CN112251818A - Wafer etching solution and etching method - Google Patents
Wafer etching solution and etching method Download PDFInfo
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- CN112251818A CN112251818A CN202011057130.0A CN202011057130A CN112251818A CN 112251818 A CN112251818 A CN 112251818A CN 202011057130 A CN202011057130 A CN 202011057130A CN 112251818 A CN112251818 A CN 112251818A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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Abstract
The invention discloses a wafer etching solution and an etching method, and relates to the technical field of semiconductor materials. The invention relates to a wafer etching solution which comprises the following components in percentage by volume: 70-77% of hydrogen peroxide, 3.8-5% of concentrated sulfuric acid, 7.7-10% of glacial acetic acid and 9.5-11.5% of concentrated hydrochloric acid, and preferably comprises the following components in percentage by volume: 77% of hydrogen peroxide, 3.8% of concentrated sulfuric acid, 7.7% of glacial acetic acid and 11.5% of concentrated hydrochloric acid. The invention discloses a wafer etching solution and an etching method, which can solve the problems of low wafer etching speed and difficulty in cleaning after etching of a wafer, and can effectively increase the success rate of the etching solution after etching to a certain extent.
Description
Technical Field
The invention relates to the technical field of semiconductor materials, in particular to a wafer etching solution and an etching method.
Background
Indium phosphide plays an important role as a compound semiconductor material in the photonic field (emission and detection capabilities at wavelengths of 1000nm or more) and the radio frequency field (high-speed and low-noise performance in high-frequency RF applications). For indium phosphide, the preparation method has the advantages of high electron mobility, good radiation resistance, large forbidden bandwidth, high thermal conductivity, high breakdown electric field and the like. The substrate is the preferred substrate material in the preparation of microwave and millimeter wave circuits and high-speed digital integrated circuits for the first choice of performance-driven niche markets for military communication, radar, radiometry and the like and automatic test equipment. In the 5G communication era, compared with other semiconductor materials, the performance of the indium phosphide material is better, and although the technology of the indium phosphide material is challenged by the technology of other semiconductor materials, the indium phosphide material still is the mainstream material of the future semiconductor materials by virtue of the excellent performance, and has a wider development prospect for the improvement and the higher pursuit of the product performance and the development and the promotion of the indium phosphide technology in the future.
The InP wafer is processed by an InP crystal bar, saw lines are generated on the surface of the wafer in the processing process, internal stress is generated inside the wafer, and the thickness of the wafer after being cut is greatly different from that of a product. After slicing, before polishing, grinding treatment is needed, defects such as saw lines, scratches and the like on the surface of the wafer are repaired, and the thickness of the wafer is ground to reach the thickness standard before polishing. And then, etching the wafer, and removing the stress layer and the damaged layer on the surface of the wafer.
Therefore, when the indium phosphide wafer is etched, research and study on the etching solution and the etching method of the indium phosphide wafer are required, and a more excellent etching solution ratio and an operation method are obtained through a large number of data experiments.
After being ground, most of the existing indium phosphide wafers are cleaned only by using deionized water, namely, the wafers are corroded once by using a corrosion solution, firstly, the wafers are corroded and cleaned by using the traditional corrosion solution, the surface cleaning speed is low, after the surface is found to be corroded, the wafers are cleaned by using the deionized water, and then the wafers are dried, so that the wafers are found to be unqualified in corrosion due to the fact that a few of stains such as corrosion chemical marks, watermarks and the like are formed on the surfaces of the wafers.
Disclosure of Invention
In view of the above problems, the present invention aims to disclose a wafer etching solution and an etching method, which can improve the problems of slow wafer etching speed and difficulty in cleaning the wafer after etching, and can effectively increase the success rate of the etching solution after etching to a certain extent.
Specifically, the wafer etching solution provided by the invention comprises the following components in percentage by volume: 70 to 77 percent of hydrogen peroxide, 3.8 to 5 percent of concentrated sulfuric acid, 7.7 to 10 percent of glacial acetic acid and 9.5 to 11.5 percent of concentrated hydrochloric acid.
Further, the corrosion liquid comprises the following components in percentage by volume: 77% of hydrogen peroxide, 3.8% of concentrated sulfuric acid, 7.7% of glacial acetic acid and 11.5% of concentrated hydrochloric acid.
In addition, the invention also discloses a preparation method of the wafer etching solution, and the etching method comprises the steps of soaking and cleaning the ground wafer, then etching for four times, finally dehydrating and drying, and entering the next procedure.
