CN113621375A - Quartz wafer etching additive and preparation method thereof - Google Patents
Quartz wafer etching additive and preparation method thereof Download PDFInfo
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- CN113621375A CN113621375A CN202110873612.1A CN202110873612A CN113621375A CN 113621375 A CN113621375 A CN 113621375A CN 202110873612 A CN202110873612 A CN 202110873612A CN 113621375 A CN113621375 A CN 113621375A
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Abstract
A quartz wafer etching additive comprises the following components in percentage by weight: 12-25% of phase stable solvent, 1-5% of penetrating agent, 4-8% of dispersing agent, 20-30% of chelating corrosion inhibitor, 15-25% of wetting agent, 8-12% of foam breaking agent, 10-20% of concave-convex point inhibitor and 1-2% of settling agent. The etching solution prepared by the additive has high removal rate, stable speed and long service life, can complete the etching operation after being soaked at normal temperature, and the etched wafer is easy to clean by water; the etching solution added with the additive has the advantages that the surface microscopic appearance of the etched wafer is flat and smooth, the thickness tolerance is less than or equal to 0.2um, the good dispersion wetting and sedimentation functions of the additive can reduce the problems of scratches and concave-convex points formed by uneven etched powder residues, suspension in the solution and adsorption on the surface of the wafer, the additive can effectively inhibit the volatilization of acid and the loss of the etching acid, and the odor is mild and has no stimulation.
Description
Technical Field
The invention relates to the technical field of semiconductor material processing, in particular to a quartz wafer etching additive and a preparation method thereof.
Background
Quartz crystal is an electronic material with the second use amount to monocrystalline silicon, is used for manufacturing electronic components for selecting and controlling frequency, is widely applied to various fields of electronic information industry, such as color TV, air conditioner, computer, DVD, wireless communication and the like, is increasingly applied to high-performance electronic equipment and digital equipment, and is a necessary material for producing SMD (surface mounted device) frequency chips and mobile phone frequency chips.
After the quartz plate is subjected to coarse, medium and fine grinding, no matter how fine the final grinding material is, the surface of the wafer always has a damage layer formed by the grinding material and quartz particles, if the damage layer is not removed, the grinding material and the quartz particles gradually fall off in the resonance process, so that the frequency is deviated, meanwhile, the firmness of an electrode film is also reduced, and in addition, the damage layer can also enable the surface of the wafer to generate a stress relaxation effect, so that the aging rate of the quartz resonator is increased. Therefore, the etching process is essential for the manufacturing process of quartz crystal.
At present, hydrofluoric acid aqueous solution with the mass concentration of 5% -30% or ammonium bifluoride aqueous solution with the mass concentration of 10% -50% is commonly used in the industry for rolling/rotating etching, a damaged layer can be effectively removed, and the production requirement is basically met, but the process has the biggest defect that the requirements on equipment, etching time and corrosive liquid concentration are extremely high, and the frequency of a quartz wafer subjected to etching corrosion is close to or exceeds the upper limit by more than 40%. At present, the production size of semiconductor materials is smaller and thinner, and the yield of the etching process is in need of improvement.
In the use process of the quartz wafer etching solution, hydrofluoric acid and ammonium bifluoride can generate selective corrosion silicon oxide, a large number of concave-convex points, lamination marks and other defects can be formed on the surface of the wafer, and the active ingredients of the etching solution are consumed too fast, so that the production cost is increased, and the environment is polluted.
CN 1648287A discloses a high-purity alkali etching solution for etching silicon wafers and an alkali etching method for silicon wafers, the invention scheme is that the solution contains 40-60% by weight of sodium hydroxide and 0.01-10% by weight of nitrate and/or nitrite, the scheme needs to be heated to 85 ℃, the residual concentrated alkali solution on the surface after treatment is extremely difficult to wash clean, the high-temperature solution is easy to cause wafer fracture and deformation, the etching rate is low at 2.45-3.34 um/min, and the surface flatness of the thickness tolerance is slightly poor at 0.23-0.38 um.
