WO2023234304A1 - エッチング方法 - Google Patents

エッチング方法 Download PDF

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Publication number
WO2023234304A1
WO2023234304A1 PCT/JP2023/020125 JP2023020125W WO2023234304A1 WO 2023234304 A1 WO2023234304 A1 WO 2023234304A1 JP 2023020125 W JP2023020125 W JP 2023020125W WO 2023234304 A1 WO2023234304 A1 WO 2023234304A1
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WIPO (PCT)
Prior art keywords
etching
gas
etched
compound
fluorodithiethane
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PCT/JP2023/020125
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English (en)
French (fr)
Japanese (ja)
Inventor
一真 松井
優希 岡
萌 谷脇
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Resonac Corp
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Resonac Corp
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Priority to KR1020247038317A priority Critical patent/KR20250016114A/ko
Priority to US18/867,945 priority patent/US20250361440A1/en
Priority to JP2024524877A priority patent/JPWO2023234304A1/ja
Publication of WO2023234304A1 publication Critical patent/WO2023234304A1/ja
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P50/00—Etching of wafers, substrates or parts of devices
    • H10P50/20—Dry etching; Plasma etching; Reactive-ion etching
    • H10P50/28—Dry etching; Plasma etching; Reactive-ion etching of insulating materials
    • H10P50/282—Dry etching; Plasma etching; Reactive-ion etching of insulating materials of inorganic materials
    • H10P50/283—Dry etching; Plasma etching; Reactive-ion etching of insulating materials of inorganic materials by chemical means
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00—Etching, surface-brightening or pickling compositions
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00—Etching, surface-brightening or pickling compositions
    • C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
    • C09K13/08—Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P50/00—Etching of wafers, substrates or parts of devices
    • H10P50/20—Dry etching; Plasma etching; Reactive-ion etching
    • H10P50/24—Dry etching; Plasma etching; Reactive-ion etching of semiconductor materials
    • H10P50/242—Dry etching; Plasma etching; Reactive-ion etching of semiconductor materials of Group IV materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P50/00—Etching of wafers, substrates or parts of devices
    • H10P50/20—Dry etching; Plasma etching; Reactive-ion etching
    • H10P50/26—Dry etching; Plasma etching; Reactive-ion etching of conductive or resistive materials
    • H10P50/264—Dry etching; Plasma etching; Reactive-ion etching of conductive or resistive materials by chemical means
    • H10P50/266—Dry etching; Plasma etching; Reactive-ion etching of conductive or resistive materials by chemical means by vapour etching only
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P50/00—Etching of wafers, substrates or parts of devices
    • H10P50/71—Etching of wafers, substrates or parts of devices using masks for conductive or resistive materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P50/00—Etching of wafers, substrates or parts of devices
    • H10P50/73—Etching of wafers, substrates or parts of devices using masks for insulating materials

Definitions

  • the present invention relates to an etching method.
  • Patent Documents 1 and 2 disclose a dry etching method in which a silicon material such as silicon oxide or silicon nitride is etched using an etching gas containing a sulfur-containing compound as an etching compound and a carbon material such as amorphous carbon as a mask. ing.
  • An object of the present invention is to provide an etching method with a high etching selectivity, which is the ratio of the etching rate of a silicon material to the etching rate of a carbon material.
  • an etching gas containing an etching compound is brought into contact with an etched member having an etched object to be etched by the etching gas and a non-etched object which is not to be etched by the etching gas, comprising an etching step of selectively etching the etching target object compared to the etching target object,
  • the etching object has a silicon material
  • the non-etching object has a carbon material
  • the etching compound is fluorodithiethane represented by the chemical formula C x F y S 2 , where x in the chemical formula is 2 or more and 6 or less, and y is 4 or more and 12 or less
  • the etching gas contains or does not contain at least one metal selected from sodium, magnesium, aluminum, potassium, calcium, chromium, manganese, iron, cobalt, nickel, copper, and molybdenum, and contains the above metal. If so, an
  • the fluorodithiethane is 2,2,4,4-tetrafluoro-1,3-dithiethane, 1,1,2,2,3,3,4,4-octafluoro-1,3-dithiethane , 2,2,4-trifluoro-4-trifluoromethyl-1,3-dithiethane, 2,4-difluoro-2,4-bis(trifluoromethyl)-1,3-dithiethane, and 2,2,
  • the etching method according to [1] comprising at least one of 4,4-tetrakis(trifluoromethyl)-1,3-dithiethane.
  • the silicon material has at least one of a silicon compound and polysilicon, and the silicon compound is a compound having a silicon atom and at least one of an oxygen atom and a nitrogen atom [1] or [2]
  • [4] The etching method according to any one of [1] to [3], wherein the carbon material includes at least one of photoresist and amorphous carbon.
  • [5] The etching method according to any one of [1] to [4], wherein the etching gas contains the fluorodithiethane and at least one of a second etching compound and an inert gas.
  • the etching selectivity ratio which is the ratio of the etching rate of silicon material to the etching rate of carbon material, is high.
  • FIG. 1 is a schematic diagram showing an example of an etching apparatus for explaining an embodiment of an etching method according to the present invention.
  • 1 is a schematic diagram showing an example of a purification apparatus for refining fluorodithiethane or sulfur hexafluoride.
  • FIG. 2 is a schematic diagram showing an example of a preparation device for preparing an aqueous nitric acid solution used for measuring the concentration of metals in fluorodithiethane. It is a schematic diagram showing an example of the preparation device which prepares the nitric acid aqueous solution used for the concentration measurement of the metal in sulfur hexafluoride.
  • an etching gas containing an etching compound is brought into contact with an etched member having an etched object to be etched by the etching gas and a non-etched object not to be etched by the etching gas. and an etching step for selectively etching the object to be etched compared to the object not to be etched.
  • the etched object has a silicon material
  • the non-etched object has a carbon material
  • the etching compound is fluorodithiethane represented by the chemical formula C x F y S 2 .