Further, the etching method specifically comprises the following steps:
soaking and cleaning: soaking the ground wafer and the clamping plug in water;
primary corrosion: preparing a dilute nitric acid solution with the mass fraction of 10%, fishing out the wafer from water, putting the wafer into the dilute nitric acid solution, carrying out primary corrosion, and cleaning and soaking the wafer by using deionized water after the corrosion is finished;
secondary corrosion: respectively measuring hydrogen peroxide and dilute sulfuric acid, stirring and mixing uniformly to obtain a first mixed solution, adding the wafer subjected to primary corrosion into the first mixed solution for secondary corrosion, and cleaning and soaking the wafer with deionized water after the corrosion is finished;
and (3) third corrosion: preparing an etching solution according to the proportion of claim 1 or 2, adding the wafer subjected to secondary etching into the etching solution, and cleaning and soaking the wafer by using deionized water after the etching is finished;
four times of corrosion: respectively measuring citric acid and hydrogen peroxide, adding into deionized water, stirring and mixing uniformly to obtain a second mixed solution, placing the wafer subjected to the three-time corrosion into the second mixed solution, and cleaning and soaking the wafer with the deionized water after the corrosion is finished;
dewatering and drying: and soaking the wafer subjected to the four-time corrosion in alcohol for dehydration, fishing out after the dehydration is finished, drying, and entering the next working procedure.
Compared with the traditional etching process, the four times of etching is carried out, and the improvement according to the invention can greatly improve the production efficiency of the wafer and reduce the occurrence of the chemical printing and the dirty printing. The cleaning effect of the wafer is more obvious
Further, the corrosion time of the primary corrosion is 10-20s, and the corrosion temperature is 25-35 ℃.
Further, in the mixed solution I, the mass ratio of hydrogen peroxide to dilute sulfuric acid is 20-25: 1.
Further, the corrosion time of the secondary corrosion is 20-30s, and the corrosion temperature is 25-30 ℃.
Further, the corrosion time of the third corrosion is 3-5min, and the corrosion temperature is 25-30 ℃.
Further, the volume ratio of the citric acid to the hydrogen peroxide to the deionized water in the mixed solution II is 1-1.5: 1-2: 3-5.
Furthermore, the corrosion time of the four times of corrosion is 2-3min, and the corrosion temperature is 25-30 ℃.
The invention has the beneficial effects that:
1. the invention discloses a wafer etching solution, which can accelerate the dropping amount of a wafer and avoid the situations of slow dropping amount and uneven dropping amount by optimizing a formula, thereby greatly improving the production efficiency of the wafer, reducing the occurrence of chemical printing and dirty printing and ensuring that the cleaning effect of the wafer is more obvious.
2. The wafer etching method of the invention can clean the residual impurities on the surface before the third etching of the volume removal etching through the steps of the first etching and the second etching, and etch the grinding fluid on the surface, and through the strong oxidation of nitric acid, the substances which can not be cleaned in the corrosive liquid can be effectively cleaned by the strong corrosion effect, the three times of corrosion are combined, so that the corrosion effect of the surface of the wafer is better, and the cleaning effect of the surface of the wafer is mainly carried out through four corrosion steps, after the etching is carried out after the amount is removed in the third etching step, part of the impurities of the grinding fluid and the impurities of the indium phosphide are remained on the wafer, and the citric acid contained in the mixed solution II can precipitate metal substances, so that impurities are dispersed and suspended, the impurities on the surface of the wafer can be quickly cleaned by using deionized water, and finally, the wafer is dehydrated and dried by combining alcohol, so that the possibility of the impurities on the surface of the wafer is effectively reduced.
