CN111925798B - Etching solution composition, preparation method and application thereof - Google Patents
Etching solution composition, preparation method and application thereof Download PDFInfo
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- CN111925798B CN111925798B CN202010817221.3A CN202010817221A CN111925798B CN 111925798 B CN111925798 B CN 111925798B CN 202010817221 A CN202010817221 A CN 202010817221A CN 111925798 B CN111925798 B CN 111925798B
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- 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
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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 at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/311—Etching the insulating layers by chemical or physical means
- H01L21/31105—Etching inorganic layers
- H01L21/31111—Etching inorganic layers by chemical means
Abstract
The invention discloses an etching solution composition, and preparation and application thereof. Specifically, the etching solution composition comprises the following components in parts by weightComprises the following components: 76.5-84.6 parts of phosphoric acid, 13.5-15 parts of water and 0.5-10 parts of a compound shown as a formula A. The compound and the composition shown in the formula A can provide high selectivity ratio, prolong the service life of the etching solution and adapt to the increase of the number of layers of a laminated structure.
Description
Technical Field
The invention relates to an etching solution composition, a preparation method and application thereof.
Background
An oxide film such as a silicon oxide film and a nitride film such as a silicon nitride film are representative insulator films, and in a semiconductor manufacturing process, the silicon oxide film or the silicon nitride film may be used alone or in the form of a stacked body (laminate) in which one or more thin films are alternately stacked. In addition, the oxide film or the nitride film is also used as a hard mask for forming a conductive pattern such as a metal wiring.
In the wet etching process for removing the nitride film, an aqueous phosphoric acid solution is generally used. There are many problems with the aqueous phosphoric acid solution alone, such as: the etching rate selection ratio of silicon oxide and silicon nitride is improper, and more particles and precipitates exist in the solution in a short time in the process, so that the service life of liquid medicine is short, the increase of the layer number of the laminated structure cannot be adapted, and the like.
In order to solve these problems, it is considered that a compound is added to the phosphoric acid aqueous solution to improve the etching capability of the phosphoric acid aqueous solution.
Disclosure of Invention
The invention aims to solve the technical problem that in the prior art, the etching rate selection ratio of silicon oxide and silicon nitride is not proper, more particles and precipitates are in the solution in a short time in the process, the service life of liquid medicine is short, the number of layers of a laminated structure cannot be increased, and the like, and provides an etching liquid composition, a preparation method and application thereof. The etching rate selection ratio of silicon oxide and silicon nitride etched by using the etching liquid composition is proper, the service life of the etching liquid is prolonged, and the etching capacity of phosphoric acid aqueous solution can be effectively improved.
The present invention solves the above technical problems by the following technical solutions.
The invention provides an etching solution composition which comprises the following components in parts by weight:
76.5-84.6 parts of phosphoric acid, 13.5-15 parts of water and 0.5-10 parts of compound shown as a formula A
In some embodiments of the present invention, the mass part of the compound represented by formula a is 0.5 to 9.5 parts, for example, 0.5 part, 1.0 part, 4.5 parts, 9.5 parts or 10.0 parts, preferably 1 to 9.5 parts, and more preferably 4.5 parts.
In some embodiments of the present invention, the content of the phosphoric acid may be 76.9 to 84.6 parts, for example 76.5 parts, 76.9 parts, 81.2 parts, 84.1 parts or 84.6 parts, preferably 76.9 to 84.1 parts, and more preferably 81.2 parts by weight.
In some embodiments of the invention, the water may be one or more of deionized water, distilled water, pure water, and ultrapure water.
In some embodiments of the present invention, the water content may be 13.5 to 14.9 parts, for example, 13.5 parts, 13.6 parts, 14.3 parts, 14.8 parts or 14.9 parts, preferably 13.6 to 14.8 parts, and more preferably 14.3 parts by weight.
In some embodiments of the present invention, the etching solution comprises the following components: a compound represented by formula A, phosphoric acid and water.
In some embodiments of the present invention, the etching solution composition comprises the following components: 76.5-84.6% of phosphoric acid, 13.5-15% of water and 0.5-10% of a compound shown as a formula A, wherein the percentage is that the mass of each component accounts for the mass of the etching solution.