  • x is 2 or more and 6 or less
  • y is 4 or more and 12 or less.
  • the etching gas contains sodium (Na), magnesium (Mg), aluminum (Al), potassium (K), calcium (Ca), chromium (Cr), manganese (Mn), iron (Fe), and cobalt (Co). , nickel (Ni), copper (Cu), and molybdenum (Mo), or if the metal is contained, the concentration of all the metals contained. The total amount is 300 mass ppb or less.
  • silicon material that is the object to be etched reacts with the etching compound in the etching gas, so that etching of the silicon material progresses.
  • the carbon material, which is not an object to be etched hardly reacts with the etching compound, the etching of the carbon material hardly progresses. Therefore, according to the etching method according to this embodiment, silicon material can be selectively etched compared to carbon material (that is, high etching selectivity can be obtained).
  • the etching method according to the present embodiment performs etching using an etching gas that does not contain metal or contains a very small amount of metal, so it is difficult to etch carbon materials.
  • the etching selectivity ratio which is the ratio of the etching speed of the silicon material to the etching speed, is high.
  • the etching selectivity ratio which is the ratio of the etching rate of the silicon material to the etching rate of the carbon material, can be set to, for example, 1.2 or more.
  • the etching selectivity ratio is preferably 2 or more, more preferably 30 or more.
  • the etching method according to this embodiment can be used for manufacturing semiconductor devices. For example, if the etching method according to this embodiment is applied to a semiconductor substrate having a thin film made of a silicon material and a thin film made of a carbon material, and the thin film made of a silicon material is etched using the thin film made of a carbon material as a mask. , three-dimensionally integrated semiconductor devices can be manufactured.
  • etching in the present invention refers to processing the etched member into a predetermined shape (for example, a three-dimensional shape) by removing part or all of the object to be etched that the etched member has (for example, when the etched member is processing of a film-like object to be etched made of a silicon material into a predetermined thickness.
  • the "metal" in "metal concentration” in the present invention includes metal atoms and metal ions.
  • etching method for the etching method according to this embodiment, either plasma etching that uses plasma or plasmaless etching that does not use plasma can be used.
  • plasma etching include reactive ion etching (RIE), inductively coupled plasma (ICP) etching, and capacitively coupled plasma (CCP) etching.
  • RIE reactive ion etching
  • ICP inductively coupled plasma
  • CCP capacitively coupled plasma
  • ECR electron cyclotron resonance
  • microwave plasma etching microwave plasma etching.
  • plasma may be generated in a chamber in which the member to be etched is installed, or the plasma generation chamber and the chamber in which the member to be etched is installed may be separated (i.e., using remote plasma).
  • Etching using remote plasma can sometimes make it possible to etch the silicon material that is the object to be etched with higher selectivity.
  • the etching compound contained in the etching gas is a compound that hardly reacts with the carbon material and reacts with the silicon material to advance the etching of the silicon material.
  • the etching compound is fluorodithiethane represented by the chemical formula C x F y S 2 , in which x is 2 or more and 6 or less and y is 4 or more and 12 or less. From the viewpoint of stability, fluorodithiethane in which x in the chemical formula is 2 or more and 4 or less and y is 4 or more and 12 or less is preferable.
  • Etching compounds may be used alone or in combination of two or more.
  • fluorodithiethane represented by the chemical formula C It can be used as an etching compound in an etching method according to the present invention.
  • fluorodithiethane having a 1,3-dithiethane structure is preferred, and fluorodithiethane having a 1,3-dithiethane structure and having no unsaturated bond is more preferred.
  • a film of a compound having a carbon-sulfur bond is formed on the surface of the carbon material.
  • Films of this compound have relatively high resistance to active species that arise from combinations of chemical species such as fluorine, chlorine, bromine, oxygen, carbon, and nitrogen atoms and are effective in etching silicon materials. have Therefore, this compound film has the effect of suppressing etching of the carbon material. As a result, the silicon material is selectively etched compared to the carbon material.
  • fluorodithiethane having a 1,3-dithiethane structure and having no unsaturated bond is 2,2,4,4-tetrafluoro-1,3-dithiethane (C 2 F 4 S 2 , chemical formula 1).
  • fluorodithiethanes include 2,2,4,4-tetrafluoro-1,3-dithiethane, 1,1,2,2,3, 3,4,4-octafluoro-1,3-dithiethane, 2,2,4-trifluoro-4-trifluoromethyl-1,3-dithiethane, 2,4-difluoro-2,4-bis(trifluoro methyl)-1,3-dithiethane and 2,2,4,4-tetrakis(trifluoromethyl)-1,3-dithiethane are more preferable, and 2,2,4, 4-tetrafluoro-1,3-dithiethane is more preferred.
  • the etching gas is a gas containing an etching compound (fluorodithiethane), but it may also be a gas consisting only of the etching compound, or a mixed gas containing the etching compound and another type of gas other than the etching compound. There may be.
  • the concentration of the etching compound contained in the etching gas is particularly limited as long as it is a concentration that allows processing of silicon materials. isn't it.
  • the concentration of the etching compound contained in the etching gas can be, for example, more than 0 volume% and less than 100 volume%, but preferably 1 volume% or more and 50 volume% or less, and 3 volume% or more and 30 volume%. It is more preferably at least 5% by volume and not more than 20% by volume, and particularly preferably at least 10% by volume and not more than 20% by volume.
  • the concentration of the etching compound in the etching gas is within the above numerical range, the etching rate of the silicon material tends to be high. Furthermore, since the plasma etching resistance of the carbon material increases, the etching selectivity ratio of the silicon material to the carbon material tends to increase.
  • gases other than the etching compound contained in the etching gas include a second etching compound and an inert gas.
  • the etching gas may contain either the second etching compound or the inert gas, or may contain both.
  • Methods for mixing each component in the etching gas include introducing gases other than the etching compound at an arbitrary ratio into a container containing the etching compound, and adjusting the flow rate of the etching compound and the gas other than the etching compound. Examples include a method of supplying the gas to a container or an etching apparatus while controlling the flow rate of each gas.
