CN114621769A - Etching composition and application thereof - Google Patents
Etching composition and application thereof Download PDFInfo
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- CN114621769A CN114621769A CN202011443394.XA CN202011443394A CN114621769A CN 114621769 A CN114621769 A CN 114621769A CN 202011443394 A CN202011443394 A CN 202011443394A CN 114621769 A CN114621769 A CN 114621769A
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- etching composition
- etching
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- 238000005530 etching Methods 0.000 title claims abstract description 74
- 239000000203 mixture Substances 0.000 title claims abstract description 51
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 27
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 27
- -1 silane compound Chemical class 0.000 claims abstract description 25
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 18
- 239000010703 silicon Substances 0.000 claims abstract description 18
- 229910000077 silane Inorganic materials 0.000 claims abstract description 14
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 13
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 12
- 239000010452 phosphate Substances 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 125000003545 alkoxy group Chemical group 0.000 claims description 9
- 125000000217 alkyl group Chemical group 0.000 claims description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- 238000001039 wet etching Methods 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 125000002431 aminoalkoxy group Chemical group 0.000 claims description 2
- 239000003945 anionic surfactant Substances 0.000 claims description 2
- 125000000051 benzyloxy group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])O* 0.000 claims description 2
- 125000005243 carbonyl alkyl group Chemical group 0.000 claims description 2
- 239000003093 cationic surfactant Substances 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 claims description 2
- 239000002270 dispersing agent Substances 0.000 claims description 2
- 239000003112 inhibitor Substances 0.000 claims description 2
- 239000002736 nonionic surfactant Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 27
- 229910052814 silicon oxide Inorganic materials 0.000 abstract description 27
- 239000002245 particle Substances 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 239000004065 semiconductor Substances 0.000 abstract description 5
- 239000000758 substrate Substances 0.000 abstract description 5
- 150000004767 nitrides Chemical class 0.000 description 8
- 230000008859 change Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical group N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical group [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000005380 borophosphosilicate glass Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Chemical group 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Chemical group 0.000 description 1
- 239000011593 sulfur Chemical group 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
- C09K13/06—Etching, surface-brightening or pickling compositions containing an inorganic acid with organic material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02008—Multistep processes
- H01L21/0201—Specific process step
- H01L21/02019—Chemical etching
Abstract
The invention provides an etching composition and application thereof. It includes: phosphoric acid, a silane compound, a silicon-based phosphate compound and deionized water. The etching composition can selectively etch silicon nitride and minimally etch silicon oxide, solves the problem of silicon oxide regrowth, avoids forming particles on a substrate, has a large operation window, and has a good application prospect in a semiconductor high-temperature etching process.
Description
Technical Field
The invention relates to the field of compositions for etching semiconductor components, in particular to a composition for etching silicon nitride and an application method thereof.
Background
In a semiconductor manufacturing process, a nitride layer and an oxide layer have been used as an insulating layer of a stack structure of a 3D-NAND flash memory gate, of which a silicon nitride layer (SiN) is representativex) And a silicon oxide layer (SiO)2) The insulating layers may be formed independently or alternately stacked on each other. In addition, the silicon oxide layer and the silicon nitride layer may also be used as hard masks to form metalsAn interconnected conductive pattern.
A wet etch process may be used to remove the nitride layer, wherein the selectivity of the etchant is an important consideration. An ideal etchant needs to have a high selectivity for the etch rate of the layer being etched much greater than the etch rate of the other layers. In a wet etching process for removing a nitride film, a mixture of phosphoric acid and deionized water is generally used. The deionized water is used to prevent the decrease in the etching rate of the nitride film and the change in the etching selectivity of the nitride film with respect to the silicon oxide film. However, even if the amount of deionized water is finely changed, the nitride film etching process may still fail and the operating window is small. Further, phosphoric acid, which is one of strong acids, is corrosive, and thus it is difficult to perform subsequent treatment.
