WO2012091426A3 - 판상형 지르코늄포스페이트 및 그의 제조 방법 - Google Patents

판상형 지르코늄포스페이트 및 그의 제조 방법 Download PDF

Info

Publication number
WO2012091426A3
WO2012091426A3 PCT/KR2011/010181 KR2011010181W WO2012091426A3 WO 2012091426 A3 WO2012091426 A3 WO 2012091426A3 KR 2011010181 W KR2011010181 W KR 2011010181W WO 2012091426 A3 WO2012091426 A3 WO 2012091426A3
Authority
WO
WIPO (PCT)
Prior art keywords
type zirconium
platelet
zirconium phosphate
present
nanoplatelet
Prior art date
Application number
PCT/KR2011/010181
Other languages
English (en)
French (fr)
Other versions
WO2012091426A2 (ko
Inventor
하봉우
김진태
김종상
최양호
Original Assignee
주식회사 포스코
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 주식회사 포스코 filed Critical 주식회사 포스코
Priority to JP2013539783A priority Critical patent/JP2014503449A/ja
Priority to US13/824,559 priority patent/US9481936B2/en
Priority to CN201180057135.6A priority patent/CN103228574B/zh
Priority to EP11852523.7A priority patent/EP2660197B1/en
Publication of WO2012091426A2 publication Critical patent/WO2012091426A2/ko
Publication of WO2012091426A3 publication Critical patent/WO2012091426A3/ko
Priority to US15/146,035 priority patent/US20160244886A1/en

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/48Stabilisers against degradation by oxygen, light or heat
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/37Phosphates of heavy metals
    • C01B25/372Phosphates of heavy metals of titanium, vanadium, zirconium, niobium, hafnium or tantalum
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08Anti-corrosive paints
    • C09D5/082Anti-corrosive paints characterised by the anti-corrosive pigment
    • C09D5/084Inorganic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/70Additives characterised by shape, e.g. fibres, flakes or microspheres
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F11/00Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
    • C23F11/08Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
    • C23F11/18Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using inorganic inhibitors
    • C23F11/184Phosphorous, arsenic, antimony or bismuth containing compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/74Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by peak-intensities or a ratio thereof only
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/20Particle morphology extending in two dimensions, e.g. plate-like
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/20Particle morphology extending in two dimensions, e.g. plate-like
    • C01P2004/24Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/328Phosphates of heavy metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/25Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • Y10T428/256Heavy metal or aluminum or compound thereof
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/29Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982Particulate matter [e.g., sphere, flake, etc.]

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Paints Or Removers (AREA)

Abstract

본 발명은 구조 내에 P-OH그룹을 포함하고, X선 회절 분석 시 11.6±2도의 2θ 값에서 결정 피크를 가지며, 11.6±2도 미만의 2θ 값에서는 결정 피크가 관찰되지 않는 판상형 지르코늄포스페이트 에 관한 것이다. 본 발명에 의해 제조된 판상형 지르코늄포스페이트는 판상형 구조로 피막 내부에 나노크기로 균일하게 분산되어 표면 광택도 및 베리어 능력이 우수하고, 표면의 P-OH 기에 의해 내식성이 우수하며, 수용액뿐 아니라, 유기용매 등에도 분산 가능하다.
PCT/KR2011/010181 2010-12-28 2011-12-27 판상형 지르코늄포스페이트 및 그의 제조 방법 WO2012091426A2 (ko)

Priority Applications (5)

Application Number Priority Date Filing Date Title
JP2013539783A JP2014503449A (ja) 2010-12-28 2011-12-27 板状ジルコニウムホスフェート及びその製造方法
US13/824,559 US9481936B2 (en) 2010-12-28 2011-12-27 Nanoplatelet-type zirconium phosphate and method for preparing same
CN201180057135.6A CN103228574B (zh) 2010-12-28 2011-12-27 板状型磷酸锆及其制造方法
EP11852523.7A EP2660197B1 (en) 2010-12-28 2011-12-27 Method for preparing nanoplatelet-type zirconium phosphate
US15/146,035 US20160244886A1 (en) 2010-12-28 2016-05-04 Platelet-Type Zirconium Phosphate and Method for Preparing Same

