DE3632748A1 - Method of coating hollow bodies - Google Patents

Method of coating hollow bodies

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Publication number
DE3632748A1
DE3632748A1 DE19863632748 DE3632748A DE3632748A1 DE 3632748 A1 DE3632748 A1 DE 3632748A1 DE 19863632748 DE19863632748 DE 19863632748 DE 3632748 A DE3632748 A DE 3632748A DE 3632748 A1 DE3632748 A1 DE 3632748A1
Authority
DE
Germany
Prior art keywords
plasma
hollow body
net
coating
coated
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.)
Granted
Application number
DE19863632748
Other languages
German (de)
Other versions
DE3632748C2 (en
Inventor
Peter Plein
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.)
Vereinigung zur Foerderung des Instituts fuer Kunststoffverarbeitung in Industrie und Handwerk an Der Rhein
Original Assignee
Vereinigung zur Foerderung des Instituts fuer Kunststoffverarbeitung in Industrie und Handwerk an Der Rhein
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.)
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Publication date
Application filed by Vereinigung zur Foerderung des Instituts fuer Kunststoffverarbeitung in Industrie und Handwerk an Der Rhein filed Critical Vereinigung zur Foerderung des Instituts fuer Kunststoffverarbeitung in Industrie und Handwerk an Der Rhein
Priority to DE19863632748 priority Critical patent/DE3632748A1/en
Publication of DE3632748A1 publication Critical patent/DE3632748A1/en
Application granted granted Critical
Publication of DE3632748C2 publication Critical patent/DE3632748C2/de
Granted legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/62—Plasma-deposition of organic layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/22—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to internal surfaces, e.g. of tubes
    • B05D7/227—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to internal surfaces, e.g. of tubes of containers, cans or the like
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/46—Polymerisation initiated by wave energy or particle radiation
    • C08F2/52—Polymerisation initiated by wave energy or particle radiation by electric discharge, e.g. voltolisation

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Treatments Of Macromolecular Shaped Articles (AREA)
  • Physical Vapour Deposition (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

The invention is based on the idea of developing a method which offers the possibility of providing hollow bodies of plastics or other non-microwave-active materials (for example glass) with diffusion-inhibiting coatings. As a result, on the one hand diffusion barrier effects are to be achieved, as are accomplished by processes such as sulphonation and fluorination, on the other hand their fundamental disadvantages are to be avoided and, consequently, the coating method is to be made less expensive. This object is achieved according to the invention by the hollow body to be coated being placed in a vacuum chamber which at the same time is designed as a microwave applicator. The coating is performed by the process of plasma polymerisation. This involves introducing monomers into a plasma. Excitations induced by the plasma cause the formation of monomer radicals, which subsequently polymerise out on surfaces and are deposited there as micropore-free, highly crosslinked layers. After introducing the hollow body, the entire vacuum chamber together with the hollow body to be coated is evacuated to the necessary operating pressure. Microwaves are fed into the vacuum chamber from outside at several points and additional measures are taken to ensure that a homogeneous electric field prevails in the vacuum chamber.

Description

Dem zunehmenden Einsatz meist blasgeformter Kunststoffhohlkörper in den unterschiedlichsten Bereichen sind durch die teilweise unzureichenden Sperreigenschaften der Kunststoffe gegen Gas, Dämpfe und organische Flüssigkeiten Grenzen gesetzt. Zur Ver­ besserung der Barriereeigenschaften sind mehrere Verfahren ent­ wickelt worden. Eine Reihe von Verfahren basiert auf der Modi­ fikation von Kunststoffen (Copolymerisation, Änderung der Mor­ phologie). Andere Verfahren arbeiten mit dem Aufbau von Mehr­ schichtsystemen (Lamellenstrukturen, Coextrusion, Lackieren). Gerade im Bereich großvolumiger Hohlkörper - als Behältnisse für Kohlenwasserstoffe - wird eine chemische Veränderung der Ober­ fläche durch Sulfonieren oder Fluorieren angestrebt. Vor allem die letztgenannten Verfahren verlangen einen hohen sicherheits­ technischen Aufwand, da hierbei prozeßbedingt mit aggressiven Flüssigkeiten und Gasen (Flußsäure, Schwefelsäure, Fluorgas)­ gearbeitet werden muß. Außerdem bereitet die Entsorgung der Prozeßabfälle große Probleme und ist mit einem erheblichen finanziellen Aufwand verbunden.The increasing use of mostly blow-molded hollow plastic parts in a wide variety of areas is limited by the inadequate barrier properties of the plastics against gas, vapors and organic liquids. Several methods have been developed to improve the barrier properties. A number of processes are based on the modification of plastics (copolymerization, change in morphology). Other processes work with the construction of multilayer systems (lamella structures, coextrusion, painting). Especially in the area of large-volume hollow bodies - as containers for hydrocarbons - a chemical change in the surface by sulfonation or fluorination is sought. The last-mentioned methods in particular require a high level of technical safety, since in this process aggressive liquids and gases (hydrofluoric acid, sulfuric acid, fluorine gas) have to be used. In addition, the disposal of process waste causes great problems and is associated with a considerable financial outlay.

