CN107907576B - Method for prolonging service life of polishing solution for C-direction sapphire substrate - Google Patents
Method for prolonging service life of polishing solution for C-direction sapphire substrate Download PDFInfo
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- CN107907576B CN107907576B CN201711221272.4A CN201711221272A CN107907576B CN 107907576 B CN107907576 B CN 107907576B CN 201711221272 A CN201711221272 A CN 201711221272A CN 107907576 B CN107907576 B CN 107907576B
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Abstract
The invention relates to a method for prolonging the service life of C-direction sapphire substrate polishing solution, which comprises the following specific processes: 1) in the chemical mechanical polishing process of the C-direction sapphire, taking the polishing solution of the C-direction sapphire substrate, measuring the potential by using a Zeta potential analyzer, and monitoring the Zeta potential change condition of the polishing solution of the C-direction sapphire substrate; 2) when the Zeta potential absolute value of the C-to-sapphire substrate polishing solution is not more than 20mv, directly adding a nonionic surfactant into the C-to-sapphire substrate polishing solution in use, stopping adding when the Zeta potential absolute value of the C-to-sapphire substrate polishing solution is not less than 30.0mv, then monitoring the Zeta potential again every 0.5-1.5 hours, and repeating the process; the nonionic surfactant is one or a mixture of sodium dodecyl sulfate, isomeric dodecyl alcohol polyoxyethylene ether and nonylphenol polyoxyethylene ether. The method obviously prolongs the service life of the polishing solution to more than 12 hours and reduces the use cost of the polishing solution by more than 30 percent.
Description
Technical Field
The invention relates to the technical field of sapphire substrate polishing, in particular to a method for prolonging the service life of C-direction sapphire substrate polishing solution by controlling a Zeta potential.
Background
With the development of LED substrate technology, sapphire wafers are developed from 4 inches to 6 inches or more in size. When the size of the wafer is 4 inches, the transition layer is grown on the ultra-smooth wafer surface (the general surface roughness Ra is less than or equal to 0.2nm) to overcome the defect that the gallium nitride is in Al2O3The problem of lattice mismatch during substrate growth, however, with the development of wafers to 6 inches or even larger sizes and the higher requirement of devices on flatness (surface roughness Ra is less than or equal to 0.1nm), how to reduce the surface roughness of the sapphire substrate and improve the polishing rate of the wafer and the service life of the polishing solution becomes a problem to be solved urgently.
At present, the chemical mechanical polishing technology is generally adopted for sapphire substrates by using polishing solution of silica sol abrasive, the industrial standard of the roughness of the polished substrate surface is that Ra is less than or equal to 0.3nm, and the polishing removal rate is 3-4 mu m/h, which is required by general enterprises. Wherein, the content of the silica sol abrasive material is more than 90 percent of the solid content of the polishing solution, the service life of the polishing solution is generally 7-8 hours when in use, and enterprises generally choose to pour the polishing solution in use and replenish new polishing solution after working for 7-8 hours.
The sapphire polishing solution takes silica sol as an abrasive, and the colloid stability can be gradually reduced in the use process of polishing C to sapphire in-process C to sapphire substrate polishing solution, and the main reasons are as follows: 1. the consumption of effective chemical components in the solution for helping the colloid to be stable is gradually reduced along with the chemical mechanical polishing process; 2. the temperature of the polishing solution rises due to the heat release of the chemical mechanical polishing reaction and the heat release of the polishing pad and the sapphire wafer under a certain pressure by continuous friction, and the stability of the colloidal solution is reduced due to the rise of the temperature to a certain extent. The reduction of the colloid stability directly promotes the aggregation of particles in the polishing solution to generate the increase of large agglomerated particles, the particles are agglomerated together, the effective contact area between the particle surface and the wafer surface in the polishing process is reduced, the polishing efficiency is reduced, and the service life of the polishing solution is seriously influenced; meanwhile, the agglomerated large particles may cause scratches on the wafer surface, resulting in a decrease in yield.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for prolonging the service life of a C-direction sapphire substrate polishing solution by controlling a Zeta potential. The method controls the Zeta potential value of the solution to be always kept in a certain range by adding the nonionic surfactant, improves the Zeta potential of the polishing solution, obviously prolongs the service life of the polishing solution to more than 12 hours, and reduces the use cost of the polishing solution by more than 30%.