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR10-2010-0136802 2010-12-28
KR1020100136802A KR101263086B1 (ko) 2010-12-28 2010-12-28 판상형 지르코늄포스페이트 및 그의 제조 방법

Related Child Applications (2)

Application Number Title Priority Date Filing Date
US13/824,559 A-371-Of-International US9481936B2 (en) 2010-12-28 2011-12-27 Nanoplatelet-type zirconium phosphate and method for preparing same
US15/146,035 Division US20160244886A1 (en) 2010-12-28 2016-05-04 Platelet-Type Zirconium Phosphate and Method for Preparing Same

Publications (2)

Publication Number Publication Date
WO2012091426A2 WO2012091426A2 (ko) 2012-07-05
WO2012091426A3 true WO2012091426A3 (ko) 2012-08-23

Family

ID=46383699

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/KR2011/010181 WO2012091426A2 (ko) 2010-12-28 2011-12-27 판상형 지르코늄포스페이트 및 그의 제조 방법

Country Status (6)

Country Link
US (2) US9481936B2 (ko)
EP (1) EP2660197B1 (ko)
JP (2) JP2014503449A (ko)
KR (1) KR101263086B1 (ko)
CN (1) CN103228574B (ko)
WO (1) WO2012091426A2 (ko)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6447968B2 (ja) * 2014-08-06 2019-01-09 国立大学法人京都大学 リン酸ジルコニウム粒子とその製造方法
JP6190023B1 (ja) * 2015-10-07 2017-08-30 日本化学工業株式会社 リン酸タングステン酸ジルコニウムの製造方法
US10630481B2 (en) 2016-11-07 2020-04-21 Ford Global Technologies, Llc Controller area network message authentication
KR101980270B1 (ko) * 2017-06-13 2019-05-21 한국과학기술연구원 P형 반도체의 오믹 컨택 형성을 위한 페이스트 및 이를 이용한 p형 반도체의 오믹 컨택 형성 방법
US10746225B2 (en) * 2018-03-30 2020-08-18 Minebea Mitsumi Inc. Photocurable resin composition and sliding member
CN108864905A (zh) * 2018-05-31 2018-11-23 华南理工大学 一种含片层状磷酸锆和碳纳米管的海洋防腐粉末涂料及其制备方法与应用
US20220259437A1 (en) * 2019-08-23 2022-08-18 Toyo Seikan Group Holdings, Ltd. Gas barrier film, and paint composition for forming gas barrier layer
CN112430414B (zh) * 2020-11-11 2021-12-14 江阴恒兴涂料有限公司 一种耐候性有色电泳涂料其制备方法
CN113279029B (zh) * 2021-05-15 2022-05-13 西南石油大学 一种Ni-W-P-Zr多元微晶镀层、镀液及其制备方法
CN114620698B (zh) * 2022-04-06 2023-05-05 晋大纳米科技(厦门)有限公司 一种大颗粒磷酸锆及其制备方法
CN116180432A (zh) * 2022-12-13 2023-05-30 南方科技大学 一种可自修复的超疏水织物及其制备方法与应用

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4381289A (en) * 1980-12-10 1983-04-26 National Research Development Corporation Process for preparing zirconium phosphate
US6312821B1 (en) * 1999-09-03 2001-11-06 Honda Giken Kogyo Kabushiki Kaisha Coating structure having corrosion resistance
US20080159940A1 (en) * 2004-06-22 2008-07-03 Rhodia Chimie High Form Factor Crystalline Zirconium Phosphate, Method for the Preparation Thereof and Use Thereof in a Macromolecular Material
US20100293788A1 (en) * 2007-11-26 2010-11-25 Henkel Ag & Co. Kgaa Zirconium phosphating of metal components, in particular iron

