EP2723923B1 - Pièces de pompe à vide ne comprenant pas de couche de conversion - Google Patents
Pièces de pompe à vide ne comprenant pas de couche de conversion Download PDFInfo
- Publication number
- EP2723923B1 EP2723923B1 EP12728262.2A EP12728262A EP2723923B1 EP 2723923 B1 EP2723923 B1 EP 2723923B1 EP 12728262 A EP12728262 A EP 12728262A EP 2723923 B1 EP2723923 B1 EP 2723923B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- components
- alloys
- aluminum
- titanium
- zirconium
- 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
Links
- 238000006243 chemical reaction Methods 0.000 title claims description 7
- 238000000576 coating method Methods 0.000 claims description 23
- 229910052751 metal Inorganic materials 0.000 claims description 23
- 239000002184 metal Substances 0.000 claims description 23
- 229910045601 alloy Inorganic materials 0.000 claims description 19
- 239000000956 alloy Substances 0.000 claims description 19
- 239000011248 coating agent Substances 0.000 claims description 19
- 150000002739 metals Chemical class 0.000 claims description 17
- 229910052782 aluminium Inorganic materials 0.000 claims description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 14
- 239000010936 titanium Substances 0.000 claims description 14
- 229910052719 titanium Inorganic materials 0.000 claims description 13
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 11
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 11
- 239000011777 magnesium Substances 0.000 claims description 11
- 229910052749 magnesium Inorganic materials 0.000 claims description 11
- 229910052726 zirconium Inorganic materials 0.000 claims description 10
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 8
- 238000007743 anodising Methods 0.000 claims description 7
- 229910052758 niobium Inorganic materials 0.000 claims description 7
- 239000010955 niobium Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 5
- 229910052732 germanium Inorganic materials 0.000 claims description 5
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 5
- 229910052735 hafnium Inorganic materials 0.000 claims description 5
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 150000002222 fluorine compounds Chemical class 0.000 claims description 2
- 238000009713 electroplating Methods 0.000 claims 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 11
- 238000000034 method Methods 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- 229910052574 oxide ceramic Inorganic materials 0.000 description 8
- 239000011224 oxide ceramic Substances 0.000 description 8
- 238000002048 anodisation reaction Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 229910000789 Aluminium-silicon alloy Inorganic materials 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 238000005524 ceramic coating Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 229910016570 AlCu Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229920002313 fluoropolymer Polymers 0.000 description 2
- 239000004811 fluoropolymer Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910010038 TiAl Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 239000010407 anodic oxide Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007739 conversion coating Methods 0.000 description 1
- 238000012217 deletion Methods 0.000 description 1
- 230000037430 deletion Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000052 poly(p-xylylene) Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
- C25D9/06—Electrolytic coating other than with metals with inorganic materials by anodic processes
-
- Y—GENERAL 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
- Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
- Y10T428/264—Up to 3 mils
-
- Y—GENERAL 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
- Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
- Y10T428/264—Up to 3 mils
- Y10T428/265—1 mil or less
Definitions
- the invention relates to conversion-layer-free components of vacuum pumps made of valve metals and their alloys.
- DE 101 63 864 A1 relates to a process for coating articles of valve metals or their alloys with a thin barrier layer of the metal and oxide ceramic layer thereon, the surface of which is coated with fluoropolymers, characterized in that the fluoropolymers in the form of a solution are impregnated by vacuum impregnation into the capillary system Insert oxide ceramic layer and dried after removing the non-wetting solution components.
- the group of valve metals aluminum, magnesium, titanium, niobium or zirconium and their alloys.
- this document also defines other components of vacuum pumps made of valve metals, such as rotors and stators of turbomolecular pumps.
- pure aluminum and AlMn alloys AlMnCu; AlMg 1 ; AlMg 1.5 ; E-AlMgSi; AlMgSi 0.5 ; AlZnMgCu 0.5 ; AlZnMgCu 1.5 ; G-AlSi 1.2 ; G-AlSi 5 MW; G-AlSi 8 Cu 3 ; G-AlCu 4 Ti; G-AlCu 4 TiMg understood.
- the magnesium casting alloys of the ASTM designations AS41, AM60, AZ61, AZ63, AZ81 are also suitable for the purposes of the invention.
