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Ultra-hydrophilic Diamond-like Carbon Coating on an Inner Surface of a Small-diameter Long Tube with an Amino Group by AC High-voltage Plasma Discharge

MetadataDetails
Publication Date2023-06-15
JournalJournal of Photopolymer Science and Technology
AuthorsYuichi Imai, Hiroyuki Fukue, Tatsuyuki Nakatani, Shinsuke Kunitsugu, Noriaki Kuwada
InstitutionsIndustrial Technology Center of Okayama Prefecture, Kawasaki Medical School
Citations1
AnalysisFull AI Review Included

Technical Documentation & Analysis: Ultra-hydrophilic Diamond-like Carbon Coating

Section titled “Technical Documentation & Analysis: Ultra-hydrophilic Diamond-like Carbon Coating”

This research successfully demonstrates a robust, dry-coating method for creating ultra-hydrophilic, positively charged biomimetic surfaces on small-diameter medical tubing using Diamond-Like Carbon (DLC) and subsequent ammonia (NH3) plasma treatment.

  • Core Achievement: AC high-voltage plasma CVD followed by NH3 plasma treatment reduced the water contact angle (WCA) from 83.3° (DLC only) to an ultra-hydrophilic 12.2° in pure water.
  • Surface Potential Control: The process successfully shifted the surface zeta potential to a highly positive value (+20.7 ± 4.5 mV), attributed to the introduction of primary amino groups (-NH2).
  • Biomimetic Application: Controlling both hydrophilicity and positive surface charge is critical for inhibiting biofilm adhesion and thrombosis in advanced medical devices (catheters, vascular grafts).
  • Methodology: The two-step process utilized AC high-voltage burst plasma deposition (CH4 source) followed by NH3 plasma modification, demonstrating precise control over surface chemistry (C:N:O ratio).
  • 6CCVD Relevance: While the paper focuses on DLC, 6CCVD provides the highest quality MPCVD diamond substrates (SCD/PCD/BDD) essential for next-generation biomedical devices and high-purity plasma processing equipment components.
  • Sales Driver: This work highlights the need for advanced, high-purity carbon materials and precise surface engineering, areas where 6CCVD excels with custom material specifications and metalization services.

The following hard data points were extracted from the experimental results and deposition parameters:

ParameterValueUnitContext
DLC Deposition MethodAC High-voltage Plasma CVDN/AInner surface coating
Deposition GasCH4N/ACarbon source
Working Pressure36.2PaDuring DLC deposition
AC Voltage5kVPlasma power supply
Offset Voltage2kVPlasma power supply
Initial WCA (DLC only)83.3°Before NH3 plasma treatment
Final WCA (20s NH3 plasma)12.2°Ultra-hydrophilic surface
Zeta Potential (DLC only)+4.2mVPositively charged surface
Zeta Potential (5s NH3 plasma)+20.7 ± 4.5mVHighly positive surface charge
Primary Surface Bond (XPS)C-C, C-HN/A71.2 at% (DLC component)
Amide Bond Content (XPS)15at%Estimated surface concentration (-NHCO-)
Amino Group Content (XPS)5at%Estimated surface concentration (-NH2)
XPS Analysis Depth2 to 6nmSurface layer analysis

The experiment utilized a two-step dry coating process involving AC high-voltage burst plasma CVD for film deposition, followed by surface modification using NH3 plasma discharge.

  1. DLC Film Deposition (AC High-Voltage Plasma CVD):

    • Equipment: AC high-voltage plasma CVD system utilizing an IWATSU SG-4105 voltage generator and NF Corporation HVA4321 amplifier (1000x amplification).
    • Substrate: 0.15 ”m thick Polyurethane (PU) sheets (25 mm x 7 mm) encapsulated within silicone tubes (e.g., ID5 mm x OD7 mm x L100 mm).
    • Parameters: CH4 gas flow rate of 96.2 sccm, 5 kV AC voltage, 2 kV offset voltage, and 20 min deposition time.
    • Result: Formation of an amorphous carbon DLC thin film on the inner surface of the tube.
  2. Surface Modification (NH3 Plasma Treatment):

    • Process: Plasma discharge performed under NH3 gas distribution after DLC deposition.
    • Parameters: Constant NH3 gas flow rate of 96.2 sccm.
    • Duration: Varied from 5, 10, 20, 30, and 60 s to optimize surface properties.
    • Result: Introduction of nitrogen-containing functional groups (-NH2, O=C-N) leading to ultra-hydrophilicity and positive zeta potential.
  3. Characterization:

    • Hydrophilicity: Measured using a Dropmaster 500 to determine the pure water contact angle (1.5 ”L distilled water droplet).
    • Surface Potential: Measured using an ELSZ-1000 zeta-potential-measuring device, analyzing electroosmotic flow.
    • Chemical Bonding: Investigated using X-ray Photoelectron Spectroscopy (XPS) with an Al-K source (1486.6 eV) and pseudo-Voigt function fitting (R2 > 0.995).