Der Erfindung liegt die Idee zugrunde, ein Verfahren zu ent­ wickeln, das die Möglichkeit bietet, Hohlkörper aus Kunststoffen oder anderen nicht mikrowellenaktiven Materialien (z.B. Glas) mit diffusionshemmenden Schichten zu versehen. Hierdurch sollen zum einen Diffusionssperrwirkungen erreicht werden, wie sie mit Verfahren wie Sulfonieren und Fluorieren erzielt werden, zum anderen sollen deren prinzipielle Nachteile vermieden und dadurch das Beschichtungsverfahren kostengünstiger gestaltet werden.The invention is based on the idea of developing a method wrap, which offers the possibility of plastic hollow bodies or other non-microwave active materials (e.g. glass) to provide diffusion-inhibiting layers. This is intended to a diffusion barrier effects can be achieved, as with Processes such as sulfonation and fluorination can be achieved to others should avoid their basic disadvantages and thereby the coating process can be made more cost-effective.

Diese Aufgabe wird erfindungsgemäß dadurch gelöst, daß der zu beschichtende Hohlkörper in eine Vakuumkammer eingebracht wird, die gleichzeitig als Mikrowellenapplikator ausgebildet ist. Die Beschichtung erfolgt mit dem Verfahren der Plasmapolymerisation. Hierbei werden Monomere in ein Plasma eingeleitet. Aufgrund von Anregungen durch das Plasma bilden sich Monomerradikale, die an­ schließend auf Oberflächen auspolymerisieren und sich dort als mikroporenfreie, hochvernetzte Schichten abscheiden. Nach dem Einbringen des Hohlkörpers wird die gesamte Vakuumkammer zusammen mit dem zu beschichtenden Hohlkörper auf den notwendigen Arbeits­ druck evakuiert. Von außen werden an mehreren Stellen Mikrowellen in die Vakuumkammer eingespeist, durch zusätzliche Maßnahmen wird dafür gesorgt, daß ein homogenes elektrisches Feld in der Vakuum­ kammer herrscht.This object is achieved in that the coating hollow body is placed in a vacuum chamber, which is also designed as a microwave applicator. The Coating is done using the plasma polymerization process. Here monomers are introduced into a plasma. Owing to Excitation by the plasma forms monomer radicals, which then polymerize on surfaces and there as Deposit micro-pore-free, highly cross-linked layers. After this  The entire vacuum chamber is brought together by inserting the hollow body with the hollow body to be coated on the necessary work pressure evacuated. There are microwaves from outside at several points fed into the vacuum chamber through additional measures ensured that a homogeneous electric field in the vacuum chamber rules.

Anschließend werden über eine mikrowellenmäßig abgeschirmte Düse entweder das zur Beschichtung vorgesehene Monomere oder ein Gemisch von Monomerem und einem Plasmaträgergas (Argon, Helium, Sauerstoff, Stickstoff) in das Innere des Hohlkörpers injiziert, so daß - an­ geregt durch das Mikrowellenfeld - ein Plasma gezündet und die Plasmapolymerisation durchgeführt wird.Subsequently, either the monomer intended for coating or a mixture of monomers and a plasma carrier gas (argon, helium, oxygen, nitrogen) are injected into the interior of the hollow body via a microwave-shielded nozzle, so that - excited by the microwave field - a plasma is ignited and the plasma polymerization is carried out.

Der eigentlichen Beschichtung vorgeschaltet werden kann eine Be­ handlung des Hohlkörpers in einem Sauerstoffplasma zur Reinigung und Aktivierung der Oberfläche. Desgleichen kann eine Nachbehand­ lung der zu beschichtenden Flächen in einem Sauerstoffplasma oder ein Spülen mit Sauerstoff vorgesehen werden, um eine weitere Ver­ besserung der Diffusionsschutzwirkung zu erreichen.The actual coating can be preceded by a loading treatment of the hollow body in an oxygen plasma for cleaning and activation of the surface. Aftertreatment can also be used the surfaces to be coated in an oxygen plasma or an oxygen purge may be provided to further ver to achieve better diffusion protection.