Family Cites Families (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3416884A (en) * 1966-11-04 1968-12-17 Nat Lead Co Crystalline zirconium phosphates
JPS62226807A (ja) 1986-03-27 1987-10-05 Rasa Kogyo Kk 結晶性層状リン酸ジルコニウムの製造方法
JP2581653B2 (ja) * 1987-10-03 1997-02-12 株式会社 アドバンス リン酸ジルコニウムの製造方法
JP3004291B2 (ja) 1989-11-02 2000-01-31 テイカ株式会社 結晶性層状リン酸化合物の製造方法
JP3211215B2 (ja) 1991-07-12 2001-09-25 東亞合成株式会社 結晶質リン酸ジルコニウム化合物の製造方法
KR100379630B1 (ko) 2000-12-15 2003-04-10 현대자동차주식회사 차량용 클러치 윤활구조
DE10131723A1 (de) 2001-06-30 2003-01-16 Henkel Kgaa Korrosionsschutzmittel und Korrosionsschutzverfahren für Metalloberflächen
US20030103888A1 (en) * 2001-11-13 2003-06-05 Ton That Hai Granular zirconium phosphate and methods for synthesis of same
KR100491122B1 (ko) 2002-08-14 2005-05-25 주식회사 포스코 환경친화형 크롬 무함유 내지문강판의 제조방법
JP2006040556A (ja) * 2004-07-22 2006-02-09 Mitsubishi Chemicals Corp 無機薄膜の製造方法及び無機薄膜並びに蛍光体前駆体粒子及び蛍光体粒子
JP4788186B2 (ja) * 2005-04-28 2011-10-05 東亞合成株式会社 新規リン酸ジルコニウム
WO2008053694A1 (en) * 2006-10-27 2008-05-08 Toagosei Co., Ltd. Novel lamellar zirconium phosphate
JP5088095B2 (ja) * 2006-12-13 2012-12-05 Jfeスチール株式会社 平板部耐食性、耐黒変性およびプレス成形後の外観と耐食性に優れた表面処理亜鉛系めっき鋼板、並びに亜鉛系めっき鋼板用水系表面処理液
CN100463848C (zh) * 2007-01-26 2009-02-25 北京化工大学 一种制备类球形α-磷酸锆的简便方法
KR20080088862A (ko) 2007-03-30 2008-10-06 (주)아진 경화장치
KR101198456B1 (ko) 2008-09-09 2012-11-06 삼화페인트공업주식회사 방사선경화성 수지 조성물 및 이를 포함하는 내지문성 수지조성물
US8640887B2 (en) * 2008-10-03 2014-02-04 Fresenius Medical Care Holdings, Inc. Zirconium phosphate particles having improved adsorption capacity and method of synthesizing the same
KR101132668B1 (ko) 2009-12-30 2012-04-03 주식회사 포스코 내열성, 내화학성, 열전도성, 열방사성 및 부착성이 우수한 강판
JP5821258B2 (ja) * 2011-04-20 2015-11-24 東亞合成株式会社 層状リン酸ジルコニウムの製造方法
JP5724578B2 (ja) * 2011-04-20 2015-05-27 東亞合成株式会社 層状リン酸ジルコニウムの製造方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4381289A (en) * 1980-12-10 1983-04-26 National Research Development Corporation Process for preparing zirconium phosphate
US6312821B1 (en) * 1999-09-03 2001-11-06 Honda Giken Kogyo Kabushiki Kaisha Coating structure having corrosion resistance
US20080159940A1 (en) * 2004-06-22 2008-07-03 Rhodia Chimie High Form Factor Crystalline Zirconium Phosphate, Method for the Preparation Thereof and Use Thereof in a Macromolecular Material
US20100293788A1 (en) * 2007-11-26 2010-11-25 Henkel Ag & Co. Kgaa Zirconium phosphating of metal components, in particular iron

