CN105773399A - Polishing solution, polishing machine and polishing method - Google Patents
Polishing solution, polishing machine and polishing method Download PDFInfo
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- CN105773399A CN105773399A CN201610186551.0A CN201610186551A CN105773399A CN 105773399 A CN105773399 A CN 105773399A CN 201610186551 A CN201610186551 A CN 201610186551A CN 105773399 A CN105773399 A CN 105773399A
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- 238000005498 polishing Methods 0.000 title claims abstract description 300
- 238000000034 method Methods 0.000 title claims abstract description 46
- 239000011941 photocatalyst Substances 0.000 claims abstract description 74
- 239000002245 particle Substances 0.000 claims abstract description 70
- 239000007800 oxidant agent Substances 0.000 claims abstract description 62
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012530 fluid Substances 0.000 claims description 136
- 230000001590 oxidative effect Effects 0.000 claims description 50
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 33
- 239000004065 semiconductor Substances 0.000 claims description 28
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000008187 granular material Substances 0.000 claims description 24
- 239000003002 pH adjusting agent Substances 0.000 claims description 22
- 239000013078 crystal Substances 0.000 claims description 17
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000004408 titanium dioxide Substances 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229910003460 diamond Inorganic materials 0.000 claims description 8
- 239000010432 diamond Substances 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 6
- 239000012286 potassium permanganate Substances 0.000 claims description 6
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 6
- 239000000463 material Substances 0.000 abstract description 94
- 230000000694 effects Effects 0.000 abstract description 38
- 238000007254 oxidation reaction Methods 0.000 abstract description 31
- 230000003647 oxidation Effects 0.000 abstract description 18
- 238000007517 polishing process Methods 0.000 abstract description 13
- 230000001678 irradiating effect Effects 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 25
- 235000012431 wafers Nutrition 0.000 description 25
- 230000003197 catalytic effect Effects 0.000 description 21
- 230000008569 process Effects 0.000 description 15
- 238000006555 catalytic reaction Methods 0.000 description 14
- 239000000203 mixture Substances 0.000 description 11
- 238000005260 corrosion Methods 0.000 description 10
- 230000007797 corrosion Effects 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 10
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 8
- 238000007146 photocatalysis Methods 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- 229910002601 GaN Inorganic materials 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 230000001105 regulatory effect Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000003754 machining Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000003670 easy-to-clean Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000006748 scratching Methods 0.000 description 2
- 230000002393 scratching effect Effects 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000005422 blasting Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000007521 mechanical polishing technique Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
- B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
- B24B37/044—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/34—Accessories
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B57/00—Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents
- B24B57/02—Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents for feeding of fluid, sprayed, pulverised, or liquefied grinding, polishing or lapping agents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention provides a polishing solution, a polishing machine and a polishing method. The polishing method includes the steps that the polishing solution is added to the surface of a wafer to be polished and irradiated with an ultraviolet lamp, so that chemico-mechanical polishing is completed, wherein the polishing solution includes polishing particles, an oxidizing agent, photocatalyst and deionized water. By irradiating the polishing solution with the ultraviolet lamp, the photocatalyst can be made to catalyze matter adhering to the surface of the photocatalyst to be subjected to the oxidation reaction, more strong oxidants are generated, and accordingly the oxidation effect of the polishing solution to materials to be polished can be improved, the degree of removal of the chemico-mechanical polishing process to matter on the surfaces of the materials to be polished can be enhanced, and smooth and flat surfaces can be better obtained rapidly.
Description
Technical field
The present invention relates to field of semiconductor manufacture, in particular it relates to a kind of auxiliary finishing method for CMP process, more particularly, to polishing fluid, buffing machine and finishing method.
Background technology
Chemically mechanical polishing (chemicalmechanicalpolishing, CMP) is the important technology that can realize global planarizartion at present.CMP, under the synergism of mechanical grinding and chemical attack, is removed by the material of crystal column surface, it is achieved the polishing to wafer.Current chemically mechanical polishing, is generally adopted buffing machine and polishing fluid completes to process by the planarization of polished material.Specifically, polished material is placed on rubbing head, utilizes pull of vacuum to be adsorbed by polished material tight, and adopt rubbing head to treat the pressure that polishing material applying is downward so that it is be fully contacted with polishing pad；Polishing disk and rubbing head all can rotate, now drip polishing fluid at polished material surface, polishing fluid is evenly distributed on polishing pad under centrifugal action, containing polishing particles and oxidant in polishing fluid, oxidant can be treated polishing material surface in polishing process and aoxidize, polishing particles then can be treated polishing material surface by polishing pad and carry out mechanical lapping, such that it is able to realize the synergism of mechanical grinding and chemical attack, the planarization completing to treat polishing material surface processes.
But, it is currently used for the polishing fluid of chemically mechanical polishing, buffing machine and finishing method and still haves much room for improvement.
Summary of the invention
It is contemplated that one of technical problem solved at least to a certain extent in correlation technique.