Detailed Description
The present invention will be described in detail with reference to specific examples below:
the invention relates to a wafer etching solution which comprises the following components in percentage by volume: 70-77% of hydrogen peroxide, 3.8-5% of concentrated sulfuric acid, 7.7-10% of glacial acetic acid and 9.5-11.5% of concentrated hydrochloric acid, wherein the wafer is etched by using the etching solution provided by the invention, and the formula composition of the etching solution in the first to fifth embodiments is shown in table 1:
TABLE 1
| Hydrogen peroxide (%) | Concentrated sulfuric acid (%) | Glacial acetic acid (%) | Concentrated hydrochloric acid (%) | |
| Example one | 77 | 3.8 | 7.7 | 11.5 |
| Example two | 73.5 | 5 | 10 | 11.5 |
| EXAMPLE III | 75 | 4 | 10 | 11 |
| Example four | 76 | 5 | 9 | 10 |
| EXAMPLE five | 80 | - | 8 | 12 |
| EXAMPLE six | 83.4 | 4 | - | 12.6 |
| EXAMPLE seven | 87 | 4.2 | 8.8 | - |
| Example eight | 70 | 3.8 | 7.7 | 18.5 |
The wafers were etched using the etching solutions of the formulations in table 1, all using the following methods:
soaking and cleaning: soaking the ground wafer and the clamping plug in water;
primary corrosion: preparing a dilute nitric acid solution with the mass fraction of 10%, fishing out the wafer from water, placing the wafer in the dilute nitric acid solution, carrying out first corrosion for 10-20s at the temperature of 25-35 ℃, preferably carrying out first corrosion for 15s at the temperature of 30 ℃, shaking up and down in the corrosion process to uniformly corrode the surface of the wafer, and cleaning and soaking the wafer by using deionized water after the corrosion is finished;
secondary corrosion: respectively measuring hydrogen peroxide and dilute sulfuric acid according to the mass ratio of 20:1, stirring and mixing uniformly to obtain a mixed solution I, adding the wafer subjected to primary corrosion into the mixed solution I, carrying out secondary corrosion for 20-30s at the temperature of 25-30 ℃, preferably carrying out primary corrosion for 25s at the temperature of 25 ℃, rotating the wafer in the corrosion process to enable the wafer to be corroded uniformly, and cleaning and soaking the wafer by using deionized water after the corrosion is finished;
and (3) third corrosion: respectively measuring hydrogen peroxide, concentrated sulfuric acid, glacial acetic acid and concentrated hydrochloric acid according to the proportion in the table 1, stirring and mixing uniformly to prepare corrosion liquid, adding a wafer subjected to secondary corrosion into the corrosion liquid, carrying out third corrosion at the temperature of 25-30 ℃, preferably at the temperature of 30 ℃, putting the wafer into the corrosion liquid to rotate the wafer for 1min by adopting an intermittent corrosion mode, taking out the wafer to be washed by deionized water, cleaning, putting the wafer into the corrosion liquid to rotate the wafer for 1min after cleaning, repeating the processes of corrosion and taking out for washing, and sequentially circulating for 3-5 times, wherein the total time for corroding the wafer is 3-5min, preferably 5min, and washing and soaking the wafer by using deionized water after the corrosion is finished;
four times of corrosion: respectively measuring citric acid, hydrogen peroxide and deionized water according to the volume ratio of 1:1:3, uniformly stirring and mixing to obtain a mixed solution II, placing the wafer subjected to three times of corrosion into the mixed solution II, carrying out fourth time of corrosion at the temperature of 25-30 ℃, preferably at the temperature of 25 ℃, shaking the wafer to ensure that the surface of the wafer is corroded, then placing the wafer into a corrosion solution to soak for 2-3min, preferably for 3min, and cleaning and soaking the wafer by using deionized water after the corrosion is finished;
dewatering and drying: and soaking the wafer subjected to the four-time corrosion in alcohol for dehydration for 30s, fishing out after the dehydration is finished, drying, and entering the next working procedure.
The amount of the wafer removed and the surface of the wafer after the etching were observed and detected, and the detection results are shown in table 2:
TABLE 2
As can be seen from the above table, in the first to sixth embodiments, the recipe of the etching solution affects the etching process of the whole wafer, in the etching process, when any one of concentrated sulfuric acid, glacial acetic acid, and concentrated hydrochloric acid is lacked, the etching rate of the wafer is reduced, and the etching cleaning condition of the wafer surface is affected, and in the preparation process of the etching solution, the reaction temperature of the etching solution is affected by the increase of the components of hydrochloric acid and sulfuric acid, so that the temperature of the solution is not easily controlled, the etching rate of the wafer is greatly increased, the amount of the wafer surface is not uniform, and the wafer is not cleaned cleanly.