- the oxide ceramic layer is formed essentially by a conversion layer of the surface of the component, so that here virtually a portion of the substrate material is removed and converted into the oxidation barrier layer.
- EP 1 818 428 A1 For example, there is known a method of electrolytic ceramic coating for metal and an electrolyte for use in electrolytic ceramic coating of metals and metallic materials.
- EP 1 050 606 A1 discloses a method of making hard protective coatings on particles made from aluminum alloys.
- WO 2005/014892 A2 describes a method for producing a coating on a plastic component of a vacuum pump.
- a metallic layer is applied to the component and the coating electrolytic plasma oxidation of the metallic layer.
- valve metal objects in particular components of vacuum pumps with an oxide ceramic layer formed from the metal, which has a thin barrier layer as an interface to the metal, provided with a further polymeric coating, which is formed on the basis of parylenes.
- DE 10 2005 040 648 A1 also describes the composition of this surface coating and an application method.
- WO 03/029529 A1 WO 2006/047501 A2 and WO 2006/047526 A2 describe the production of an article with a corrosion, heat and abrasion resistant ceramic coating of titanium and / or zirconia applied by the DC or AC anodization on the aluminum and / or titanium article.
- the objects underlying this prior art are not defined further. Also, no information on the chemical resistance, in particular the resistance to citric acid or hydrochloric and / or Flußsääuredämpfe present.
- the object of the present invention is to provide conversion-layer-free components of vacuum pumps made of valve metals and their alloys, which in addition to corrosion, heat and abrasion resistance have a galvanically generated conversion coating coating, which is also resistant to chemicals, especially resistant to citric acid or hydrochloric acid vapors. This is particularly important in the manufacture of components of vacuum pumps that come in contact with aggressive gases, such as HCl and / or HF vapor / gas, especially in the vacuum range.
- the solution of the above object consists in a first embodiment of conversion-free components of vacuum pumps made of valve metals and their alloys, which is characterized in that the surface of a galvanically produced coating of at least one oxide and / or an oxifluoride of an element of the group consisting of boron, germanium , Aluminum, magnesium, titanium, niobium, hafnium and / or zirconium and mixtures thereof and / or an oxifluoride of the group consisting of Aluminum, titanium and / or zirconium has a layer thickness in the range of 5 to 50 microns.
- the solution of the abovementioned object utilizes contoured covering of surfaces, as is possible with known conversion layers such as KEPLA-Coat® or anodization layers.
- conversion layers such as KEPLA-Coat® or anodization layers.
- the deposited layers can have a hardness of about 700 HV.
- Components according to the invention of vacuum pumps made of valve metals and their alloys include, in particular, rotors, stators, stator disk halves, threaded steps, housings and bearing shells.
- valve metals is in accordance with the prior art here for metals of the group aluminum, magnesium, titanium, niobium and / or zirconium and their alloys.
- the special alloys of aluminum, magnesium and titanium mentioned in the introduction to the description are also particularly preferred for the purposes of the present invention.
- At least one oxide and / or oxifluorides of the group consisting of aluminum, titanium and / or zirconium are particularly preferably selected.
- an embodiment of the present invention is that the thickness of the surface coating is 5 to 50 ⁇ m. Particularly preferred according to the present invention, the thickness of the surface coating is 15 to 30 microns. If the thickness of the surface coating is chosen to be too thin, adequate protection against corrosion, heat, abrasion and chemicals is not guaranteed. If, however, the thickness of the surface coating chosen too large, so appropriate coatings tend to flake off. In addition, correspondingly thick layers are uneconomical.
- a sample plate of AlMgSi 1 with the dimensions of 100 x 50 x 1.5 mm was at 400 volts for 5 minutes in a WO 03/029529 .
- WO 2006/047501 A2 and WO 2006/047526 A2 electrolytes coated anodically over a period of 5 minutes. The determined layer thickness was about 10 ⁇ m.
- a sample sheet as described in Example 2 was coated analogously within 10 minutes.
- the determined layer thickness was about 12 ⁇ m.
- test panels coated according to Examples 1 and 2 were exposed to a hydrochloric acid atmosphere which forms over an initial charge of 15% strength by weight hydrochloric acid master.