  • the second etching compound is a compound capable of etching at least a portion of the member to be etched, and is a compound other than the fluorodithiethane.
  • the second etching compound include halogen-containing compounds, oxygen-containing compounds, and hydrogen gas (H 2 ).
  • a halogen-containing compound is a compound having a halogen atom such as a fluorine atom, a chlorine atom, a bromine atom, or an iodine atom in its molecule.
  • An oxygen-containing compound is a compound having an oxygen atom in its molecule.
  • the second etching compound may be used alone or in combination of two or more. Note that the second etching compound does not include compounds that will be exemplified later as impurities.
  • the etching characteristics may be improved.
  • improvements in etching characteristics include improved accuracy in vertical processability, improved etching rate of silicon materials, improved etching selectivity, and improved uniformity of etching rate distribution within the wafer surface.
  • the concentration of hydrogen gas contained in the etching gas can be, for example, 0% by volume or more and 30% by volume or less, and 0% by volume.
  • the excess is preferably 20% by volume or less, and more preferably 3% by volume or more and 10% by volume or less.
  • the etching selectivity ratio which is the ratio of the etching rate of the silicon material to the etching rate of the material, may be improved by 1.2 times or more. If favorable conditions are established, the etching selectivity may be improved by a factor of 1.5 or more, and if more favorable conditions are established, the etching selectivity may be improved by a factor of 2 or more.
  • halogen-containing compounds include fluorine gas (F 2 ), methyl chloride (CH 3 Cl), dichloromethane (CH 2 Cl 2 ), chloroform (CHCl 3 ), carbon tetrachloride (CCl 4 ), and chlorine gas (Cl 2 ), boron trichloride (BCl 3 ), bromine (Br 2 ), hydrogen bromide (HBr), iodine (I 2 ), hydrogen iodide (HI), oxygen difluoride (OF 2 ), chlorine trifluoride ( ClF 3 ), bromine trifluoride (BrF 3 ), bromine pentafluoride (BrF 5 ), iodine pentafluoride (IF 5 ), iodine heptafluoride (IF 7 ), nitrogen trifluoride (NF 3 ), Examples include sulfur fluoride (SF 6 ), nitrosyl fluoride (NOF), and fluorocarbons.
  • F 2 fluorine gas
  • a fluorocarbon is a compound in which some or all of the hydrogen atoms of a hydrocarbon are replaced with fluorine atoms.
  • fluorocarbons from the viewpoint of easy availability, those having carbon numbers of 1 to 7 are preferred, those having 1 to 5 carbon atoms are more preferred, and those having 1 to 4 carbon atoms are even more preferred.
  • fluorocarbons may have atoms other than carbon atoms and fluorine atoms, such as hydrogen atoms (H), nitrogen atoms (N), oxygen atoms (O), sulfur atoms (S), chlorine atoms ( Cl), bromine atom (Br), and iodine atom (I).
  • fluorocarbons include tetrafluoromethane (CF 4 ), trifluoromethane (CHF 3 ), difluoromethane (CH 2 F 2 ), fluoromethane (CH 3 F), dibromodifluoromethane (CBr 2 F 2 ), and iodo.
  • Trifluoromethane (CF 3 I), carbonyl fluoride (COF 2 ), hexafluoroethane (C 2 F 6 ), chlorotrifluoroethylene, (C 2 F 3 Cl), 1-chloro-1-fluoroethylene (C 2 H 2 FCl), bromotrifluoroethylene (C 2 F 3 Br), 1-bromo-1-fluoroethylene (C 2 H 2 FBr), octafluoropropane (C 3 F 8 ), octafluorocyclobutane (c-C 4 F 8 ), hexafluorobutadiene (e.g.
  • chlorine gas, nitrogen trifluoride, sulfur hexafluoride, tetrafluoromethane, octafluorocyclobutane, trifluoromethane, difluoromethane, hexafluoro-1,3- Butadiene is preferred, and chlorine gas, nitrogen trifluoride, sulfur hexafluoride, tetrafluoromethane, difluoromethane, and hexafluoro-1,3-butadiene are more preferred.
  • the concentration of the halogen-containing compound contained in the etching gas is not particularly limited. Although it depends on the type of halogen-containing compound, the concentration of the halogen-containing compound contained in the etching gas can be, for example, 0 volume % or more and less than 100 volume %, and must be more than 0 volume % and 30 volume % or less.
  • the content is preferably 3% by volume or more and 25% by volume or less, and even more preferably 10% by volume or more and 20% by volume or less.
  • oxygen-containing compounds examples include oxygen gas (O 2 ), ozone (O 3 ), nitrous oxide (N 2 O), nitric oxide (NO), nitrogen dioxide (NO 2 ), and sulfur trioxide (SO 3 ) . ).
  • oxygen gas O 2
  • ozone O 3
  • nitrous oxide N 2 O
  • nitric oxide NO
  • nitrogen dioxide NO 2
  • SO 3 sulfur trioxide
  • concentration of the oxygen-containing compound contained in the etching gas depends on the type of oxygen-containing compound, but can be, for example, 0 volume % or more and 30 volume % or less, and should be more than 0 volume % and 20 volume % or less. is preferable, and more preferably 3% by volume or more and 10% by volume or less.
  • inert gas is not particularly limited as long as it hardly reacts with fluorodithiethane or the second etching compound under conditions where plasma is not generated.
  • inert gases include rare gases such as helium (He), neon (Ne), argon (Ar), krypton (Kr), and xenon (Xe).
  • rare gases such as helium (He), neon (Ne), argon (Ar), krypton (Kr), and xenon (Xe).
  • helium and argon are preferred, and argon is more preferred.
  • One type of inert gas may be used alone, or two or more types may be used in combination.
  • the concentration of the inert gas contained in the etching gas can be, for example, 0 volume% or more and less than 100 volume%, preferably 30 volume% or more and 95 volume% or less, and 50 volume% or more and 90 volume% or less. It is more preferably the following, and even more preferably 60 volume % or more and 80 volume % or less.
