and the main components of the etching solution comprise phosphoric acid accounting for 75-88% of the etching solution by mass, 0.01-0.5% of mononitro compound, 0.1-1% of nitro stabilizer, 0.01-0.5% of surfactant and the balance of water.
In the scheme, the phosphoric acid is electronic grade phosphoric acid, the nitrate content is less than 0.05ppm, and the metal ion content is less than 10ppb.
In the scheme, the boiling point of the mononitro compound is more than 160 ℃.
In the scheme, the mononitro compound is one or a mixture of more of 3-nitropyridine, 2-nitroimidazole, 3-nitrobutanol and 3-nitropropanol.
In the above scheme, the nitro stabilizer is one or a mixture of several of N-methylaniline, aniline, N-dimethylaniline and N, N '-dimethyl-N, N' -diphenylurea.
In the above scheme, the surfactant is perfluoroalkyl carboxylic acid selected from at least one of perfluorooctanoic acid, perfluoropentanoic acid, perfluoroheptanoic acid, perfluorobutanoic acid, perfluorononanoic acid, perfluorodecanoic acid, and perfluoroundecanoic acid.
In the scheme, the etching rate ratio of the etching liquid to etch the silicon nitride and the P-type polysilicon is stabilized at 1.0 +/-0.1.
The invention has the advantages of
1. The phosphoric acid in the constant-speed etching solution of the silicon nitride and the P-type polycrystalline silicon is electronic-grade phosphoric acid with nitrate content less than 0.05ppm and metal ion content less than 10ppb, so that the etching rate of the etching solution on the P-type polycrystalline silicon cannot be influenced by the nitrate content and the metal ion content in the phosphoric acid, and the component regulation and control of the etching solution are facilitated.
2. The mononitro compound in the constant-speed etching solution for the silicon nitride and the P-type polycrystalline silicon can improve the etching rate of the etching solution on the P-type polycrystalline silicon without influencing the etching rate of the etching solution on the silicon nitride, so that the etching rate ratio of the etching solution for etching the silicon nitride and the P-type polycrystalline silicon reaches 1:1 or so.
3. The nitro stabilizer in the constant-speed etching solution of the silicon nitride and the P-type polycrystalline silicon can stabilize the oxidation capability of the mononitro compound, so that the mononitro compound can generate long-acting stable controllable oxidation in the etching process, and the etching rate ratio of the etching solution to the silicon nitride to the P-type polycrystalline silicon is stabilized at 1.0 +/-0.1.
4. The constant-speed etching solution for the silicon nitride and the P-type polycrystalline silicon can realize constant-speed etching of the silicon nitride layer and the P-type polycrystalline silicon layer, and the problems that the etching appearance is difficult to control and the etching end point is difficult to judge when two kinds of etching solutions are used for step-by-step etching are solved.
5. The surfactant used in the constant-speed etching solution of the silicon nitride and the P-type polycrystalline silicon ensures that the etching solution has similar wettability (the contact angle difference is less than 2 ℃) to the silicon dioxide hard mask and the silicon substrate, and is favorable for preventing the etching solution from generating difference in etching morphology due to the difference of the upper wettability and the lower wettability when the silicon nitride and the P-type polycrystalline silicon are etched.
Drawings
FIG. 1 is a schematic view of a layered structure of an initial structural layer.
FIG. 2 is a schematic diagram illustrating the etching effect of the etching solution.
FIG. 3 is a photograph showing the contact angle of the etchant to the silicon dioxide layer in example 1.
Fig. 4 is a graph of the contact angle of the etching solution to the silicon substrate in example 1.
FIG. 5 is a photograph showing the contact angle of the etchant with the silicon dioxide layer in comparative example 4.
FIG. 6 is a graph of the contact angle of the etching solution to the silicon substrate in comparative example 4.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Examples 1 to 11:
the contents of the components of examples and comparative examples according to the inventive concept are shown in table 1, and the balance is water.
