CN109706455B - Aluminum etching solution with high etching rate and selectivity ratio and preparation method thereof - Google Patents
Aluminum etching solution with high etching rate and selectivity ratio and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an aluminum etching solution with high etching rate and selectivity ratio and a preparation method thereof. The aluminum etching liquid consists of phosphoric acid, nitric acid, acetic acid, hydrochloric acid and deionized water, and in the etching liquid, nitrosyl chloride formed by the reaction of the nitric acid and the hydrochloric acid has stronger oxidation performance, so that the nitrosyl chloride has high-efficiency etching rate on metal aluminum, and has extremely low etching influence on metal barrier layers such as titanium nitride on the surface of a silicon substrate, thereby forming high etching selection ratio. In the preparation process, by controlling the addition amount and sequence of the components, phosphoric acid, nitric acid, acetic acid and deionized water are added according to the mass ratio, and then hydrochloric acid is added after uniform stirring, so that a strong oxidation substance chlorinated nitrosyl can be generated to the maximum extent, and the etching rate of the aluminum etching solution is improved. The aluminum etching solution can greatly shorten the time of an aluminum etching process and meet the requirement of high selection ratio.
Description
Technical Field
The invention relates to the technical field of intersection of chemical etching and semiconductors, in particular to an aluminum etching solution with high etching rate and selectivity ratio and metal etching of chips, panels and the like by using the aluminum etching solution as an electronic grade chemical.
Background
In recent years, due to rapid development of industries such as semiconductors and display panels, electronic chemicals are in great demand and have higher and higher requirements for quality. Etching technology is also continuously advancing as an essential process link for semiconductors, display panels, and the like. Wet etching has long been used by the industry as the most efficient, stable and widespread etching technique. Aluminum metal has excellent comprehensive properties such as excellent electrical conductivity, low cost, and good adhesion to a silicon substrate, and is used as a metal interconnection line. Thus, current etching is mostly spread around aluminum or aluminum alloys. Because metallic aluminum is easy to diffuse on the surface of a silicon substrate, a layer of barrier metal such as titanium nitride is often deposited between aluminum and the silicon substrate in the industries such as semiconductors, and the barrier metal can effectively prevent the diffusion of the aluminum to the silicon wafer and has the property of being well combined with the silicon substrate. In the etching process, people usually want the etching solution to etch the aluminum faster, so as to save the process time, and meanwhile, expect that the barrier metal is not etched away as much as possible, the ratio of the etching rate of the aluminum to the etching rate of the barrier metal or the substrate is called as the etching selectivity ratio, and the higher the ratio is, the better the product yield is.
Based on the quality requirement of the industry for etching metal aluminum, how to increase the etching rate of metal aluminum without aggravating the etching of metal barrier layers such as titanium nitride and the like, which faces the bottleneck of the etching rate of the etching solution in the industry at present, becomes a direction to be urgently broken through in the field. Under the condition of keeping etching stability, uniformity and etching life, the faster the metal aluminum is etched, the higher the etching selection ratio of the aluminum etching liquid is, the shorter the period can be shortened, and the yield is improved, so that the production cost of the semiconductor is saved. The development of the aluminum etching solution with excellent performance is urgent and has a wide market. According to the invention, a phosphoric acid, nitric acid and acetic acid system is used, hydrochloric acid without oxidability is introduced, and the hydrochloric acid reacts with nitric acid to generate nitrosyl chloride (NOCl) with stronger oxidability, so that the etching rate and the selectivity of the aluminum etching solution are greatly improved.
Disclosure of Invention
In view of the above, an object of the present invention is to provide an aluminum etching solution with high etching rate and selectivity.
The second purpose of the invention is to provide a preparation method of the aluminum etching solution with high etching rate and selectivity.
In order to achieve the purpose, the technical scheme of the invention provides the aluminum etching liquid with high etching rate and selectivity ratio, and the aluminum etching liquid consists of phosphoric acid, nitric acid, acetic acid, hydrochloric acid and deionized water.
Wherein the phosphoric acid is concentrated phosphoric acid, and the weight content of the phosphoric acid is 85-86%; the nitric acid is concentrated nitric acid, and the weight content of the nitric acid is 68-72%; the acetic acid is concentrated acetic acid, and the weight content of the acetic acid is 99-99.8%; the hydrochloric acid is concentrated hydrochloric acid, and the weight content of the hydrochloric acid is 36.5-37.5%; the deionized water has a metal ion content of less than 0.15 ppb.
