CN115287071B - C-free high-selectivity silicon nitride etching solution - Google Patents
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Abstract
The invention discloses a C-free high-selectivity silicon nitride etching solution, which mainly comprises inorganic acid, inorganic silicon compound, pre-solvent, inorganic dispersing agent and water.
Description
Technical Field
The invention belongs to the field of electronic chemicals, and in particular relates to a C-free high-selectivity silicon nitride etching solution and a preparation method thereof
Background
With the rapid increase of the global data volume, planar NAND flash memory has approached its practical expansion limit, and each large memory vendor has been developing toward 3D NAND with higher storage capacity, and 3D NAND technology has increased in multiple times as compared with planar NAND storage capacity.
In the NAND manufacturing process of the planar structure, the silicon nitride layer is covered on the silicon oxide layer, phosphoric acid contacts the silicon nitride during etching, the silicon oxide layer contacts the phosphoric acid after the silicon nitride layer is completely etched, and the etching rate of the phosphoric acid to the silicon oxide is slow. So that the effect of phosphoric acid on the silicon oxide layer is negligible as long as the etching time is controlled. However, in the 3D NAND process, the silicon nitride layer and the silicon oxide layer are alternately laminated, phosphoric acid etches silicon nitride from the side, the silicon nitride layer and the silicon oxide layer are simultaneously contacted with phosphoric acid, and the common phosphoric acid etches the silicon nitride layer and the silicon oxide layer at the same time. Therefore, the etching liquid is required to have high selectivity to the silicon nitride layer, and the silicon nitride layer is etched while the silicon oxide layer is hardly etched.
The high selectivity silicon nitride etching solutions disclosed in the prior art have more or less drawbacks: the etching solution disclosed in the series of patent CN111925796-CN111925805 comprises: the silicon-containing additive, phosphoric acid and water, wherein the silicon-containing additive belongs to organic silicon; the etching solution disclosed in KR1020160111073 comprises: the fluorine silicon compound, the organic sulfonic acid imine adsorption inhibitor, the organic polymer adsorbent and the aqueous silicon nitride etchant also contain more organic components.
With the increase of the number of layers of the 3D NAND structure, the etching process time of the silicon nitride is continuously increased, and the problems of repeated utilization of liquid medicine and the like are considered, wherein the etching solution needs to be kept at a high temperature (150 ℃/160 ℃) for tens of hours to hundreds of hours, the typical etching solution in the prior art is prepared by adding an organic additive into phosphoric acid, and the serious problems of discoloration (deterioration) of the etching solution, rapid increase of C-containing colloid residues on a wafer, increase of the number of particles in the etching solution and the like are caused by the strong dehydration property of the high-temperature phosphoric acid due to the prolonged etching time.
Disclosure of Invention
The invention provides a C-free high-selectivity silicon nitride etching solution and a preparation method thereof, aiming at the defects that when the existing etching solution is used for selectively etching silicon nitride and silicon dioxide, the service life of the etching solution is short due to more particles and precipitates in the solution in a short time in the process, colloid residues appear on a wafer after etching, and discoloration appears when the etching solution is used for a long time.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
the etching liquid is an electronic grade product, and comprises the main components of inorganic acid accounting for 50-90% of the etching liquid by mass, inorganic silicon compound accounting for 0.1-3% of the etching liquid by mass, pre-solvent accounting for 0.3-5% of the etching liquid by mass, inorganic dispersant accounting for 0.01-0.5% of the etching liquid by mass, and water accounting for the rest.
In the above scheme, the etching solution preferably comprises the following components in percentage by weight: 70-90% of inorganic acid, 0.2-2% of inorganic silicon compound, 0.4-4% of pre-solvent, 0.01-0.4% of inorganic dispersant and the balance of water.
In the above scheme, the etching solution more preferably comprises the following components: 84-90% of inorganic acid, 0.5-1.5% of inorganic silicon compound, 1-3% of pre-solvent, 0.01-0.2% of inorganic dispersant and the balance of water.
In the above scheme, the inorganic acid is a high boiling point acid.
In the scheme, the high boiling point acid is one or a combination of more of phosphoric acid and sulfuric acid.
In the above scheme, the high boiling point acid is preferably phosphoric acid.
In the scheme, the general formula of the inorganic silicon compound is as follows;
wherein X is 1 -X 8 Is halogen, n is a natural number from 0 to 5, such as a natural number of 0, 1, 2, 3, 4, or 5.