To overcome this drawback of conventional etching compositions, the prior art proposes to include a composition comprising hydrofluoric acid (HF) and nitric acid (HNO)3) Phosphoric acid (H) mixed with one of (1)3PO4) The etching composition of (1). However, this etching composition deteriorates the etching selectivity of the nitride layer and the oxide layer. In addition to this, another etching composition comprising phosphoric acid and one of silicate and silicic acid is proposed. However, silicates and silicic acid produce particles that can seriously affect the substrate material.
In order to solve the above problems, CN103160282B discloses an etching composition containing a silyl phosphate compound, which, although it can selectively etch a nitride film with respect to an oxide film without causing problems such as generation of particles, has low selectivity to LP-TEOS and may have a silicon oxide regrowth problem. US9368647B2 discloses an etching composition containing a silicon compound (containing at least one atom of nitrogen, phosphorus and sulfur bonded to silicon), but this composition requires the addition of an additional ammonium ion, which complicates the system and, at the same time, increases the etching rate of silicon nitride and silicon oxide, which may result in a decrease in the etching selectivity of silicon nitride to silicon oxide. CN105273718B discloses an etching composition containing a silane phosphate compound, which requires the synthesis of the silane phosphate compound first and has low selectivity to BPSG. CN109689838A discloses an etching composition containing a silane compound having an alkoxy group, but it is sensitive to the silicon concentration in the solution.
Disclosure of Invention
It is an object of the present invention to provide an etching composition that can be used for highly selective removal of silicon nitride, which can minimize the silicon oxide etching rate while highly selectively removing silicon nitride while avoiding silicon oxide regrowth and formation of substrate particles.
Specifically, the present invention provides an etching composition comprising: phosphoric acid, a silane compound, a silicon-based phosphate compound and deionized water.
Preferably, the silane compound has the general formula:
wherein R is1To R4Are respectively selected from hydrogen, hydroxyl and (C)1-C10) Alkyl, (C)1-C10) Alkoxy group, (C)1-C10) Aminoalkyl radical, (C)1-C10) Aminoalkoxy, (C)1-C10) Carbonylalkyl, (C)1-C10) Isocyanatoalkyl, (C)1-C10) Ureidoalkyl, (C)1-C10) One or more of dithiocarbonate alkyl groups; r1To R4At least one of (A) is (C)1-C10) Isocyanatoalkyl, (C)1-C10) Ureidoalkyl, (C)1-C10) One of dithiocarbonate alkyl groups.
Preferably, the mass percentage concentration of the silane compound is 0.1-1%.
Preferably, the silicon-based phosphate compound has the general formula:
wherein i) R5To R7Are respectively selected from hydrogen, hydroxyl and (C)1-C10) Alkyl, (C)1-C10) One or more of alkoxy groups;
ii)R8is selected from (C)1-C10) Alkyl, (C)1-C10) One of alkoxy groups;
iii)R9is selected from (C)1-C10) Alkyl, (C)1-C10) One of alkoxy groups;
iv)R10one selected from hydroxyl, ammonium oxy and benzyloxy.
Preferably, the mass percentage concentration of the silicon-based phosphate ester compound is 0.01-5%.
Preferably, the mass percentage concentration of the phosphoric acid is 80-99.8%.
Preferably, the mass percentage concentration of the deionized water is 0.01-19.89%.
Preferably, the etching composition further comprises one or more additives selected from the group consisting of surfactants, dispersants, and corrosion inhibitors; wherein the surfactant is selected from one or more of cationic surfactant, anionic surfactant and nonionic surfactant.
In another aspect of the invention there is provided the use of an etching composition as described in any of the above for wet etching silicon nitride.
Compared with the prior art, the invention has the positive improvement effects that:
the silane compound contained in the etching composition disclosed by the invention does not contain halogen, so that the silicon nitride film can be removed at high selectivity while the silicon oxide etching rate is minimized, and meanwhile, the problems of silicon oxide regrowth, particle formation on a substrate and the like are solved. The etching composition disclosed by the invention has a larger operation window and has a good application prospect in a semiconductor high-temperature etching process.