  • Etching gas can be obtained by mixing multiple components that make up the etching gas (etching compound, second etching compound, inert gas, etc.). You can do it either inside or outside. That is, a plurality of components constituting an etching gas may be introduced into a chamber independently and mixed within the chamber, or a plurality of components constituting an etching gas may be mixed to obtain an etching gas. The etching gas may be introduced into the chamber.
  • the etching gas may contain impurities.
  • the impurity is a component of the etching gas that is different from the etching compound and the other gases.
  • impurities that can be contained in the etching gas include impurity gases such as water (H 2 O), hydrogen fluoride (HF), hydrogen chloride (HCl), hydrogen sulfide (H 2 S), and sulfur dioxide (SO 2 ). and metals. Metals will be explained in detail later.
  • the impurity gases mentioned above such as water (steam), hydrogen fluoride, hydrogen chloride, hydrogen sulfide, and sulfur dioxide, corrode the gas piping that supplies the gas, the chamber where etching is performed, the fluorodithiethane storage container, etc. There is a risk. Therefore, it is preferable to remove the impurity gas from the etching gas as much as possible. In this way, the reproducibility of etching tends to be high.
  • the concentration of impurity gas in the etching gas is preferably at most 1% by volume, more preferably at most 1000 ppm by volume, even more preferably at most 100 ppm by volume.
  • a metal is present in the etching gas, the metal may remain on the surface of the carbon material and bond with the sulfur atoms derived from fluorodithiethane.
  • the bond between the carbon atom on the surface of the carbon material and the sulfur atom derived from fluorodithiethane may not be sufficiently formed, or the proportion of active species generated from fluorodithiethane may decrease. There is a risk that it may change.
  • the carbon material becomes more easily etched and the etching rate of the silicon material decreases, so there is a risk that the etching selectivity ratio, which is the ratio of the etching rate of the silicon material to the etching rate of the carbon material, decreases. Therefore, it is preferable that the concentration of metal in the etching gas is as low as possible, and if the etching gas or the etching compound contains metal, it is preferable to remove it as much as possible by purification.
  • general purification methods such as distillation, sublimation, filtration, membrane separation, adsorption, and recrystallization can be used.
  • the types of metals whose concentration should be lowered include metal elements in periods 3 to 6 of the periodic table, such as sodium, magnesium, aluminum, potassium, calcium, chromium, manganese, iron, cobalt, nickel, Examples include copper, zinc (Zn), antimony (Sb), molybdenum, and tungsten (W).
  • etching gas e.g., metal piping, storage containers. Because it is often mixed with etching gas, it is easy to get mixed in with the etching gas.
  • the etching gas contains or does not contain at least one metal among sodium, magnesium, aluminum, potassium, calcium, chromium, manganese, iron, cobalt, nickel, copper, and molybdenum as an impurity,
  • the etching gas contains the metal, the total concentration of all the metals contained must be 300 mass ppb or less.
  • etching selectivity ratio is the ratio of the etching rate of the silicon material to the etching rate of the carbon material.
  • the etching selectivity ratio is the ratio of the etching rate of the silicon material to the etching rate of the carbon material, compared to the case of using an etching gas that contains and has a total concentration of all metals exceeding 300 mass ppb. may be improved by a factor of 1.1 or more. If favorable conditions are established, the etching selectivity may be improved by a factor of 1.2 or more, and if more favorable conditions are established, the etching selectivity may be improved by a factor of 1.3 or more.
  • the metal compound means a compound containing a metal element, and includes, for example, metal oxides, metal nitrides, metal oxynitrides, metal chlorides, metal bromides, metal iodides, metal sulfides, and the like.
  • the concentration of metal in the etching gas can be determined using an inductively coupled plasma mass spectrometer (ICP-MS).
  • ICP-MS inductively coupled plasma mass spectrometer
  • not containing metal means that it cannot be quantitatively determined by an inductively coupled plasma mass spectrometer.
  • the total concentration of all the metals contained in the etching gas is preferably 1 mass ppb or more and 300 mass ppb or less, more preferably 5 mass ppb or more and 200 mass ppb or less, and 10 mass ppb. More preferably, the amount is not less than 100 ppb by mass.
  • the member to be etched that is etched by the etching method according to the present embodiment includes an etching object that is an object to be etched with an etching gas and a non-etching object that is not an object to be etched with an etching gas.
  • the etched object has a silicon material
  • the non-etched object has a carbon material.
  • the member to be etched may be a member having a portion formed of an etching object and a portion formed of a non-etching object, or a member formed of a mixture of an etching object and a non-etching object. good. Further, the member to be etched may include other objects than the etched object and the non-etched object. Further, the shape of the member to be etched is not particularly limited, and may be, for example, plate-like, foil-like, film-like, powder-like, or lump-like. An example of the member to be etched is the aforementioned semiconductor substrate.
  • the object to be etched includes a silicon material, but may be formed only of silicon material, or may have a portion formed only of silicon material and a portion formed of another material. It may be made of a mixture of silicon material and other materials. Further, the shape of the object to be etched is not particularly limited, and may be, for example, plate-like, foil-like, film-like, powder-like, or lump-like.
  • a silicon material refers to a material having silicon (Si) in a composition of 10 mol% or more and 100 mol% or less, preferably 20 mol% or more and 100 mol% or less, and 30 mol% or more and 100 mol% or less. It is more preferable to have the following silicon.
  • the silicon material may contain elements such as hydrogen (H), carbon (C), nitrogen (N), oxygen (O), and germanium (Ge).
  • silicon materials include single crystal silicon, polysilicon, amorphous silicon, silicon nitride, silicon oxide, silicon oxynitride (SiON), and silicon germanium (Si t Ge 100-t , where t is a coefficient).
  • silicon compounds and polysilicon are preferred.