The present invention is based on the following discovery of inventor and completes:
Current chemical Mechanical Polishing Technique, when being polished for high rigidity, stable chemical nature, dysoxidizable semi-conducting material (such as gallium nitride, carborundum etc.), it is common to there is the problem that material surface clearance is relatively low, be difficult to quickly obtain flawless smooth planar surface.Inventor finds through further investigation and great many of experiments, it is due to above-mentioned semi-conducting material stable chemical nature, it is difficult to be corroded by the efficient oxidation in common CMP process, cause that in polishing process, the synergism of mechanical grinding and chemical attack is poor, thus material surface clearance is low, it is difficult to quickly obtained smooth planar surface by chemically mechanical polishing.
In view of this, in a first aspect of the present invention, the present invention proposes a kind of method assisting polishing outside the venue.The method includes: be added on by polishing fluid on polished crystal column surface, adopts polishing fluid described in ultra violet lamp, in order to completing described chemically mechanical polishing, wherein, described polishing fluid includes: polishing particles simultaneously；Oxidant；Photocatalyst；And deionized water.Utilize uviol lamp that polishing fluid is irradiated, photocatalyst catalysis can be made to be attached to the material generation oxidation reaction of photocatalyst surface, produce more strong oxidizer, and then this polishing fluid can be improved treat the oxidation effectiveness of polishing material, such that it is able to strengthen CMP process to treat the material removal degree on polishing material surface, be conducive to quickly obtaining the surface of smooth planar.
According to embodiments of the invention, based on the gross mass of described polishing fluid, the content of described polishing particles is 3wt%～6wt%；The content of described oxidant is 1wt%～4wt%；The content of described photocatalyst is 1wt%～3wt%, and surplus is described deionized water.Thus, it is possible to mechanical lapping and oxide etch synergism preferably in guarantee polishing process, such that it is able to improve efficiency and the effect of polishing, be conducive to quickly obtaining the surface of smooth planar.
According to embodiments of the invention, in this polishing fluid, described photocatalyst contains N-type semiconductor granule.The above-mentioned N-type semiconductor granule photocatalyst with photocatalysis performance, under the light such as ultraviolet light irradiate, catalysis can be attached to the material generation oxidation reaction of photocatalyst surface, produce more strong oxidizer, and then polished material surface out-of-flatness position can be corroded better, in conjunction with the polishing particles in this polishing fluid and oxidant, it is possible to improve the effect treating the corrosion of polishing material surface chemistry, be conducive to quickly obtaining the surface of smooth planar.
According to embodiments of the invention, in this polishing fluid, described N-type semiconductor granule is to be formed by selected from least one of titanium dioxide, tin ash and ferrum oxide.Above-mentioned N-type semiconductor granule is under irradiation under ultraviolet ray, catalysis can be attached to the material generation oxidation reaction of photocatalyst surface, produce more strong oxidizer, such that it is able to improve the chemical attack effect treating polishing material in CMP process, be conducive to quickly obtaining the surface of smooth planar.
According to embodiments of the invention, in this polishing fluid, the particle diameter of described photocatalyst is 30～200nm.The particle diameter of appropriateness can speed up the catalytic oxidation of photocatalyst, such that it is able to accelerated oxidation corrosion, such that it is able to improve the efficiency and the effect that utilize the method to carry out chemically mechanical polishing further.
According to embodiments of the invention, in this polishing fluid, described polishing particles is to be formed by selected from least one of silicon oxide, aluminium oxide and diamond, and optionally, the particle diameter of described polishing particles is 50～300nm.Thus, it is possible to mechanical lapping efficiency in raising polishing process and effect, be conducive to quickly obtaining the surface of smooth planar.
According to embodiments of the invention, in this polishing fluid, described oxidant contains at least one of hydrogen peroxide and potassium permanganate.Thus, it is possible to treat polishing material to carry out oxide etch, improve efficiency and the effect of polishing.
According to embodiments of the invention, in this polishing fluid, farther including: pH adjusting agent, described pH adjusting agent contains at least one of potassium hydroxide and nitric acid, and the content of described pH adjusting agent is not higher than 0.1wt%.PH value has material impact for oxidation and the catalytic performance of oxidant and photocatalyst, therefore according to the particular make-up of polishing fluid, the pH value of this polishing fluid can be adjusted, such that it is able to further enhance polishing effect.In another aspect of this invention, the present invention proposes a kind of chemical-mechanical polishing mathing.According to embodiments of the invention, this buffing machine includes: workbench, and described worktable upper surface is provided with sample area；Polishing tool, described polishing tool is arranged on above described workbench, described polishing tool and limit sample space between described workbench；Polishing fluid feedway, described polishing fluid feedway is configured to supply foregoing polishing fluid to described sample area；And uviol lamp, described uviol lamp is configured to irradiate described sample area.Thus, it is possible to utilize ultraviolet to cause polishing fluid generation light-catalyzed reaction, the Strong oxdiative material of generation can act on polished sample in real time, such that it is able to strengthen efficiency and the effect of oxide etch, and then improves the treatment effect of polishing.
In another aspect of this invention, the present invention proposes a kind of polishing fluid, and according to embodiments of the invention, this polishing fluid includes: polishing particles；Oxidant；Photocatalyst；And deionized water.Photocatalyst is under proper condition, catalysis can be attached to the material generation oxidation reaction of photocatalyst surface, produce more strong oxidizer, and then this polishing fluid can be improved treat the oxidation effectiveness of polishing material, such that it is able to strengthen CMP process to treat the material removal degree on polishing material surface, be conducive to quickly obtaining the surface of smooth planar.