TABLE 1
The constant-speed etching solution for the silicon nitride and the P-type polycrystalline silicon is prepared by the following steps:
1. taking the raw materials according to the types and the quantities of the raw materials in the table for later use;
2. uniformly mixing a nitro compound and a nitro stabilizer, and adding the mixture into phosphoric acid;
3. adding a surfactant into the mixed solution, uniformly mixing, and ultrasonically dispersing to prepare a constant-speed etching solution of silicon nitride and P-type polycrystalline silicon;
the etching process is carried out according to the following steps:
1. cutting the wafer of the Si3N4 and the P-type polycrystalline silicon into small pieces of 1 x 1cm, washing with water, drying by using nitrogen, and measuring the initial thicknesses of the two wafers by using an ellipsometer;
2. heating the constant-speed etching solution to 158 ℃, etching at the stirring speed of 300r/min, and etching Si3N4 and the P-type polycrystalline silicon for 5min respectively;
3. after etching, the post-etching thicknesses of the two wafers were measured using an ellipsometer after rinsing with water and drying with nitrogen gas immediately, and the etching rates were calculated from the difference between the pre-and post-etching thicknesses and the etching time, and the results are shown in table 2.
TABLE 2
Comparing the above examples and comparative examples, the data shows that the addition of the nitro compound can significantly improve the etching rate of the etching solution to the P-type polysilicon, and by comparing the data of examples 1 and 4, comparative examples 2 and 3, it can be seen that the addition of the nitro stabilizer can effectively stabilize the acceleration effect of the nitro compound on the etching of the P-type polysilicon, which is beneficial to achieving the purpose of stabilizing the etching rate ratio of the silicon nitride layer and the P-type polysilicon layer at 1.0 ± 0.1, and by the data of examples and comparative examples 4, the addition of the perfluoroalkyl carboxylic acid can flatten the difference of the wettability of the etching solution on silicon dioxide and silicon substrate, and by the data of examples 14 and 15, when the low-boiling-point nitro compound is added, because the boiling point of the low-point nitro compound is lower than the working temperature, the volatilization amount of the low-boiling-point nitro compound at the working temperature is increased sharply, and the effect that can be played is unstable and very limited.
It is apparent that the above embodiments are only examples for clearly illustrating and do not limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications are therefore intended to be included within the scope of the invention as claimed.
Claims (4)
1. The constant-speed etching solution for the silicon nitride and the P-type polycrystalline silicon is characterized by being an electronic-grade product, and mainly comprising phosphoric acid accounting for 75-88% of the etching solution by mass, a mononitro compound accounting for 0.01-0.5%, a nitro stabilizer accounting for 0.1-1%, a surfactant accounting for 0.01-0.5% of the etching solution by mass, and the balance of water, wherein the mononitro compound is one or a mixture of more of 3-nitropyridine, 2-nitroimidazole, 3-nitrobutanol and 3-nitropropanol, the nitro stabilizer is one or a mixture of more of N-methylaniline, aniline, N, N-dimethylaniline and N, N '-dimethyl-N, N' -diphenylurea, and the surfactant is perfluoroalkyl carboxylic acid.
2. The etching solution of silicon nitride and P-type polysilicon in constant velocity as claimed in claim 1, wherein the phosphoric acid is electronic grade phosphoric acid, nitrate content is less than 0.05ppm, and metal ion content is less than 10ppb.
3. The etching solution of claim 1, wherein the perfluoroalkyl carboxylic acid is at least one selected from the group consisting of perfluorooctanoic acid, perfluoropentanoic acid, perfluoroheptanoic acid, perfluorobutanoic acid, perfluorononanoic acid, perfluorodecanoic acid, and perfluoroundecanoic acid.
4. The constant-speed etching solution for silicon nitride and P-type polysilicon according to claim 1, wherein the etching rate ratio of the etching solution to etch silicon nitride and P-type polysilicon is stabilized at 1.0 ± 0.1.
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