CN112251233B - Silicon etching solution for removing grinding lines - Google Patents
Silicon etching solution for removing grinding lines Download PDFInfo
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- 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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- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
- C09K13/08—Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound
Abstract
The invention relates to a silicon etching solution for removing grinding lines. The etching solution consists of nitric acid, hydroxylamine nitrate, fluorosulfonic acid, ammonium bifluoride, xenon difluoride, sulfuric acid, a thickening agent and deionized water. Wherein the thickening agent can be any one of polyacrylamide, hexanol, octanol, polyethylene glycol, polyvinylpyrrolidone and the like. In the invention, hydroxylamine nitrate reacts with fluorosulfonic acid to generate hydrofluoric acid, and xenon difluoride is slowly decomposed in an acidic environment to generate the hydrofluoric acid, so that the concentration of the hydrofluoric acid in the etching solution composition is increased, the temporal change of the etching solution composition can be inhibited, and the stable etching rate is maintained. The etching solution for removing the grinding lines can be directly used for the back roughening process of the grinding sheet, deeper mechanical grinding lines are etched, the working procedure of polishing and removing the grinding lines is omitted, the cost is saved, the production efficiency is improved, and meanwhile, the stable etching service life can be maintained.
Description
Technical Field
The invention belongs to the technical field of intersection of wet electronic chemicals and wafer back roughening processing, and particularly relates to a silicon etching solution for removing grinding lines.
Background
In the manufacture of integrated circuit chips, it is necessary to implant metal on the back of the silicon wafer, and this metal layer can be used as electrode, bonding, and heat conducting metal layer, thereby achieving the effects of heat dissipation and resistance reduction. However, the wafer back surface needs to be roughened before the back surface metallization process, otherwise, the silicon wafer surface is too smooth, metal ions are difficult to adhere and stay on the surface, and the metal layer is difficult to be tightly connected with the substrate, which results in peeling of the metal layer, increase of resistance, and influence on the reliability of the semiconductor device. Several silicon etching solutions have been proposed to roughen the back surface of a wafer, for example, patent documents 1 and 2. Patent document 1 has a low etching rate and a small removal amount per unit time, and is only applicable to silicon wafers treated with a chemical wafer thinning liquid, and cannot satisfy the etching of a mechanical polishing sheet with deep polishing lines. Thus, patent document 2 first uses 10 to 16% of HF and 20 to 30% of HNO 315% -25% of H2SO414-20% of H3PO4And 20% -30% of water to carry out damage etching and remove mechanical grinding marks; then 3 to 7 percent of HF and 3 to 7 percent of HNO are used375% -85% of H2SO45% -15% of water, if the silicon wafer is treated by the etching solution with the damage, the etching rate is too fast and difficult to control, so that the etching surface is not uniform, the stability of the liquid medicine is poor, and if the silicon wafer is etched by the etching solution with the rough surface, the grinding lines still appear after etching, so that two processes are needed. And because the process equipment for grinding silicon wafers of different manufacturers is different, the grinding lines of some silicon wafers are deep, and deep lines can be left if the silicon wafers are directly treated by the roughening liquid, so that the mechanical grinding lines are generally treated by the wafer thinning liquid before the back grinding liquid is used, and the manufacturing cost is increased by the long and complicated process.
Therefore, the grinding line removing etching solution can be directly used for the back roughening process of the grinding sheet, deeper mechanical grinding lines are etched, the working procedure of polishing and removing the grinding lines is omitted, the cost can be saved, and the production efficiency is improved.
Patent document 1: silicon wafer polishing solution CN 109913222A
Patent document 2: process for rough etching silicon solar cell CN 1411612A
Disclosure of Invention
In view of the above, the present invention provides a high etching rate etching solution for removing grinding lines, which can be directly applied to a mechanical grinding sheet with deep grinding lines, so as to shorten the process time, save the cost, and obtain a rough surface with a uniform and flat etching surface and no mechanical grinding line residue;
the high-service-life anti-abrasion etching solution provided by the invention can supplement the consumption of effective components, reduce the volatilization of effective gas and maintain stable etching life under the condition of higher etching rate.
In order to achieve the purpose, the technical scheme of the invention provides a silicon etching solution for removing grinding lines, which contains nitric acid, hydroxylamine nitrate, fluorosulfonic acid, ammonium bifluoride, xenon difluoride, sulfuric acid, a thickening agent and deionized water, and the etching solution is directly used for a back roughening process of a mechanical grinding sheet.