According to embodiments of the invention, based on the gross mass of described polishing fluid, the content of described polishing particles is 3wt%～6wt%；The content of described oxidant is 1wt%～4wt%；The content of described photocatalyst is 1wt%～3wt%, and surplus is described deionized water.Thus, it is possible to mechanical lapping and oxide etch synergism preferably in guarantee polishing process, such that it is able to improve efficiency and the effect of polishing, be conducive to quickly obtaining the surface of smooth planar.
According to embodiments of the invention, in this polishing fluid, described photocatalyst contains N-type semiconductor granule.The above-mentioned N-type semiconductor granule photocatalyst with photocatalysis performance, under the light such as ultraviolet light irradiate, catalysis can be attached to the material generation oxidation reaction of photocatalyst surface, produce more strong oxidizer, and then polished material surface out-of-flatness position can be corroded better, in conjunction with the polishing particles in this polishing fluid and oxidant, it is possible to improve the effect treating the corrosion of polishing material surface chemistry, be conducive to quickly obtaining the surface of smooth planar.
According to embodiments of the invention, in this polishing fluid, described N-type semiconductor granule is to be formed by selected from least one of titanium dioxide, tin ash and ferrum oxide.Above-mentioned N-type semiconductor granule is under irradiation under ultraviolet ray, catalysis can be attached to the material generation oxidation reaction of photocatalyst surface, produce more strong oxidizer, such that it is able to improve the chemical attack effect treating polishing material in CMP process, be conducive to quickly obtaining the surface of smooth planar.
According to embodiments of the invention, in this polishing fluid, the particle diameter of described photocatalyst is 30～200nm.The particle diameter of appropriateness can speed up the catalytic oxidation of photocatalyst, such that it is able to accelerated oxidation corrosion, such that it is able to improve the efficiency and the effect that utilize this polishing fluid to carry out chemically mechanical polishing further.
According to embodiments of the invention, in this polishing fluid, described polishing particles is to be formed by selected from least one of silicon oxide, aluminium oxide and diamond, and optionally, the particle diameter of described polishing particles is 50～300nm.Thus, it is possible to mechanical lapping efficiency in raising polishing process and effect, be conducive to quickly obtaining the surface of smooth planar.
According to embodiments of the invention, in this polishing fluid, described oxidant contains at least one of hydrogen peroxide and potassium permanganate.Thus, it is possible to treat polishing material to carry out oxide etch, improve efficiency and the effect of polishing.
According to embodiments of the invention, in this polishing fluid, farther including: pH adjusting agent, described pH adjusting agent contains at least one of potassium hydroxide and nitric acid, and the content of described pH adjusting agent is not higher than 0.1wt%.PH value has material impact for oxidation and the catalytic performance of oxidant and photocatalyst, therefore according to the particular make-up of polishing fluid, the pH value of this polishing fluid can be adjusted, such that it is able to further enhance polishing effect.
According to embodiments of the invention, the pH value of described polishing fluid is 5～9.5.Thus, it is possible to improve oxidation and the catalytic performance of oxidant and photocatalyst, such that it is able to improve polishing effect.Further, the pH value polishing fluid not higher than 10 is conducive to completing chemically mechanical polishing under relatively mild condition, without the associated components of buffing machine is caused corrosion.
Accompanying drawing explanation
Fig. 1 shows the photocatalyst TEM figure of according to embodiments of the present invention 1；
Fig. 2 shows polisher structure schematic diagram according to an embodiment of the invention；
Fig. 3 shows CMP process schematic diagram according to an embodiment of the invention；
Fig. 4 shows the original wafer surface white light scanning interferogram of according to embodiments of the present invention 5；And
Fig. 5 shows crystal column surface white light scanning interferogram after the polishing of according to embodiments of the present invention 5.
Detailed description of the invention
Being described below in detail embodiments of the invention, the example of described embodiment is shown in the drawings.The embodiment described below with reference to accompanying drawing is illustrative of, it is intended to is used for explaining the present invention, and is not considered as limiting the invention.
In a first aspect of the present invention, the present invention proposes a kind of method of chemically mechanical polishing.According to embodiments of the invention, the method includes: be added on by polishing fluid on polished crystal column surface, adopts ultra violet lamp polishing fluid, in order to complete chemically mechanical polishing simultaneously.Under the irradiation of uviol lamp, photocatalyst in polishing fluid catalysis can be attached to the material generation oxidation reaction of photocatalyst surface, produce more strong oxidizer, raising is treated polishing material and is carried out efficiency and the effect of chemical attack, such that it is able to quickly obtain smooth surface, polishing effect is better.
