The present invention relates to a polishing processing method for efficiently polishing a surface of a GaN single crystal material into a mirror surface.
Although electronic devices such as semiconductor integrated circuits are often constructed on silicon single crystal substrates, single crystal substrates made of gallium nitride GaN having better electric characteristics are expected to be used for power devices etc. requiring a function of controlling comparatively large electric power, instead of the silicon single crystal substrates. Since a power device using such a single crystal substrate made of gallium nitride GaN can deal with a large amount of electric power, generates small amount of heat, and can be miniaturized, the power device is preferably used as a control element controlling the number of rotations or torque of a motor or an electric generator in a hybrid vehicle, a fuel-cell vehicle, etc. The single crystal substrates made of gallium nitride GaN are excellent in high frequency characteristics and are expected to be developed into wireless communication stations, relay stations, mobile stations, etc.
In a typically employed manufacturing method employed for manufacturing of VLSI, a multiplicity of chips are formed on a semiconductor wafer, which is cut into respective chip sizes in a final process. Since a degree of integration is recently dramatically increased in association with improvements in VLSI manufacturing technology and wirings are increasingly multilayered, planarization of an entire semiconductor wafer (global planarization) is required in a process of forming each layer. One of the techniques of achieving such planarization of an entire semiconductor wafer is a polishing method referred to as a CMP (chemical mechanical polishing) method. In the CMP method, while a nonwoven fabric or a polishing pad such as a foam pad affixed to a surface plate is pressed against a wafer and forcibly rotated, a slurry (a dense suspension with fine powder dispersed in liquid such as an aqueous alkali solution) containing fine polishing particles (loose abrasive grains) is allowed to flow thereto for polishing. This CMP method achieves comparatively accurate polishing processing because of a synergetic effect between chemical polishing with a liquid component and mechanical polishing with polishing abrasive grains.
However, in such a conventional CMP method, a considerable time is spent for the polishing processing. If a loose abrasive grain polishing processing using diamond abrasive grains as polishing particles is performed, surface roughness becomes as large as Ra=10 nm, for example, although a certain level of processing efficiency is provided. In contrast, if a loose abrasive grain polishing processing is performed by using silica abrasive grains, the surface roughness becomes smaller; however, the processing efficiency deteriorates and scratches of unknown cause inconveniently tend to occur.
In this regard, a polishing processing method for polishing a SiC single crystal substrate is proposed. For example, this corresponds to a polishing processing method described in Patent Document 1.
Patent Document
Patent Document 1: Japanese Laid-Open Patent Publication No. 2008-068390
The polishing processing method of Patent Document 1 is based on finding of a specific polishing processing condition on which a high polishing efficiency is provided along with a low surface roughness of a SiC single crystal substrate with respect to ranges of hydrogen ion concentration pH and oxidation-reduction potential Eh of a polishing liquid. However, it is inappropriate to apply such a polishing processing condition directly to a single crystal substrate made of gallium nitride GaN, polishing processing of which is more difficult than the SiC single crystal substrate, and it is difficult to efficiently reduce the surface roughness of the single crystal substrate made of gallium nitride GaN.
The present invention was conceived in view of the situations and it is therefore an object of the present invention to provide a polishing processing method achieving sufficient polishing efficiency and polishing performance in polishing using a CMP method for a single crystal substrate made of gallium nitride GaN which is a material more difficult to process.
As a result of intensive continuous studies for developing such a method of polishing a material difficult to process by using a CMP method, the present inventors found out that, in a polishing processing method using a CMP method for polishing a surface of a crystal material to be smooth by using a polishing pad in the presence of a polishing liquid and polishing particles, polishing efficiency and polishing performance are made remarkably excellent for a single crystal substrate made of gallium nitride GaN which is the material difficult to process, by dissolving an oxidizing agent to impart oxidizability to the polishing liquid in specific regions existing respectively for a fixed polishing abrasive grain type polishing pad and a loose polishing abrasive grain type polishing pad with respect to ranges of oxidation-reduction potential Eh and pH of the polishing liquid. The present invention was conceived based on this knowledge.
That is, a first aspect of the invention provides a polishing processing method (a) using a CMP method for polishing a surface of a crystal material to be smooth by using a loose polishing abrasive grain type polishing pad in the presence of a polishing liquid and a plurality of polishing abrasive grains, wherein (b) the crystal material is a single crystal of GaN, and wherein (c) the polishing liquid is an oxidizing polishing liquid having an oxidation-reduction potential between Ehmin (determined by Eq. (1)) mV and Ehmax (determined by Eq. (2)) mV and pH between 0.1 and 6.5:
Ehmin (mV)=−33.9 pH+750 (1)
Ehmax (mV)=−82.1 pH+1491 (2).
That is, a second aspect of the invention provides a polishing processing method (d) using a CMP method for polishing a surface of a crystal material to be smooth by using a fixed polishing abrasive grain type polishing pad in the presence of a polishing liquid and a plurality of polishing abrasive grains, wherein (e) the crystal material is a single crystal of GaN, and wherein (f) the polishing liquid is an oxidizing polishing liquid having an oxidation-reduction potential between Ehmin (determined by Eq. (3)) mV and Ehmax (determined by Eq. (4)) mV and pH between 0.12 and 5.7:
Ehmin (mV)=−27.2 pH+738.4 (3)
Ehmax (mV)=−84 pH+1481 (4).