The further preferable scheme is that the phosphoric acid is concentrated phosphoric acid, and the weight content of the phosphoric acid is 85.7 percent; the nitric acid is concentrated nitric acid, and the weight content of the nitric acid is 70.2%; the acetic acid is concentrated acetic acid, and the weight content of the acetic acid is 99.5 percent; the hydrochloric acid is concentrated hydrochloric acid, and the weight content of the hydrochloric acid is 37.0 percent; the deionized water has a metal ion content of less than 0.1 ppb.
Wherein the mass fraction of phosphoric acid in the etching solution is 65-85%; the mass fraction of the nitric acid is 1-7%; the mass fraction of the acetic acid is 1-10%; the mass fraction of the hydrochloric acid is 0.5-7%; the mass fraction of the deionized water is the balance.
In the technical scheme of the invention, the method utilizes the reaction between hydrochloric acid and nitric acid in the etching solution
HNO3+3HCl (NOCl + Cl2+2H 2O) generates a small amount of nitrosyl chloride, and has stronger oxidizability; the chloride ions generated in the solution have excellent coordination and complexation capability, and are combined with phosphate radicals to strengthen the complexation of aluminum ions.
The technical scheme of the invention also provides a preparation method of the aluminum etching liquid with high etching rate and selectivity ratio, which comprises the following steps:
s1, respectively weighing phosphoric acid, nitric acid, acetic acid, deionized water and hydrochloric acid according to the proportion;
s2, adding phosphoric acid, nitric acid, acetic acid and deionized water one by one, and stirring uniformly and keeping the temperature at room temperature when adding one component;
s3, adding weighed hydrochloric acid slowly into the mixed solution prepared in the S2, and stirring uniformly.
In the preparation process, phosphoric acid, nitric acid, acetic acid and deionized water can be added in any order, but must be added one by one.
Wherein, in the S2, each component is added for 5-10 minutes and the stirring time is kept at room temperature during the adding process.
In the preparation method, the prepared mixed solution is uniformly mixed and is not stirred before the hydrochloric acid is added.
In the preparation method, the hydrochloric acid is slowly added at the speed of 0.5-50mL/min when being added.
In the preparation method, the hydrochloric acid is required to be stirred when being added, the stirring speed is 30-100r/min, and the stirring is stopped when the hydrochloric acid is added.
The invention has the advantages and beneficial effects that: in the invention, components such as a surfactant and the like are not used, and on the basis of phosphoric acid, nitric acid and acetic acid, hydrochloric acid is introduced to enable the etching solution to generate chlorinated nitrosyl with stronger oxidability so as to accelerate the etching rate, avoid the problem of foam caused by the surfactant, and simultaneously give consideration to the stability, the etching uniformity and the etching life of the aluminum etching solution. And aiming at the aluminum wire with the titanium nitride layer, the aluminum etching liquid has higher etching selection ratio. In addition, the preparation method of the aluminum etching liquid with high etching rate and selectivity has the process advantages of few components, simple preparation and the like.
Detailed Description
The invention will be further described in detail with reference to the following figures and examples for better understanding of the invention, but the scope of the invention as claimed is not limited to the scope of the examples.
Example 1:
the embodiment provides a preparation method and an etching effect of an aluminum etching solution with high etching rate and selectivity ratio, which specifically comprises the following steps:
the aluminum etching solution consists of phosphoric acid, nitric acid, acetic acid and deionized water,
wherein the phosphoric acid is concentrated phosphoric acid, and the weight content of the phosphoric acid is 85.7 percent; the nitric acid is concentrated nitric acid, and the weight content of the nitric acid is 70.2%; the acetic acid is concentrated acetic acid, and the weight content of the acetic acid is 99.5 percent; the hydrochloric acid is concentrated hydrochloric acid, and the weight content of the hydrochloric acid is 37.0 percent; the deionized water has a metal ion content of less than 0.1 ppb.
Wherein the mass fraction of phosphoric acid in the etching solution is 70%; the mass fraction of the nitric acid is 5 percent; the mass fraction of acetic acid is 10 percent; the remainder was deionized water.
