CN115287071A - 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, an inorganic silicon compound, a pre-solvent, an inorganic dispersant and water.
Description
Technical Field
The invention belongs to the field of electronic chemicals, and particularly relates to a C-free high-selectivity silicon nitride etching solution and a preparation method thereof
Background
With the dramatic increase of global data volume, NAND flash memories with planar structure are approaching to their practical expansion limit, and various large memory manufacturers are moving to 3D NAND with higher storage capacity, and 3D NAND technology is multiplied compared with NAND storage capacity with planar structure.
In the NAND manufacturing process of the planar structure, the silicon nitride layer covers the silicon oxide layer, phosphoric acid contacts the silicon nitride layer firstly during etching, the silicon oxide layer is contacted with the phosphoric acid after the silicon nitride layer is completely etched, and the etching rate of the phosphoric acid to the silicon oxide is very slow. The effect of phosphoric acid on the silicon oxide layer is negligible as long as the etching time is controlled well. However, in the 3D NAND process, the silicon nitride layer and the silicon oxide layer are alternately stacked, phosphoric acid etches silicon nitride from the side, the silicon nitride layer and the silicon oxide layer are simultaneously in contact with phosphoric acid, and ordinary phosphoric acid etches the silicon nitride layer and also etches the silicon oxide layer. Therefore, it is necessary that the etching solution has high selectivity to the silicon nitride layer and hardly etches the silicon oxide layer while etching the silicon nitride layer.
The high-selectivity silicon nitride etching solution disclosed in the prior literature has more or less some defects: the etching solution disclosed in serial patent CN111925796-CN111925805 comprises: the silicon-containing additive comprises silicon-containing additive, phosphoric acid and water, wherein the silicon-containing additive is organosilicon; patent KR1020160111073 discloses an etching solution comprising: fluorosilicone compounds, organic sulfonic acid imine adsorption inhibitors, organic polymer adsorbents, and aqueous silicon nitride etchants also contain a large amount of organic components.
With the increase of the number of layers of the 3D NAND structure, the time of a silicon nitride etching process is continuously increased, and in consideration of the problems of recycling of liquid medicine and the like, the etching solution needs to be kept for tens of hours or even hundreds of hours at a high temperature (150 ℃/160 ℃), typical etching solutions in the prior art are all formed by adding organic additives into phosphoric acid, and due to the fact that the etching time is prolonged, the typical etching solutions in the prior art have serious problems that due to the strong dehydration property of high-temperature phosphoric acid, the etching solution is discolored (deteriorated), the residual of colloid containing C on a wafer is increased sharply, the number of particles in the etching solution is increased, and the like.
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, more particles and precipitates in the solution in a short time in the process cause short service life of the etching solution, colloidal residues appear on a wafer after etching, and discoloration appears after long-time use.
In order to achieve the purpose, the invention adopts the technical scheme that:
the C-free high-selectivity silicon nitride etching solution is an electronic grade product, and mainly comprises 50-90% of inorganic acid, 0.1-3% of inorganic silicon compound, 0.3-5% of pre-solvent, 0.01-0.5% of inorganic dispersant and the balance of water by mass percent.
In the above scheme, the etching solution preferably comprises the following components: 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 preferably contains the following components: the mass fraction of the inorganic acid is 84-90%, the mass fraction of the inorganic silicon compound is 0.5-1.5%, the mass fraction of the pre-solvent is 1-3%, the mass fraction of the inorganic dispersant is 0.01-0.2%, and the balance is water.
In the scheme, the inorganic acid is a high-boiling-point acid.
In the scheme, the high-boiling-point acid is one or a combination of phosphoric acid and sulfuric acid.
In the above scheme, the high boiling point acid is preferably phosphoric acid.
In the above scheme, the general formula of the inorganic silicon compound is;
wherein, X 1 -X 8 Is halogen, n isA 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 from 0 to 2, such as 0, 1, or 2, more preferably 0 or 1.
In the above scheme, the pre-solvent is one or a combination of more than 98% phosphoric acid, more than 96% 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.
In the scheme, the inorganic dispersant is one or a combination of more of ammonium tripolyphosphate, ammonium hexametaphosphate and ammonium pyrophosphate.
In the scheme, the water is one of ultrapure water, deionized water or distilled water with the resistivity of 15-18M omega cm at 25 ℃.
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 C-free means that the total carbon TC content of the etching solution is less than 20ppm.