  • the silicon compound is a compound having a silicon atom and at least one of an oxygen atom and a nitrogen atom, and includes, for example, silicon nitride, silicon oxide, and silicon oxynitride.
  • silicon oxide is silicon dioxide (SiO 2 ).
  • silicon nitride refers to a compound containing silicon and nitrogen in any proportion, and an example thereof is Si 3 N 4 .
  • the purity of silicon nitride is not particularly limited, but is preferably 30% by mass or more, more preferably 60% by mass or more, and still more preferably 90% by mass or more.
  • silicon material may be used alone, or two or more kinds of silicon materials may be used in combination.
  • chemical formula representing silicon germanium has been added, these are merely examples, and those skilled in the art can easily imagine that the chemical composition and coefficients change depending on the film forming conditions and the raw materials used.
  • Non-etched object Since the non-etching target material does not substantially react with the above-mentioned etching compound or reacts with the above-mentioned etching compound very slowly, even if it is etched by the etching method according to the present embodiment, etching hardly progresses. It's something you don't do.
  • the non-etching object includes a carbon material, but may be formed only of carbon material, or may have a portion formed only of carbon material and a portion formed of another material. It may be made of a carbon material or a mixture of a carbon material and other materials. Further, the shape of the non-etching object is not particularly limited, and may be, for example, plate-like, foil-like, film-like, powder-like, or block-like.
  • a carbon material refers to a material having 20% by mass or more and 100% by mass of carbon in its composition, preferably 50% by mass or more and 100% by mass or less of carbon, and 60% by mass or more and 100% by mass or less of carbon. It is more preferable to have the following.
  • the carbon material may contain elements other than carbon.
  • carbon materials examples include amorphous carbon, carbon-doped silicon oxide, and photoresist.
  • amorphous carbon and photoresist are preferred.
  • one type of carbon material may be used alone, or two or more types may be used in combination.
  • the non-etching object can be used as a resist or mask for suppressing etching of the etching object by the etching gas. Therefore, in the etching method according to the present embodiment, a patterned non-etching object is used as a resist or a mask to process the etching object into a predetermined shape (for example, a film-like etching object included in a member to be etched) is processed into a predetermined shape. Since it can be used for methods such as processing a material to a predetermined film thickness, it can be suitably used for manufacturing semiconductor devices. In addition, since the non-etched objects are hardly etched, it is possible to suppress etching of parts of the semiconductor element that should not be etched, and it is possible to prevent the characteristics of the semiconductor element from being lost due to etching. can.
  • a predetermined shape for example, a film-like etching object included in a member to be etched
  • the method for forming the carbon material there is no particular restriction on the method for forming the carbon material, and methods commonly used for forming carbon material films, such as spray coating, spin coating, thermal deposition method (CVD), plasma deposition method (PECVD), etc. can be used. can.
  • the PECVD method using a hydrocarbon precursor is generally used for film formation of amorphous carbon, but the type of hydrocarbon precursor is not particularly limited, and any of alkanes, alkenes, and alkynes can be used.
  • hydrocarbon precursors include methane (CH 4 ), ethane (C 4 H 6 ), ethylene (C 2 H 4 ), propylene (C 3 H 6 ), propyne (C 3 H 4 ). , propane (C 3 H 8 ), butane (C 4 H 10 ), butene (C 4 H 8 , including isomers), butadiene (C 4 H 6 ), acetylene (C 2 H 2 ), toluene (C 7 H 8 ), and mixtures thereof.
  • the temperature conditions of the etching step in the etching method according to the present embodiment are not particularly limited, it is preferable that the temperature of the member to be etched during etching is -60°C or higher and 100°C or lower, and -40°C or higher and 80°C or higher.
  • the temperature is more preferably at most -20°C and at most 60°C, and particularly preferably at least 10°C and at most 40°C. If etching is performed with the temperature of the member to be etched within the above range, the etching selectivity will tend to be higher.
  • the pressure in the chamber where etching is performed is preferably 0.1 Pa or more and 100 Pa or less, and 0.5 Pa or more and 20 Pa or less. More preferably, the pressure is 1 Pa or more and 10 Pa or less. If the pressure conditions are within the above range, the plasma will be easily stabilized and uniform plasma will be easily obtained.
  • the amount of etching gas used in the etching method according to the present embodiment depends on the internal volume of the chamber and the exhaust equipment for reducing the pressure inside the chamber. It may be adjusted as appropriate depending on the capacity, pressure in the chamber, etc.
  • the etching apparatus shown in FIG. 1 is a plasma etching apparatus that performs etching using capacitively coupled plasma as a plasma source. First, the etching apparatus shown in FIG. 1 will be explained.
  • the etching apparatus 200 in FIG. 1 includes a chamber 210 in which plasma etching is performed, an upper electrode 220 that forms an electric field and a magnetic field in the chamber 210 for turning etching gas into plasma, and an etched member 400 to be plasma etched.
  • a lower electrode 221 that supports the inside of the chamber 210, a vacuum pump 230 that reduces the pressure inside the chamber 210, and a pressure gauge 240 that measures the pressure inside the chamber 210.
  • a high frequency power source 260 that generates high frequency is connected to the upper electrode 220 and the lower electrode 221. Further, the lower electrode 221 and the high frequency power source 260 are connected via a matching box 261.
  • the matching box 261 has a circuit for matching the output impedance of the high frequency power supply 260 and the impedances of the upper electrode 220 and the lower electrode 221. Note that high frequency power sources having different frequencies may be connected to the upper electrode 220 and the lower electrode 221, respectively. In that case, it is preferable that the connections between the upper electrode 220 and the lower electrode 221 and the high frequency power source be made through a matching box.
  • the etching apparatus 200 in FIG. 1 includes an etching gas supply section that supplies etching gas into the chamber 210.
  • This etching gas supply section includes a fluorodithiethane gas supply section 300 that supplies a fluorodithiethane gas, an inert gas supply section 310 that supplies an inert gas, and a second etching gas supply section that supplies a second etching compound gas.