Specifically, according to embodiments of the invention, with reference to Fig. 3, it is possible to adopt buffing machine, polishing fluid is used to complete polished sample, such as the chemically mechanical polishing of wafer.For example, it is possible to be arranged on rubbing head by wafer, polishing disk arranges polishing pad (not shown).Utilize the pull of vacuum of rubbing head so that it is be in close contact with wafer.Meanwhile, by rubbing head, wafer is applied downward pressure.Polishing fluid is dripped by polishing fluid exit, is distributed in crystal column surface.Due to polishing disk and rubbing head all rotatable (along figure curve arrow direction), therefore polishing fluid can be evenly distributed on polishing pad under the influence of centrifugal force.As it was previously stated, ultraviolet light field is dispersed, various location light intensity is different, therefore to obtain maximum luminous energy, polishing fluid exit can be directed at the direction of illumination of ultraviolet light.Further, for avoiding powerful light according to the materials such as the plastic pipe on machine are caused damage, the associated components of uviol lamp and buffing machine need to be kept to have certain distance.To there is the time short for the oxidizing species produced due to photocatalysis oxidation reaction, therefore can by polishing fluid exit close proximity to wafer position, it is ensured that oxidizing species utilizes as early as possible, participates in oxide etch reaction.Realize the catalytic performance of photocatalyst owing to the method adopts ultra-violet lamp to irradiate polishing fluid exit, be therefore more widely applicable for the preparation process of various sizes wafer, be not limited to 2 inches of small size wafers, be conducive to large-scale promotion to utilize.
Understand in order to convenient, first below the concrete composition of this polishing fluid is described in detail.
According to embodiments of the invention, polishing particles is containing at least one of silica, aluminium oxide and diamond, and the content of polishing particles can be 3wt%～6wt%, and the particle diameter of polishing particles can be 50～300nm.Thus, it is possible to effectively treat polishing material surface in CMP process to carry out mechanical lapping, in order to remove, by mechanical grinding, the material that polished material surface is prominent, it is thus achieved that smooth surface.It should be noted that, in the present invention, the concrete kind of polishing particles and content are not particularly limited, the concrete condition (such as parameters such as hardness) of the material that those skilled in the art can polish according to actual needs, in above-mentioned scope, composition and content to polishing particles select.Such as, according to a particular embodiment of the invention, the particle diameter of silicon dioxide can be 100nm；The particle diameter of aluminium oxide can be 300nm；The particle diameter of diamond can be 100nm.There is the above-mentioned material going through scope and under the premise not scratching polished material surface, CMP process can provide comparatively strong mechanical lapping, such that it is able to improve polishing efficiency and effect.
According to embodiments of the invention, oxidant contains at least one of hydrogen peroxide and potassium permanganate, and the content of oxidant can be 1wt%～4wt%.Thus, it is possible in polishing process, treat polishing material surface and carry out oxide etch, in conjunction with the mechanical abrasive action of polishing process, it is possible to more effectively improve the flatness of polished material surface, improve efficiency and the effect of chemically mechanical polishing.It should be noted that, in the present invention, the concrete kind of oxidant and content are not particularly limited, the concrete condition (such as chemical composition, chemical stability etc.) of the material that those skilled in the art can polish according to actual needs, in above-mentioned scope, composition and content to oxidant select.
According to embodiments of the invention, photocatalyst contains N-type semiconductor granule, and the content of photocatalyst can be 1wt%～3wt%.N-type semiconductor granule has photocatalysis performance, under the light such as ultraviolet light irradiate, catalysis can be attached to the material generation oxidation reaction of photocatalyst surface, produce more strong oxidizer, and then polished material surface out-of-flatness position can be corroded better, in conjunction with the polishing particles in this polishing fluid and oxidant, it is possible to improve the effect treating the corrosion of polishing material surface chemistry, be conducive to quickly obtaining the surface of smooth planar.It should be noted that, particular make-up and the concrete content of above-mentioned N-type semiconductor granule are not particularly limited, those skilled in the art can according to the content of oxidant, polishing particles in the concrete chemical composition of polished material, chemical inertness degree and polishing fluid, and the parameter at above-mentioned scope interior focusing catalyst carries out selecting and regulating.Above-mentioned substance has good photocatalysis performance under irradiation under ultraviolet ray, and price is less expensive, and technology of preparing is ripe, is conducive to the polishing fluid large-scale application containing above-mentioned substance.It will be appreciated to those of skill in the art that in actual applications, it is possible to the ultraviolet wavelength of its decomposition, coupling can produce the ultra-violet lamp of respective wavelength and polishing fluid is irradiated to select optimum to promote according to the particular type of oxidant in polishing fluid.In order to improve the catalytic effect of photocatalyst further, it is possible to selecting the N-type semiconductor granule that energy gap is narrower, particle diameter is less, more little energy gap and particle diameter easily produce better catalytic performance.Such as, according to some embodiments of the present invention, N-type semiconductor granule can be formed by selected from least one of titanium dioxide, tin ash and ferrum oxide.It is for instance possible to use anatase titanium dioxide is as photocatalyst.In order to improve catalytic effect further, titanium dioxide can be nano-particle, and the particle diameter of nano-particle can be 30nm～100nm.Thus, it is possible to granule narrower by above-mentioned energy gap, that particle diameter is less constitutes photocatalyst, such that it is able to improve the polishing effect of this polishing fluid.
It will be appreciated to those of skill in the art that ultraviolet light field is dispersed, various location light intensity is different.Therefore, in actual use in order to enable photocatalyst to obtain maximum luminous energy, it is possible to polishing fluid exit to be directed at the direction of illumination of ultraviolet light.Polishing fluid exit can be irradiated by ultra-violet lamp due to the present invention and realize catalysis, therefore be more widely applicable for the preparation process of various sizes wafer, be not limited to 2 inches of small size wafers, be conducive to large-scale promotion to utilize.