In some embodiments of the invention, the etching solution composition comprises the following components: 76.9-84.6 wt% of phosphoric acid, 13.1-15 wt% of water and 0.5-9.5 wt% of a compound shown as a formula A, wherein the percentage is that the mass of each component accounts for the mass of the etching solution.
In some embodiments of the invention, the etching solution composition comprises the following components: 76.9-84.1% of phosphoric acid, 13.6-15.7% of water and 1-9.5% of a compound shown as a formula A, wherein the percentage is that the mass of each component accounts for the mass of the etching solution.
In some embodiments of the present invention, the etching solution composition comprises the following components: 0.5 percent of compound shown as formula A, 84.6 percent of phosphoric acid and 14.9 percent of water, wherein the percentage is that the mass of each component accounts for the mass of the etching solution.
In some embodiments of the present invention, the etching solution composition comprises the following components: 1% of a compound shown as a formula A, 84.1% of phosphoric acid and 14.9% of water, wherein the percentage is that the mass of each component accounts for the mass of the etching solution.
In some embodiments of the present invention, the etching solution composition comprises the following components: 4.5 percent of the compound shown as the formula A, 81.2 percent of phosphoric acid and 14.3 percent of water, wherein the percentage is that the mass of each component accounts for the mass of the etching solution.
In some embodiments of the present invention, the etching solution comprises the following components: 9.5 percent of the compound shown as the formula A, 76.9 percent of phosphoric acid and 13.5 percent of water, wherein the percentage is that the mass of each component accounts for the mass of the etching solution.
In some embodiments of the present invention, the etching solution comprises the following components: 10 percent of compound shown as formula A, 76.5 percent of phosphoric acid and 13.5 percent of water, wherein the percentage is the percentage of the mass of each component in the etching solution.
In some embodiments of the present invention, when the etching liquid composition is an etching liquid composition for etching a silicon nitride film, the etching is performed in the presence of a silicon oxide film. The silicon nitride film may be a silicon nitride film formed on a patterned silicon semiconductor wafer. The thickness of the silicon nitride film can be
The silicon oxide film may be a silicon oxide film formed on a patterned silicon semiconductor wafer; the thickness of the silicon oxide film is
The silicon oxide film and the silicon nitride film are of a laminated structure of the silicon oxide film and the silicon nitride film, and the number of layers of the laminated structure can be 10-200.
The invention also provides application of the etching solution in etching silicon oxide and/or silicon nitride. The etching conditions and operations described may be those conventional in the art.
In the application, the etching solution is preferably used for etching silicon nitride.
In the application, when the etching is carried out in the presence of a silicon oxide film and a silicon nitride film, the etching solution composition is used for selectively etching the silicon nitride film; the silicon oxide film may be a silicon oxide film formed on a patterned silicon semiconductor wafer.
In the application, the silicon oxide and/or the silicon nitride can be applied to semiconductor materials.
In said application, said silicon nitride and/or silicon nitride film may have a thickness of
For example
Also for example
Or
In the application, the silicon oxide and/or the silicon nitride can be a laminated structure. In the laminated structure, the number of layers of the laminated structure can be 10-200, such as 32, 64, 128 or 192.
In such applications, the etching temperature may be 150 ℃ to 170 ℃, for example 159 ℃. + -. 2 ℃.
In the application, the etching time may be 600 seconds and 6500 seconds, for example, 720 seconds or 6000 seconds.
In the application, the etching may include the steps of: and etching the silicon oxide and/or the silicon nitride at the temperature of 150 ℃ and 170 ℃ for 600 seconds and 6500 seconds, taking out the silicon oxide and/or the silicon nitride, cleaning, drying, and observing the etching condition of the silicon oxide and/or the silicon nitride by using a TEM section.
The invention provides a preparation method of the etching solution, which comprises the following steps: and mixing the compound shown as the formula A, phosphoric acid and water to obtain the etching solution composition.