Verfahrensbedingt können als zu beschichtende Materialien nur mikrowelleninaktive Materialien, die selbst keine Energie aus dem Mikrowellenfeld aufnehmen, oder nur schwach mikrowellenaktive Stoffe dienen.Due to the process, materials can only be coated microwave inactive materials that do not themselves generate energy from the Record microwave field, or only weakly microwave active Serve fabrics.

Die mit dieser Erfindung erzielbaren Vorteile liegen zum einen darin, daß der gesamte Beschichtungsprozeß in einem geschlossenen System stattfindet. Somit sind keine Entsorgungsmaßnahmen notwen­ dig, eine Belastung der Umwelt findet nicht statt. Die notwen­ digen sicherheitstechnischen Maßnahmen beschränken sich auf Maßnahmen zur Erzielung einer Mikrowellendichtigkeit der Anlage.The advantages that can be achieved with this invention are on the one hand in that the entire coating process in a closed System takes place. Therefore no disposal measures are necessary dig, there is no environmental pollution. The necessary Other safety measures are limited to Measures to achieve microwave tightness of the system.

Zum anderen sind aufgrund der Mikroporenfreiheit der entstehenden Schichten, ihres hohen Vernetzungsgrades und ihrer hohen Dichte Verbesserungen der Diffusionsschutzwirkung erreichbar, die die der bisher üblichen Verfahren übertrifft. Secondly, due to the absence of micropores, the resulting Layers, their high degree of cross-linking and their high density Improvements in the diffusion protection effect achievable that the exceeds the usual procedures.  

Zur Beschichtung von Hohlkörpern, deren Wände hinreichend steif sind, um einer Druckdifferenz von 0,9 bar zwischen Außen- und Innenseite ohne große Verformungen zu widerstehen, wird erfin­ dungsgemäß eine zweite Verfahrensvariante vorgeschlagen.For coating hollow bodies, the walls of which are sufficiently rigid are to a pressure difference of 0.9 bar between outside and It is invented to withstand the inside without large deformations In accordance with the invention, a second method variant is proposed.

Hierbei besteht die Mikrowellenkammer aus zwei oder mehreren Tei­ len, die mit Hilfe geeigneter Verbindungen mikrowellendicht zu­ sammengefügt werden können. Eine Vakuumdichtigkeit der Mikrowel­ lenkammer ist nicht erforderlich.The microwave chamber consists of two or more parts len, which are microwave-proof with the help of suitable connections can be put together. A vacuum tightness of the microwave Steering chamber is not required.

Der zu beschichtende Hohlkörper wird in die geöffnete Mikrowel­ lenkammer gebracht und mit Hilfe einer geeigneten Vorrichtung so an eine Vakuumpumpe angeflanscht, daß der Hohlkörper durch seine Öffnung auf den Arbeitsdruck evakuiert werden kann. Die Mikrowel­ lenkammer wird geschlossen; der Hohlkörper wird evakuiert. Durch eine in das Absaugsystem integrierte oder davon getrennte Mono­ mereinspritzdüse wird das zu verwendende Monomer und eventuell ein zusätzliches Trägergas in das Innere des Hohlkörpers gebracht. Das durch das anschließend angelegte Mikrowellenfeld gezündete Plasma brennt nur im Innern des Hohlkörpers, da die erforderliche Zündspannung für ein Plasma mit steigendem Gasdruck stark ansteigt und da der Hohlkörper nur im Innern evakuiert ist.The hollow body to be coated is placed in the opened microwave brought to the steering chamber and with the help of a suitable device flanged to a vacuum pump that the hollow body through its Opening can be evacuated to the working pressure. The microwave steering chamber is closed; the hollow body is evacuated. By a mono integrated in or separate from the suction system mer injector becomes the monomer to be used and possibly brought an additional carrier gas into the interior of the hollow body. The ignited by the subsequently created microwave field Plasma only burns inside the hollow body as the required Ignition voltage for a plasma rises sharply with increasing gas pressure and since the hollow body is only evacuated inside.

Die mit diesem Teil der Erfindung erreichbaren Vorteile liegen zusätzlich darin, daß der vakuumtechnische Aufwand der Anlage auf ein Minimum reduziert wird. Außerdem können die Zykluszeiten bei der Beschichtung weiter reduziert werden.The advantages achievable with this part of the invention are In addition, the fact that the system requires a vacuum is reduced to a minimum. In addition, the cycle times at the coating can be further reduced.