What skilled artisans appreciate that is, the pH value of polishing fluid has a certain impact for oxidation effectiveness and the catalytic performance tool of previously described oxidant and photocatalyst, therefore, according to embodiments of the invention, this polishing fluid can further include pH adjusting agent.Specifically, pH adjusting agent can contain at least one of potassium hydroxide and nitric acid, and the content of pH adjusting agent is very low, for the pH value of polishing fluid is finely tuned.Specifically, based on the gross mass of this polishing fluid, the content of pH adjusting agent can not higher than 0.1wt%.In actual applications, those skilled in the art according to the particular make-up of polishing fluid, can utilize above-mentioned pH adjusting agent that the pH value of this polishing fluid is adjusted, such that it is able to further enhance polishing effect.According to embodiments of the invention, the pH value of this polishing fluid can be 5～9.5.Thus, namely oxidation and the catalytic performance of oxidant and photocatalyst can be improved, such that it is able to raising polishing effect, chemically mechanical polishing can be completed again, it is to avoid the acid or alkaline associated components excessively treating by force polishing material (such as gallium nitride wafer) or buffing machine of polishing fluid causes corrosion under relatively mild condition.
According to embodiments of the invention, in order to improve the polishing effect of the method further, the method may further include: adopts dehydrated alcohol that the wafer through chemically mechanical polishing is carried out ultrasonic cleaning.Thus, it is possible to removing is attached to the materials such as the remaining polishing fluid of crystal column surface easily, it is thus achieved that smooth surface.
In sum, cmp method according to embodiments of the present invention has following characteristics and advantage:
1, containing photocatalyst in polishing fluid, it is achieved that effective utilization of unstable strong oxidizer, accelerating oxide etch reaction, thus improving planarization working (machining) efficiency, being conducive to quickly obtaining the crystal column surface of smooth planar；
2, polishing fluid exit can be irradiated by ultra-violet lamp and realize the catalytic performance of photocatalyst, be more widely applicable for the preparation process of various sizes wafer, be not limited to 2 inches of small size wafers, be conducive to large-scale promotion to utilize.
3, after the method polishing, residual is few, and quality of finish is high, and speed is fast, it is easy to clean.
Another aspect of the present invention, the present invention proposes a kind of chemical-mechanical polishing mathing.According to embodiments of the invention, with reference to Fig. 2, this buffing machine includes: workbench 100, polishing tool 200, polishing fluid feedway 300 and uviol lamp 400.Specifically, workbench 100 upper surface is provided with sample area, it is possible to by polished sample, for instance polished wafer is arranged in the sample area on workbench 100.Polishing tool 200 is arranged on above workbench 100, polishing tool 200 and limit sample space between workbench 100, in order to utilize the part place that polished sample is arranged in sample space by polishing tool 200 to be processed by shot blasting.Polishing fluid feedway 300 is configured to supply previously described polishing fluid to sample area, uviol lamp 400 is configured to irradiate sample area, to make the photocatalyst generation light-catalyzed reaction in the polishing fluid of sample area, generate Strong oxdiative material, and this Strong oxdiative material is used for chemical mechanical polish process in real time.Thus, it is possible to utilize ultraviolet to cause polishing fluid generation light-catalyzed reaction, the Strong oxdiative material of generation can act on polished sample in real time, such that it is able to strengthen efficiency and the effect of oxide etch, and then improves the treatment effect of polishing.
It should be noted that, particular type and the concrete polishing mode of above-mentioned workbench 100, polishing tool 200 and polishing fluid feedway 300 are not particularly limited, as long as the chemically mechanical polishing of complete paired samples under previously described polishing fluid existent condition of this buffing machine can be utilized.Such as, with reference to Fig. 3, polishing tool 200 can be rubbing head, workbench 100 can have polishing pad (not shown), and rubbing head can for can be rotatably set in the top of workbench 100 (i.e. polishing disk shown in figure), in order to rotate by surrounding the direction of arrow of rubbing head in figure, utilize the pull of vacuum of rubbing head, make rubbing head and polished sample, for instance, it is possible to it is in close contact for polished wafer.Polishing fluid is dripped by polishing fluid exit, is distributed in crystal column surface.Additionally, polishing disk is it can also be provided that rotatable, thus, polishing fluid can be evenly distributed on polishing pad under the influence of centrifugal force, such that it is able to improve efficiency and the effect of polishing.