Wherein, the weight content of nitric acid in the silicon etching solution for removing the grinding lines is 3 to 7 percent; the weight content of hydroxylamine nitrate is 0.01-0.5%; the weight content of the fluorosulfonic acid is 0.1-1%; the weight content of the ammonium bifluoride is 4-8 percent; the weight content of xenon difluoride is 0.1-2%; the weight content of the sulfuric acid is 75-85 percent; the weight content of the thickening agent is 0.01 to 0.1 percent; the weight content of the deionized water is the balance.
Wherein, the thickening agent in the silicon etching solution for removing the grinding lines comprises at least one of polyacrylamide, hexanol, octanol, polyethylene glycol and polyvinylpyrrolidone; and preferably polyacrylamide or polyethylene glycol.
In the technical scheme of the invention, nitric acid is used as a main oxidant, and nitrous acid generated by the reaction of hydroxylamine nitrate and nitric acid improves the oxidation rate of silicon and supplements the consumption of nitric acid.
The fluorosulfonic acid reacts with hydroxylamine nitrate to produce hydroxylamine-O-sulfonic acid and hydrofluoric acid, which react as follows: FHO3S+NH2OH→NH2OSO2OH + HF, increasing the concentration of hydrofluoric acid in the etching solution compositionAnd a step of controlling the change of the etching liquid composition with time.
The ammonium bifluoride exists mainly in the form of difluoride in etching liquid, because difluoride can help the protonated hydroxyl group on the surface of silicon dioxide to be separated and HF2 -In the process, the bond angle of F-H-F is close to 180 degrees, so that fluorine can easily attack silicon atoms, and the dissolution rate of silicon dioxide is greatly improved.
The oxygen generated by the xenon difluoride slowly decomposing in an acid environment is used as an auxiliary oxidant to enhance the oxidation performance of the solution, and meanwhile, the xenon difluoride slowly decomposes in the acid environment to generate hydrofluoric acid, so that the consumption of the hydrofluoric acid in the etching solution composition is supplemented, and the stable etching rate is maintained.
The sulfuric acid provides oxidation reaction activation energy to enable the reaction to start rapidly, and bubbles generated in the corrosion process are attached to the surface of the silicon wafer to form a masking effect, so that a rough frosted surface is formed.
The thickening agent can be any one of polyacrylamide, hexanol, octanol, polyethylene glycol, polyvinylpyrrolidone and the like, increases the viscosity of the solution, influences the size, stability and the like of bubbles generated by nitrogen oxides and the like, increases the solubility of reactive gases, reduces the volatilization of effective components in the reaction process, and prolongs the service life of the etching solution. Meanwhile, the mass transfer resistance of the etching solution is increased due to the increase of the viscosity of the etching solution, and the etching rate of the wave crest is far greater than that of the wave trough, so that the etching surface is more and more flat.
The invention has the advantages and beneficial effects that: in the invention, nitrous acid generated by the reaction of hydroxylamine nitrate and nitric acid and oxygen generated by xenon difluoride are slowly decomposed in an acid environment, so that the oxidation rate of silicon is improved, ammonium bifluoride mainly exists in an etching solution in a bifluoride form, so that the dissolution rate of silicon dioxide is greatly improved, the etching rate is increased, the removal amount is improved, meanwhile, the thickening agent increases the viscosity of the etching solution, the mass transfer resistance of the etching solution is increased, the etching rate of a wave crest is far greater than that of a wave trough, the surface roughness is reduced, and the etched surface is more and more smooth. Therefore, the method can be directly used for the back roughening process of the grinding sheet, deeper mechanical grinding lines are etched, the working procedure of polishing and removing the grinding lines is omitted, the cost is saved, and the production efficiency is improved. In addition, nitrous acid generated by the reaction of hydroxylamine nitrate and nitric acid maintains the oxidability of nitric acid, hydrofluoric acid generated by the reaction of strong amine nitrate and fluorosulfonic acid and xenon difluoride are slowly decomposed to generate hydrofluoric acid in an acid environment, the concentration of the hydrofluoric acid in the etching solution composition is increased, the problem that the etching rate is greatly reduced due to consumption of HF is solved, meanwhile, the thickening agent increases the viscosity of the solution, influences the size, stability and the like of bubbles generated by nitrogen oxides and the like, increases the solubility of reactive gases, reduces the volatilization of effective components such as nitric acid, nitrogen oxides, hydrofluoric acid and the like in the reaction process, and maintains the long-acting stability of the etching solution.
