WO2022172823A1 - 電解めっき液用添加剤、電解めっき液、電解めっき方法及び金属層の製造方法 - Google Patents

電解めっき液用添加剤、電解めっき液、電解めっき方法及び金属層の製造方法 Download PDF

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Publication number
WO2022172823A1
WO2022172823A1 PCT/JP2022/004007 JP2022004007W WO2022172823A1 WO 2022172823 A1 WO2022172823 A1 WO 2022172823A1 JP 2022004007 W JP2022004007 W JP 2022004007W WO 2022172823 A1 WO2022172823 A1 WO 2022172823A1
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WO
WIPO (PCT)
Prior art keywords
electrolytic plating
additive
plating solution
electroplating
metal layer
Prior art date
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Ceased
Application number
PCT/JP2022/004007
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English (en)
French (fr)
Japanese (ja)
Inventor
拓也 ▲高▼橋
伸哉 石渡
朋子 廿日出
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Adeka Corp
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Adeka Corp
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Publication date
Application filed by Adeka Corp filed Critical Adeka Corp
Priority to JP2022580575A priority Critical patent/JP7808062B2/ja
Priority to CN202280014793.5A priority patent/CN116888308A/zh
Priority to KR1020237030640A priority patent/KR20230142785A/ko
Priority to US18/275,517 priority patent/US20240132453A1/en
Publication of WO2022172823A1 publication Critical patent/WO2022172823A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/38—Electroplating: Baths therefor from solutions of copper
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
    • C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
    • C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
    • C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
    • C07D251/30—Only oxygen atoms
    • C07D251/32—Cyanuric acid; Isocyanuric acid
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D405/00—Heterocyclic compounds containing both one or more hetero rings having oxygen atoms as the only ring hetero atoms, and one or more rings having nitrogen as the only ring hetero atom
    • C07D405/14—Heterocyclic compounds containing both one or more hetero rings having oxygen atoms as the only ring hetero atoms, and one or more rings having nitrogen as the only ring hetero atom containing three or more hetero rings
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/12—Semiconductors