Detailed Description
The advantages of the invention are further illustrated below with reference to specific examples.
Etching compositions of examples 1 to 12 and comparative examples 1 to 6 were prepared according to the components and contents described in table 1. The reagents and raw materials used in the invention are commercially available, wherein the phosphoric acid is 85% phosphoric acid aqueous solution. The composition of the invention can be prepared by simply and uniformly mixing the components.
TABLE 1 Components and amounts of compositions of examples 1-12 and comparative examples 1-6
In order to investigate the etching rates of the composition on silicon oxide and silicon nitride and the etching selection ratio of the composition on the silicon oxide and the silicon nitride, the invention adopts the following technical means: the etching composition liquid was heated to 160 ℃ in a reactor, and then a silicon nitride film was placed in each composition to be etched for 10min, and then the change in thickness before and after etching was measured by an ellipsometer to calculate the etching rate. Each etching composition was heated to 160 ℃ in a reactor, and a silicon oxide film was placed therein and etched for 60min, and then the change in thickness before and after etching was measured by a non-metal film thickness tester to calculate the etching rate. The etch selectivity ratio of the etch rate of silicon nitride to the etch rate of silicon oxide was calculated. The etch rates and etch selectivity of the compositions for silicon nitride and silicon oxide are shown in table 2.
TABLE 2 etching rates and selectivity ratios of etching compositions of examples 1 to 12 and comparative examples 1 to 6
As can be seen from table 2: the etching combination liquid can selectively etch and remove silicon nitride, simultaneously, the etching rate of silicon oxide is minimized, and the operation window is larger.
As can be seen from the comparison of comparative example 1 with example 1, selective removal of silicon nitride was not achieved using pure phosphoric acid. As can be seen from comparison of comparative examples 3, 4, 5 and 6 with examples 4, 8 and 11, the addition of the silane compound or the silicon-based phosphate compound alone has no great effect on the etching of silicon nitride, but none of them can effectively suppress the etching of silicon oxide. Therefore, the etching selection ratio of the singly added silane compound or the silicon-based phosphate compound to silicon nitride and silicon oxide is lower than the effect of compounding the silane compound and the silicon-based phosphate compound.
To further determine the silicon content increasing loading of the etching composition of the present invention, a silicon nitride film and a silicon oxide film were separately dissolved in a part of the etching composition prepared as described above and the silicon concentration in the solution was increased. The specific technical means is as follows: the etching composition liquid of the present embodiment was placed in a reactor and heated to 160 c, and when the silicon concentration in the solution was 0ppm, 60ppm, 120ppm and 180ppm, respectively, a silicon nitride film was placed therein and etched for 10min, and then the change in thickness before and after etching was measured by an ellipsometer to calculate the etching rate. Under the same conditions and silicon concentration, a silicon oxide film was left to etch for 60min, and then the change in thickness before and after etching was measured by a non-metal film thickness tester to calculate the etching rate, and further the etching selectivity of the etching rate of silicon nitride to that of silicon oxide was calculated. The etching rates of the etching composition liquid of the present invention for silicon nitride and silicon oxide and the etching selectivity for both are shown in table 3.
Table 3 test results of example 4 and example 8
As can be seen from table 3, the etching composition of the present invention can etch silicon nitride with high selectivity at a silicon content of 120ppm and an etch selectivity of 2066.67 for silicon nitride and silicon oxide. Thus, the etching composition of the invention can have a silicon content increase loading of greater than 120 ppm.
In summary, the etching composition of the present invention provides an etching composition for selectively removing silicon nitride and minimizing the etching rate of silicon oxide, which solves the problem of silicon oxide regrowth, and simultaneously avoids forming particles on the substrate, and has a large operation window and good application prospect in the semiconductor high-temperature etching process.