- the oxide ceramic layer on the sample plates was examined for detachment after 144 h and after 300 h of the test period. The oxide ceramic layer on the sample plates was intact after this exposure time.
- test panels coated according to Examples 1 and 2 were exposed to citric acid solutions at concentrations of 2%, 3.5% and 5%.
- the oxide ceramic layer on the sample plates was after 90h trial period for deletions examined.
- the oxide ceramic layer on the sample plates was intact after this exposure time.
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Structures Of Non-Positive Displacement Pumps (AREA)
- Physical Vapour Deposition (AREA)
Claims (5)
- Composants de pompe à vide sans couches de conversion, en métaux de soupape ou des alliages de ceux-ci, caractérisés en ce que leurs surfaces présentent un revêtement d'au moins un oxyde d'un élément du groupe consistant en bore, germanium, aluminium, magnésium, titane, niobium, hafnium et/ou zirconium, et des mélanges de ceux-ci, et/ou un oxyfluorure du groupe consistant en aluminium, titane et/ou zirconium, préparés par revêtement galvanique, et ayant une épaisseur de couche comprise dans la gamme allant de 5 à 50 µm.
- Composants selon la revendication 1, incluant des rotors, des stators, des demi-disques de stators, des étages à filetage, des boîtiers, et des coussinets.
- Composants selon la revendication 1 ou 2, caractérisés en ce que ledit métal de soupape est choisi parmi l'aluminium, le magnésium, le titane, le niobium, et /ou le zirconium et leurs alliages.
- Composants selon l'une quelconque des revendications 1 à 3, caractérisés en ce que l'épaisseur du revêtement de surface est de 15 à 30 µm.
- Procédé pour préparer des composants de pompe à vide sans couches de conversion, en métaux de soupape ou des alliages de ceux-ci, préparés par revêtement galvanique, caractérisé par l'étape consistant à(a) procurer une solution d'anodisation contenant, outre l'eau, au moins un autre composant choisi dans le groupe de fluorures et oxyfluorures complexes, dispersibles dans l'eau, d'éléments du groupe consistant en bore, germanium, aluminium, magnésium, titane, niobium, hafnium et/ou zirconium, et des mélanges de ceux-ci,(b) mettre une cathode en contact avec ladite solution d'anodisation,(c) introduire les composants en tant qu'anodes dans ladite solution d'anodisation, et(d) appliquer une tension électrique entre l'anode et la cathode pour appliquer un revêtement de surface auxdits composants.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102011105455A DE102011105455A1 (de) | 2011-06-24 | 2011-06-24 | Konversionsschichtfreie Bauteile von Vakuumpumpen |
PCT/EP2012/061491 WO2012175429A1 (fr) | 2011-06-24 | 2012-06-15 | Pièces exemptes de couches de conversion pour des pompes à vide |
Publications (2)
Publication Number | Publication Date |
---|---|
EP2723923A1 EP2723923A1 (fr) | 2014-04-30 |
EP2723923B1 true EP2723923B1 (fr) | 2017-09-06 |
Family
ID=46319764
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP12728262.2A Active EP2723923B1 (fr) | 2011-06-24 | 2012-06-15 | Pièces de pompe à vide ne comprenant pas de couche de conversion |
Country Status (8)
Country | Link |
---|---|
US (1) | US20140154503A1 (fr) |
EP (1) | EP2723923B1 (fr) |
JP (1) | JP5957075B2 (fr) |
KR (1) | KR20140043129A (fr) |
CN (1) | CN103620091A (fr) |
DE (1) | DE102011105455A1 (fr) |
TW (1) | TWI560327B (fr) |
WO (1) | WO2012175429A1 (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US10933592B2 (en) | 2016-06-29 | 2021-03-02 | Valinge Innovation Ab | Method and device for inserting a tongue |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109707628A (zh) * | 2018-12-17 | 2019-05-03 | 陈鑫 | 真空泵的铝合金泵体结构及用于该泵体加工的珩磨头 |