The technical scheme adopted by the invention for solving the technical problems is as follows: the method for prolonging the service life of the polishing solution for the C-direction sapphire substrate is provided, and the specific process of the method is as follows:
1) in the chemical mechanical polishing process of the C-direction sapphire, taking the polishing solution of the C-direction sapphire substrate, measuring the potential by using a Zeta potential analyzer, and monitoring the Zeta potential change condition of the polishing solution of the C-direction sapphire substrate;
2) when the Zeta potential absolute value of the C-to-sapphire substrate polishing solution is not more than 20mv, directly adding a nonionic surfactant into the C-to-sapphire substrate polishing solution in use, stopping adding when the Zeta potential absolute value of the C-to-sapphire substrate polishing solution is not less than 30.0mv, then monitoring the Zeta potential again every 0.5-1.5 hours, and repeating the process; the nonionic surfactant is one or a mixture of sodium dodecyl sulfate, isomeric dodecyl alcohol polyoxyethylene ether and nonylphenol polyoxyethylene ether.
Compared with the prior art, the invention has the beneficial effects that:
the method detects the change of the Zeta potential value of the solution at any time in the use process of the polishing solution of the sapphire substrate C, and adds the nonionic surfactant when the Zeta potential absolute value is lower than 20mv, thereby not only improving the Zeta potential of the polishing solution, but also obviously prolonging the service life of the polishing solution to more than 12 hours and reducing the use cost of the polishing solution to more than 30 percent.
Detailed Description
The present invention is further explained by the following examples, which should not be construed as limiting the scope of the claims of the present application.
The invention discloses a method for prolonging the service life of C-direction sapphire substrate polishing solution (method for short), which comprises the following specific steps:
1) in the process of chemically and mechanically polishing the C-direction sapphire, taking a small amount of C-direction sapphire substrate polishing solution, measuring the potential by using a Zeta potential analyzer, and monitoring the Zeta potential change condition of the C-direction sapphire substrate polishing solution;
2) when the Zeta potential absolute value of the C-to-sapphire substrate polishing solution is not more than 20mv, directly adding a proper amount of nonionic surfactant into the C-to-sapphire substrate polishing solution in use, stopping adding when the Zeta potential absolute value of the C-to-sapphire substrate polishing solution is not less than 30.0mv, then monitoring the Zeta potential again every 0.5-1.5 hours, and repeating the process; the nonionic surfactant is one or a mixture of sodium dodecyl sulfate, isomeric dodecyl alcohol polyoxyethylene ether and nonylphenol polyoxyethylene ether.
The present invention is further characterized in that the amount of the nonionic surfactant added is 0.001 to 0.1wt% of the total content of the remaining C to the sapphire substrate polishing solution.
The invention is further characterized in that the number of times of adding the nonionic surfactant into the sapphire substrate polishing solution C is 2-4, the nonionic surfactant cannot be added all the time without limit, when the number of times of adding is too large, although the Zeta potential can be ensured to be higher, the polishing temperature is too low to achieve the required polishing efficiency in practical use.
The polishing machine used in the invention is provided with a polishing solution container, and the polishing solution container is always in a stirring state in the polishing process. In the stirring process, the nonionic surfactant is directly added to ensure uniform stirring.
Example 1
The C-direction sapphire substrate polishing solution used in this example was a nano-silica polishing solution (5010(E), SiO) from Shanghai micelle chemical Co., Ltd235% by mass and 70-110nm in abrasive particle size), and deionized water in a ratio of 1: 1, and adding 10 wt% KOH solution to adjust the pH value of the polishing solution to 10.5 to obtain the prepared C-direction sapphire substrate polishing solution. The chemical mechanical polishing test was performed using polishing equipment CP4 from CETR corporation, usa.