The preparation method comprises the following specific steps:
(1) the method comprises the following steps: weighing 81.67g of phosphoric acid, 7.12g of nitric acid, 10.01g of acetic acid and 1.2g of deionized water according to 100g of aluminum etching solution;
(2) step two: adding the weighed phosphoric acid into a beaker, and uniformly stirring to ensure that the phosphoric acid is in a room temperature state;
(3) step three: on the basis of the second step, adding the weighed nitric acid into a beaker, and stirring for 5 minutes to ensure that the nitric acid is in a room temperature state;
(4) step four: on the basis of the third step, adding the weighed acetic acid into a beaker, and stirring for 5 minutes to ensure that the acetic acid is in a room temperature state;
(5) step five: finally, adding the weighed deionized water into a beaker, and stirring for 5 minutes to ensure that the beaker is in a room temperature state;
and (3) carrying out an etching experiment on the metal aluminum on the silicon wafer by using the prepared aluminum etching solution at 40 ℃, recording the time required for etching the aluminum with a certain thickness, and calculating the etching rate. In addition, the sample containing the titanium nitride coating is also etched in the aluminum etching solution, and the etching rate ratio of aluminum to titanium nitride is calculated to obtain the etching selection ratio.
Example 2:
the embodiment provides a preparation method and an etching effect of an aluminum etching solution with high etching rate and selectivity ratio, which specifically comprises the following steps:
the aluminum etching liquid consists of phosphoric acid, nitric acid, acetic acid, hydrochloric acid and deionized water,
wherein the phosphoric acid is concentrated phosphoric acid, and the weight content of the phosphoric acid is 85.7 percent; the nitric acid is concentrated nitric acid, and the weight content of the nitric acid is 70.2%; the acetic acid is concentrated acetic acid, and the weight content of the acetic acid is 99.5 percent; the hydrochloric acid is concentrated hydrochloric acid, and the weight content of the hydrochloric acid is 37.0 percent; the deionized water has a metal ion content of less than 0.1 ppb.
Wherein the weight content of phosphoric acid in the etching solution is 68.6 percent; the weight content of the nitric acid is 5 percent; the weight content of acetic acid is 10 percent; the weight content of the hydrochloric acid is 1 percent, and no additional deionized water is added. The prepared etching solution can generate 0.05-0.33 wt% of chlorinated nitrosyl.
The preparation method comprises the following specific steps:
(1) the method comprises the following steps: respectively weighing 80.09g of phosphoric acid, 7.12g of nitric acid, 10.01g of acetic acid and 2.78g of hydrochloric acid according to 100g of the aluminum etching solution;
(2) step two: adding the weighed phosphoric acid into a beaker, and uniformly stirring to ensure that the phosphoric acid is in a room temperature state;
(3) step three: on the basis of the second step, adding the weighed nitric acid into a beaker, and stirring for 5 minutes to ensure that the nitric acid is in a room temperature state;
(4) step four: on the basis of the third step, adding the weighed acetic acid into a beaker, and stirring for 5 minutes to ensure that the acetic acid is in a room temperature state;
(5) step five: finally, the weighed hydrochloric acid is slowly dripped into the beaker for 1 minute, and the stirring is stopped after the dripping at 30 r/min.
And (3) carrying out an etching experiment on the metal aluminum on the silicon wafer by using the prepared aluminum etching solution at 40 ℃, recording the time required for etching the aluminum with a certain thickness, and calculating the etching rate. In addition, the sample containing the titanium nitride coating is also etched in the aluminum etching solution, and the etching rate ratio of aluminum to titanium nitride is calculated to obtain the etching selection ratio.
Example 3:
the embodiment provides a preparation method and an etching effect of an aluminum etching solution with high etching rate and selectivity ratio, which specifically comprises the following steps:
the aluminum etching liquid consists of phosphoric acid, nitric acid, acetic acid, hydrochloric acid and deionized water,
wherein the phosphoric acid is concentrated phosphoric acid, and the weight content of the phosphoric acid is 85.7 percent; the nitric acid is concentrated nitric acid, and the weight content of the nitric acid is 70.2%; the acetic acid is concentrated acetic acid, and the weight content of the acetic acid is 99.5 percent; the hydrochloric acid is concentrated hydrochloric acid, and the weight content of the hydrochloric acid is 37.0 percent; the deionized water has a metal ion content of less than 0.1 ppb.
Wherein the weight content of phosphoric acid in the etching solution is 69%; the weight content of the nitric acid is 5 percent; the weight content of acetic acid is 10 percent; the weight content of the hydrochloric acid is 0.5 percent; the balance being deionized water. The prepared etching solution can generate 0.025-0.17 wt% of chlorinated nitrosyl.
