EP3536827B1 - Procédé de traitement de surface destiné à une tête de repoussage de tantale - Google Patents

Procédé de traitement de surface destiné à une tête de repoussage de tantale Download PDF

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Publication number
EP3536827B1
EP3536827B1 EP18761041.5A EP18761041A EP3536827B1 EP 3536827 B1 EP3536827 B1 EP 3536827B1 EP 18761041 A EP18761041 A EP 18761041A EP 3536827 B1 EP3536827 B1 EP 3536827B1
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EP
European Patent Office
Prior art keywords
spinneret
tantalum
lithium
film
coating
Prior art date
Legal status (The legal status 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 status listed.)
Active
Application number
EP18761041.5A
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German (de)
English (en)
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EP3536827B9 (fr
EP3536827A4 (fr
EP3536827A1 (fr
Inventor
Yuzhong Liu
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.)
Beijing Huayu Chuangxin Science & Trade Co Ltd
Beijing Huayu Chuangxin Ta-Nb Science & Technology Co Ltd
Original Assignee
Beijing Huayu Chuangxin Science & Trade Co Ltd
Beijing Huayu Chuangxin Ta-Nb Science & Technology Co Ltd
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Publication date
Application filed by Beijing Huayu Chuangxin Science & Trade Co Ltd, Beijing Huayu Chuangxin Ta-Nb Science & Technology Co Ltd filed Critical Beijing Huayu Chuangxin Science & Trade Co Ltd
Priority claimed from PCT/CN2018/077938 external-priority patent/WO2018157867A1/fr
Publication of EP3536827A1 publication Critical patent/EP3536827A1/fr
Publication of EP3536827A4 publication Critical patent/EP3536827A4/fr
Application granted granted Critical
Publication of EP3536827B1 publication Critical patent/EP3536827B1/fr
Publication of EP3536827B9 publication Critical patent/EP3536827B9/fr
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    • 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
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • C23C28/042Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material including a refractory ceramic layer, e.g. refractory metal oxides, ZrO2, rare earth oxides
    • 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
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/26Anodisation of refractory metals or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00Electrolytic coating other than with metals
    • C25D9/04Electrolytic coating other than with metals with inorganic materials
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D4/00Spinnerette packs; Cleaning thereof
    • D01D4/02Spinnerettes
    • D01D4/022Processes or materials for the preparation of spinnerettes

Definitions

  • the method of the present invention further comprises a polishing step (d): subjecting the fiber outlet face of the tantalum spinneret treated in step (c) to a polishing treatment to remove the film layer containing lithium-containing compound on the surface of the fiber outlet face.
  • a layer of amorphous Ta 2 O 5 film is formed on the tantalum spinneret by anodization in step (a).
  • the tantalum spinneret is placed in an oxygen-containing electrolyte solution at room temperature to 380°C, preferably room temperature to 300°C, and an anode voltage of 3 to 800V is applied constantly for 0.01 to 2 hours, with a voltage-increasing current density of 1 to 200 mA/cm 2 to form a layer of amorphous Ta 2 O 5 film.
  • the non-aqueous oxygen-containing electrolyte may be anhydrous concentrated sulfuric acid or a molten salt or a mixture of a molten salt and a base, such as potassium nitrate, sodium nitrate, lithium nitrate, or a mixture thereof with a base such as lithium, sodium or potassium-containing base.
  • the melting temperature should be controlled to the melting point of the molten salt to below 380°C, because tantalum will be significantly oxidized above 400°C. A voltage of 3 to 66V is applied.
  • step (c) When the coating temperature in step (c) is from 250°C to 430°C, preferably from 300°C to 400°C, more preferably from 300°C to 350°C, step (a) of forming a layer of Ta 2 O 5 film before coating on the tantalum spinneret may be omitted.
  • the mixed melt or the mixed melt liquid has a temperature of 300°C to 520°C, the applied anode voltage is 5 to 25V, and the voltage-increasing current density is 5 to 20 mA/cm 2 .
  • an ultrasonic generator can be placed in the mixed melt or the mixed melt liquid in step (c).

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Ceramic Engineering (AREA)
  • Textile Engineering (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Claims (12)