According to the first aspect of the invention, in polishing processing using a CMP method, a loose polishing abrasive grain type polishing pad is used for polishing a surface of a crystal material that is a single crystal of GaN in the presence of an oxidizing polishing liquid having an oxidation-reduction potential between Ehmin (determined by Eq. (1)) [mV] and Ehmax (determined by Eq. (2)) [mV] and pH between 0.1 and 6.5, and therefore, a high polishing efficiency can preferably be provided while a low surface roughness is achieved.
According to the second aspect of the invention, in polishing processing using a CMP method, a fixed polishing abrasive grain type polishing pad is used for polishing a surface of a crystal material that is a single crystal of GaN in the presence of an oxidizing polishing liquid having an oxidation-reduction potential between Ehmin (determined by Eq. (3)) [mV] and Ehmax (determined by Eq. (4)) [mV] and pH between 0.12 and 5.7, and therefore, a high polishing efficiency can preferably be provided while a low surface roughness is achieved.
Preferably, the loose polishing abrasive grain type polishing pad is made of a hard polyurethane resin, and the polishing abrasive grains are loose abrasive grains contained in the polishing liquid supplied to the polishing pad. As a result, a higher polishing efficiency and a low surface roughness are provided, and a polishing accuracy is improved in terms of flatness etc.
Preferably, the oxidizing polishing liquid has potassium permanganate, potassium bichromate, or potassium thiosulphate added thereto as an oxidation-reduction potential adjustment agent. As a result, a preferable oxidizing polishing liquid is easily acquired.
Preferably, the fixed polishing abrasive grain type polishing pad has a matrix resin with independent pores or communicating pores, and the plurality of polishing abrasive grains is housed in the matrix resin such that the polishing abrasive grains are partially fixed inside the independent pores or communicating pores formed in the matrix resin or are partially separated from the matrix resin. As a result, since the polishing abrasive grains are contained in the communicating pores of the matrix resin, a higher polishing efficiency and a low surface roughness are provided. A consumed amount of the polishing abrasive grains is reduced, which enables the use of expensive polishing abrasive grains.
Preferably, the matrix resin of the fixed polishing abrasive grain type polishing pad is made of an epoxy resin or a polyethersulfone (PES) resin. As a result, a higher polishing effect is provided. However, for example, a synthetic resin etc. are also preferably used that include at least one of fluorine-based synthetic resins such as polyvinyl fluoride, vinyl fluoride-hexafluoropropylene copolymer, polyvinylidene fluoride, and vinylidene fluoride-hexafluoropropylene copolymer, polyethylene resins, and polymethylmethacrylate.
Preferably, the polishing abrasive grains contain at least one of diamond, CBN (cubic boron nitride), B4C (boron carbide), silicon carbide, silica, ceria, alumina, zirconia, titania, manganese oxide, barium carbonate, chromium oxide, and iron oxide. This advantageously enables the use of polishing abrasive grains with hardness corresponding to an object to be polished on which a favorable surface roughness can be achieved. Preferably, the polishing abrasive grains have the average grain diameter in a range of 0.005 to 10 (μm) and, in the case of silica, for example, fumed silica (silica microparticles acquired by high-temperature combustion of silicon tetrachloride, chlorosilane, etc. in the presence of hydrogen and oxygen) etc. are preferably used. Preferably, the volume percentage of the polishing abrasive grains to the polishing pad is within a range of 20 to 50(%) and the weight percentage thereof is within a range of 51 to 90(%).
Preferably, in the case of polishing using the fixed polishing abrasive grain type polishing pad, an amount of the polishing liquid is extremely small and is 0.1 to 200 ml/min/m2 per unit area of a polishing surface plate. As a result, a higher polishing efficiency is provided, and a surface roughness is reduced.
An application example of the present invention will now be described in detail with reference to the drawings.
The polishing processing apparatus 10 is provided as needed with an adjustment tool holding member not shown disposed rotatably around an axial center C3 parallel to the axial center C1 of the polishing surface plate 12 and movably in the direction of the axial center C3 and in the radial direction of the polishing surface plate 12 and a polishing object adjustment tool (conditioner) such as a diamond wheel not shown attached to a lower surface of the adjustment tool holding member, i.e., a surface facing the polishing pad 14, and the adjustment tool holding member and the polishing object adjustment tool attached thereto are pressed against the polishing pad 14 and reciprocated in the radial direction of the polishing surface plate 12 while being rotationally driven by an adjustment tool drive motor not shown, for adjustment of a polishing surface of the polishing pad 14, so that a surface state of the polishing pad 14 is always maintained in a state suitable for polishing processing.