CN 106024675A discloses a semiconductor silicon wafer etching solution and an etching method thereof, the scheme is that nitric acid, hydrofluoric acid and glacial acetic acid are mixed according to the volume ratio of 4-14: 6-18, the concentration of the nitric acid is 65-70%, the concentration of the hydrofluoric acid is 45-55%, the concentration of the glacial acetic acid is 95-99%, inert gas is introduced at the temperature of-12 ℃ to-8 ℃ in the etching process, the etching acid solution is fast in loss and short in service life, etching residues are poor in dispersion and sedimentation, and used acids are mixed with stock solutions and are pungent in smell.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention needs to provide an etching solution additive which has high removal rate, stable speed and long service life, the etched wafer is easy to clean by water, the etching solution additive can finish the etching operation by soaking at normal temperature, the surface of the etched wafer has flat and smooth microscopic appearance, the thickness tolerance is less than or equal to 0.2um, the etching rate is more than or equal to 4.00um/min, the etching solution additive has good dispersion wetting and sedimentation functions, the problems of scratches and concave-convex points formed by uneven etched powder slag, suspension in the solution and adsorption on the surface of the wafer can be solved, the acid volatilization and the etching acid loss can be effectively inhibited, and the odor is mild and has no stimulation.
The purpose of the invention is realized by the following technical scheme: a quartz wafer etching additive comprises the following components in percentage by mass: 12-25% of phase stable solvent, 1-5% of penetrating agent, 4-8% of dispersing agent, 20-30% of chelating corrosion inhibitor, 15-25% of wetting agent, 8-12% of foam breaking agent, 10-20% of concave-convex point inhibitor and 1-2% of settling agent.
The phase stable solvent is one or a combination of ultrapure water, absolute ethyl alcohol, n-propyl alcohol and isopropyl alcohol.
The penetrating agent is one or more of JFC (sea rock flower), JFC-G (sea rock flower), JFC-E (sea rock flower), JFC-M (sea rock flower), 10M08(CECA special chemical industry), Softanol-90 (Japanese catalyst) and Softanol-70 (Japanese catalyst).
The dispersing agent is one or more of secondary alkyl sodium sulfonate, sodium dodecyl benzene sulfonate, sodium naphthol sulfonate, sodium butyl naphthalene sulfonate, sodium octyl sulfonate and carboxylate-sulfonate-nonionic terpolymer.
The chelating corrosion inhibitor is one or more of iminodisuccinic acid sodium, N-diethyl propyne amine sulfate, nitrilotriacetic acid sodium salt, polyaspartic acid sodium salt, potassium silicate (M2.4) and potassium fluosilicate.
The wetting agent is formed by compounding at least two of surfadol440 (Chongqing aikemi), surfadol465 (Chongqing aikemi), surfadol541 (Chongqing aikemi) and surfadol604 (Chongqing aikemi).
The foam breaking agent is prepared by compounding at least two of 3, 5-dimethyl-1-hexyne-3-ol, 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol, PE6400 and PE 6800.
The concave-convex point inhibitor is
SF-921A (Guangzhou Damei),
SF-337B (Kyowa Bigmei), Actyflon-S200 (Harbin snow good fluorine silicon chemistry), TEGO Twin 4100 (Germany Digao), TEGO Wet 251 (Germany Digao), Silsoft 860 (Germany Digao).
The settling agent is composed of one or more of cationic polyacrylamide, hydroxyethyl cellulose ether and hydroxypropyl cellulose ether.
A preparation method of a quartz wafer etching additive comprises the steps of using a temperature-controlled stirring liquid tank, weighing a specified amount of phase-state stable solvent according to mass percent, adding the solvent into the temperature-controlled stirring liquid tank, setting the temperature to normal temperature, weighing a dispersing agent and a chelating corrosion inhibitor according to mass percent after stirring at a stirring speed of 60-80r/min, and stirring for 20-25 minutes; heating to 50-60 ℃ under the condition of continuous stirring, stirring at constant temperature, setting the rotating speed at 200-220r/min, sequentially adding the penetrating agent and the wetting agent, stirring for 2-2.5 hours until the materials are completely and uniformly dissolved, adjusting the stirring rotating speed to 120-150r/min, setting the temperature at 25-35 ℃, adding the concave-convex point inhibitor, the foam breaker and the settling agent after the temperature is reduced to 25-28 ℃, stirring for 30 minutes, and uniformly dissolving to obtain the finished product of the quartz wafer etching additive.
The invention has the advantages and beneficial effects that:
adding the etching solution additive into hydrofluoric acid or ammonium bifluoride aqueous solution for use; the additive can effectively improve the etching selectivity of the etching solution after being added, and avoid the generation of concave convex points after the wafer is etched.