Definitions

  • the present invention provides an additive for an electrolytic plating solution containing a reaction product of an epoxy compound having a specific structure and a tertiary amine compound, an electrolytic plating solution containing the additive for an electrolytic plating solution, and the electrolytic plating solution. and a method for producing a metal layer using the electroplating method.
  • Electroplating is one of the representative methods for embedding metal, and among them, electrolytic copper plating for embedding copper as metal is widely known.
  • problems such as poor uniformity of the thickness of the embedded copper layer and the occurrence of voids inside the grooves and holes, which causes circuit connection failures.
  • additives such as smoothing agents and suppressing agents have been introduced into the electrolytic copper plating solution, and the effect of these additives has been investigated to increase the embedding rate and improve the uniformity of the thickness, and to embed copper. rice field.
  • Patent Literature 1 discloses polyvinylpyrrolidone as a smoothing agent used in an aqueous copper electroplating solution for embedding fine copper wiring.
  • Patent Document 2 discloses polyethyleneimine as a smoothing agent used in a copper plating solution for forming a copper film.
  • Patent Document 3 discloses polyethyleneimine as a smoothing agent used in a non-cyanide acidic silver plating bath.
  • Patent Document 4 discloses a reaction product of 1,4-butanediol diglycidyl ether and 2,4-dimethylimidazole as a smoothing agent.
  • Patent Document 5 discloses a reaction product of glycerol diglycidyl ether and imidazole.
  • Patent Document 6 discloses reaction products of 1,4-butanediol diglycidyl ether with N-methylaniline or diphenylamine.
  • an object of the present invention is to provide an additive for an electrolytic plating solution capable of forming a metal layer with a high embedding rate and a highly uniform thickness.
  • the present inventors solved the above problems by using, as an additive for an electrolytic plating solution, a compound obtained by reacting an epoxy compound having a specific structure with a tertiary amine compound.
  • the inventors have found that it is possible to achieve the present invention.
  • the present invention provides an electrolytic plating solution containing a reaction product of at least one epoxy compound (a1) represented by the following general formula (1) and at least one tertiary amine compound (a2): It is an additive.
  • L 1 and L 2 each independently represent a hydrogen atom, an alkyl group having 1 to 5 carbon atoms, or a group represented by the following general formulas (L-1) to (L-3), and n is represents an integer from 1 to 5.
  • n 1 to m 3 each independently represent an integer of 1 to 5, and * represents a bond.
  • the present invention is an electrolytic plating solution containing the additive for an electrolytic plating solution.
  • the present invention is an electrolytic plating method using the above electrolytic plating solution.
  • the present invention is a method for manufacturing a metal layer using the electroplating method described above.
  • an additive for an electrolytic plating solution capable of forming a metal layer with a high embedding rate and a highly uniform thickness.
  • the electrolytic plating solution additive of the present invention contains a reaction product of at least one epoxy compound (a1) represented by the general formula (1) and at least one tertiary amine compound (a2). do.
  • L 1 and L 2 each independently represent a hydrogen atom, an alkyl group having 1 to 5 carbon atoms, or a group represented by general formulas (L-1) to (L-3) above. and n represents an integer of 1-5.
  • alkyl group having 1 to 5 carbon atoms examples include methyl group, ethyl group, propyl group, isopropyl group, butyl group, isobutyl group, sec-butyl group, tert-butyl group, pentyl group and isopentyl group. , a neopentyl group, and the like.
  • n 1 , m 2 and m 3 each independently represent an integer of 1 to 5, and * represents a bond.
  • L 1 is preferably a group represented by the general formula (L-3) from the viewpoint that a metal layer having a high embedding rate and a highly uniform thickness can be formed.
  • L 2 is preferably a group represented by general formula (L-2) or (L-3).
  • a group represented by general formula (L-3) is preferred, and more preferred.
  • n is preferably an integer of 1 to 3, more preferably an integer of 1 to 2, from the viewpoint of forming a metal layer with a high embedding rate and high thickness uniformity.
  • m 1 , m 2 , and m 3 are preferably integers of 1 to 3, and preferably integers of 1 to 2, from the viewpoint of forming a metal layer with a high embedding rate and high uniformity of thickness. is more preferable.
  • Preferred specific examples of the epoxy compound (a1) represented by the general formula (1) include the following No. 1 to No. 16 epoxy compounds are mentioned.
  • epoxy compounds (a1) from the viewpoint of being able to form a metal layer with a higher embedding rate and a higher thickness uniformity, No. More preferred is the epoxy compound of 13 (triglycidyl isocyanurate).
  • tertiary amine compound (a2) well-known general tertiary amine compounds can be used, and specific examples thereof include trialkylamine compounds and azole compounds.
  • trialkylamine compounds include trimethylamine, triethylamine, tripropylamine, tributylamine, dimethylethylamine, and diethylmethylamine.
  • azole compounds include pyrrole, imidazole, 1,2,3-triazole, 1,2,4-triazole, tetrazole, pyrazole, oxazole, isoxazole, thiazole, isothiazole, oxadiazole, thiadiazole, and dihydrooxazole.