This research demonstrates the critical role of advanced carbon materials and precise plasma processing in developing next-generation biomedical surfaces. 6CCVD is uniquely positioned to supply the high-purity diamond materials and custom engineering required to replicate or extend this work into high-performance applications.

To advance research requiring controlled surface potential, high stability, and biocompatibility beyond amorphous DLC, 6CCVD recommends the following MPCVD diamond materials:

  • Boron-Doped Diamond (BDD): Essential for applications requiring precise electrochemical control and stable surface potential. BDD electrodes offer superior stability and wide potential windows compared to traditional carbon materials, ideal for advanced biosensors or in vivo sensing components.
  • Optical Grade Single Crystal Diamond (SCD): For plasma CVD systems requiring high-purity, robust optical windows or viewports that must withstand harsh plasma environments (like the AC high-voltage discharge used here). 6CCVD offers SCD up to 500 ”m thick with Ra < 1 nm polishing.
  • Polycrystalline Diamond (PCD) Wafers: Suitable for large-area deposition tooling or substrates where high thermal conductivity and chemical inertness are required in the plasma reactor environment. 6CCVD offers PCD plates up to 125 mm diameter.

The paper utilized specific, small-scale PU sheets and silicone tubes. 6CCVD’s manufacturing capabilities allow researchers to scale up or customize substrates for complex reactor geometries:

Research Requirement6CCVD CapabilitySpecification Range
Custom Substrate DimensionsPrecision laser cutting and shaping of diamond plates/wafers.Plates/wafers up to 125 mm (PCD).
Thickness ControlSCD and PCD materials available in ultra-thin to thick formats.SCD/PCD from 0.1 ”m up to 500 ”m.
Surface FinishUltra-smooth surfaces are critical for minimizing friction and maximizing uniformity in medical applications.Polishing to Ra < 1 nm (SCD) and Ra < 5 nm (Inch-size PCD).
Surface ModificationInternal metalization services for creating custom contacts or bonding layers on diamond substrates.Au, Pt, Pd, Ti, W, Cu metalization available.

The successful control of hydrophilicity and zeta potential relies heavily on precise material selection and plasma parameters. 6CCVD’s in-house PhD team specializes in the physical and chemical properties of CVD diamond and can assist with material selection for similar Biomimetic Surface Engineering and Advanced Plasma Processing projects.

We provide consultation on:

  • Optimizing diamond substrate orientation and doping levels (e.g., BDD concentration) for specific electrochemical or surface modification goals.
  • Designing custom diamond components (e.g., plasma reactor windows, high-power electrodes) that require extreme purity and durability.
  • Selecting the appropriate diamond grade (SCD vs. PCD) based on required thermal, optical, or mechanical performance.

Call to Action: For custom specifications or material consultation, visit 6ccvd.com or contact our engineering team directly.

View Original Abstract

Medical tubing includes artificial vascular grafts and catheters, each has a different purpose of use, but they both need to hydrophilize the lumen surface. Diamond-like carbon (DLC) is a dry coating technology, and its surface can be easily modified with hydrophilic functional groups. AC high-voltage plasma chemical vapor deposition has been developed for DLC deposition on the inner surface of small-diameter long tubes. In addition, oxygen plasma treatment of the DLC-deposited surface has been performed to enhance the hydrophilicity of the tube lumen and to inhibit biofilm adhesion in urinary catheters. However, the oxygen plasma treatment using silicone as the base material had only a slight inhibitory effect on biofilm adhesion, with a water contact angle of 104.4° for the DLC film and 90.6° for the DLC film, compared with oxygen plasma treatment, with an average value of 119.5° for the blank film. Recently, a new ammonia plasma treatment method has been developed, and an ultra-hydrophilic water contact angle of nearly 10° has been achieved with polyurethan (PU) as the base material. Furthermore, the zeta potential was found to be negative in oxygen plasma treatment and positive in ammonia plasma treatment, indicating that the hydrophilicity, and surface potential can be arbitrarily controlled by combining these plasmas, thereby achieving surface properties suitable for various applications.