Before C-direction sapphire chemical mechanical polishing, adding 70L C-direction sapphire substrate polishing solution into a polishing solution container, starting chemical mechanical polishing, taking about 3mL of polishing solution every 1 hour, measuring the potential of the polishing solution by using a Zeta potential analyzer, and monitoring the Zeta potential change condition of the C-direction sapphire substrate polishing solution; monitoring that the Zeta potential absolute value of the polishing solution of the sapphire substrate is 19mv after polishing for about 7 hours, indicating that the colloid stability in the polishing solution is poor, adding sodium dodecyl sulfate into the polishing solution of the sapphire substrate, wherein the addition amount of the sodium dodecyl sulfate is 0.005 wt% of the total content of the residual polishing solution of the sapphire substrate, and continuously stirring at the stirring speed of 60 rpm; and when the Zeta potential absolute value of the C-direction sapphire substrate polishing solution is detected to be greater than 30.0mv, stopping adding, monitoring the Zeta potential again after 1 hour, continuing polishing the C-direction sapphire at the moment, then continuing monitoring, monitoring that the Zeta potential absolute value of the C-direction sapphire substrate polishing solution is 20mv after working for 4 hours, adding sodium dodecyl sulfate, repeating the process for 2 times, abandoning the residual polishing solution, and finishing the polishing process.
The service life of the polishing solution of the embodiment can be prolonged to about 15 h.
Example 2
The C-directional sapphire substrate polishing solution used in this embodiment is a C-directional sapphire polishing stock solution of model JN-z820 produced by soft nano new materials ltd in Shenzhen city, and the stock solution and deionized water are mixed according to a ratio of 1: 1 to obtain the prepared C-direction sapphire substrate polishing solution, and performing a chemical mechanical polishing test.
Before C-sapphire is subjected to chemical mechanical polishing, adding 70L C sapphire substrate polishing solution into a polishing solution container, starting to perform chemical mechanical polishing, after 7 hours of working, taking 3mL of polishing solution every 0.5 hour, measuring the potential of the polishing solution by using a Zeta potential analyzer, monitoring the Zeta potential change condition of the C-sapphire substrate polishing solution, when 8 hours of working, monitoring that the Zeta potential absolute value of the C-sapphire substrate polishing solution is 19.5mv, indicating that the colloid stability in the polishing solution is poor, starting to add nonylphenol polyoxyethylene ether into the C-sapphire substrate polishing solution, wherein the adding amount of the nonylphenol polyoxyethylene ether is 0.003 wt% of the total content of the residual C-sapphire substrate polishing solution, and stirring is constant at the stirring speed of 70 rpm; and when the absolute value of the Zeta potential of the C-direction sapphire substrate polishing solution is detected to be greater than 30.0mv, stopping adding, continuing to polish the C-direction sapphire, then continuing to monitor every 1h, after working for 5h, monitoring that the absolute value of the Zeta potential of the C-direction sapphire substrate polishing solution is 20mv, adding nonylphenol polyoxyethylene ether, repeating the process for 3 times, abandoning the residual polishing solution, and finishing the polishing process.
The service life of the polishing solution of the embodiment can be prolonged to about 16 h.
Example 3
The polishing solution for a sapphire substrate C used in this example, the equipment used in this example, and the method for prolonging the lifetime were the same as in example 1, except that the nonionic surfactant added in this example was a mixture of isomeric dodecyl alcohol polyoxyethylene ether and nonylphenol polyoxyethylene ether in a volume ratio of 1: 2.
The embodiment can prolong the service life of the existing C-direction sapphire substrate polishing solution in a limited way, the added nonionic surfactant can improve the Zeta potential of the polishing solution and the colloid stability of the polishing solution, improve the removal rate of the polishing solution, remarkably prolong the service life of the polishing solution to more than 12 hours, reduce the use cost of the existing polishing solution for manufacturers, almost reduce the use cost by more than 30 percent, and bring huge economic benefits.