Das erfindungsgemäß entwickelte Verfahren kann - außer in dem vorstehend beschriebenen Einsatzbereich - auch in anderen Bereichen eingesetzt werden. So können mit dem Verfahren z.B. polymere Deck­ schichten aufgebracht werden, die Aufgaben im Bereich des Korro­ sionsschutzes übernehmen. Andere realisierbare Aufgabenbereiche sind die Erhöhung der mechanischen Festigkeit der Oberflächen oder die Erzielung dekorativer Effekte.The method according to the invention developed can - except in the above-described area of application - also be used in other areas. The process can be used, for example, to apply polymeric top layers that take on corrosion protection tasks. Other realizable tasks are increasing the mechanical strength of the surfaces or achieving decorative effects.

Die Fig. 1 und 2 zeigen zwei mögliche Ausführungsformen der Erfindung. Hierbei bezeichnet Figs. 1 and 2 show two possible embodiments of the invention. Inscribed here

  • 1 ein Mikrowellengenerator,
    2 die Mikrowelleneinkopplungen in die Beschichtungskammer,
    3 die Monomereinlaßdüse,
    4 die Vakuum- bzw. Mikrowellenkammer,
    5 den Anschluß der Vakuumpumpen und
    6 den lösbaren Vakuumausschluß des Hohlkörpers.     1 a microwave generator,
    2 the microwave coupling into the coating chamber,
    3 the monomer inlet nozzle,
    4 the vacuum or microwave chamber,
    5 the connection of the vacuum pumps and
    6 the releasable vacuum exclusion of the hollow body.

Claims (14)

1. Verfahren zur Beschichtung von Hohlkörpern mit polymeren Deckschichten, dadurch gekennzeichnet, daß die Beschichtung mit dem Verfahren der Plasmapolymerisation erfolgt.1. Process for coating hollow bodies with polymeric cover layers, characterized in that the coating is carried out with the process of plasma polymerization. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die zu beschichtenden Hohlkörper aus nicht mikrowellenaktiven Kunst­ stoffen bestehen.2. The method according to claim 1, characterized in that the to coating hollow body made of non-microwave active art fabrics exist. 3. Verfahren nach Anspruch 1 und 2, dadurch gekennzeichnet, daß die zu beschichtenden Hohlkörper aus anderen nicht mikro­ wellenaktiven Materialien bestehen.3. The method according to claim 1 and 2, characterized in that the hollow body to be coated from other non-micro wave-active materials exist. 4. Verfahren nach den Ansprüchen 1 bis 3, dadurch gekennzeich­ net, daß die zu beschichtenden Hohlkörper aus schwach mikrowellen­ aktiven bzw. durch den Zusatz von Ruß schwach mikrowellen­ aktiv gemachten Kunststoffen bestehen.4. The method according to claims 1 to 3, characterized in net that the hollow body to be coated from weak microwaves active or weak microwave due to the addition of soot actively made plastics exist. 5. Verfahren nach den Ansprüchen 1 bis 4, dadurch gekennzeich­ net, daß die Beschichtung nur auf den Innenseiten der Hohl­ körper erfolgt.5. The method according to claims 1 to 4, characterized in net that the coating only on the inside of the hollow body takes place. 6. Verfahren nach den Ansprüchen 1 bis 5, dadurch gekennzeich­ net, daß ein Plasma in einem Plasmareaktor mit Metallwänden gezündet wird und daß die Anregung des Plasmas durch von außen eingekoppelte Mikrowellen erfolgt.6. The method according to claims 1 to 5, characterized in net that a plasma in a plasma reactor with metal walls is ignited and that the excitation of the plasma by from outside Coupled microwaves takes place. 7. Verfahren nach den Ansprüchen 1 bis 6, dadurch gekennzeich­ net, daß der Plasmareaktor als Vakuumgefäß ausgeführt ist. 7. The method according to claims 1 to 6, characterized in net that the plasma reactor is designed as a vacuum vessel.   8. Verfahren nach den Ansprüchen 1 bis 7, dadurch gekennzeich­ net, daß der Plasmareaktor so ausgelegt ist, daß in seinem Innern ein möglichst homogenes Mikrowellenfeld und damit ein homogenes Plasma herrscht.8. The method according to claims 1 to 7, characterized in net that the plasma reactor is designed so that in its Inside, a microwave field that is as homogeneous as possible and thus a homogeneous plasma prevails. 9. Verfahren nach den Ansprüchen 1 bis 8, dadurch gekennzeich­ net, daß der zu beschichtende Hohlkörper evakuiert wird, während eine ihn umgebende Mikrowellenkammer nicht evakuiert wird, so daß ein Plasma nur im Innern des Hohlkörpers brennt.9. The method according to claims 1 to 8, characterized in net that the hollow body to be coated is evacuated, while a microwave chamber surrounding it does not evacuate is so that a plasma burns only inside the hollow body. 10. Verfahren nach den Ansprüchen 1 bis 9, dadurch gekennzeich­ net, daß das im Plasma zu polymerisierende Monomere über eine Monomer-Einspritzdüse ins Innere des zu beschichtenden Hohl­ körpers injiziert wird.10. The method according to claims 1 to 9, characterized in net that the monomer to be polymerized in plasma via a Monomer injector inside the hollow to be coated body is injected. 11. Verfahren nach den Ansprüchen 1 bis 10, dadurch gekennzeich­ net, daß die Mikrowellenkammer zwecks schnelleren Öffnens und Schließens mehrgeteilt ist und durch geeignete Schnell­ verbindungen mikrowellendicht verschlossen werden kann.11. The method according to claims 1 to 10, characterized in net that the microwave chamber for faster opening and closing is divided and by appropriate quick connections can be sealed microwave-tight. 12. Verfahren nach den Ansprüchen 1 bis 11, dadurch gekennzeich­ net, daß während der Beschichtung als Trägergas des Plasmas Sauerstoff, Stickstoff, Helium oder Argon zugegeben wird.12. The method according to claims 1 to 11, characterized in net that during the coating as the carrier gas of the plasma Oxygen, nitrogen, helium or argon is added. 13. Verfahren nach den Ansprüchen 1 bis 12, dadurch gekennzeich­ net, daß die zu beschichtenden Hohlkörper vor der Beschichtung einer Vorbehandlung in einem Sauerstoffplasma unterzogen werden.13. The method according to claims 1 to 12, characterized in net that the hollow body to be coated before coating pretreated in an oxygen plasma will. 14. Verfahren nach den Ansprüchen 1 bis 13, dadurch gekennzeich­ net, daß die beschichteten Hohlkörper einer Nachbehandlung in einem Sauerstoffplasma oder mit Sauerstoffgas unterzogen wurde.14. The method according to claims 1 to 13, characterized in net that the coated hollow body of an aftertreatment subjected in an oxygen plasma or with oxygen gas has been.
DE19863632748 1986-09-26 1986-09-26 Method of coating hollow bodies Granted DE3632748A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE19863632748 DE3632748A1 (en) 1986-09-26 1986-09-26 Method of coating hollow bodies