In still another aspect of the invention, the present invention proposes a kind of polishing fluid.According to embodiments of the invention, this polishing fluid includes: polishing particles；Oxidant；Photocatalyst；And deionized water.According to embodiments of the invention, photocatalyst is under proper condition, catalysis can be attached to the material generation oxidation reaction of photocatalyst surface, produce more strong oxidizer, and then the oxidation effectiveness treating polishing material can be improved, such that it is able to strengthen chemical machinery throwing process to treat the material removal degree on polishing material surface, be conducive to quickly obtaining the surface of smooth planar.Such as, under the irradiation of the light such as ultraviolet light, photocatalyst can catalytic adsorption in the oxidant generation oxidation reaction of photocatalyst surface, produce the unstable Strong oxdiative materials such as free radical.Now polishing fluid contacts with polished material, it is ensured that Strong oxdiative material utilizes as early as possible, participates in oxide etch reaction.And above-mentioned Strong oxdiative material is due to chemical property extremely unstable, it is added directly in polishing fluid and can not play a role.Inventor finds through great many of experiments, by adding the photocatalyst with catalytic oxidation function in polishing fluid, can in use by providing the environment (laser irradiation etc.) that can make photocatalyst generation catalytic performance, produce Strong oxdiative material in real time, such that it is able to be effectively improved the effect of chemical attack, be conducive to quickly obtaining smooth surface.
Below according to embodiments of the invention, the concrete composition of this polishing fluid is described in detail.According to embodiments of the invention, polishing particles is to be formed by selected from least one of silicon oxide, aluminium oxide and diamond, and the content of polishing particles can be 3wt%～6wt%, and the particle diameter of polishing particles can be 50～300nm.Thus, it is possible to effectively treat polishing material surface in CMP process to carry out mechanical lapping, in order to remove, by mechanical grinding, the material that polished material surface is prominent, it is thus achieved that smooth surface.It should be noted that, in the present invention, the concrete kind of polishing particles and content are not particularly limited, the concrete condition (such as parameters such as hardness) of the material that those skilled in the art can polish according to actual needs, in above-mentioned scope, composition and content to polishing particles select.Such as, according to a particular embodiment of the invention, the particle diameter of silicon dioxide can be 100nm；The particle diameter of aluminium oxide can be 300nm；The particle diameter of diamond can be 100nm.There is the above-mentioned material going through scope and under the premise not scratching polished material surface, CMP process can provide comparatively strong mechanical lapping, such that it is able to improve polishing efficiency and effect.
According to embodiments of the invention, oxidant contains hydrogen peroxide with at least one of potassium permanganate, and the content of oxidant can be 1wt%～4wt%.Thus, it is possible in polishing process, treat polishing material surface and carry out oxide etch, in conjunction with the mechanical abrasive action of polishing process, it is possible to more effectively improve the flatness of polished material surface, improve efficiency and the effect of chemically mechanical polishing.It should be noted that, in the present invention, the concrete kind of oxidant and content are not particularly limited, the concrete condition (such as chemical composition, chemical stability etc.) of the material that those skilled in the art can polish according to actual needs, in above-mentioned scope, composition and content to oxidant select.
According to embodiments of the invention, photocatalyst contains N-type semiconductor granule, and the content of photocatalyst can be 1wt%～3wt%.N-type semiconductor granule has photocatalysis performance, under the light such as ultraviolet light irradiate, catalysis can be attached to the material generation oxidation reaction of photocatalyst surface, produce more strong oxidizer, and then polished material surface out-of-flatness position can be corroded better, in conjunction with the polishing particles in this polishing fluid and oxidant, it is possible to improve the effect treating the corrosion of polishing material surface chemistry, be conducive to quickly obtaining the surface of smooth planar.It should be noted that, particular make-up and the concrete content of above-mentioned N-type semiconductor granule are not particularly limited, those skilled in the art can according to the content of oxidant, polishing particles in the concrete chemical composition of polished material, chemical inertness degree and polishing fluid, and the parameter at above-mentioned scope interior focusing catalyst carries out selecting and regulating.Above-mentioned substance has good photocatalysis performance under irradiation under ultraviolet ray, and price is less expensive, and technology of preparing is ripe, is conducive to the polishing fluid large-scale application containing above-mentioned substance.It will be appreciated to those of skill in the art that in actual applications, it is possible to the ultraviolet wavelength of its decomposition, coupling can produce the ultra-violet lamp of respective wavelength and polishing fluid is irradiated to select optimum to promote according to the particular type of oxidant in polishing fluid.In order to improve the catalytic effect of photocatalyst further, it is possible to selecting the N-type semiconductor granule that energy gap is narrower, particle diameter is less, more little energy gap and particle diameter easily produce better catalytic performance.Such as, according to some embodiments of the present invention, N-type semiconductor granule can be formed by selected from least one of titanium dioxide, tin ash and ferrum oxide.It is for instance possible to use anatase titanium dioxide is as photocatalyst.In order to improve catalytic effect further, titanium dioxide can be nano-particle, and the particle diameter of nano-particle can be 30nm～100nm.Thus, it is possible to granule narrower by above-mentioned energy gap, that particle diameter is less constitutes photocatalyst, such that it is able to improve the polishing effect of this polishing fluid.