Comparative example 1
Compared with the method of the application, the difference of the comparative example is that the etching step is not carried out once, and the method specifically comprises the following steps:
soaking and cleaning: soaking the ground wafer and the clamping plug in water;
primary corrosion: respectively measuring hydrogen peroxide and dilute sulfuric acid according to the mass ratio of 20:1, stirring and mixing uniformly to obtain a mixed solution I, adding the wafer subjected to primary corrosion into the mixed solution I, carrying out primary corrosion for 20s at the temperature of 25-30 ℃, rotating the wafer in the corrosion process to enable the wafer to be corroded uniformly, and cleaning and soaking the wafer by using deionized water after the corrosion is finished;
secondary corrosion: respectively measuring hydrogen peroxide, concentrated sulfuric acid, glacial acetic acid and concentrated hydrochloric acid according to the proportion of the first embodiment in the table 1, stirring and mixing uniformly to prepare an etching solution, adding the wafer subjected to primary etching into the etching solution, performing secondary etching at the temperature of 25-30 ℃, placing the wafer in the etching solution in an intermittent etching mode to etch for 1min, taking out the wafer to clean with deionized water, placing the wafer in the etching solution to etch for 1min, repeating the etching and taking out the cleaning processes for 5 times, wherein the total time of etching the wafer is 5min, and cleaning and soaking the wafer with deionized water after etching;
and (3) third corrosion: respectively measuring citric acid, hydrogen peroxide and deionized water according to the volume ratio of 1:1:3, stirring and mixing uniformly to obtain a mixed solution II, placing the wafer subjected to secondary corrosion in the mixed solution II, carrying out third corrosion at the temperature of 25-30 ℃, shaking the wafer firstly to ensure that the surface of the wafer is corroded, then placing the wafer in a corrosion solution to soak for 3min, and cleaning and soaking the wafer by using the deionized water after the corrosion is finished;
dewatering and drying: and soaking the wafer subjected to the three-time corrosion in alcohol for dehydration for 30s, fishing out after the dehydration is finished, drying, and entering the next working procedure.
Comparative example No. two
Compared with the method, the comparative example has the following difference that the secondary etching step is not carried out in the process of etching the wafer, and specifically comprises the following steps:
soaking and cleaning: soaking the ground wafer and the clamping plug in water;
primary corrosion: preparing a dilute nitric acid solution with the mass fraction of 10%, fishing out the wafer from water, placing the wafer in the dilute nitric acid solution, carrying out first corrosion for 20s at the temperature of 25-35 ℃, shaking up and down in the corrosion process to uniformly corrode the surface of the wafer, and cleaning and soaking the wafer by using deionized water after the corrosion is finished;
secondary corrosion: respectively measuring hydrogen peroxide, concentrated sulfuric acid, glacial acetic acid and concentrated hydrochloric acid according to the proportion of the first embodiment in the table 1, stirring and mixing uniformly to prepare an etching solution, adding the wafer subjected to primary etching into the etching solution, performing secondary etching at the temperature of 25-30 ℃, placing the wafer in the etching solution in an intermittent etching mode to etch for 1min, taking out the wafer to clean with deionized water, placing the wafer in the etching solution to etch for 1min, repeating the etching and taking out the cleaning processes for 5 times, wherein the total time of etching the wafer is 5min, and cleaning and soaking the wafer with deionized water after etching;
and (3) third corrosion: respectively measuring citric acid, hydrogen peroxide and deionized water according to the volume ratio of 1:1:3, stirring and mixing uniformly to obtain a mixed solution II, placing the wafer subjected to secondary corrosion in the mixed solution II, carrying out third corrosion at the temperature of 25-30 ℃, shaking the wafer firstly to ensure that the surface of the wafer is corroded, then placing the wafer in a corrosion solution to soak for 3min, and cleaning and soaking the wafer by using the deionized water after the corrosion is finished;
dewatering and drying: and soaking the wafer subjected to the three-time corrosion in alcohol for dehydration for 30s, fishing out after the dehydration is finished, drying, and entering the next working procedure.