The preparation method comprises the following specific steps:
(1) the method comprises the following steps: respectively weighing 80.5g of phosphoric acid, 7.12g of nitric acid, 10.01g of acetic acid, 1.39g of hydrochloric acid and 0.98g of deionized water according to 100g of aluminum etching solution;
(2) step two: adding the weighed phosphoric acid into a beaker, and uniformly stirring to ensure that the phosphoric acid is in a room temperature state;
(3) step three: on the basis of the second step, adding the weighed nitric acid into a beaker, and stirring for 5 minutes to ensure that the nitric acid is in a room temperature state;
(4) step four: on the basis of the third step, adding the weighed acetic acid into a beaker, and stirring for 5 minutes to ensure that the acetic acid is in a room temperature state;
(5) step five: finally, adding the weighed deionized water into a beaker, and stirring for 5 minutes to ensure that the beaker is in a room temperature state;
(6) step six: finally, the weighed hydrochloric acid is slowly dripped into the beaker for 0.5 minute, and the stirring is carried out at 30r/min, and the stirring is stopped after the dripping is finished.
And (3) carrying out an etching experiment on the metal aluminum on the silicon wafer by using the prepared aluminum etching solution at 40 ℃, recording the time required for etching the aluminum with a certain thickness, and calculating the etching rate. In addition, the sample containing the titanium nitride coating is also etched in the aluminum etching solution, and the etching rate ratio of aluminum to titanium nitride is calculated to obtain the etching selection ratio.
Example 4:
the embodiment provides a preparation method and an etching effect of an aluminum etching solution with high etching rate and selectivity ratio, which specifically comprises the following steps:
the aluminum etching liquid consists of phosphoric acid, nitric acid, acetic acid, hydrochloric acid and deionized water,
wherein the phosphoric acid is concentrated phosphoric acid, and the weight content of the phosphoric acid is 85.7 percent; the nitric acid is concentrated nitric acid, and the weight content of the nitric acid is 70.2%; the acetic acid is concentrated acetic acid, and the weight content of the acetic acid is 99.5 percent; the hydrochloric acid is concentrated hydrochloric acid, and the weight content of the hydrochloric acid is 37.0 percent; the deionized water has a metal ion content of less than 0.1 ppb.
Wherein the weight content of phosphoric acid in the etching solution is 70%; the weight content of nitric acid is 3.5%; the weight content of acetic acid is 10 percent; the weight content of the hydrochloric acid is 1 percent; the balance being deionized water. The prepared etching solution can generate 0.05-0.33 wt% of chlorinated nitrosyl.
The preparation method comprises the following specific steps:
(1) the method comprises the following steps: weighing 81.67g of phosphoric acid, 4.98g of nitric acid, 10.01g of acetic acid, 2.78g of hydrochloric acid and 0.56g of deionized water according to 100g of aluminum etching solution;
(2) step two: adding the weighed phosphoric acid into a beaker, and uniformly stirring to ensure that the phosphoric acid is in a room temperature state;
(3) step three: on the basis of the second step, adding the weighed nitric acid into a beaker, and stirring for 5 minutes to ensure that the nitric acid is in a room temperature state;
(4) step four: on the basis of the third step, adding the weighed acetic acid into a beaker, and stirring for 5 minutes to ensure that the acetic acid is in a room temperature state;
(5) step five: finally, adding the weighed deionized water into a beaker, and stirring for 5 minutes to ensure that the beaker is in a room temperature state;
(6) step six: finally, the weighed hydrochloric acid is slowly dripped into the beaker for 1 minute, and the stirring is stopped after the dripping at 30 r/min.
And (3) carrying out an etching experiment on the metal aluminum on the silicon wafer by using the prepared aluminum etching solution at 40 ℃, recording the time required for etching the aluminum with a certain thickness, and calculating the etching rate. In addition, the sample containing the titanium nitride coating is also etched in the aluminum etching solution, and the etching rate ratio of aluminum to titanium nitride is calculated to obtain the etching selection ratio.
Example 5:
the embodiment provides a preparation method and an etching effect of an aluminum etching solution with high etching rate and selectivity ratio, which specifically comprises the following steps:
the aluminum etching liquid consists of phosphoric acid, nitric acid, acetic acid, hydrochloric acid and deionized water,
wherein the phosphoric acid is concentrated phosphoric acid, and the weight content of the phosphoric acid is 85.7 percent; the nitric acid is concentrated nitric acid, and the weight content of the nitric acid is 70.2%; the acetic acid is concentrated acetic acid, and the weight content of the acetic acid is 99.5 percent; the hydrochloric acid is concentrated hydrochloric acid, and the weight content of the hydrochloric acid is 37.0 percent; the deionized water has a metal ion content of less than 0.1 ppb.
Wherein the weight content of phosphoric acid in the etching solution is 65%; the weight content of the nitric acid is 2 percent; the weight content of acetic acid is 10 percent; the weight content of the hydrochloric acid is 4 percent; the balance being deionized water. The prepared etching solution can generate 0.2 to 1.33 weight percent of nitrosyl chloride.