  1. Procédé de traitement de surface d'une filière de tantale, caractérisé en ce que le procédé comprend les étapes suivantes :
    (a) placer la filière de tantale dans une solution d'électrolyte contenant de l'oxygène à une température ambiante de 380°C et appliquer une tension anodique de 3 à 800V de façon constante pendant 0,01 à 2 heures, avec une densité de courant augmentant la tension de 1 à 200 mA/cm2pour former une couche de film de Ta2O5 amorphe ;
    (b) éventuellement polissage : polissage d'une face de sortie de fibre de la filière de tantale traitée à l'étape (a) pour éliminer le 5film de Ta2O5 sur une surface de la face de sortie de fibre ; et
    (c) revêtement : soumettre la filière de tantale traitée dans l'étape (b) à un traitement de revêtement par un procédé électrochimique à sel fondu pour former une couche de film contenant un composé contenant du lithium.
  2. Procédé selon la revendication 1, comprenant en outre une étape de polissage (d) :
    soumettre la face de sortie de fibre de la filière de tantale traitée à l'étape (c) à un traitement de polissage pour éliminer la couche de film contenant un composé contenant du lithium sur la surface de la face de sortie de fibre.
  3. Procédé selon la revendication 1, dans lequel la solution d'électrolyte contenant de l'oxygène est une solution aqueuse, une solution non aqueuse, ou un mélange d'un électrolyte aqueux et d'un composé organique.
  4. Procédé selon la revendication 1, dans lequel à l'étape (c), le procédé électrochimique à sel fondu est un procédé électrochimique à sel de lithium fondu.
  5. Procédé selon la revendication 1, dans lequel, à l'étape (c), la filière est placée dans un sel inorganique de lithium contenant de l'oxygène ou un liquide fondu mixte d'un sel inorganique de lithium contenant de l'oxygène et d'hydroxyde de lithium, ou un liquide de fusion mixte d'un sel et d'hydroxyde de lithium ou un liquide de fusion mixte d'un sel de lithium et d'un sel contenant de l'oxygène à une température de 250°C à 650°C, de préférence de 250°C à 430°C, plus préférentiellement de 300°C à 400°C, encore plus préférentiellement de 300°C à 350°C, et une tension anodique de 1 à 66V est appliquée constamment pendant 0,01 à 200 heures, avec une densité de courant augmentant la tension de 1 à 1000 mA/cm2 pour former une couche de film contenant un composé contenant du lithium.
  6. Procédé selon la revendication 5, dans lequel le mélange fondu ou le liquide de mélange fondu a une température de 300°C à 520°C, de préférence de 300°C à 350°C, la tension anodique appliquée est de 5 à 25V, et la densité de courant augmentant la tension est de 5 à 20 mA/cm2.
  7. Procédé selon la revendication 5, dans lequel le sel de lithium inorganique contenant de l'oxygène est LiNO3.
  8. Procédé selon la revendication 5, dans lequel un générateur d'ultrasons est disposé dans le mélange fondu ou le liquide de mélange fondu à l'étape (c).
  9. Procédé selon la revendication 1, dans lequel la filière tantale est nitrurée ou non nitrurée avant l'étape (a).
  10. Procédé selon la revendication 1, dans lequel la filière de tantale comprend une filière de tantale pur et une filière d'alliage de tantale, de préférence une filière d'alliage de tantale-niobium.
  11. Procédé selon la revendication 1, dans lequel le procédé est un procédé de traitement de surface de la filière tantale pour le filage au mouillé.
  12. Une filière de tantale comprenant :
    (a) une couche de film amorphe de Ta2O5 ; et
    (b) une couche de film contenant un composé contenant du lithium formé à partir de la couche de film de Ta2O5 amorphe.
EP18761041.5A 2017-03-03 2018-03-02 Procédé de traitement de surface destiné à une tête de repoussage de tantale Active EP3536827B9 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
CN201710124797 2017-03-03
CN201710587999.8A CN108531906B (zh) 2017-03-03 2017-07-19 钽喷丝头的表面处理方法
PCT/CN2018/077938 WO2018157867A1 (fr) 2017-03-03 2018-03-02 Procédé de traitement de surface destiné à une tête de repoussage de tantale

Publications (4)

Publication Number Publication Date
EP3536827A1 EP3536827A1 (fr) 2019-09-11
EP3536827A4 EP3536827A4 (fr) 2020-04-29
EP3536827B1 true EP3536827B1 (fr) 2022-01-26
EP3536827B9 EP3536827B9 (fr) 2022-05-18

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EP18761041.5A Active EP3536827B9 (fr) 2017-03-03 2018-03-02 Procédé de traitement de surface destiné à une tête de repoussage de tantale

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EP (1) EP3536827B9 (fr)
JP (1) JP6808848B2 (fr)
CN (1) CN108531906B (fr)
ES (1) ES2908746T3 (fr)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110835786B (zh) * 2019-11-19 2021-11-30 中国石油化工股份有限公司 一种扁平形腈纶纤维的制备方法
CN111005050B (zh) * 2020-02-19 2021-08-03 南昌航空大学 一种提高烧结钕铁硼磁体耐蚀性双涂层的制备方法

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4678546A (en) * 1985-03-27 1987-07-07 North China Research Institute Of Electro-Optics Process for providing lithium tantalum oxide coated tantalum articles with improved wear resistance
CN85101505B (zh) * 1985-04-01 1988-03-30 华北光电技术研究所 钽铌器件熔盐电解法制膜及产品
JPH0660436B2 (ja) * 1986-03-28 1994-08-10 ユ ツオン リユ タンタル、ニオブまたはその合金製物品の保護膜およびその製法
CN86102269B (zh) * 1986-04-09 1988-11-23 华北光电技术研究所 带膜钽铌喷丝头(板)的制造方法及应用
CN2151155Y (zh) * 1992-11-15 1993-12-29 李士华 钽材制品离子电解镀膜
CN1279224C (zh) * 2001-04-09 2006-10-11 北京华宇创新科贸有限责任公司 用于湿法纺丝的钽喷丝头的表面处理方法
CN1428465A (zh) * 2001-12-27 2003-07-09 北京华宇创新科贸有限责任公司 用于湿法纺丝的钽喷丝头的表面处理方法
CN100443629C (zh) * 2006-06-22 2008-12-17 上海交通大学 钽喷丝头表面化学气相沉积金刚石薄膜强化方法

Also Published As

Publication number Publication date
EP3536827B9 (fr) 2022-05-18
ES2908746T9 (es) 2022-06-13
CN108531906B (zh) 2020-05-29
EP3536827A4 (fr) 2020-04-29
ES2908746T3 (es) 2022-05-03
JP2020509250A (ja) 2020-03-26
EP3536827A1 (fr) 2019-09-11
JP6808848B2 (ja) 2021-01-06
CN108531906A (zh) 2018-09-14

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