X in the general formula of the inorganic silicon compound 1 -X 8 Preferably Cl, n is preferably a natural number of 0 to 2, such as 0, 1, or 2, more preferably 0 or 1.
In the scheme, the pre-solvent is one or a combination of more than 98% of phosphoric acid, more than 96% of sulfuric acid, anhydrous phosphorous acid and anhydrous hypophosphorous acid.
In the above scheme, the pre-solvent is preferably phosphoric acid with a concentration of more than 98% or sulfuric acid with a concentration of more than 96%.
In the scheme, the mass ratio of the inorganic silicon compound to the pre-solvent is 1:1-1:5.
In the scheme, the inorganic dispersing agent is one or a combination of more of ammonium tripolyphosphate, ammonium hexametaphosphate and ammonium pyrophosphate.
In the above scheme, the water is one of ultrapure water, deionized water or distilled water with resistivity of 15-18MΩ cm at 25deg.C.
In the above scheme, the high selectivity means that the etching selectivity ratio of the etching solution to the silicon nitride and the silicon dioxide is more than 500.
In the scheme, the total carbon TC content of the etching solution without C is less than 20ppm.
In the scheme, the etching solution has high-temperature stability, and when the temperature of the etching solution is more than 150 ℃ and the etching solution is maintained for more than 40 hours, the chromaticity change of the etching solution is less than 30Hazen.
In the scheme, the etching solution has high-temperature stability, and when the temperature of the etching solution is more than 160 ℃ and is maintained for more than 50 hours, the chromaticity change of the etching solution is less than 30Hazen.
In the above scheme, the method for disposing the etching solution includes the following steps:
(1) Weighing proper pre-solvent and inorganic silicon compound in proportion;
(2) Adding inorganic silicon compound into the pre-solvent, mixing uniformly, heating to 80-100 ℃ under stirring, condensing and refluxing state, keeping for 40-60 minutes, cooling and storing for standby;
(3) Adding an inorganic dispersing agent into inorganic acid, and uniformly mixing for later use;
(4) Adding the mixture in the step 2 into the mixture in the step 3, and uniformly mixing to prepare the C-free high-selectivity silicon nitride etching solution
The reagents and materials used in the present invention are commercially available.
The beneficial effects of the invention are that
1. The inorganic silicon compound in the high-selectivity SiN etching solution can be well dissolved in inorganic acid under the action of a pre-solvent, and is different from a common surfactant which has hydrophilic and lipophilic different parts with amphiphilicity. The filter element is not blocked due to the generation of foam during stirring or turbulence, and adverse effects such as influencing the etching effect of the bottom layer of the structure are avoided.
2. The high-selectivity silicon nitride etching solution does not contain organic components and C element, does not generate color change or organic carbonization due to strong dehydration of high-temperature phosphoric acid/sulfuric acid in the long-time heating use process, and has good high-temperature stability. No colloid residue phenomenon appears on the wafer after the silicon nitride etching is completed.
3. The high-selectivity silicon nitride etching solution also contains an inorganic dispersing agent, and the etching effect is not affected under normal conditions, but if the etched wafer contains photoresist residues, the inorganic dispersing agent in the high-selectivity silicon nitride etching solution can reduce colloid residues on the wafer and plays a foolproof role.
Drawings
Fig. 1 is an optical image of a wafer without gum residue.
Fig. 2 is an optical image of a wafer with gum residue.
Fig. 3 is an SEM image of a wafer without gum residue.
Fig. 4 is an SEM image of gum residue on a wafer.
Detailed Description
For a better understanding of the present invention, the following examples are further illustrated, but are not limited to the following examples.
The inorganic silicon compounds described herein may be represented by chemical formulas (1) to (3) in some embodiments, but these are merely examples, and the inventive concept is not limited thereto.
Chemical formula (1):
hexachlorodisiloxane (CAS: 14986-21-1)
Chemical formula (2):
octachlorotrisiloxane (CAS: 31323-44-1)
Chemical formula (3):
ten-chloro-tetrasiloxane (CAS: 56240-64-3)
The organosilicon compound in the comparative example may be represented by the formulae (4) to (5)
Chemical formula (4):
hexamethyldisiloxane (CAS: 107-46-0)
Chemical formula (5):
hexaethyldisiloxane (CAS: 994-49-0)
Examples 1 to 12
The contents of the components according to the examples and comparative examples contemplated by the present invention are shown in Table 1, with the balance being water.