  • the tertiary amine compound (a2) is preferably an azole compound, such as imidazole, pyrazole, isothiazole, or It is more preferably an azole compound selected from the group consisting of isoxazole, 1,2,3-triazole, 1,2,4-triazole and benzimidazole, even more preferably imidazole or benzimidazole, imidazole is most preferred.
  • an azole compound such as imidazole, pyrazole, isothiazole, or It is more preferably an azole compound selected from the group consisting of isoxazole, 1,2,3-triazole, 1,2,4-triazole and benzimidazole, even more preferably imidazole or benzimidazole, imidazole is most preferred.
  • the reaction product contained in the additive for electrolytic plating solution of the present invention includes at least one epoxy compound (a1) and at least one tertiary amine compound (a2) represented by the general formula (1). It is produced by reacting with As the epoxy compound (a1) represented by the general formula (1), one type may be used, or two or more types may be used. As the tertiary amine compound (a2), one kind may be used, or two or more kinds may be used.
  • the production method is not particularly limited except that the component (a1) and the component (a2) are reacted.
  • the component (a1) and the component (a2) are mixed in an aqueous solution of diethylene glycol, It can be obtained by removing the solvent after heating, stirring, and filtration.
  • the heating temperature is preferably 50 to 200°C, more preferably 70 to 150°C, from the viewpoint of reducing unreacted substances.
  • the heating time is preferably 30 minutes to 10 hours, more preferably 1 to 5 hours, from the viewpoint of reducing unreacted substances.
  • the molar ratio of the component (a1) to the sum of the components (a1) and (a2) [component (a1) / ((a1) component + (a2) component)] is preferably 0.05 to 0.95, more preferably 0.1 to 0.8, and 0.2 to 0.6 Most preferably there is.
  • a metal layer having a high embedding rate and a highly uniform thickness is formed on a substrate by an electrolytic plating method using an electrolytic plating solution to which the additive for an electrolytic plating solution of the present invention containing the reaction product is added.
  • the electrolytic plating method using the electrolytic plating solution to which the additive for electrolytic plating solution of the present invention is added even for a substrate having a fine structure (for example, grooves and holes) on the surface, the embedding rate is high and the thickness is high.
  • a metal layer with high thickness uniformity can be formed.
  • the additive for an electrolytic plating solution of the present invention is added to an electrolytic copper plating solution, the resulting copper layer has a very high embedding rate and a very high thickness uniformity. It is particularly suitable as an additive for liquids.
  • the electrolytic plating solution of the present invention is an aqueous solution containing the additive for electrolytic plating solution as an essential active ingredient. From the viewpoint of making the effect of the present invention more remarkable, the concentration of the electrolytic plating solution additive in the electrolytic plating solution is preferably 1 mg/L to 1000 mg/L, more preferably 10 mg/L to 500 mg/L, and still more preferably. is between 20 mg/L and 300 mg/L.
  • the electrolytic plating solution of the present invention contains, as components other than the additive for the electrolytic plating solution, a metal salt as a metal supply source, an electrolyte, a chloride ion source, and a plating accelerator, similarly to conventionally known electrolytic plating solutions. agent, plating inhibitor, and the like.
  • the metal of the metal salt used in the electrolytic plating solution of the present invention is not particularly limited as long as it is a metal capable of forming a film by an electrolytic plating method, and examples thereof include copper, tin, and silver.
  • the additive for an electrolytic plating solution of the present invention is used in an electrolytic copper plating solution, the uniformity of the thickness of the resulting copper layer is improved, which is preferable.
  • Copper salts to be blended in the electrolytic copper plating solution include copper sulfate, copper acetate, copper fluoroborate, copper nitrate, and the like.
  • the concentration of copper sulfate (as CuSO 4 .5H 2 O) in the electrolytic plating solution is preferably 10 g/L to 300 g/L, more preferably 100 g/L to 250 g/L. efficient from the point of view of From the viewpoint of plating speed, the concentration of sulfuric acid in the electrolytic plating solution is preferably 30 g/L to 400 g/L, more preferably 50 g/L to 200 g/L.
  • a chloride ion source can be used in the electrolytic plating solution of the present invention in order to form a smooth metal layer with a uniform thickness.
  • the chloride ion source in the electrolytic plating solution is preferably blended at a concentration of 5 mg/L to 200 mg/L, more preferably 20 mg/L to 150 mg/L.
  • the chloride ion source is not particularly limited, but NaCl, HCl, and the like can be used, for example.
  • the electroplating solution of the present invention can also contain a plating accelerator (brightener) such as an organic compound containing sulfur element and a salt compound thereof.
  • Plating accelerators include compounds represented by the following general formulas (2) to (4).
  • R is an optionally substituted alkyl group, preferably an alkyl group having 1 to 6 carbon atoms, more preferably an alkyl group having 1 to 4 carbon atoms. be.
  • Ar is an optionally substituted aryl group, such as an optionally substituted phenyl group or naphthyl group.