Nothing in this specification is said to apply to the prior art.
Claims (3)
1. A method for prolonging the service life of C-direction sapphire substrate polishing solution comprises the following specific processes:
1) in the chemical mechanical polishing process of the C-direction sapphire, taking the polishing solution of the C-direction sapphire substrate, measuring the potential by using a Zeta potential analyzer, and monitoring the Zeta potential change condition of the polishing solution of the C-direction sapphire substrate;
2) when the Zeta potential absolute value of the C-to-sapphire substrate polishing solution is not more than 20mv, directly adding a nonionic surfactant into the C-to-sapphire substrate polishing solution in use, stopping adding when the Zeta potential absolute value of the C-to-sapphire substrate polishing solution is not less than 30.0mv, then monitoring the Zeta potential again every 0.5-1.5 hours, and repeating the process; the nonionic surfactant is one or a mixture of sodium dodecyl sulfate, isomeric dodecyl alcohol polyoxyethylene ether and nonylphenol polyoxyethylene ether.
2. The method for prolonging the service life of the polishing solution for the C-direction sapphire substrate according to claim 1, wherein the nonionic surfactant is added in an amount of 0.001 to 0.1wt% based on the total content of the remaining polishing solution for the C-direction sapphire substrate.
3. The method for prolonging the service life of the C-directed sapphire substrate polishing solution according to claim 1, wherein the number of times of adding the nonionic surfactant to the C-directed sapphire substrate polishing solution is 2 to 4.
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| CN201711221272.4A CN107907576B (en) | 2017-11-29 | 2017-11-29 | Method for prolonging service life of polishing solution for C-direction sapphire substrate |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009028814A (en) * | 2007-07-25 | 2009-02-12 | Sumitomo Metal Mining Co Ltd | Sapphire substrate polishing method |
| CN102190962A (en) * | 2010-03-10 | 2011-09-21 | 福吉米株式会社 | Polishing composition and polishing method using the same |
| CN102190963A (en) * | 2010-03-10 | 2011-09-21 | 福吉米株式会社 | Polishing composition and polishing method using the same |
| JP2014042861A (en) * | 2012-08-24 | 2014-03-13 | Sumitomo Electric Ind Ltd | Method for treating an effluent |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040055993A1 (en) * | 1999-10-12 | 2004-03-25 | Moudgil Brij M. | Materials and methods for control of stability and rheological behavior of particulate suspensions |
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2017
- 2017-11-29 CN CN201711221272.4A patent/CN107907576B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009028814A (en) * | 2007-07-25 | 2009-02-12 | Sumitomo Metal Mining Co Ltd | Sapphire substrate polishing method |
| CN102190962A (en) * | 2010-03-10 | 2011-09-21 | 福吉米株式会社 | Polishing composition and polishing method using the same |
| CN102190963A (en) * | 2010-03-10 | 2011-09-21 | 福吉米株式会社 | Polishing composition and polishing method using the same |
| JP2014042861A (en) * | 2012-08-24 | 2014-03-13 | Sumitomo Electric Ind Ltd | Method for treating an effluent |
Non-Patent Citations (4)
| Title |
|---|
| Characteristics of Sapphire Wafers Polishing Depending on Ion Conductivity of Silica Sol;Na, Cho et al.;《Korean Journal of Materials Research》;20150131;第25卷(第1期);全文 * |
| Novel rapid polishing process for fabrication of sapphire windows;Singh, Arjunan et al.;《Material Technologies and Applications to Optics, Structures, Components, and Sub-Systems》;20130930;全文 * |
| Two-Step Chemical Mechanical Polishing of Sapphire Substrate;Zhang, Liu et al.;《Journal of The Electrochemical Society》;20100503;第157卷(第6期);全文 * |
| 纳米碳化硅抛光液的制备及其对蓝宝石晶片抛光性能的研究;熊伟, 储向峰 et al.;《金刚石与磨料磨具工程》;20131020;第33卷(第5期);全文 * |
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