  • It has an active gas supply piping 311 and a second etching compound gas supply piping 321 that connects a second etching compound gas supply section 320 to an intermediate portion of the etching gas supply piping 330.
  • fluorodithiethane gas When fluorodithiethane gas is supplied to the chamber 210 as an etching gas, the fluorodithiethane gas is sent from the fluorodithiethane gas supply section 300 to the etching gas supply piping 330. Fluorodithiethane gas is supplied to the chamber 210 via 330 .
  • the pressure in the chamber 210 before the etching gas is supplied is not particularly limited as long as it is less than or equal to the etching gas supply pressure or lower than the etching gas supply pressure, but is, for example, 10 -5 Pa or more. It is preferably less than 100 kPa, and more preferably 1 Pa or more and 80 kPa or less.
  • the fluorodithiethane gas is sent from the fluorodithiethane gas supply section 300 to the etching gas supply piping 330, and , inert gas is sent from the inert gas supply section 310 to the middle part of the etching gas supply pipe 330 via the inert gas supply pipe 311 .
  • the fluorodithiethane gas and the inert gas are mixed in the middle part of the etching gas supply pipe 330 to form a mixed gas, and this mixed gas is supplied to the chamber 210 via the etching gas supply pipe 330. It has become.
  • a mixed gas of fluorodithiethane gas and a second etching compound gas or a mixture of fluorodithiethane gas, a second etching compound gas, and an inert gas.
  • a gas may be supplied to chamber 210 as an etching gas.
  • the fluorodithiethane gas supply section 300 may be heated with an external heater (not shown), or the etching gas containing fluorodithiethane may be liquefied within the pipe.
  • the inert gas supply pipe 311, the second etching compound gas supply pipe 321, and the etching gas supply pipe 330 may be heated with an external heater (not shown) or the like.
  • the member to be etched 400 is placed on the lower electrode 221 arranged inside the chamber 210, and the inside of the chamber 210 is depressurized by the vacuum pump 230. After that, an etching gas is supplied into the chamber 210 by an etching gas supply section. Then, when high-frequency power is applied to the upper electrode 220 and the lower electrode 221 by the high-frequency power supply 260, an electric field and a magnetic field are formed inside the chamber 210, which accelerates electrons, and these accelerated electrons New ions and electrons are generated by collision with dithiethane, etc., and as a result, discharge occurs and plasma is formed.
  • the member to be etched 400 is etched.
  • the amount of etching gas supplied to the chamber 210 and the concentration of fluorodithiethane in the etching gas (mixed gas) are determined by the etching gas supply piping 330, the second etching compound gas supply piping 321, and the inert gas supply piping 330.
  • the flow rates of the fluorodithiethane gas, the second etching compound gas, and the inert gas can be controlled by mass flow controllers (not shown) installed in the pipes 311, respectively.
  • Fluorodithiethane was purified using the purification apparatus shown in FIG.
  • a raw material container 10 made of manganese steel, capacity 3 L
  • a gas filter 12 Entegris Co., Ltd.
  • the raw material container 10 is equipped with a main stopper.
  • the outlet side of the gas filter 12 is connected to one branch pipe of a cross-shaped branch pipe 13 made of SUS316.
  • the other three branch pipes of the branch pipe 13 are connected to a vacuum pump 60, a vacuum gauge 40, and a receiving container 50 (made of manganese steel, capacity 3 L), respectively.
  • the raw material container 10, the piping 11, and the branch piping 13 can be heated to any temperature by an external heater (not shown).
  • a vacuum pump line valve 30 is provided in the middle of the branch pipe to which the vacuum pump 60 is connected.
  • the receiving container 50 is a container that contains fluorodithiethane purified by passing it through the gas filter 12, and is installed on a receiving container mass meter 41 that measures the mass of the receiving container 50. Further, the receiving container 50 is equipped with a main stopper.
  • a branch pipe 15 extends from the middle of the branch pipe to which the receiving container 50 is connected, and is connected to a vaporizer 70 (made of manganese steel, capacity 30 mL).
  • the vaporizer 70 is a container that contains fluorodithiethane purified by passing it through the gas filter 12, and is installed on a vaporizer mass meter 73 that measures the mass of the vaporizer 70.
  • the vaporizer 70 is equipped with an inlet vaporizer valve 71 and an outlet vaporizer valve 72, the inlet vaporizer valve 71 is connected to the branch pipe 15, and the outlet vaporizer valve 72 is normally closed.
  • the raw material container 10 was heated to 70° C., the piping 11, the branch piping 13, and the branch piping 15 were heated to 100° C., the main valve of the raw material container 10 was closed, and the main valve of the receiving container 50 and the inlet vaporizer valve 71 were opened. Then, the vacuum pump line valve 30 was opened, and the pressure inside the pipe 11, branch pipe 13, branch pipe 15, receiving container 50, and vaporizer 70 was reduced to 10 Pa or less using the vacuum pump 60.
  • the concentration (M) of metal contained in Sample 1-2 and Sample 1-3 was determined as follows. First, a mixed solution of fluorodithiethane and an aqueous nitric acid solution was prepared using the preparation apparatus shown in FIG. The method for preparing the mixed liquid will be explained below.
  • the vaporizer 70 filled with purified fluorodithiethane was removed from the purification apparatus of FIG. 2 and attached to the preparation apparatus of FIG. 3. That is, an inlet vaporizer valve 71 of the vaporizer 70 is connected to a mass flow controller 75 and an argon supply section 74 via an argon pipe 76, and an outlet vaporizer valve 72 is connected to a nitric acid container 79 via a connecting pipe 77. It is connected to the.
  • the nitric acid container 79 contains 40 g of a nitric acid aqueous solution 78 having a concentration of 1% by mass, and the tip of the connecting pipe 77 is placed in the nitric acid aqueous solution 78 . Further, the nitric acid container 79 is provided with an exhaust port 80.