What skilled artisans appreciate that is, the pH value of polishing fluid has a certain impact for oxidation effectiveness and the catalytic performance tool of previously described oxidant and photocatalyst, therefore, according to embodiments of the invention, this polishing fluid can further include pH adjusting agent.Specifically, pH adjusting agent can contain at least one of potassium hydroxide and nitric acid, and the content of pH adjusting agent is very low, for the pH value of polishing fluid is finely tuned.Specifically, based on the gross mass of this polishing fluid, the content of pH adjusting agent can not higher than 0.1wt%.In actual applications, those skilled in the art according to the particular make-up of polishing fluid, can utilize above-mentioned pH adjusting agent that the pH value of this polishing fluid is adjusted, such that it is able to further enhance polishing effect.Owing to the oxidability of the oxidant in this polishing fluid and the Strong oxdiative material of photocatalyst generation is relevant to environmental pH, therefore pH value is adjusted to suitable scope, be conducive to improving the oxidability of oxidant and Strong oxdiative material, such that it is able to improve the polishing effect of this polishing fluid further.According to embodiments of the invention, it is possible to regulating the pH value making polishing fluid is 5～9.5.Thus, namely oxidation and the catalytic performance of oxidant and photocatalyst can be improved, such that it is able to raising polishing effect, chemically mechanical polishing can be completed again, it is to avoid the acid or alkaline associated components excessively treating by force polishing material (such as gallium nitride wafer) or buffing machine of polishing fluid causes corrosion under relatively mild condition.In sum, polishing fluid according to embodiments of the present invention has following characteristics and advantage:
1, containing photocatalyst, it is achieved that effective utilization of unstable strong oxidizer, accelerating oxide etch reaction, thus improving planarization working (machining) efficiency, being conducive to quickly obtaining the crystal column surface of smooth planar；
2, polishing fluid exit can be irradiated by ultra-violet lamp and realize the catalytic performance of photocatalyst, be more widely applicable for the preparation process of various sizes wafer, be not limited to 2 inches of small size wafers, be conducive to large-scale promotion to utilize.
3, the Component Source contained in this polishing fluid group is extensive, it is easy to obtain, and preparation technology is simple, with low cost.
4, after the polishing of this polishing fluid, residual is few, and quality of finish is high, and speed is fast, it is easy to clean.
5, the pH value of this polishing fluid is moderate, it is possible to ensures the oxidation susceptibility of oxidant and Strong oxdiative material, and prevents from the associated components of buffing machine is caused corrosion.
Below by specific embodiment, the present invention will be described, it should be noted that, following specific embodiment is only used for descriptive purpose, and the scope not limited the present invention in any way, additionally, if no special instructions, then the method specifically not recording condition or step is conventional method, and the reagent and the material that adopt all commercially obtain.
The preparation of embodiment 1 polishing fluid
Adopting titanium dioxide as photocatalyst, hydrogen peroxide and nitric acid as oxidant, silicon oxide is polishing particles, adds deionized water and is configured to polishing fluid, and with potassium hydroxide regulate to pH value be 9.5.In solution, each component proportion is as follows:
| Title | Content |
| Polishing particles | 6% |
| Oxidant | 4% |
| Photocatalyst | 3% |
| Deionized water | Surplus |
The titanium dioxide adopted in the present embodiment is nano-particle, and particle diameter is 30nm～100nm.With reference to Fig. 1, this titania nanoparticles has less particle diameter and good dispersibility.
Weigh each component according to said ratio, polishing particles, oxidant, photocatalyst are scattered in deionized water, and are sufficiently stirred for agitator.PH meter is put in the sufficient above-mentioned solution of stirring, add a small amount of potassium hydroxide or nitric acid, pH value is regulated to 9.5.The polishing fluid regulating pH value being covered preservative film continue to be sufficiently stirred for, mixing time is 1～2h so that it is mix homogeneously.
The preparation of embodiment 2 polishing fluid
Adopt the material in embodiment 1 and method to prepare polishing fluid, institute the difference is that, adopt potassium hydroxide regulate to pH value be 9.In solution, each component proportion is as follows:
| Title | Content |
| Polishing particles | 4% |
| Oxidant | 4% |
| Photocatalyst | 2% |
| Deionized water | Surplus |
The preparation of embodiment 3 polishing fluid
Adopt the material in embodiment 1 and method to prepare polishing fluid, institute the difference is that, adopt potassium hydroxide regulate to pH value be 8.In solution, each component proportion is as follows:
| Title | Content |
| Polishing particles | 3% |
| Oxidant | 2% |
| Photocatalyst | 2.5% |
| Deionized water | Surplus |
The preparation of embodiment 4 polishing fluid
Adopt the material in embodiment 1 and method to prepare polishing fluid, institute the difference is that, adopt potassium hydroxide regulate to pH value be 5.In solution, each component proportion is as follows:
| Title | Content |
| Polishing particles | 6% |
| Oxidant | 4% |
| Photocatalyst | 3% |
| Deionized water | Surplus |
Embodiment 5 polishing wafer
Adopt CP-4 chemical-mechanical polishing mathing (being furnished with a rubbing head), utilize the polishing fluid of preparation in embodiment 1 that 2 inches of gallium nitride wafers are polished.Regulating the position of uviol lamp distance buffing machine, make alignment ultra violet lamp direction, polishing fluid exit, other parameters are as follows:
Downforce 5.6psi, rubbing head rotating speed 120rpm and polishing disk 160rpm: specifically set according to semiconductor crystal wafer situation；
Polishing time: 10～20min；Polishing pad: polyurethane polishing pad；Polishing fluid flow: 100～150ml/min；Polishing process temperature: 20～25 DEG C
Crystal column surface quality testing after throwing:
Use the crystal column surface pattern before and after the observation polishing of white light scanning interferometer, use 50 times of object lens observations.By observe throw rear surface white light scanning two dimension and graphics, surface roughness (Ra) assesses flatness and surface quality after throwing.For avoiding the crystal column surface attachment impurity impact on experimental result, need wafer ultrasonic cleaning 20～30 minutes in dehydrated alcohol afterwards on pretreatment.With reference to Fig. 4 and Fig. 5, crystal column surface rough whole (Fig. 4) before polishing, the obvious flat smooth of crystal column surface (Fig. 5) after polishing.