The invention also provides the application of the compound shown as the formula A in serving as an etching liquid compound;
in the application, the content of the compound shown in the formula A can be 0.5-10%, preferably 1.00-9.50%, and more preferably 4.50%, wherein the percentage is the mass of the compound shown in the formula A in the etching solution.
In the application, the content of the phosphoric acid is 13.5-14.9%, preferably 13.6-14.8%, and more preferably 14.3%, wherein the percentage is the mass percentage of the phosphoric acid in the etching solution.
In the application, the content of the water is 76.9-84.6%, preferably 76.9-84.1%, and more preferably 81.2%, wherein the percentage is the mass percentage of the water in the etching solution.
In the application, the etching solution can be as described in any of the above embodiments.
In the application, the etching solution can be used for etching silicon oxide and/or silicon nitride, preferably silicon nitride.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
In the present invention, said compound represented by formula a is prepared by referring to patent application CN 108586518B.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows: the compound and the composition of the invention can provide high selectivity ratio, prolong the service life of the etching solution and adapt to the increase of the number of laminated structure layers.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
1 preparation of etching liquid composition
Structure of compound a:
structure of compound B:
the preparation methods of the compound A and the compound B refer to patent CN 105254674B;
respectively adding A or B into pure phosphoric acid raw materials at room temperature to obtain etching solutions in examples 1-5 and comparative example 1; the etching solution in comparative example 2 was pure phosphoric acid as a raw material.
The pure phosphoric acid raw materials used in the invention are all concentrated phosphoric acid with the mass percentage of 85%. In the case of other concentrations of concentrated phosphoric acid, the amount of concentrated phosphoric acid converted to that concentration can be calculated by equivalent amounts.
2 detection of etch Rate
Etching an object: a silicon oxide film and a silicon nitride film; wherein the two films are deposited on the patterned silicon semiconductor wafer to a thickness of
And forming a deposit on the patterned silicon semiconductor wafer to a thickness of
The silicon nitride film of (1).
Etching temperature: 159 ℃ plus or minus 2 ℃.
Etching container: a quartz tank.
Etching time: the silicon oxide film and the silicon nitride film were etched for 720 seconds and 6000 seconds, respectively.
The speed measurement method comprises the following steps: the film thicknesses of the silicon oxide film and the nitride film were measured before and after etching using a film thickness measuring apparatus (NANO VIEW, SEMG-1000), 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 nitride film etching rate (SiNE/R) to the oxide film etching rate (SiO E/R).
The concentration of the compound in the invention is mass percent, namely the mass of the compound accounts for the total mass of the etching solution.
3 detection of Life
In both of silicon oxide film etching and silicon nitride film etching, the etching metabolite contains silicon dioxide, and the concentration of silicon dioxide dissolved in the etching solution gradually increases as the etching time increases. Thus, an etching solution in which the concentration of silicon dioxide was gradually increased (0ppm/80ppm/120ppm/300ppm/500ppm) was prepared as an initial etching solution, and the etching rates and the selectivity of silicon oxide and silicon nitride were measured, respectively.
The silicon oxide and silicon nitride etch rates and selectivity for various concentrations of a or B as phosphoric acid etch liquid compounds at an initial silicon dioxide concentration of 0ppm are detailed in table 1:
TABLE 1 etch rates and selectivity for silicon oxide and silicon nitride at an initial silicon dioxide concentration of 0ppm
Within the error range of the experimental system of the present invention, the selection ratio is preferably within the range of 500-900. The higher the rewet is, the more the overfetching is.