TABLE 1
The above examples 1 to 12 and comparative examples 1 to 5 were each configured as follows:
(1) Sampling according to the proportion in the table for standby;
(2) Adding inorganic silicon compound (or organic silicon compound) into the pre-solvent, uniformly mixing, heating to 80 ℃ under stirring, condensing and refluxing state, keeping for 60 minutes, cooling and storing for standby;
(3) Adding inorganic dispersant (if any) into inorganic acid, and uniformly mixing for later use;
(4) And (3) adding the mixture in the step (2) into the mixture in the step (3), and uniformly mixing to prepare the C-free high-selectivity silicon nitride etching solution.
The method for detecting the etching rate is carried out in the following manner:
etching object: silicon nitride film and silicon oxide film (thickness of about 1000A and 300A, respectively)
Etching temperature: 160 ℃ +/-1 ℃.
Etching container: quartz groove.
Etching time: the silicon nitride film was etched for 300 seconds, and the silicon oxide film was etched for 7200 seconds. .
The etching rate measuring method comprises the following steps: the film thicknesses of the silicon nitride film and the silicon oxide film were measured before etching and after etching using an ellipsometer, and the etching rate was calculated by dividing the difference between the initial thickness and the thickness after etching by the etching time (minutes). The selectivity represents the ratio of the silicon nitride film etching rate to the silicon oxide film etching rate.
The residual number measuring method comprises the following steps: immersing the silicon oxide film layer residue in 160 ℃ etching solution for 300 seconds, taking out, washing with water, cleaning with SC1, drying with IPA, scanning with a microscopic optical detector, and analyzing the particle residue number of the surface unit area of the wafer with software.
The chromaticity detection method comprises the following steps: after the etching solutions of examples and comparative examples were kept at 160℃for 50 hours, the samples were cooled and the chromaticity of the solutions was measured by using a single wavelength chromaticity detection method of ultraviolet-visible spectrophotometer at 455 nm.
The results of the etching and heating experiments performed with the high selectivity silicon nitride etching solutions formulated in various combinations according to the embodiments of the present invention are shown in table 2.
TABLE 2
Note that: the initial chromaticity of the etching solution is less than 1.
In examples 1-12, the technical effects achieved are the same as those of fig. 1 and 3, namely, the optical pictures and SEM pictures of the wafer without gum residue. Comparative examples 1-3 contained relatively little gum residue, as shown in FIGS. 2 and 4.
Comparing the above examples with the comparative examples, the data shows that, compared with the organic silicon additive, the silicon oxide inorganic additive used in the invention can ensure that the whole high-selectivity silicon nitride etching solution belongs to a C-free system, has obvious advantages in the aspect of high temperature resistance, the temperature of the etching solution is above 160 ℃, and the chromaticity change of the etching solution is less than 30Hazen when the temperature of the etching solution is maintained for more than 50 hours; meanwhile, the silicon oxide inorganic additive added in the invention can improve the effective silicon concentration in the solution, reduce the etching rate of phosphoric acid to silicon oxide, thereby improving the etching selectivity to silicon nitride, and the etching solution is an inorganic system, so that the phenomenon of colloid residue on a wafer due to the strong dehydration of high-temperature phosphoric acid/sulfuric acid in the use process is avoided. The addition of the pre-solvent can enable the inorganic silicon compound to be well dissolved in the inorganic acid to form a uniform system; the inorganic dispersant does not bring in the organic component, and can also play a role in reducing loss when the organic component is mixed in the etching system.
It is apparent that the above examples are only examples made for the sake of clarity and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. And thus obvious variations or modifications to the disclosure are within the scope of the invention.
Claims (5)
1. The C-free high-selectivity silicon nitride etching solution is characterized in that the etching solution is an electronic grade product, the components of the etching solution are phosphoric acid accounting for 82-85% of the etching solution by mass percent and used as inorganic acid, inorganic silicon compounds accounting for 0.5-1.5% of the etching solution by mass percent, pre-solvent accounting for 1-3% of the etching solution by mass percent, inorganic dispersing agent accounting for 0.05-0.15% of the etching solution by mass percent, and the balance of water, wherein the inorganic silicon compounds have the general formula of;
wherein X is 1 -X 8 Selected from Cl, n is a natural number of 0-2, the inorganic dispersant is ammonium tripolyphosphate or ammonium hexametaphosphate, and the pre-solvent is phosphoric acid with concentration of more than 98% or sulfuric acid with concentration of more than 96%.