Drawings
Fig. 1 is a surface state of a mechanical grinding chip visually observed before etching.
FIG. 2 shows the surface state of a mechanical lapping under a microscope 500 times before etching.
FIG. 3 is a surface state of a mechanical grinding chip visually observed after etching in example 1.
FIG. 4 shows the surface state of a 500-fold mechanically lapped piece under a microscope after etching in example 1.
Fig. 5 is a surface state of the mechanical grinding chip visually observed after etching of comparative example 1.
FIG. 6 shows the surface state of a mechanical lapping under a microscope 500 times after etching in comparative example 1.
FIG. 7 shows the etching life of example 1.
Fig. 8 shows the loss amount of the effective component during the etching process of example 1 and comparative example 2.
Fig. 9 shows the etching life of comparative example 2.
Detailed Description
For a better understanding of the present invention, the present invention is further described in detail below with reference to the following figures and examples, but the scope of the present invention is not limited to the following examples.
Example 1
Example 1 provides a graining-removing etching solution and an etching result, specifically:
the weight content of the nitric acid is 5 percent; the weight content of hydroxylamine nitrate is 0.3 percent; the weight content of the fluorosulfonic acid is 0.6%; the weight content of the ammonium bifluoride is 6 percent; the weight content of xenon difluoride is 1%; the weight content of the sulfuric acid is 82 percent; the weight content of polyacrylamide is 0.05%; the weight content of the deionized water is the balance.
Performing an etching experiment on a mechanical grinding sheet (3cm multiplied by 3cm) by using the silicon etching solution without the grinding patterns at 25 ℃, wherein the etching mode is rotary spray etching, the etching time is 1min, the thickness of the silicon wafer before and after etching is detected by using a micrometer screw, and the etching rate is calculated, and the etching rate is (H)1-H2) And/t, and roughnesss, Ra1, Ra2 of the front and rear surfaces before and after etching were examined by a surface Roughness meter, and the removal of surface scratches was observed with the naked eye and a 500-fold microscope.
H1Thickness of the silicon wafer before reaction, H2The thickness of the silicon wafer after the reaction, t the reaction time, Ra1 the surface roughness before the reaction, and Ra2 the surface roughness after the reaction. The etching effect is recorded in table 1, the surface state before etching is shown in fig. 1 and 2, and the surface after etching has no wear marks, as shown in fig. 3 and 4.
Performing an etching life test on the mechanical grinding sheet with the silicon etching solution without the grinding patterns at 25 deg.C by rotary spray etching, respectively circularly etching with 500ml of the above medicinal solution for 60s, 300s, and 600s, then etching a new grinding sheet for 1min, measuring the etching rate, and detecting HF and HNO in the medicinal solution after circularly etching for 60s, 300s, and 600s with fluorine ion electrode and spectrophotometer3Content of (a), HF and HNO thereof3The loss situation of (2) is shown in fig. 8.
Example 2
A graining-removing etching solution and an etching result are specifically as follows: the weight content of the nitric acid is 6 percent; the weight content of hydroxylamine nitrate is 0.5 percent; the weight content of the fluorosulfonic acid is 1%; the weight content of the ammonium bifluoride is 5 percent; the weight content of xenon difluoride is 2%; the weight content of the sulfuric acid is 80 percent; the weight content of polyethylene glycol is 0.1%; the weight content of the deionized water is the balance.
The etching effect was measured in the same manner as in example 1, and the etching effect is shown in Table 1.
Example 3
A graining-removing etching solution and an etching result are specifically as follows: the weight content of the nitric acid is 5 percent; the weight content of hydroxylamine nitrate is 0.5 percent; the weight content of the fluorosulfonic acid is 0.4%; the weight content of ammonium bifluoride is 6.5 percent; the weight content of xenon difluoride is 0.5%; the weight content of the sulfuric acid is 82 percent; the weight content of polyacrylamide is 0.03%; the weight content of the deionized water is the balance.
The etching effect was measured in the same manner as in example 1, and the etching effect is shown in Table 1.
Comparative example 1:
comparative example 1 provides a desmear etchant and etching results, specifically:
the weight content of the nitric acid is 5 percent; the weight content of the ammonium bifluoride is 6 percent; the weight content of the sulfuric acid is 82 percent; the weight content of the deionized water is the balance.
The etching effect was measured in the same manner as in example 1, and the etching effect was recorded in table 1, and the surface still had the burr remained after etching, as shown in fig. 5 and 6.