In the polishing processing of the CMP method by the polishing processing apparatus 10, while the polishing surface plate 12 and the polishing pad 14 affixed thereto as well as the workpiece holding member 18 and the object to be polished 16 held on the lower surface thereof are rotationally driven around respective axial centers by the surface plate drive motor 13 and the workpiece drive motor, the polishing liquid 20 is supplied from the dropping nozzle 22 and/or the spray nozzle 24 onto the surface of the polishing pad 14, and the object to be polished 16 held by the workpiece holding member 18 is pressed against the polishing pad 14. As a result, a surface to be polished of the object to be polished 16, i.e., a surface facing the polishing pad 14 is polished to be flat by a chemical polishing action due to the polishing liquid 20 and a mechanical polishing action due to polishing abrasive grains 26 contained in the polishing pad 14 and self-supplied from the polishing pad 14. For example, silica with an average grain diameter of about 80 nm is used for the polishing abrasive grains 26.
The polishing pad 14 affixed onto the polishing surface plate 12 is a loose polishing abrasive grain type polishing pad made of a hard foamed polyurethane resin or a fixed polishing abrasive grain type polishing pad made of an epoxy resin or a PES resin having independent pores or communicating pores housing the polishing abrasive grains 26 and has dimensions of about 300 (mmø)×5 (mm), for example.
In the polishing processing in the polishing processing apparatus 10 configured as described above, while the polishing surface plate 12 and the polishing pad 14 affixed thereto as well as the workpiece holding member 18 and the object to be polished 16 held on the lower surface thereof are rotationally driven around the respective axial centers by the surface plate drive motor 13 and the workpiece drive motor not shown, for example, the oxidizing polishing liquid 20 such as a potassium permanganate aqueous solution is supplied from the dropping nozzle 22 onto the surface of the polishing pad 14, and the object to be polished 16 held by the workpiece holding member 18 is pressed against the surface of the polishing pad 14. As a result, the surface to be polished of the object to be polished 16, i.e., the facing surface contacting with the polishing pad 14, is polished to be flat by the chemical polishing action due to the polishing liquid 20 and the mechanical polishing action due to the polishing abrasive grains 26 self-supplied from the polishing pad 14.
An experimental example 1 performed by the present inventors will hereinafter be described. First, an apparatus having the same configuration as the polishing processing apparatus 10 shown in
[Loose Abrasive Grain Polishing Conditions]
less and the polishing rates of 7 nm/h or more.
Ehmin (mV)=−33.9 pH+750 (1)
Ehmax (mV)=−82.1 pH+1491 (2)
An experimental example 2 performed by the present inventors will hereinafter be described. First, an apparatus having the same configuration as the polishing processing apparatus 10 shown in
[Fixed Abrasive Grain Polishing Conditions]
Ehmin (mV)=−27.2 pH+738.4 (3)
Ehmax (mV)=−84 pH+1481 (4)
Although not exemplarily illustrated one by one, the present invention is used with other various modifications without departing from the spirit thereof.
Number | Date | Country | Kind |
---|---|---|---|
2014-074202 | Mar 2014 | JP | national |
Filing Document | Filing Date | Country | Kind |
---|---|---|---|
PCT/JP2015/059526 | 3/26/2015 | WO | 00 |
Publishing Document | Publishing Date | Country | Kind |
---|---|---|---|
WO2015/152021 | 10/8/2015 | WO | A |
Number | Name | Date | Kind |
---|---|---|---|
7416604 | Ishibashi | Aug 2008 | B2 |
20050150172 | Sato | Jul 2005 | A1 |
20070254401 | Nishiura et al. | Nov 2007 | A1 |
20070281484 | Ishibashi et al. | Dec 2007 | A1 |
20090317638 | Kawabata | Dec 2009 | A1 |
20100248478 | Nishiura et al. | Sep 2010 | A1 |
20130075867 | Nishiura et al. | Mar 2013 | A1 |
20130149945 | Misra | Jun 2013 | A1 |
20130292802 | Ishibashi | Nov 2013 | A1 |
20160257854 | Omori | Sep 2016 | A1 |
Number | Date | Country |
---|---|---|
101066583 | Nov 2007 | CN |
1 852 480 | Nov 2007 | EP |
1 863 074 | Dec 2007 | EP |
2514858 | Oct 2012 | EP |
2006-179647 | Jul 2006 | JP |
2007-103457 | Apr 2007 | JP |
2007-299979 | Nov 2007 | JP |
2008-010835 | Jan 2008 | JP |
2008-068390 | Mar 2008 | JP |
2011-129752 | Jun 2011 | JP |
2012-253259 | Dec 2012 | JP |
2008102672 | Aug 2008 | WO |
Entry |
---|
Oct. 4, 2016 Written Opinion issued in International Patent Application No. PCT/JP2015/059526. |
May 12, 2015 Search Report issued in International Patent Application No. PCT/JP2015/059526. |
May 24, 2018 extended European Search Report issued in European Application No. 15774319.6. |
Jul. 17, 2018 Office Action issued in Japanese Patent Application No. 2017-215116. |
Oct. 26, 2018 Office Action issued in Taiwan Patent Application No. 104110016. |
Number | Date | Country | |
---|---|---|---|
20170100815 A1 | Apr 2017 | US |