The surface tension of the etching solution is reduced from 75N/m to 23N/m by adding the additive, and the additive can ensure that the additive penetrates into a wafer gap to avoid lamination print generation even if the conditions of factory equipment are poor and a wafer cannot be scattered by mechanical force in a rolling etching process.
The addition of the additive can ensure that the thickness tolerance of the surface of the etched wafer is less than or equal to 0.2um, can effectively improve the etching rate, and has stable and no obvious reduction of the rate and long service life in the use process.
The additive can effectively reduce the volatilization of the etching acid liquor, inhibit the pungent odor diffusion of the acid liquor and effectively improve the production environment.
The etching solution prepared by the additive has high removal rate, stable speed and long service life, can complete the etching operation after being soaked at normal temperature, and the etched wafer is easy to clean by water; the etching solution added with the additive has the advantages that the surface microscopic appearance of the etched wafer is flat and smooth, the thickness tolerance is less than or equal to 0.2um, the good dispersion wetting and sedimentation functions of the additive can reduce the problems of scratches and concave-convex points formed by uneven etched powder residues, suspension in the solution and adsorption on the surface of the wafer, the additive can effectively inhibit the volatilization of acid and the loss of the etching acid, and the odor is mild and has no stimulation.
Drawings
FIG. 1: the additive of example 3 was added to the etching solution to etch the wafer and then the surface of the wafer was magnified.
FIG. 2: magnifier picture of the wafer surface after etching the wafer with 8% hydrofluoric acid solution (acid solution 2 in table 2).
FIG. 3: comparative example 3 magnifier picture of the wafer surface after the etching solution etched the wafer.
Detailed Description
The invention relates to a quartz wafer etching additive which is characterized by comprising the following materials in percentage by mass: 12-25% of phase stable solvent, 1-5% of penetrating agent, 4-8% of dispersing agent, 20-30% of chelating corrosion inhibitor, 15-25% of wetting agent, 8-12% of foam breaking agent, 10-20% of concave-convex point inhibitor and 1-2% of settling agent.
The phase stable solvent is one or a combination of ultrapure water, absolute ethyl alcohol, n-propyl alcohol and isopropyl alcohol.
The penetrant is one or more of JFC (sea rock flower), JFC-G (sea rock flower), JFC-E (sea rock flower), JFC-M (sea rock flower), 10M08(CECA special chemical industry), Softanol-90 (Japanese catalyst) and Softanol-70 (Japanese catalyst), and the dispersant is one or more of secondary alkyl sodium sulfonate, sodium dodecyl benzene sulfonate, sodium naphthol sulfonate, sodium butyl naphthalene sulfonate, sodium octyl sulfonate and carboxylate-sulfonate-nonionic terpolymer.
The chelating corrosion inhibitor is one or more of iminodisuccinic acid sodium, N-diethyl propyne amine sulfate, nitrilotriacetic acid sodium salt, polyaspartic acid sodium salt, potassium silicate (M2.4) and potassium fluosilicate.
The wetting agent is formed by compounding at least two of surfadol440 (Chongqing aikemi), surfadol465 (Chongqing aikemi), surfadol541 (Chongqing aikemi) and surfadol604 (Chongqing aikemi).
The foam breaking agent is prepared by compounding at least two of 3, 5-dimethyl-1-hexyne-3-alcohol, 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol, PE6400 (basf) and PE6800 (basf).
The concave-convex point inhibitor is
SF-921A (Guangzhou Damei),
SF-337B (Kyowa Bigmei), Actyflon-S200 (Harbin snow good fluorine silicon chemistry), TEGO Twin 4100 (Germany Digao), TEGO Wet 251 (Germany Digao), Silsoft 860 (Germany Digao).
The settling agent is one or more of Cationic Polyacrylamide (CPAM), hydroxyethyl cellulose ether (HEC) and hydroxypropyl cellulose ether (HPC).
The present invention will be described in more detail with reference to examples, although the present invention is not limited thereto.
Examples 1 to 10: using a No. 1 temperature-controlled stirring liquid tank according to the mixture ratio of a formula table 1, weighing a specified amount of phase-state stable solvent according to the mass percentage, adding the phase-state stable solvent into the No. 1 tank, setting the temperature and the normal temperature, weighing the dispersing agent and the chelating corrosion inhibitor according to the mass percentage after stirring at a stirring speed of 60r/min, and stirring for 20 minutes; heating to 50 ℃ under the condition of continuous stirring, stirring at constant temperature, setting the rotating speed at 200r/min, sequentially adding a penetrating agent and a wetting agent, stirring for 2 hours until the materials are completely and uniformly dissolved, adjusting the stirring rotating speed to 120r/min, setting the temperature at 25 ℃, adding a concave-convex point inhibitor, a foam breaker and a settling agent after the temperature is reduced to 25 ℃, stirring for 30 minutes, and uniformly dissolving to obtain a finished product of the quartz wafer etching additive.