  • the vaporizer 70 was heated to 80°C with an external heater (not shown), and the connecting pipe 77 was heated to 100°C with an external heater (not shown). Then, fluorodithiethane in the vaporizer 70 was bubbled into the nitric acid aqueous solution 78 in the nitric acid container 79 by supplying argon at a flow rate of 40 mL/min from the argon supply section 74 to the vaporizer 70 via the argon pipe 76.
  • the mass of the vaporizer 70 was measured with a vaporizer mass meter 73 after bubbling was completed, it was found to be 10 g (A) lower than before bubbling. Therefore, it is considered that the entire amount of fluorodithiethane in the vaporizer 70 was vaporized and supplied to the nitric acid aqueous solution 78 in the nitric acid container 79.
  • an aqueous nitric acid solution having a concentration of 1% by mass was added so that the mass of the contents in the nitric acid container 79 was 50 g (B) to obtain a mixed solution of fluorodithiethane and an aqueous nitric acid solution.
  • 1 g of the aqueous layer of this mixed solution was extracted and analyzed for metals using an inductively coupled plasma mass spectrometer. The signal intensities of cobalt, nickel, copper, and molybdenum were each measured (y). Then, the concentration of each metal was calculated from the signal intensity using a calibration curve, and the total concentration of the metals was determined by summing them.
  • the calibration curve used was created as follows. That is, nitric acid standard solutions with metal concentrations of 0 mass ppb (contains no metal), 10 mass ppb, 100 mass ppb, 300 mass ppb, 700 mass ppb, and 1200 mass ppb are prepared, and the solutions are subjected to an inductively coupled plasma mass spectrometer. The analysis was performed using Then, a calibration curve was created in which the concentration of metal was plotted on the horizontal axis and the signal intensity was plotted on the vertical axis, and its slope (a) and intercept (b) were determined. Similar operations were performed for sodium, magnesium, aluminum, potassium, calcium, chromium, manganese, iron, cobalt, nickel, copper, and molybdenum, and calibration curves for each metal were created.
  • the fluorodithiethane of Preparation Example 2 is 1,1,2,2,3,3,4,4-octafluoro-1,3-dithiethane, and the unpurified product is Sample 2-1 and the purified product is Sample 2- Set it to 2.
  • the fluorodithiethane of Preparation Example 3 is 2,2,4-trifluoro-4-trifluoromethyl-1,3-dithiethane, and the unpurified product is designated as Sample 3-1 and the purified product is designated as Sample 3-2.
  • the fluorodithiethane of Preparation Example 4 is 2,4-difluoro-2,4-bis(trifluoromethyl)-1,3-dithiethane, and the unpurified product is called Sample 4-1 and the purified product is called Sample 4-2. do.
  • the fluorodithiethane of Preparation Example 5 is 2,2,4,4-tetrakis(trifluoromethyl)-1,3-dithiethane, and the unpurified product is designated as Sample 5-1 and the purified product is designated as Sample 5-2.
  • the nitric acid container 96 contains 100 mL of a nitric acid aqueous solution 94 having a concentration of 1% by mass, and the tip of the connecting pipe 93 is placed in the nitric acid aqueous solution 94 . Further, the nitric acid container 96 is provided with an exhaust port 95. Furthermore, a pressure regulator 91 and a mass flow controller 92 are installed in the middle of the connecting pipe 93.
  • the main valve of the container 90 is opened, and sulfur hexafluoride gas is bubbled into the nitric acid aqueous solution 94 in the nitric acid container 96 via the connecting pipe 93 while controlling the supply pressure and flow rate using the pressure regulator 91 and mass flow controller 92, respectively. , was discharged from the exhaust port 95.
  • the pressure during bubbling was 0.1 MPa gauge pressure, the flow rate was 100 mL/min, and bubbling was continued until 10 g of sulfur hexafluoride was bubbled. Thereby, a mixed solution of sulfur hexafluoride and nitric acid aqueous solution was obtained.
  • the mixed solution thus prepared was analyzed in the same manner as in Preparation Example 1, and the concentration of each metal contained in Sample 6-1 and the total thereof were determined. The results are shown in Table 1.
  • Example 1 Using an ICP etching apparatus RIE-200iP manufactured by Samco Co., Ltd., five types of etching test specimens were simultaneously subjected to plasma etching.
  • the five types of etching test specimens were one in which a polysilicon (Poly-Si) film with a thickness of 2000 nm was formed on a silicon substrate (manufactured by Seiren KST Co., Ltd.), and a silicon dioxide film with a thickness of 1000 nm formed on a silicon substrate.
  • a silicon nitride (Si 3 N 4 ) film with a thickness of 1000 nm on a silicon substrate manufactured by Seiren KST Co., Ltd.
  • a photo film with a thickness of 1000 nm on a silicon substrate A resist film was formed, and an amorphous carbon film with a thickness of 1000 nm was formed on a silicon substrate (APF (registered trademark) manufactured by Applied Materials Co., Ltd.).
  • the photoresist film was formed by coating a photoresist TSCR (registered trademark) manufactured by Tokyo Ohka Kogyo Co., Ltd. on a silicon substrate and then curing it by exposing it to light. Furthermore, the silicon substrates used in these five types of etching test specimens were all square-shaped with a side of 2 cm.
  • the volume of the chamber of the ICP etching apparatus was 46,000 cm 3
  • the etching gas was a mixed gas of 2,2,4,4-tetrafluoro-1,3-dithiethane and argon of sample 1-3.
  • the flow rate of sample 1-3 introduced into the chamber was 20 mL/min and the flow rate of argon to 80 mL/min
  • 2,2,4,4-tetrafluoro-1,3-dithiethane in the etching gas in the chamber was The concentration of was adjusted to 20% by volume.
  • the concentration of metals contained in the argon used here was below the detection limit.
  • Total concentration of each metal in the etching gas M 1 ⁇ V 1 ⁇ X 1 / (M 1 ⁇ V 1 +M 2 ⁇ V 2 )
  • M 1 is the molecular weight of fluorodithiethane
  • M 2 is the atomic weight of the inert gas (argon)
  • V 1 is the flow rate of the fluorodithiethane gas
  • V 2 is the flow rate of the inert gas
  • X 1 is the molecular weight of the fluorodithiethane. This is the total concentration of each metal contained.