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
FRANCESCA BELLEZA ET AL., COLLOID POLYM SCI, vol. 285, no. 1, 3 August 2006 (2006-08-03), pages 19 - 25, XP019442828 *

Also Published As

Publication number Publication date
EP2660197A2 (en) 2013-11-06
EP2660197A4 (en) 2015-12-02
KR101263086B1 (ko) 2013-05-09
JP5969058B2 (ja) 2016-08-10
US20160244886A1 (en) 2016-08-25
JP2015129080A (ja) 2015-07-16
US9481936B2 (en) 2016-11-01
CN103228574B (zh) 2016-09-14
EP2660197B1 (en) 2019-08-21
JP2014503449A (ja) 2014-02-13
CN103228574A (zh) 2013-07-31
KR20120074841A (ko) 2012-07-06
US20130330539A1 (en) 2013-12-12
WO2012091426A2 (ko) 2012-07-05

Similar Documents

Publication Publication Date Title
WO2012091426A3 (ko) 판상형 지르코늄포스페이트 및 그의 제조 방법
WO2008090554A3 (en) Modified conductive surfaces prepared by electrografting of diazonium salts
EP2767529A3 (en) Formulations and methods for oxidation protection of composite articles
WO2014107641A3 (en) Surface-modified, exfoliated nanoplatelets as mesomorphic structures in solutions and polymeric matrices
WO2011022175A3 (en) Compositions with improved dirt pickup resistance comprising layered double hydroxide particles
WO2009044478A1 (ja) 銀系無機抗菌剤
WO2012142057A3 (en) Multi-layer films and methods of forming same
WO2010039721A3 (en) Zirconium phosphate particles having improved adsorption capacity and method of synthesizing the same
MX355473B (es) Método para recubrir superficies metálicas con un agente de recubrimiento que contiene un polímero, el agente de recubrimiento y uso del mismo.
WO2009043850A3 (en) Heat-processable thermally conductive polymer composition
WO2013064643A8 (de) Beschichtete, nasschemisch oxidierte aluminiumeffektpigmente, verfahren zu deren herstellung, beschichtungsmittel und beschichteter gegenstand
WO2011139702A3 (en) Modified nucleosides and oligomeric compounds prepared therefrom
BR112015027133A2 (pt) nanopartículas de fitoglicogênio e métodos de fabricação dos mesmos
WO2009075802A3 (en) Method of preparing a pigment composition
WO2011088056A3 (en) Method and system for producing graphene and graphenol
MX365187B (es) Material compuesto tribológico, de estructuración fina, pigmentado.
EP2290013A3 (en) Methods of making nanosized particles of benzimidazolone pigments
ATE518921T1 (de) Pvd-metalleffektpigment mit gradient an nanoskaligen metallteilchen, verfahren zu deren herstellung und verwendung derselben
WO2010080242A3 (en) Uzm-27 family of crystalline aluminosilicate compositions, a method of preparing the compositions and methods of using the compositions
WO2014051529A3 (en) Catalyst systems
IN2015DN01140A (ko)
WO2012052265A3 (de) Stabilisiertes, reines lithiummetallpulver und verfahren zu dessen herstellung
WO2011106075A3 (en) A microelectronic structure including a low k dielectric and a method of controlling carbon distribution in the structure
EP2698142A3 (de) Zahnfüllungsmaterialien und Zahnlacke zur Hemmung der Biofilmbildung von Streptococcus mutans und deren Herstellung
WO2011103969A3 (en) Process for the co-encapsulation of biocidally active compounds in clay minerals functionalized by nitrogen compounds

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 11852523

Country of ref document: EP

Kind code of ref document: A2

ENP Entry into the national phase

Ref document number: 2013539783

Country of ref document: JP

Kind code of ref document: A

WWE Wipo information: entry into national phase

Ref document number: 2011852523

Country of ref document: EP

NENP Non-entry into the national phase

Ref country code: DE

WWE Wipo information: entry into national phase

Ref document number: 13824559

Country of ref document: US