Table 1 examples of formulations for several quartz wafer etching additives
With the use concentration of 0.5% as the actual addition concentration, a 15% aqueous solution of ammonium bifluoride (acid 1 in the following table), an 8% aqueous solution of hydrofluoric acid (acid 2 in the following table), the CN 1648287a version of the invention as comparative example 3, and the CN 106024675a version of the invention as comparative example 4; the etching solution containing the additive obtained in examples 1 to 15 was subjected to comparative tests, the average etching rate per 5 hours was measured, the average tolerance value of the thickness of the etched product was measured, and the total amount of wafers treated with the etching solution, the ratio of concave and convex points after etching, and the ratio of scratches were recorded, and the comparative conditions are shown in table 2.
The experimental data test evaluation method comprises the following steps:
(1) etching speed (average thickness before etching-average thickness after etching)/etching time
(2) Thickness tolerance: maximum post-etch average thickness-minimum post-etch average thickness
(3) The wafers used in the test process are all products processed by machines with the same size and model and the same type
(4) Counting concave and convex points by observing surface morphology through EDS
(5) And (4) calculating the scratch proportion by observing the surface appearance by using a quadratic element imager
TABLE 2 data for several quartz wafer etching additive applications
As can be seen from table 2, the effect of each example is significantly improved compared to the comparative example by adding the etching additive for quartz wafers of the present invention, wherein the effects of the additives of examples 1 to 10 are significantly improved in controlling the concave and convex points, reducing scratches, increasing etching flatness, and prolonging the service life, and the magnifier pictures of the surface of the wafer after the additives of examples 1, 2, and 4 to 10 are added to the etching solution to etch the wafer are substantially the same as the drawings of example 3, and the effects of concave and convex points, less scratches, and increasing etching flatness are achieved.
In example 11, the phase-stable solvent was removed, and the prepared additive solution itself had sediment and was easily delaminated, and was difficult to use.
Example 12 the penetrant was removed, and the flatness of the wafer surface was slightly deteriorated after the treatment, resulting in a smaller amount of treatment.
In example 13, the dispersant was removed, the wafer scratch ratio was significantly increased, and the concave-convex ratio was increased after the treatment.
Example 14 removes the chelating corrosion inhibitor, the scratch ratio of the wafer after treatment is obviously improved, the concave-convex point ratio is increased, and the service life of the solution is shortened.
Example 15, in which the wetting agent was removed, the flatness of the wafer surface after treatment was poor and the raised ratio of asperities and scratches was significant.
Example 16 the defoaming agent was removed and the surface flatness was poor.
In example 17, the irregularity inhibitor was removed, the solution life was shortened, and the irregularity and scratch ratio were sharply increased.
Example 18, with the settling agent removed, the scratch rate increased significantly.
Example 19 the ratio of the concavo-convex point inhibitor is increased to 24% which exceeds the normal ratio by 4%, and the test comprehensive effect slightly declines compared with the normal ratio range.
Example 20 the ratio of the concave-convex inhibitor is reduced to 6% and is lower than the normal ratio of 4%, and the proportion of concave-convex and scratch on the surface of the wafer after treatment is obviously increased.
Taking a 15% aqueous solution of ammonium bifluoride base liquid (hereinafter, conveniently expressed as acid solution 1) adopted in mass production in the industry at present as a comparison example, the addition mass concentration of a quartz wafer etching additive (hereinafter, conveniently expressed as additive) is explored in example 1, and test data are shown in Table 3
TABLE 3 additive concentration experimental data for quartz wafer etch additives
As can be seen from Table 3, by adding the quartz wafer etching additive of the invention, the etching efficiency is obviously improved, the etching speed is kept stable, the etching precision is higher, the etched surface tends to be uniform, the comprehensive performance is much higher than the effect of mass production of the ammonium bifluoride 15% aqueous solution at present, the optimum addition amount of the ammonium bifluoride 15% aqueous solution of the invention is 0.5% mass concentration, and the addition amount is too high, which can cause the etching speed to be greatly reduced.