The silicon oxide and silicon nitride etch rates and selectivity for various concentrations of a or B as phosphoric acid etch liquid compounds at an initial silicon dioxide concentration of 80ppm are detailed in table 2:
TABLE 2 etch rates and selectivity for silicon oxide and silicon nitride at an initial silicon dioxide concentration of 80ppm
The silicon oxide and silicon nitride etch rates and selectivity for various concentrations of a or B as phosphoric acid etch liquid compounds at an initial silicon dioxide concentration of 120ppm are detailed in table 3:
TABLE 3 etch rates and selectivity for silicon oxide and silicon nitride at an initial silicon dioxide concentration of 120ppm
The silicon oxide and silicon nitride etch rates and selectivity for various concentrations of a or B as phosphoric acid etch liquid compounds at an initial silicon dioxide concentration of 300ppm are detailed in table 4:
TABLE 4 etch rates and selectivity for silicon oxide and silicon nitride at an initial silicon dioxide concentration of 300ppm
The silicon oxide and silicon nitride etch rates and selectivity for various concentrations of a or B as phosphoric acid etch liquid compounds at an initial silicon dioxide concentration of 500ppm are detailed in table 5:
TABLE 5 etch rates and selectivity for silicon oxide and silicon nitride at an initial silicon dioxide concentration of 500ppm
Etching of 4 layers of a laminated structure
Etching an object: silicon wafer having a cross-laminated structure of
And a silicon oxide layer of
The silicon nitride layers of (2) are cross-laminated. The number of layers of the laminated structure is respectively as follows: 32 layers/64 layers/128 layers/192 layers.
Etching conditions: the initial concentration of silicon dioxide in the etching solution was 0 ppm.
The detection method comprises the following steps: after etching the wafer at 159 ℃. + -. 2 ℃ for 10min, the wafer was taken out, washed, dried and the etching of the layered structure in the wafer was observed by TEM section.
Evaluation criteria: the A level is the etching completion of the silicon nitride layer and the silicon oxide layer is not damaged; the B level is the silicon nitride layer which is etched but damaged; the C level is that the silicon nitride layer is not etched.
From examples 1 to 3, it is found that when the concentration of the compound a represented by the formula a is in the range of 1.00% to 9.50%, the etching solution was used in the above-described etching experiment to complete the etching of the silicon wafers having 32, 64, 128 and 192 layers without damaging the silicon oxide layer. The etching solution in example 4 was subjected to the above-described etching experiment to etch the silicon nitride layers of the silicon wafers of 32 layers, 64 layers, 128 layers and 192 layers, but the silicon oxide layers were damaged. The etching solutions in example 5 and comparative example 1 were subjected to the above-described etching experiment to finish etching of the silicon nitride layer. The etching solution in comparative example 2 was subjected to the above-described etching experiment to completely etch the silicon nitride layers of the 32-layer and 64-layer silicon wafers but to damage the silicon oxide layers, and to incompletely etch the silicon nitride layers of the 128-layer and 192-layer silicon wafers.
Claims (13)
1. The etching solution composition is characterized by comprising the following components in parts by mass: 76.9 to 84.1 portions of phosphoric acid, 13.6 to 14.9 portions of water and 1.0 to 9.5 portions of compound shown as the formula A
2. The etching solution composition according to claim 1,
the etching solution composition is used for etching the silicon nitride film;
and/or the water is one or more of deionized water, distilled water, pure water and ultrapure water.
3. The etching solution composition according to claim 2,
when the etching solution composition is an etching solution composition for etching a silicon nitride film, the etching is performed in the presence of a silicon oxide film;
and/or, when the etching solution composition is an etching solution composition for etching a silicon nitride film, the silicon nitride film is a silicon nitride film formed on a patterned silicon semiconductor wafer;
and/or, when the etching solution composition is used for etching a silicon nitride film, the thickness of the silicon nitride film is
4. The etching solution composition according to claim 3,
the content of the compound shown as the formula A is 4.5 parts by weight;
and/or, the content of the phosphoric acid is 81.2 parts by mass;
and/or, the content of the water is 14.3 parts by mass;
and/or, when the etching solution composition is an etching solution composition for etching a silicon nitride film, the etching is performed in the presence of a silicon oxide film, the silicon oxide film being a silicon oxide film formed on a patterned silicon semiconductor wafer;
and/or, when the etching solution composition is used for etching a silicon nitride film, the silicon oxide film has a thickness of
And/or, when the etching solution composition is an etching solution composition for etching a silicon nitride film, and the etching is performed in the presence of a silicon oxide film, the silicon oxide film and the silicon nitride film have a laminated structure of the silicon oxide film and the silicon nitride film.