Comparative example No. three
Compared with the method, the comparative example has the following difference that the secondary etching step is not carried out in the process of etching the wafer, and specifically comprises the following steps:
soaking and cleaning: soaking the ground wafer and the clamping plug in water;
primary corrosion: preparing a dilute nitric acid solution with the mass fraction of 10%, fishing out the wafer from water, placing the wafer in the dilute nitric acid solution, carrying out first corrosion for 20s at the temperature of 25-35 ℃, shaking up and down in the corrosion process to uniformly corrode the surface of the wafer, and cleaning and soaking the wafer by using deionized water after the corrosion is finished;
secondary corrosion: respectively measuring hydrogen peroxide and dilute sulfuric acid according to the mass ratio of 20:1, stirring and mixing uniformly to obtain a mixed solution I, adding the wafer subjected to primary corrosion into the mixed solution I, carrying out secondary corrosion for 20s at the temperature of 25-30 ℃, rotating the wafer in the corrosion process to enable the wafer to be corroded uniformly, and cleaning and soaking the wafer by using deionized water after the corrosion is finished;
and (3) third corrosion: respectively measuring hydrogen peroxide, concentrated sulfuric acid, glacial acetic acid and concentrated hydrochloric acid according to the proportion of the first embodiment in the table 1, stirring and mixing uniformly to prepare an etching solution, adding a wafer subjected to secondary etching into the etching solution, carrying out third etching at the temperature of 25-30 ℃, placing the wafer in the etching solution in an intermittent etching mode to etch for 1min, taking out the wafer to clean with deionized water, placing the wafer in the etching solution to etch for 1min, repeating the etching and taking out the cleaning processes for 5 times, wherein the total time of etching the wafer is 5min, and cleaning and soaking the wafer with deionized water after etching;
dewatering and drying: and soaking the wafer subjected to the three-time corrosion in alcohol for dehydration for 30s, fishing out after the dehydration is finished, drying, and entering the next working procedure.
The amount of the wafer removed and the surface of the wafer after the etching were observed and detected, and the detection results are shown in table 3:
TABLE 3
As shown in Table 3, the etching method of the present invention as a whole may increase the failure rate of wafer etching in the absence of any one of the etching steps, and the etching of the wafer surface is more uniform, clean and smooth under the combined action of the four etching steps, and meets the requirements of customers.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims. The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.
Claims (10)
1. The wafer etching solution is characterized by comprising the following components in percentage by volume: 70 to 77 percent of hydrogen peroxide, 3.8 to 5 percent of concentrated sulfuric acid, 7.7 to 10 percent of glacial acetic acid and 9.5 to 11.5 percent of concentrated hydrochloric acid.
2. The wafer etching solution of claim 1, wherein the etching solution comprises the following components in percentage by volume: 77% of hydrogen peroxide, 3.8% of concentrated sulfuric acid, 7.7% of glacial acetic acid and 11.5% of concentrated hydrochloric acid.
3. The etching method of the wafer is characterized in that the wafer after being ground is soaked and cleaned, then is etched for four times, and finally is dehydrated and dried to enter the next procedure.
4. The method of claim 3, wherein the etching method comprises the following steps:
soaking and cleaning: soaking the ground wafer and the clamping plug in water;
primary corrosion: preparing a dilute nitric acid solution with the mass fraction of 10%, fishing out the wafer from water, putting the wafer into the dilute nitric acid solution, carrying out primary corrosion, and cleaning and soaking the wafer by using deionized water after the corrosion is finished;
secondary corrosion: respectively measuring hydrogen peroxide and dilute sulfuric acid, stirring and mixing uniformly to obtain a first mixed solution, adding the wafer subjected to primary corrosion into the first mixed solution for secondary corrosion, and cleaning and soaking the wafer with deionized water after the corrosion is finished;
and (3) third corrosion: preparing an etching solution according to the proportion of claim 1 or 2, adding the wafer subjected to secondary etching into the etching solution, and cleaning and soaking the wafer by using deionized water after the etching is finished;
four times of corrosion: respectively measuring citric acid and hydrogen peroxide, adding into deionized water, stirring and mixing uniformly to obtain a second mixed solution, placing the wafer subjected to the three-time corrosion into the second mixed solution, and cleaning and soaking the wafer with the deionized water after the corrosion is finished;
dewatering and drying: and soaking the wafer subjected to the four-time corrosion in alcohol for dehydration, fishing out after the dehydration is finished, drying, and entering the next working procedure.
5. The method as claimed in claim 4, wherein the etching time of the first etching is 10-20s, and the etching temperature is 25-35 ℃.
6. The method as claimed in claim 4, wherein the mass ratio of hydrogen peroxide to dilute sulfuric acid in the first mixed solution is 20-25: 1.
7. The method as claimed in claim 4, wherein the etching time of the second etching is 20-30s, and the etching temperature is 25-30 ℃.
8. The method as claimed in claim 4, wherein the etching time of the third etching is 3-5min, and the etching temperature is 25-30 ℃.
9. The method of claim 4, wherein the volume ratio of the citric acid to the hydrogen peroxide to the deionized water in the second mixed solution is 1-1.5: 1-2: 3-5.
10. The method as claimed in claim 4, wherein the etching time of the fourth etching is 2-3min, and the etching temperature is 25-30 ℃.
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