Comparative example 2
Comparative example 2 provides a graining-removing etching solution and etching results, specifically:
the weight content of the nitric acid is 8 percent; the weight content of the ammonium bifluoride is 10 percent; the weight content of the sulfuric acid is 76 percent; the weight content of the deionized water is the balance.
The etching effect was measured in the same manner as in example 1, and the etching effect is shown in Table 1.
Performing an etching life test on the mechanical grinding plate with the above silicon etching solution without grinding patterns at 25 deg.C by rotary spray etching, respectively etching with 500ml of the above medicinal solution for 60s, 300s, and 600s, then etching for 1min, measuring the etching rate, and measuring the etching life as shown in FIG. 9Detecting HF and HNO in the liquid medicine after cyclic etching for 60s, 300s and 600s by using a fluorine ion electrode and a spectrophotometer3Content of (a), HF and HNO thereof3The loss situation of (2) is shown in fig. 8.
Example 4
A graining-removing etching solution and an etching result are specifically as follows:
the weight content of the nitric acid is 6 percent; the weight content of hydroxylamine nitrate is 0.5 percent; the weight content of the fluorosulfonic acid is 1%; the weight content of the ammonium bifluoride is 5 percent; the weight content of the sulfuric acid is 80 percent; the weight content of polyethylene glycol is 0.1%; the weight content of the deionized water is the balance.
The etching effect was measured in the same manner as in example 1, and the etching effect is shown in Table 1.
Example 5
A graining-removing etching solution and an etching result are specifically as follows:
the weight content of the nitric acid is 6 percent; the weight content of hydroxylamine nitrate is 0.5 percent; the weight content of the fluorosulfonic acid is 1%; the weight content of the ammonium bifluoride is 5 percent; the weight content of xenon difluoride is 2.4%; the weight content of the sulfuric acid is 80 percent; the weight content of polyethylene glycol is 0.1%; the weight content of the deionized water is the balance.
The etching effect was measured in the same manner as in example 1, and the etching effect is shown in Table 1.
Example 6
A graining-removing etching solution and an etching result are specifically as follows:
the weight content of the nitric acid is 5 percent; the weight content of hydroxylamine nitrate is 0.5 percent; the weight content of the fluorosulfonic acid is 0.4%; the weight content of ammonium bifluoride is 9 percent; the weight content of xenon difluoride is 0.5%; the weight content of the sulfuric acid is 80 percent; the weight content of polyacrylamide is 0.03%; the weight content of the deionized water is the balance.
The etching effect was measured in the same manner as in example 1, and the etching effect is shown in Table 1.
Example 7
A graining-removing etching solution and an etching result are specifically as follows:
the weight content of the nitric acid is 5 percent; the weight content of hydroxylamine nitrate is 0.5 percent; the weight content of the fluorosulfonic acid is 0.4%; the weight content of the ammonium bifluoride is 3 percent; the weight content of xenon difluoride is 0.5%; the weight content of the sulfuric acid is 82 percent; the weight content of polyacrylamide is 0.03%; the weight content of the deionized water is the balance.
The etching effect was measured in the same manner as in example 1, and the etching effect is shown in Table 1.
Example 8
A graining-removing etching solution and an etching result are specifically as follows:
the weight content of the nitric acid is 5 percent; the weight content of the fluorosulfonic acid is 0.6%; the weight content of the ammonium bifluoride is 6 percent; the weight content of xenon difluoride is 1%; the weight content of the sulfuric acid is 82 percent; the weight content of polyacrylamide is 0.05%; the weight content of the deionized water is the balance.
The etching effect was measured in the same manner as in example 1, and the etching effect is shown in Table 1.
Example 9
A graining-removing etching solution and an etching result are specifically as follows:
the weight content of the nitric acid is 5 percent; the weight content of hydroxylamine nitrate is 1 percent; the weight content of the fluorosulfonic acid is 0.6%; the weight content of the ammonium bifluoride is 6 percent; the weight content of xenon difluoride is 1%; the weight content of the sulfuric acid is 82 percent; the weight content of polyacrylamide is 0.05%; the weight content of the deionized water is the balance.
The etching effect was measured in the same manner as in example 1, and the etching effect is shown in Table 1.