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19863632748 DE3632748A1 (en) 1986-09-26 1986-09-26 Method of coating hollow bodies

Publications (2)

Publication Number Publication Date
DE3632748A1 true DE3632748A1 (en) 1988-04-07
DE3632748C2 DE3632748C2 (en) 1989-04-13

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EP0622111A1 (en) * 1993-04-21 1994-11-02 Bend Research, Inc. Plasma polymerization and surface modification inside hollow micro-substrates
WO1994027745A1 (en) * 1993-06-01 1994-12-08 Kautex Werke Reinold Hagen Aktiengesellschaft Method and device for producing a polymer coating inside hollow plastic articles
WO1995021948A1 (en) * 1994-02-09 1995-08-17 The Coca-Cola Company Hollow containers with inert or impermeable inner surface through plasma-assisted deposition of a primarily inorganic substance
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US5521351A (en) * 1994-08-30 1996-05-28 Wisconsin Alumni Research Foundation Method and apparatus for plasma surface treatment of the interior of hollow forms
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US9878101B2 (en) 2010-11-12 2018-01-30 Sio2 Medical Products, Inc. Cyclic olefin polymer vessels and vessel coating methods
US9903782B2 (en) 2012-11-16 2018-02-27 Sio2 Medical Products, Inc. Method and apparatus for detecting rapid barrier coating integrity characteristics
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DE102016124209A1 (en) 2016-12-13 2018-06-14 Jokey Plastik Wipperfürth GmbH Coating device and coating method for plastic containers
US10189603B2 (en) 2011-11-11 2019-01-29 Sio2 Medical Products, Inc. Passivation, pH protective or lubricity coating for pharmaceutical package, coating process and apparatus
US10201660B2 (en) 2012-11-30 2019-02-12 Sio2 Medical Products, Inc. Controlling the uniformity of PECVD deposition on medical syringes, cartridges, and the like
US11066745B2 (en) 2014-03-28 2021-07-20 Sio2 Medical Products, Inc. Antistatic coatings for plastic vessels
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US11624115B2 (en) 2010-05-12 2023-04-11 Sio2 Medical Products, Inc. Syringe with PECVD lubrication
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