  • X is a counterion such as sodium or potassium.
  • each of R 11 and R 12 independently has a hydrogen atom, a linear or branched alkyl group having 1 to 6 carbon atoms, or a substituent having 1 to 3 carbon atoms; a cycloalkyl group having 5 to 9 carbon atoms or an optionally substituted aryl group having 1 to 3 carbon atoms, M represents an alkali metal, ammonium or monovalent organic ammonium; ⁇ represents a number from 1 to 7;
  • sodium 3,3'-dithiobis(1-propanesulfonate) (hereinafter sometimes referred to as SPS) is preferable because it has a high effect of promoting the formation of a metal layer.
  • the concentration of the plating accelerator in the electrolytic plating solution is preferably 1 mg/L to 1000 mg/L, more preferably 1 mg/L to 1000 mg/L, more preferably 5 mg/L to 500 mg/L, more preferably 30 mg/L to 300 mg/L.
  • a plating inhibitor for example, an oxygen-containing high-molecular weight organic compound can be used, and specifically, polyethylene glycol, polypropylene glycol, polyoxyethylene-polyoxypropylene random copolymer, polyoxyethylene-polyoxypropylene block copolymer. etc., among which polyethylene glycol is preferred. From the viewpoint of making the effect of the present invention remarkable, these oxygen-containing high molecular weight organic compounds preferably have a molecular weight of 500 to 100,000, more preferably 1,000 to 10,000. Polyethylene glycol having a molecular weight of 1,000 to 10,000 is particularly preferred. From the same point of view, the concentration of the oxygen-containing high molecular organic compound in the electroplating solution is preferably 20 mg/L to 5,000 mg/L, more preferably 50 mg/L to 3,000 mg/L.
  • any other additive known to be added to the plating solution can be used in the electrolytic plating solution of the present invention as long as it does not impair the effects of the present invention.
  • additives include anthraquinone derivatives, cationic surfactants, nonionic surfactants, anionic surfactants, amphoteric surfactants, alkanesulfonic acids, alkanesulfonates, alkanesulfonate esters, and hydroxyalkanesulfones. acids, hydroxyalkanesulfonates, hydroxyalkanesulfonic acid esters, hydroxyalkanesulfonic acid organic acid esters, and the like.
  • the concentration of other additives in the electrolytic plating solution is preferably 0.1 mg/L to 500 mg/L, More preferably 0.5 mg/L to 100 mg/L.
  • the electroplating method of the present invention may be carried out in the same manner as conventional electroplating methods except that the electroplating solution of the present invention is used as the electroplating solution.
  • an electrolytic copper plating method for forming a copper layer on a substrate will be described.
  • an electrolytic plating apparatus for example, a paddle stirring type plating apparatus is used, and the substrate is immersed in an electrolytic copper plating bath filled with the electrolytic copper plating solution of the present invention in a plating tank.
  • the substrate is, for example, a Si substrate with a copper seed layer on which a resist pattern is formed using a photoresist.
  • the temperature of the electrolytic copper plating bath is, for example, 10° C. to 70° C., preferably 20° C. to 50° C., from the viewpoint of forming a metal layer with a high embedding rate and high uniformity in thickness.
  • ° C. and the current density is 1 A/dm 2 to 70 A/dm 2 , preferably 2 A/dm 2 to 50 A/dm 2 , more preferably 5 A/dm 2 to 30 A/dm 2 .
  • a method for stirring the electroplating solution air stirring, rapid liquid flow stirring, mechanical stirring using a stirring blade or the like can be used.
  • the plated products manufactured using the electroplating method of the present invention are not particularly limited. , electronic industrial materials (contacts, circuits, semiconductor packages, printed circuit boards, thin film resistors, capacitors, hard disks, magnetic materials, lead frames, nuts, magnets, resistors, stems, computer parts, electronic parts, laser oscillation elements, optical memory elements , optical fibers, filters, thermistors, heating elements, high-temperature heating elements, varistors, magnetic heads, various sensors (gas, temperature, humidity, light, speed, etc.), MEMS, etc.), precision equipment (copier parts, optical equipment parts, watch parts, etc.), aviation and marine materials (water pressure equipment, screws, engines, turbines, etc.), chemical industry materials (balls, gates, plugs, checks, etc.), various molds, machine tool parts, vacuum equipment parts, etc.
  • electronic industrial materials contacts, circuits, semiconductor packages, printed circuit boards, thin film resistors, capacitors, hard disks, magnetic materials, lead frames, nuts, magnets, resistors, stems, computer parts
  • the electroplating method of the present invention is preferably used for electronic industrial materials that particularly require fine patterns, and more particularly for use in the manufacture of semiconductor packages and printed circuit boards typified by TSV formation and bump formation.
  • the semiconductor package is more preferable.
  • the embedding rate is large and the thickness is small. It was found that a highly uniform metal layer can be formed. In particular, when the electrolytic plating bath containing the additive for electrolytic plating solution of Example 1 was used, it was confirmed that a metal layer having a high embedding rate and particularly high thickness uniformity could be formed.
  • first metal layer width 30 ⁇ m
  • second metal layer width 75 ⁇ m
  • substrate 4 height of first metal layer (H 1 ) 5 Height of second metal layer (H 2 ) 6 difference ( ⁇ H) between the height of the first metal layer 1 and the height of the second metal layer 2