It can be seen from the experimental data in table 1 and fig. 1-6 that, in comparative example 1, the etching rate is slow, the etching removal amount is small, the mass transfer effect is weak, and the etched surface has deep burr residue, and in examples 1, 2 and 3, the etching rate is improved by nearly 3 times by adding hydroxylamine nitrate, xenon difluoride and difluoride, and the mass transfer resistance of the solution is increased by the synergistic action of the thickener, so that the etched surface is flat and has no burr. Comparative example 2 although the etching rate was increased by increasing the contents of nitric acid and hydrofluoric acid, the etching rate was drastically decreased as the nitric acid and hydrofluoric acid were consumed and volatilized, as shown in fig. 9. Comparing example 1 with examples 8 and 9, when hydroxylamine nitrate is not added, the etching rate is low, and shallow grinding lines still exist, when 1% hydroxylamine nitrate is added, the reaction rate is difficult to control, a large amount of brown smog emerges, and brown spots appear on the surface of the silicon wafer after etching. Comparing example 2 with examples 4 and 5, when xenon difluoride is not added, the etching rate is slow and the service life is short, and when the xenon difluoride is added in excess, dot-shaped black porous silicon is generated on the surface of a silicon wafer. Comparing example 3 with examples 6 and 7, after adding excessive ammonium bifluoride, black porous silicon is generated due to the excessive hydrofluoric acid, and when the ammonium bifluoride content is only 3%, the etching rate is slow, so that shallow burr residues still exist at the edge of the silicon wafer. As shown in fig. 7 and 8, in example 1, the loss of nitric acid and hydrofluoric acid is compensated by adding hydroxylamine nitrate, fluorosulfonic acid and xenon difluoride, and meanwhile, the addition of the thickening agent increases the viscosity of the solution, increases the solubility of the reactive gas, reduces the volatilization of effective components in the reaction process, and prolongs the service life of the etching solution. Therefore, the anti-abrasion silicon etching solution has a remarkable improvement effect.
Table 1 experimental results of etching experiments performed in examples 1 to 3 and comparative examples 1 to 8.
Claims (2)
1. The silicon etching liquid for removing the grinding lines is characterized by comprising the components of nitric acid, hydroxylamine nitrate, fluorosulfonic acid, ammonium bifluoride, xenon difluoride, sulfuric acid, a thickening agent and deionized water; the weight content of nitric acid in the silicon etching solution is 3% -7%; the weight content of hydroxylamine nitrate is 0.01-0.5%; the weight content of the fluorosulfonic acid is 0.1% -1%; the weight content of the ammonium bifluoride is 4-8%; the weight content of xenon difluoride is 0.1% -2%; the weight content of the sulfuric acid is 75-85%; the weight content of the thickening agent is 0.01% -0.1%; the weight content of the deionized water is the balance.
2. The silicon etching solution for removing the grinding lines as claimed in claim 1, wherein: the thickening agent comprises at least one of polyacrylamide, hexanol, octanol, polyethylene glycol and polyvinylpyrrolidone.
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| CN114573931B (en) * | 2022-03-04 | 2023-05-09 | 中国工程物理研究院激光聚变研究中心 | Preparation and application of colloid for repairing surface damage pits of optical elements |
Citations (4)
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| CN1411612A (en) * | 1999-12-22 | 2003-04-16 | 默克专利有限公司 | Method for raw etching silicon solar cells |
| CN102443395A (en) * | 2010-09-30 | 2012-05-09 | 韩国泰科诺赛美材料株式会社 | Compound for wet etching silicon dioxide |
| CN109575923A (en) * | 2018-12-11 | 2019-04-05 | 湖北兴福电子材料有限公司 | A kind of etching solution of low-doped silicon electrode |
| CN109913222A (en) * | 2019-02-18 | 2019-06-21 | 湖北兴福电子材料有限公司 | A kind of silicon wafer polishing liquid |
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| US20100112728A1 (en) * | 2007-03-31 | 2010-05-06 | Advanced Technology Materials, Inc. | Methods for stripping material for wafer reclamation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1411612A (en) * | 1999-12-22 | 2003-04-16 | 默克专利有限公司 | Method for raw etching silicon solar cells |
| CN102443395A (en) * | 2010-09-30 | 2012-05-09 | 韩国泰科诺赛美材料株式会社 | Compound for wet etching silicon dioxide |
| CN109575923A (en) * | 2018-12-11 | 2019-04-05 | 湖北兴福电子材料有限公司 | A kind of etching solution of low-doped silicon electrode |
| CN109913222A (en) * | 2019-02-18 | 2019-06-21 | 湖北兴福电子材料有限公司 | A kind of silicon wafer polishing liquid |
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