Semiconductor crystal wafer ultrasonic cleaning crossed before and after experiment and dry weighs quality on electronic balance, with reference to formula (I), calculate material remove rate MRR (nm/h) according to the decreasing value of quality and density of material, wafer area and polishing time etc.:
Wherein, Δ m is quality decreasing value (unit g) after throwing.Gallium nitride material clearance after polishing is 122nm/h, and adopting the gallium nitride material clearance that tradition CMP method obtains is 41nm/h, absolutely prove that polishing fluid and the finishing method of the present invention can significantly improve planarization working (machining) efficiency in field of semiconductor manufacture, save man-hour.
Comparative example 1
Adopt the method in embodiment 5 that 2 inches of gallium nitride wafers are polished, institute the difference is that, polishing process does not adopt uviol lamp polishing fluid is irradiated.After polishing, gallium nitride material clearance is 42nm/h, and clearance is basic identical with the clearance of tradition CMP method.
In the description of this specification, specific features, structure, material or feature that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means in conjunction with this embodiment or example describe are contained at least one embodiment or the example of the present invention.In this manual, the schematic representation of above-mentioned term is necessarily directed to identical embodiment or example.And, the specific features of description, structure, material or feature can combine in one or more embodiments in office or example in an appropriate manner.Additionally, when not conflicting, the feature of the different embodiments described in this specification or example and different embodiment or example can be carried out combining and combining by those skilled in the art.
Although above it has been shown and described that embodiments of the invention, it is understandable that, above-described embodiment is illustrative of, it is impossible to be interpreted as limitation of the present invention, and above-described embodiment can be changed, revises, replace and modification by those of ordinary skill in the art within the scope of the invention.
Claims (10)
1. the method for a chemically mechanical polishing, it is characterised in that including: be added on by polishing fluid on polished crystal column surface, adopts polishing fluid described in ultra violet lamp, in order to complete described chemically mechanical polishing simultaneously,
Wherein, described polishing fluid includes: polishing particles；Oxidant；Photocatalyst；And deionized water.
2. method according to claim 1, it is characterised in that based on the gross mass of described polishing fluid, the content of described polishing particles is 3wt%～6wt%；The content of described oxidant is 1wt%～4wt%；The content of described photocatalyst is 1wt%～3wt%, and surplus is described deionized water.
3. method according to claim 1, it is characterised in that described photocatalyst contains N-type semiconductor granule, described N-type semiconductor granule is to be formed by selected from least one of titanium dioxide, tin ash and ferrum oxide；
Optionally, the particle diameter of described photocatalyst is 30～200nm.
4. method according to claim 1, it is characterised in that described polishing particles is to be formed by selected from least one of silicon oxide, aluminium oxide and diamond；
Optionally, the particle diameter of described polishing particles is 50～300nm；
Optionally, described oxidant contains at least one of hydrogen peroxide and potassium permanganate.
5. method according to claim 1, it is characterised in that described polishing fluid farther includes pH adjusting agent, described pH adjusting agent contains at least one of potassium hydroxide and nitric acid, and the content of described pH adjusting agent is not higher than 0.1wt%.
6. a chemical-mechanical polishing mathing, it is characterised in that including:
Workbench, described worktable upper surface is provided with sample area；
Polishing tool, described polishing tool is arranged on above described workbench, described polishing tool and limit sample space between described workbench；
Polishing fluid feedway, described polishing fluid feedway is configured to supply the polishing fluid described in any one of claim 1-5 to described sample area；And
Uviol lamp, described uviol lamp is configured to irradiate described sample area.
7. a polishing fluid, it is characterised in that including:
Polishing particles；
Oxidant；
Photocatalyst；And
Deionized water.
8. polishing fluid according to claim 7, it is characterised in that based on the gross mass of described polishing fluid, the content of described polishing particles is 3wt%～6wt%；The content of described oxidant is 1wt%～4wt%；The content of described photocatalyst is 1wt%～3wt%, and surplus is described deionized water.
9. polishing fluid according to claim 7, it is characterised in that described photocatalyst contains N-type semiconductor granule, described N-type semiconductor granule is to be formed by selected from least one of titanium dioxide, tin ash and ferrum oxide；
Optionally, the particle diameter of described photocatalyst is 30～200nm；
Optionally, described polishing particles is to be formed by selected from least one of silicon oxide, aluminium oxide and diamond,
Optionally, the particle diameter of described polishing particles is 50～300nm；
Optionally, described oxidant contains at least one of hydrogen peroxide and potassium permanganate.
10. polishing fluid according to claim 7, it is characterised in that farther include: pH adjusting agent, described pH adjusting agent contains at least one of potassium hydroxide and nitric acid, and the content of described pH adjusting agent is not higher than 0.1wt%.
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