2. The C-free high selectivity silicon nitride etching solution according to claim 1, wherein the mass ratio of the inorganic silicon compound to the pre-solvent is 1:1 to 1:5.
3. The C-free high selectivity silicon nitride etching solution according to claim 1, wherein the water is one of ultrapure water, deionized water or distilled water having a resistivity of 15 to 18mΩ×cm at 25 ℃.
4. The C-free high selectivity silicon nitride etching solution according to claim 1, wherein the C-free etching solution has a total carbon TC content of < 20ppm.
5. The C-free high selectivity silicon nitride etching solution according to claim 1, wherein the method for disposing the etching solution comprises the steps of:
(1) Weighing proper pre-solvent and inorganic silicon compound in proportion;
(2) Adding inorganic silicon compound into the pre-solvent, mixing uniformly, heating to 80-100 ℃ under stirring, condensing and refluxing state, keeping for 40-60 minutes, cooling and storing for standby;
(3) Adding an inorganic dispersing agent into inorganic acid, and uniformly mixing for later use;
(4) And (3) adding the mixture in the step (2) into the mixture in the step (3), and uniformly mixing to prepare the C-free high-selectivity silicon nitride etching solution.
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| CN202210790396.9A CN115287071B (en) | 2022-07-06 | 2022-07-06 | C-free high-selectivity silicon nitride etching solution |
| PCT/CN2023/083354 WO2024007627A1 (en) | 2022-07-06 | 2023-03-23 | C-free high-selectivity silicon nitride etching solution |
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| CN109689838A (en) * | 2016-12-26 | 2019-04-26 | 秀博瑞殷株式公社 | Etching composition and the method for using the etching composition manufacturing semiconductor devices |
| CN110804441A (en) * | 2019-11-08 | 2020-02-18 | 湖北兴福电子材料有限公司 | Phosphoric acid etching solution for inhibiting silicon dioxide etching |
| CN110846040A (en) * | 2019-11-08 | 2020-02-28 | 湖北兴福电子材料有限公司 | High-silicon-content phosphate etching solution and preparation method thereof |
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| JP2021086943A (en) * | 2019-11-28 | 2021-06-03 | 花王株式会社 | Etching liquid |
| CN114250077A (en) * | 2020-09-21 | 2022-03-29 | 易安爱富科技有限公司 | Silicon nitride film etching composition and etching method using the same |
| CN114369461A (en) * | 2021-12-09 | 2022-04-19 | 湖北兴福电子材料有限公司 | High-selectivity etching solution for aluminum nitride and silicon |
| CN114621769A (en) * | 2020-12-11 | 2022-06-14 | 安集微电子（上海）有限公司 | Etching composition and application thereof |
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| JP5302551B2 (en) * | 2008-02-28 | 2013-10-02 | 林純薬工業株式会社 | Silicon anisotropic etchant composition |
| JP7233252B2 (en) * | 2019-03-07 | 2023-03-06 | 関東化学株式会社 | Silicon nitride etchant composition |
| 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 |
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Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109689838A (en) * | 2016-12-26 | 2019-04-26 | 秀博瑞殷株式公社 | Etching composition and the method for using the etching composition manufacturing semiconductor devices |
| CN110804441A (en) * | 2019-11-08 | 2020-02-18 | 湖北兴福电子材料有限公司 | Phosphoric acid etching solution for inhibiting silicon dioxide etching |
| CN110846040A (en) * | 2019-11-08 | 2020-02-28 | 湖北兴福电子材料有限公司 | High-silicon-content phosphate etching solution and preparation method thereof |
| JP2021086943A (en) * | 2019-11-28 | 2021-06-03 | 花王株式会社 | Etching liquid |
| CN111849487A (en) * | 2020-08-14 | 2020-10-30 | 上海新阳半导体材料股份有限公司 | High-selectivity silicon nitride etching solution, and preparation method and application thereof |
| CN114250077A (en) * | 2020-09-21 | 2022-03-29 | 易安爱富科技有限公司 | Silicon nitride film etching composition and etching method using the same |
| CN114621769A (en) * | 2020-12-11 | 2022-06-14 | 安集微电子（上海）有限公司 | Etching composition and application thereof |
| CN114369461A (en) * | 2021-12-09 | 2022-04-19 | 湖北兴福电子材料有限公司 | High-selectivity etching solution for aluminum nitride and silicon |
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