Family Cites Families (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4332297B2 (ja) * | 1997-12-17 | 2009-09-16 | アイル・コート・リミテツド | アルミニウム合金からつくられた物品上に硬質保護用コーティングを施す方法 |
KR100417580B1 (ko) * | 2000-12-29 | 2004-02-05 | 주식회사 엘지이아이 | 스크롤 압축기용 베어링 제조방법 |
ATE389045T1 (de) | 2001-09-29 | 2008-03-15 | Oerlikon Heberlein Temco Wattw | Verfahren und vorrichtung zur herstellung von kontengarn |
US7578921B2 (en) * | 2001-10-02 | 2009-08-25 | Henkel Kgaa | Process for anodically coating aluminum and/or titanium with ceramic oxides |
US7820300B2 (en) * | 2001-10-02 | 2010-10-26 | Henkel Ag & Co. Kgaa | Article of manufacture and process for anodically coating an aluminum substrate with ceramic oxides prior to organic or inorganic coating |
US6916414B2 (en) * | 2001-10-02 | 2005-07-12 | Henkel Kommanditgesellschaft Auf Aktien | Light metal anodization |
US7452454B2 (en) | 2001-10-02 | 2008-11-18 | Henkel Kgaa | Anodized coating over aluminum and aluminum alloy coated substrates |
DE10163864A1 (de) * | 2001-12-22 | 2003-07-10 | Leybold Vakuum Gmbh | Beschichtung von Gegenständen |
JP4694771B2 (ja) * | 2003-03-12 | 2011-06-08 | 財団法人国際科学振興財団 | ポンプおよびポンプ部材の製造方法 |
DE202004010821U1 (de) * | 2003-07-23 | 2004-12-23 | The Boc Group Plc, Windlesham | Vakuumpumpenbauteil |
GB0317126D0 (en) * | 2003-07-23 | 2003-08-27 | Boc Group Plc | Coating |
US20080093223A1 (en) * | 2004-11-05 | 2008-04-24 | Nobuaki Yoshioka | Method for electrolytically depositing a ceramic coating on a metal, electrolyte for such electrolytic ceramic coating method, and metal member |
DE102005040648A1 (de) | 2005-08-27 | 2007-03-01 | Leybold Vacuum Gmbh | Beschichtete Gegenstände |
DE102008024764A1 (de) * | 2008-05-23 | 2009-11-26 | Oerlikon Leybold Vacuum Gmbh | Mehrstufige Vakuumpumpe |
US9701177B2 (en) * | 2009-04-02 | 2017-07-11 | Henkel Ag & Co. Kgaa | Ceramic coated automotive heat exchanger components |
CN102362015B (zh) * | 2009-04-10 | 2014-06-18 | 株式会社爱发科 | 构成机械增压泵、涡轮分子泵或干式泵的部件的表面处理方法及通过该表面处理方法处理过的机械增压泵、涡轮分子泵或干式泵 |
-
2011
- 2011-06-24 DE DE102011105455A patent/DE102011105455A1/de not_active Withdrawn
-
2012
- 2012-06-06 TW TW101120284A patent/TWI560327B/zh active
- 2012-06-15 CN CN201280028749.6A patent/CN103620091A/zh active Pending
- 2012-06-15 WO PCT/EP2012/061491 patent/WO2012175429A1/fr active Application Filing
- 2012-06-15 US US14/126,715 patent/US20140154503A1/en not_active Abandoned
- 2012-06-15 JP JP2014516291A patent/JP5957075B2/ja active Active
- 2012-06-15 KR KR1020147001902A patent/KR20140043129A/ko not_active Application Discontinuation
- 2012-06-15 EP EP12728262.2A patent/EP2723923B1/fr active Active
Non-Patent Citations (1)
Title |
---|
None * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US10933592B2 (en) | 2016-06-29 | 2021-03-02 | Valinge Innovation Ab | Method and device for inserting a tongue |
Also Published As
Publication number | Publication date |
---|---|
TW201303090A (zh) | 2013-01-16 |
US20140154503A1 (en) | 2014-06-05 |
DE102011105455A1 (de) | 2013-01-10 |
EP2723923A1 (fr) | 2014-04-30 |
TWI560327B (en) | 2016-12-01 |
KR20140043129A (ko) | 2014-04-08 |
JP2014520211A (ja) | 2014-08-21 |
CN103620091A (zh) | 2014-03-05 |
WO2012175429A1 (fr) | 2012-12-27 |
JP5957075B2 (ja) | 2016-07-27 |
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Legal Events
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PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
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17P | Request for examination filed |
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