5. The etching solution composition according to claim 3, wherein when the etching solution composition is an etching solution composition for etching a silicon nitride film, and the etching is performed in the presence of a silicon oxide film, the silicon oxide film and the silicon nitride film have a laminated structure of a silicon oxide film and a silicon nitride film, and the number of layers of the laminated structure is 10 to 200.
6. The etching solution composition according to any one of claims 1 to 5, wherein the etching solution composition is any one of the following:
scheme 1:
the etching solution composition comprises the following components: 1% of a compound shown as a formula A, 84.1% of phosphoric acid and 14.9% of water, wherein the percentage is that the mass of each component accounts for the mass of the etching solution;
scheme 2:
the etching solution composition comprises the following components: 4.5% of a compound shown as a formula A, 81.2% of phosphoric acid and 14.3% of water, wherein the percentage is that the mass of each component accounts for the mass of the etching solution;
scheme 3:
the etching solution composition comprises the following components: 9.5 percent of the compound shown as the formula A, 76.9 percent of phosphoric acid and 13.6 percent of water, wherein the percentage is that the mass of each component accounts for the mass of the etching solution.
7. Use of an etchant composition according to any one of claims 1 to 6 for etching silicon oxide and/or silicon nitride.
8. Use of the etching liquid composition according to claim 7 for etching silicon oxide and/or silicon nitride,
when the etching is carried out in the presence of a silicon oxide film and a silicon nitride film, the etching liquid composition is used for selectively etching the silicon nitride film;
and/or, the silicon oxide and/or the silicon nitride are applied to a semiconductor material;
and/or the thickness of the silicon oxide and/or the silicon nitride is
And/or the silicon oxide and/or the silicon nitride are in a laminated structure, and the number of layers of the laminated structure in the laminated structure is 10-200;
and/or the etching temperature is 150-170 ℃;
and/or the etching time is 600-6500 seconds;
and/or, the etching comprises the following steps: and etching the silicon oxide and/or the silicon nitride at the temperature of 150 ℃ and 170 ℃ for 600 seconds and 6500 seconds, taking out the silicon oxide and/or the silicon nitride, cleaning, drying, and observing the etching condition of the silicon oxide and/or the silicon nitride by using a TEM section.
9. Use of the etching solution composition according to claim 7 for etching silicon oxide and/or silicon nitride, wherein the etching solution composition is a selective etching silicon nitride film etching when the etching is in the presence of a silicon oxide film and a silicon nitride film; the silicon oxide film is formed on a patterned silicon semiconductor wafer.
10. A method for preparing the etching solution composition according to any one of claims 1 to 6, comprising the steps of: and (2) mixing the compound shown as the formula A, the phosphoric acid and the water to obtain the etching solution composition.
11. An application of a compound shown as a formula A in preparing an etching solution composition;
12. the use of a compound of formula A according to claim 11 for the preparation of an etching solution composition,
in the etching solution composition, the content of the compound shown as the formula A is 1.00-9.50%, wherein the percentage is the mass percentage of the compound shown as the formula A in the etching solution;
and/or the etching solution contains water, and the content of the water is 13.6% -14.9%, wherein the percentage is the percentage of the mass of the water in the mass of the etching solution;
and/or the etching solution contains phosphoric acid with the content of 76.9-84.1%, wherein the percentage is the mass percentage of the phosphoric acid in the etching solution;
and/or the etching solution is used for etching the silicon nitride film.
13. The use of a compound of formula A according to claim 11 for the preparation of an etching solution composition,
in the etching solution composition, the content of the compound shown in the formula A is 4.50%, wherein the percentage is the mass percentage of the compound shown in the formula A in the etching solution;
and/or the etching solution contains 14.3% of water, wherein the percentage is the percentage of the mass of the water in the etching solution;
and/or the etching solution contains phosphoric acid with the content of 81.2 percent, wherein the percentage is the percentage of the mass of the phosphoric acid in the mass of the etching solution;
and/or the etching solution is used for etching a silicon nitride film, the etching is carried out in the presence of a silicon oxide film, and the silicon nitride film is formed on a patterned silicon semiconductor wafer; the silicon oxide film is formed on a patterned silicon semiconductor wafer.
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