The etching solution additive is added on the basis of keeping the original etching solution unchanged, is used for etching quartz wafers, solves the problems of concave-convex points and lamination marks formed on the surfaces of wafers etched by the traditional process in the field of semiconductor material processing, reduces the equipment investment cost, prolongs the service life of the etching solution, prolongs the liquid changing period, reduces the production cost, effectively improves the surface quality of the etched wafers, provides good binding force for coating films of the quartz wafers in the post-process, and plays a positive role in improving the overall efficiency and benefits of factories.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and all simple modifications, equivalent variations and modifications made to the above embodiment according to the technical spirit of the present invention still fall within the scope of the technical solution of the present invention.
Claims (10)
1. The quartz wafer etching additive is characterized by comprising the following materials in percentage by mass: 12-25% of phase stable solvent, 1-5% of penetrating agent, 4-8% of dispersing agent, 20-30% of chelating corrosion inhibitor, 15-25% of wetting agent, 8-12% of foam breaking agent, 10-20% of concave-convex point inhibitor and 1-2% of settling agent.
2. The quartz wafer etching additive of claim 1, wherein the phase stable solvent is one or more of ultrapure water, absolute ethyl alcohol, n-propanol and isopropanol.
3. The quartz wafer etching additive of claim 1, wherein the infiltrant is comprised of one or more of JFC, JFC-G, JFC-E, JFC-M, 10M08, Softanol-90, Softanol-70.
4. The quartz wafer etching additive of claim 1, wherein the dispersant is comprised of one or more of secondary sodium alkyl sulfonate, sodium dodecyl benzene sulfonate, sodium naphthol sulfonate, sodium butyl naphthalene sulfonate, sodium octyl sulfonate, carboxylate-sulfonate-nonionic terpolymer.
5. The quartz wafer etching additive of claim 1, wherein the chelating corrosion inhibitor is one or more of sodium iminodisuccinate, N-diethylpropynylamine sulfate, sodium nitrilotriacetate, sodium polyaspartate, potassium silicate (M = 2.4), potassium fluorosilicate.
6. The quartz wafer etching additive of claim 1, wherein the wetting agent is a combination of at least two of sufadol 440, sufadol 465, sufadol 541, and sufadol 604.
7. The quartz wafer etching additive of claim 1, wherein the foam breaker is a combination of at least two of 3, 5-dimethyl-1-hexyne-3-ol, 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol, PE6400, and PE 6800.
8. The concave-convex point inhibitor according to claim 1, characterized in that: the concave-convex point inhibitor is formed by compounding at least two of SiFast SF-921A, SiFast SF-337B, Actyflon-S200, TEGO Twin 4100, TEGO Wet 251 and Silsoft 860.
9. The quartz wafer etching additive of claim 1, wherein the settling agent is comprised of one or more of cationic polyacrylamide, hydroxyethyl cellulose ether, hydroxypropyl cellulose ether.
10. A method for preparing the quartz wafer etching additive according to any one of claims 1 to 9, wherein a temperature-controlled stirring liquid tank is used, a specified amount of phase-state stable solvent is weighed according to the mass percentage and then added into the temperature-controlled stirring liquid tank, the temperature and the normal temperature are set, and after the stirring speed is 60 to 80r/min, the dispersant and the chelating corrosion inhibitor are weighed according to the mass percentage and stirred for 20 to 25 minutes; heating to 50-60 ℃ under the condition of continuous stirring, stirring at constant temperature, setting the rotating speed at 200-220r/min, sequentially adding the penetrating agent and the wetting agent, stirring for 2-2.5 hours until the materials are completely and uniformly dissolved, adjusting the stirring rotating speed to 120-150r/min, setting the temperature at 25-35 ℃, adding the concave-convex point inhibitor, the foam breaker and the settling agent after the temperature is reduced to 25-28 ℃, stirring for 30 minutes, and uniformly dissolving to obtain the finished product of the quartz wafer etching additive.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115011348A (en) * | 2022-06-30 | 2022-09-06 | 湖北兴福电子材料有限公司 | Aluminum nitride etching solution and application thereof |
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| CN115011348A (en) * | 2022-06-30 | 2022-09-06 | 湖北兴福电子材料有限公司 | Aluminum nitride etching solution and application thereof |
| CN115011348B (en) * | 2022-06-30 | 2023-12-29 | 湖北兴福电子材料股份有限公司 | Aluminum nitride etching solution and application thereof |
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