The preparation method comprises the following specific steps:
(1) the method comprises the following steps: respectively weighing 75.84g of phosphoric acid, 2.85g of nitric acid, 10.01g of acetic acid, 11.1g of hydrochloric acid and 0.2g of deionized water according to 100g of aluminum etching solution;
(2) step two: adding the weighed phosphoric acid into a beaker, and uniformly stirring to ensure that the phosphoric acid is in a room temperature state;
(3) step three: on the basis of the second step, adding the weighed nitric acid into a beaker, and stirring for 5 minutes to ensure that the nitric acid is in a room temperature state;
(4) step four: on the basis of the third step, adding the weighed acetic acid into a beaker, and stirring for 5 minutes to ensure that the acetic acid is in a room temperature state;
(5) step five: finally, adding the weighed deionized water into a beaker, and stirring for 5 minutes to ensure that the beaker is in a room temperature state;
(6) step six: finally, the weighed hydrochloric acid is slowly dripped into the beaker for 4 minutes, and the stirring is stopped after the dripping is finished at the stirring speed of 30 r/min.
And (3) carrying out an etching experiment on the metal aluminum on the silicon wafer by using the prepared aluminum etching solution at 40 ℃, recording the time required for etching the aluminum with a certain thickness, and calculating the etching rate. In addition, the sample containing the titanium nitride coating is also etched in the aluminum etching solution, and the etching rate ratio of aluminum to titanium nitride is calculated to obtain the etching selection ratio.
The data for the examples listed above and the results for etching, selectivity, etc. are now shown in the following table:
the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. An aluminum and titanium nitride etching solution with high etching rate and selectivity ratio is characterized in that: the aluminum and titanium nitride etching solution consists of phosphoric acid, nitric acid, acetic acid, hydrochloric acid and deionized water, and the mass fraction of the phosphoric acid in the etching solution is 65%; the mass fraction of the nitric acid is 2 percent; the mass fraction of acetic acid is 10 percent; the mass fraction of the hydrochloric acid is 4 percent; the mass fraction of the deionized water is the balance, and the prepared etching solution can generate 0.2-1.33 wt% of chlorinated nitrosyl;
the phosphoric acid is concentrated phosphoric acid, and the weight content of the phosphoric acid is 85.7 percent;
the nitric acid is concentrated nitric acid, and the weight content of the nitric acid is 70.2%;
the acetic acid is concentrated acetic acid, and the weight content of the acetic acid is 99.5 percent;
the hydrochloric acid is concentrated hydrochloric acid, and the weight content of the hydrochloric acid is 37.0 percent;
the deionized water has a metal ion content of less than 0.1 pp.
2. A preparation method of an aluminum and titanium nitride etching solution with high etching rate and selectivity ratio is characterized by comprising the following steps:
s1, respectively weighing phosphoric acid, nitric acid, acetic acid, deionized water and hydrochloric acid according to the proportion in the claim 1;
s2, adding phosphoric acid, nitric acid, acetic acid and deionized water one by one, and stirring uniformly and keeping the temperature at room temperature when adding one component;
s3, adding weighed hydrochloric acid slowly into the mixed solution prepared in the S2, and stirring uniformly.
3. The method of claim 2, wherein: the phosphoric acid, nitric acid, acetic acid and deionized water in the S2 step may be added in any order, but must be added one by one.
4. The method of claim 2, wherein: the stirring time for each component added in the step of S2 is 5-10 minutes, and the room temperature is maintained during the addition.
5. The method of claim 2, wherein: in the step S3, the prepared mixed solution is already in a uniformly mixed state and is in an unstirred state before the hydrochloric acid is added.
6. The method of claim 2, wherein: when hydrochloric acid is added into S3, the hydrochloric acid is slowly added at the speed of 0.5-50 mL/min.
7. The method of claim 2, wherein: and (3) stirring is required when hydrochloric acid is added into S3, the stirring speed is 30-100r/min, and the stirring is stopped when the hydrochloric acid is added.
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| CN112111280A (en) * | 2020-08-27 | 2020-12-22 | 江苏中德电子材料科技有限公司 | Selective etching solution for silicon oxide and application and use method thereof |
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| KR101154244B1 (en) * | 2005-06-28 | 2012-06-18 | 주식회사 동진쎄미켐 | Etchant for etching Al, Mo and ITO |
| KR20070017762A (en) * | 2005-08-08 | 2007-02-13 | 엘지.필립스 엘시디 주식회사 | Etchant composition, method of patterning electroconductive film using the same and method of fabricating flat panel display using the same |
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