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Epoxy Compounds (AREA)
  • Plural Heterocyclic Compounds (AREA)
PCT/JP2022/004007 2021-02-15 2022-02-02 電解めっき液用添加剤、電解めっき液、電解めっき方法及び金属層の製造方法 Ceased WO2022172823A1 (ja)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP2022580575A JP7808062B2 (ja) 2021-02-15 2022-02-02 電解めっき液用添加剤、電解めっき液、電解めっき方法及び金属層の製造方法
CN202280014793.5A CN116888308A (zh) 2021-02-15 2022-02-02 电镀液用添加剂、电镀液、电镀方法和金属层的制造方法
KR1020237030640A KR20230142785A (ko) 2021-02-15 2022-02-02 전해 도금액용 첨가제, 전해 도금액, 전해 도금 방법 및 금속층의 제조 방법
US18/275,517 US20240132453A1 (en) 2021-02-15 2022-02-02 Additive for electroplating solution, electroplating solution, electroplating method, and method of producing metal layer

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2021021841 2021-02-15
JP2021-021841 2021-02-15

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WO2022172823A1 true WO2022172823A1 (ja) 2022-08-18

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US (1) US20240132453A1 (https=)
JP (1) JP7808062B2 (https=)
KR (1) KR20230142785A (https=)
CN (1) CN116888308A (https=)
TW (1) TW202248198A (https=)
WO (1) WO2022172823A1 (https=)

Citations (8)

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US3879270A (en) * 1974-01-10 1975-04-22 Monsanto Co Compositions and process for the electrodeposition of metals
JPS5661374A (en) * 1979-10-08 1981-05-26 Henkel Kgaa Cytostatic drug* novel cyanuric acid derivative and manufacture thereof
JP2006037232A (ja) * 2004-07-22 2006-02-09 Rohm & Haas Electronic Materials Llc 平滑化剤化合物
CN101555609A (zh) * 2009-04-28 2009-10-14 武汉风帆电镀技术有限公司 有氰转无氰碱性环保镀锌组合物光亮剂
JP2011207878A (ja) * 2010-03-15 2011-10-20 Rohm & Haas Electronic Materials Llc めっき浴および方法
WO2011135716A1 (ja) * 2010-04-30 2011-11-03 荏原ユージライト株式会社 新規化合物およびその利用
JP2013249515A (ja) * 2012-05-31 2013-12-12 Rohm & Haas Denshi Zairyo Kk 電解銅めっき液及び電解銅めっき方法
US20180237932A1 (en) * 2015-09-10 2018-08-23 Atotech Deutschland Gmbh Copper plating bath composition and method for deposition of copper

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JP2007327127A (ja) 2006-06-09 2007-12-20 Daiwa Fine Chemicals Co Ltd (Laboratory) 銀めっき方法
JP5809055B2 (ja) 2009-07-01 2015-11-10 Jx日鉱日石金属株式会社 Ｕｌｓｉ微細ダマシン配線埋め込み用電気銅めっき水溶液
US20110220512A1 (en) 2010-03-15 2011-09-15 Rohm And Haas Electronic Materials Llc Plating bath and method
JP6142165B2 (ja) 2013-03-25 2017-06-07 石原ケミカル株式会社 電気銅メッキ浴、電気銅メッキ方法並びに当該メッキ浴を用いて銅皮膜を形成した電子部品の製造方法
US10100421B2 (en) 2015-08-06 2018-10-16 Dow Global Technologies Llc Method of electroplating photoresist defined features from copper electroplating baths containing reaction products of imidazole and bisepoxide compounds
WO2019044651A1 (ja) * 2017-08-31 2019-03-07 株式会社Adeka 電解めっき液用添加剤、該電解めっき液用添加剤を含有する電解めっき液及び該電解めっき液を用いた電解めっき方法

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3879270A (en) * 1974-01-10 1975-04-22 Monsanto Co Compositions and process for the electrodeposition of metals
JPS5661374A (en) * 1979-10-08 1981-05-26 Henkel Kgaa Cytostatic drug* novel cyanuric acid derivative and manufacture thereof
JP2006037232A (ja) * 2004-07-22 2006-02-09 Rohm & Haas Electronic Materials Llc 平滑化剤化合物
CN101555609A (zh) * 2009-04-28 2009-10-14 武汉风帆电镀技术有限公司 有氰转无氰碱性环保镀锌组合物光亮剂
JP2011207878A (ja) * 2010-03-15 2011-10-20 Rohm & Haas Electronic Materials Llc めっき浴および方法
WO2011135716A1 (ja) * 2010-04-30 2011-11-03 荏原ユージライト株式会社 新規化合物およびその利用
JP2013249515A (ja) * 2012-05-31 2013-12-12 Rohm & Haas Denshi Zairyo Kk 電解銅めっき液及び電解銅めっき方法
US20180237932A1 (en) * 2015-09-10 2018-08-23 Atotech Deutschland Gmbh Copper plating bath composition and method for deposition of copper

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US20240132453A1 (en) 2024-04-25
JP7808062B2 (ja) 2026-01-28
KR20230142785A (ko) 2023-10-11
TW202248198A (zh) 2022-12-16
JPWO2022172823A1 (https=) 2022-08-18
CN116888308A (zh) 2023-10-13

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