It should be understood that% referred to in this invention are units of mass percent.
It should be noted that the embodiments of the present invention have been described in terms of preferred embodiments, and not by way of limitation, and that those skilled in the art can make modifications and variations of the embodiments described above without departing from the spirit of the invention.
Claims (9)
1. An etching composition characterized by containing, in an organic solvent,
the method comprises the following steps: phosphoric acid, a silane compound, a silicon-based phosphate compound and deionized water.
2. The etching composition of claim 1,
the silane compound has the general formula:
wherein R is1To R4Are respectively selected from hydrogen, hydroxyl and (C)1-C10) Alkyl, (C)1-C10) Alkoxy group, (C)1-C10) Aminoalkyl radical, (C)1-C10) Aminoalkoxy, (C)1-C10) Carbonylalkyl, (C)1-C10) Isocyanatoalkyl, (C)1-C10) Ureidoalkyl, (C)1-C10) One or more dithiocarbonic acid alkyl groups;
R1to R4At least one of (A) is (C)1-C10) Isocyanatoalkyl, (C)1-C10) Ureidoalkyl, (C)1-C10) One of dithiocarbonate alkyl groups.
3. The etching composition of claim 1,
the mass percentage concentration of the silane compound is 0.1-1.0%.
4. The etching composition of claim 1,
the general formula of the silicon-based phosphate compound is as follows:
wherein i) R5To R7Are respectively selected from hydrogen, hydroxyl and (C)1-C10) Alkyl, (C)1-C10) One or more of alkoxy groups;
ii)R8is selected from (C)1-C10) Alkyl, (C)1-C10) One of alkoxy groups;
iii)R9is selected from (C)1-C10) Alkyl, (C)1-C10) One of alkoxy groups;
iv)R10one selected from hydroxyl, ammonium oxy and benzyloxy.
5. The etching composition of claim 1,
the mass percentage concentration of the silicon-based phosphate compound is 0.01-5.0%.
6. The etching composition of claim 1,
the phosphoric acid is 80-99.8% in mass percentage concentration.
7. The etching composition of claim 1,
the mass percentage concentration of the deionized water is 0.01-19.89%.
8. The etching composition of claim 1,
the etching composition further comprises one or more additives selected from the group consisting of surfactants, dispersants, and corrosion inhibitors;
wherein the surfactant is selected from one or more of cationic surfactant, anionic surfactant and nonionic surfactant.
9. Use of an etching composition as claimed in any one of claims 1 to 8 for wet etching silicon nitride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011443394.XA CN114621769A (en) | 2020-12-11 | 2020-12-11 | Etching composition and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011443394.XA CN114621769A (en) | 2020-12-11 | 2020-12-11 | Etching composition and application thereof |
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| Publication Number | Publication Date |
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| CN114621769A true CN114621769A (en) | 2022-06-14 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115011350A (en) * | 2022-07-05 | 2022-09-06 | 上海集成电路材料研究院有限公司 | Etching composition, etching method and application |
| CN115287071A (en) * | 2022-07-06 | 2022-11-04 | 湖北兴福电子材料有限公司 | C-free high-selectivity silicon nitride etching solution |
-
2020
- 2020-12-11 CN CN202011443394.XA patent/CN114621769A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115011350A (en) * | 2022-07-05 | 2022-09-06 | 上海集成电路材料研究院有限公司 | Etching composition, etching method and application |
| CN115287071A (en) * | 2022-07-06 | 2022-11-04 | 湖北兴福电子材料有限公司 | C-free high-selectivity silicon nitride etching solution |
| CN115287071B (en) * | 2022-07-06 | 2023-08-25 | 湖北兴福电子材料股份有限公司 | C-free high-selectivity silicon nitride etching solution |
| WO2024007627A1 (en) * | 2022-07-06 | 2024-01-11 | 湖北兴福电子材料股份有限公司 | C-free high-selectivity silicon nitride etching solution |
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