  • the etching test specimen was taken out from the chamber, the thickness of each film formed on the silicon substrate was measured, and the etching rate of each film was calculated.
  • the film thickness was measured using a reflectance spectroscopic film thickness meter F20 manufactured by Filmetrics. Further, the etching rate of each film was calculated by subtracting the film thickness after etching from the film thickness before etching, and dividing the difference by the etching time. The results are shown in Table 2.
  • the conditions for measuring film thickness are as follows. That is, the measurement atmosphere was air and the measurement temperature was 25°C. Moreover, the measurement wavelength range is a wavelength range in which Goodness of fit is 0.9 or more. Specifically, the following wavelength range was used as a guide. That is, polysilicon has a thickness of 500 to 1200 nm, silicon dioxide has a thickness of 300 to 1100 nm, silicon nitride has a thickness of 500 to 1500 nm, photoresist has a thickness of 400 to 1000 nm, and amorphous carbon has a thickness of 400 to 800 nm.
  • the etching selectivity was calculated from the etching rate of each film determined as described above. That is, the ratio of the polysilicon etch rate to the photoresist etch rate (polysilicon etch rate/photoresist etch rate), and the ratio of the silicon dioxide etch rate to the photoresist etch rate (silicon dioxide etch rate/photoresist etch rate). The ratio of the silicon nitride etching rate to the photoresist etching rate (silicon nitride etching rate/photoresist etching rate) was calculated.
  • the ratio of the etching rate of polysilicon to the etching rate of amorphous carbon (etching rate of polysilicon / etching rate of amorphous carbon)
  • the ratio of the etching rate of silicon dioxide to the etching rate of amorphous carbon (etching rate of silicon dioxide / amorphous
  • the ratio of the silicon nitride etching rate to the amorphous carbon etching rate was calculated. The results are shown in Table 2.
  • Example 2 Examples 2 to 7 and Comparative Examples 1 to 5
  • the etching test specimen was etched in the same manner as in Example 1, except that the fluorodithiethane shown in Table 2 was used instead of the fluorodithiethane in Sample 1-3.
  • the etching rates of the silicon material and the carbon material were measured, and the etching selectivity ratio, which is the ratio of the etching rate of the silicon material to the etching rate of the carbon material, was calculated.
  • Table 2 The results are shown in Table 2.
  • the etching gas was 2,2,4,4-tetrafluoro-1,3-dithiethane of Sample 1-3 and the second etching compound shown in Table 2 (tetrafluoromethane, nitrogen trifluoride, sulfur hexafluoride, It is a mixed gas of difluoromethane, chlorine gas, hexafluoro-1,3-butadiene, octafluorocyclobutane, or hydrogen gas) and argon, and the flow rates of these three gases are as shown in Table 2.
  • the etching test specimen was etched by performing the same operations as in Example 1 except for the above points.
  • Example 2 the etching rates of the silicon material and the carbon material were measured, and the etching selectivity ratio, which is the ratio of the etching rate of the silicon material to the etching rate of the carbon material, was calculated. The results are shown in Table 2.
  • Total concentration of each metal in the etching gas (M 1 ⁇ V 1 ⁇ X 1 +M 3 ⁇ V 3 ⁇ X 3 )/(M 1 ⁇ V 1 +M 2 ⁇ V 2 +M 3 ⁇ V 3 )
  • M 1 is the molecular weight of fluorodithiethane
  • M 2 is the atomic weight of the inert gas (argon)
  • M 3 is the molecular weight of the second etching compound
  • V 1 is the flow rate of the fluorodithiethane gas
  • V 2 is the inertness.
  • V3 is the flow rate of the second etching compound
  • X1 is the sum of the concentrations of each metal contained in the fluorodithiethane
  • X3 is the sum of the concentrations of each metal contained in the second etching compound.
  • Example 1 Comparative Examples 6 to 12 and Reference Example 1
  • the etching gas is a mixed gas of the second etching compound gas shown in Table 2 and argon, and the flow rates of these two gases are as shown in Table 2.
  • the etching test specimen was etched by performing the same operation. Then, as in Example 1, the etching rates of the silicon material and the carbon material were measured, and the etching selectivity ratio, which is the ratio of the etching rate of the silicon material to the etching rate of the carbon material, was calculated. The results are shown in Table 2.
  • Total concentration of each metal in the etching gas M 3 ⁇ V 3 ⁇ X 3 / (M 2 ⁇ V 2 +M 3 ⁇ V 3 )
  • M 2 is the atomic weight of the inert gas (argon)
  • M 3 is the molecular weight of the second etching compound
  • V 2 is the flow rate of the inert gas
  • V 3 is the flow rate of the second etching compound
  • X 3 is the second etching compound.
  • Example 6 using an etching gas in which the total concentration of each metal contained was 100 mass ppb
  • Example 7 using an etching gas in which the total concentration of each metal contained was 275 mass ppb
  • an etching gas having a total concentration of less than 50 mass ppb was used.
  • the etching selectivity of the silicon material to the carbon material was decreased slightly compared to the other examples used, it was still sufficiently high.
  • an etching gas in which the total concentration of each metal contained was 500 mass ppb or more (Comparative Examples 1 to 5)
  • the etching selectivity of the silicon material to the carbon material was low.
  • Example 15 in which hydrogen gas was used as the second etching compound, the etching selectivity of the silicon material to the carbon material was higher than in the case where an etching gas not containing hydrogen gas was used. From this, it was found that by using hydrogen gas as the second etching compound, it was possible to improve the etching selectivity of the silicon material to the carbon material.
  • Etching device 210... Chamber 220... Upper electrode 221... Lower electrode 300... Fluorodithiethane gas supply section 310... Inert gas supply section 320... Second etching Compound gas supply section 400... member to be etched

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