In the scheme, the etching solution has high-temperature stability, and when the temperature of the etching solution is above 150 ℃ and 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 above 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 preparing the etching solution comprises the following steps:
(1) Weighing proper amount of a pre-solvent and an inorganic silicon compound according to the proportion;
(2) Adding inorganic silicon compound into the pre-solvent, mixing uniformly, heating to 80-100 ℃ under the state of stirring, condensing and refluxing, keeping for 40-60 minutes, cooling and storing for later use;
(3) Adding an inorganic dispersant into inorganic acid and uniformly mixing for later use;
(4) Adding the mixture obtained in the step 2 into the mixture obtained in the step 3, and uniformly mixing to obtain the C-free high-selectivity silicon nitride etching solution
The reagents and starting materials used in the present invention are commercially available.
The invention has the advantages of
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 oleophilic different parts with two-phase affinity. The foam can not be generated during stirring or turbulence, so that the filter element is blocked, and the adverse effects such as the etching effect of the bottom layer of the structure are not influenced.
2. The high-selectivity silicon nitride etching solution does not contain organic components and C elements, does not generate the phenomenon of color change or organic matter carbonization due to strong dehydration property of high-temperature phosphoric acid/sulfuric acid in the long-time heating and using process, and has good high-temperature stability. And after the silicon nitride etching is finished, the colloid residue phenomenon on the wafer can not occur.
3. The high-selectivity silicon nitride etching solution also contains an inorganic dispersing agent, so that the etching effect cannot be influenced 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 the colloid residues on the wafer and plays a foolproof role.
Drawings
Fig. 1 is an optical image of a wafer without residual glue.
Fig. 2 is an optical image of a wafer with glue residue.
Fig. 3 is an SEM picture of the wafer without glue residue.
FIG. 4 is an SEM image of the glue residue on the wafer.
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.
The inorganic silicon compounds described herein may be represented by chemical formulas (1) - (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):
dechlorotetrasiloxane (CAS: 56240-64-3)
The organosilicon compound in the comparative example may be represented by the following chemical formula (4) - (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 respective components of examples and comparative examples in accordance with the inventive concept are shown in table 1, and the balance is water.
TABLE 1
The above examples 1 to 12 and comparative examples 1 to 5 were each prepared by the following procedure:
(1) Sampling according to the proportion in the table for standby;
(2) Adding an inorganic silicon compound (or an organic silicon compound) into a pre-solvent, uniformly mixing, heating to 80 ℃ under the state of stirring, condensing and refluxing, keeping for 60 minutes, cooling and storing for later use;
(3) Adding inorganic dispersant (if any) into inorganic acid and uniformly mixing for later use;
(4) And (3) adding the mixture obtained in the step (2) into the mixture obtained in the step (3), and uniformly mixing to obtain the C-free high-selectivity silicon nitride etching solution.
The etching rate detection method is carried out in the following way:
etching an object: silicon nitride film and silicon oxide film (thickness about 1000A and 300A, respectively)
Etching temperature: 160 ℃ plus or minus 1 ℃.
Etching container: a quartz tank.
Etching time: the silicon nitride film was etched for 300 seconds, and the silicon oxide film was etched for 7200 seconds. .
Etching rate measuring method: the film thicknesses of the silicon nitride film and the silicon oxide film were measured before 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 ratio represents the ratio of the etching rate of the silicon nitride film to the etching rate of the silicon oxide film.
The method for measuring the residual number comprises the following steps: and (3) immersing the silicon oxide film layer only when the wafer on the silicon oxide is remained in the etching solution at 160 ℃ for 300 seconds, taking out, washing with water, cleaning with SC1, drying with IPA, and analyzing the particle residue number of the wafer surface per unit area by scanning with a micro-optical detector and software.
The chroma detection method comprises the following steps: after the etching solutions in examples and comparative examples were kept at 160 ℃ for 50 hours, samples were cooled and taken, and the chromaticity of the solutions was measured by using a single-wavelength chromaticity detection method at 455nm using an ultraviolet-visible spectrophotometer.
The results of the etching and heating experiments performed with the highly selective silicon nitride etching solutions formulated in various combinations according to embodiments contemplated by the present invention are listed in table 2.
TABLE 2
Note: the initial chroma of the etching solution is less than 1.
In examples 1 to 12, the technical effects achieved in fig. 1 and 3 are optical images and SEM images of the wafer without the colloidal residue. In contrast, the comparative examples 1-3, which contain residual gum, have relatively less gum in at least the respective figures, such as fig. 2 and 4.
Comparing the above examples with comparative examples, the data shows that, compared with organosilicon additives, the silicon-oxygen inorganic additive used in the invention can ensure that the high-selectivity silicon nitride etching solution belongs to a C-free system as a whole, and has obvious advantages in the aspect of high temperature resistance, the temperature of the etching solution is above 160 ℃, and when the etching solution is maintained for more than 50 hours, the chroma change of the etching solution is less than 30Hazen; meanwhile, the silicon-oxygen 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 selection ratio to silicon nitride, and because the etching solution is an inorganic system, the colloidal residue phenomenon on the wafer due to the strong dehydration property of high-temperature phosphoric acid/sulfuric acid in the use process can be avoided. The addition of the pre-solvent enables the inorganic silicon compound to be well dissolved in the inorganic acid to form a uniform system; the inorganic dispersant does not bring organic components into the etching system, and can also play a role in reducing loss when the organic components are mixed into the etching system.
It is apparent that the above embodiments are only examples for clearly illustrating, and are not limiting to 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 (10)
1. The C-free high-selectivity silicon nitride etching solution is characterized in that the etching solution is an electronic grade product, and the main components of the C-free high-selectivity silicon nitride etching solution comprise 50-90% of inorganic acid, 0.1-3% of inorganic silicon compound, 0.3-5% of pre-solvent, 0.01-0.5% of inorganic dispersing agent and the balance of water by mass percent of the etching solution.
2. The C-free highly selective silicon nitride etching solution as set forth in claim 1, wherein the etching solution comprises the following components: 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.
3. The C-free highly selective silicon nitride etching solution as set forth in claim 2, wherein the etching solution comprises the following components: the mass fraction of the inorganic acid is 84-90%, the mass fraction of the inorganic silicon compound is 0.5-1.5%, the mass fraction of the pre-solvent is 1-3%, the mass fraction of the inorganic dispersant is 0.01-0.2%, and the balance is water.
4. The C-free highly selective silicon nitride etching solution according to claim 1, wherein the inorganic acid is a high-boiling acid; the high-boiling-point acid is phosphoric acid and/or sulfuric acid.
5. The C-free highly selective silicon nitride etching solution as claimed in claim 1, wherein the inorganic silicon compound has the formula;
wherein X 1 -X 8 Is halogen, and n is a natural number of 0 to 5.
6. The inorganic silicon compound according to claim 5, wherein X is represented by the formula 1 -X 8 Preferably, cl and n are natural numbers of 0 to 2, more preferably 0 or 1.
7. The C-free high-selectivity silicon nitride etching solution as claimed in claim 6, wherein the pre-solvent is one or more of phosphoric acid with a concentration of more than 98%, sulfuric acid with a concentration of more than 96%, anhydrous phosphorous acid and anhydrous hypophosphorous acid, and the mass ratio of the inorganic silicon compound to the pre-solvent is 1-1.
8. The C-free high-selectivity silicon nitride etching solution as claimed in claim 1, wherein the inorganic dispersant is one or a combination of ammonium tripolyphosphate, ammonium hexametaphosphate and ammonium pyrophosphate; the water is one of ultrapure water, deionized water or distilled water with the resistivity of 15-18M omega cm at 25 ℃.
9. The C-free highly selective silicon nitride etching solution according to claim 1, wherein the C-free means that the total carbon TC content of the etching solution is < 20ppm.
10. The C-free highly selective silicon nitride etching solution as set forth in claim 1, wherein the preparation method of the etching solution comprises the steps of:
(1) Weighing proper pre-solvent and inorganic silicon compound according to the proportion;
(2) Adding inorganic silicon compound into the pre-solvent, mixing uniformly, heating to 80-100 ℃ under the state of stirring, condensing and refluxing, keeping for 40-60 minutes, cooling and storing for later use;
(3) Adding an inorganic dispersant into inorganic acid and uniformly mixing for later use;
(4) And (3) adding the mixture obtained in the step (2) into the mixture obtained in the step (3), and uniformly mixing to obtain the C-free high-selectivity silicon nitride etching solution.
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| PCT/CN2023/083354 WO2024007627A1 (en) | 2022-07-06 | 2023-03-23 | C-free high-selectivity silicon nitride etching solution |
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| 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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| 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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| 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 |
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