Correction - Vertically aligned boron-doped diamond nanostructures as highly efficient electrodes for electrochemical supercapacitors

At a Glance

Metadata	Details
Publication Date	2024-01-01
Journal	Journal of Materials Chemistry A
Authors	Shradha Suman, Dhananjay K. Sharma, Ondrej Szabó, Benadict Rakesh, Marián Marton
Institutions	Academy of Scientific and Innovative Research, Czech Academy of Sciences, Institute of Physics
Citations	2
Analysis	Full AI Review Included

Technical Documentation & Analysis: Boron-Doped Diamond Nanostructures for Supercapacitors

Executive Summary

This correction notice details the precise methodology for synthesizing and structuring Boron-Doped Diamond (BDD) films for use as highly efficient electrochemical supercapacitor electrodes. The research validates the use of MPCVD diamond films for high-performance energy storage applications.

Feature	Detail	Value Proposition for 6CCVD Clients
Core Application	Electrochemical Supercapacitors	High surface area, superior chemical stability, and fast charge transfer kinetics inherent to BDD.
Material Synthesis	LA MW CVD (SCIA cube 300)	Demonstrates successful scaling and control of both Microcrystalline (BMCDp) and Ultra-Nanocrystalline (BUNCDp) BDD films.
Doping Control	Trimethyl Borate (TMBT) source	Achieved extremely high B/C ratios (up to 328,000 ppm), critical for optimizing electrical conductivity.
Structuring Method	Au Nanodroplet Masking + RIE	Confirms compatibility of 6CCVD diamond films with standard semiconductor fabrication techniques (metalization, plasma etching).
Key Parameters	Low temperature (600 °C) growth	Enables integration onto various substrates and minimizes thermal stress during deposition.

Technical Specifications

The following parameters were extracted from the corrected methodology sections detailing the preparation and fabrication of the BDD electrodes.

Parameter	Value	Unit	Context
Substrate Annealing Temp	1000	°C	Pre-treatment of Alumina (Al₂O₃) substrate
Nanodiamond Seed Size	5	nm	Used for ultrasonic nucleation
Growth Temperature	600	°C	Substrate temperature during LA MW CVD
Growth Pressure	30	Pa	Pressure during BDD film deposition
Growth Time	30	h	Total duration of BDD film growth
CO₂ / H₂ Ratio	0.2	%	Gas mixture ratio
B/C Ratio (BMCDp)	312,500	ppm	Boron concentration for Microcrystalline Diamond
B/C Ratio (BUNCDp)	328,000	ppm	Boron concentration for Ultra-Nanocrystalline Diamond
Au Mask Thickness	8	nm	Deposited layer for self-organized masking
H₂ Plasma Heat Treatment	500	°C	Used to form Au nanodroplets
RIE Etching Gas Ratio	60/3 (5% CF₄)	sccm	O₂ / CF₄ flow rates
RIE Etching Pressure	150	mTorr	Pressure during Reactive Ion Etching
RIE RF Power	150	W	Power applied during etching
RIE Etching Time	6	min	Duration of nanostructure fabrication

Key Methodologies

The fabrication process involved two distinct phases: high-quality BDD film growth and subsequent nanostructuring via plasma etching.

1. Preparation of BDD Films (LA MW CVD)

Substrate Preparation: Alumina (Al₂O₃) substrates were cleaned (NH₄OH/H₂O₂) and annealed at 1000 °C for 1 h.
Nucleation: Substrates were ultrasonically treated in a suspension of 5 nm nanodiamond powder.
Growth Setup: Linear Antenna MW CVD (SCIA cube 300) was used.
Gas Mixture: H₂ / TMBT / CO₂ mixture, maintaining a CO₂ to H₂ ratio of 0.2%.
Doping Control: Trimethyl borate (TMBT) flow was varied (1% for BMCDp, 4% for BUNCDp) to achieve high B/C ratios (312,500 ppm to 328,000 ppm).
Conditions: Substrate temperature maintained at 600 °C and pressure at 30 Pa for 30 h.

2. Fabrication of BDD Nanostructures (RIE)

Metalization: An 8 nm thick Au layer was deposited onto the BDD films.
Mask Formation: The Au-coated films were heat treated in H₂-based microwave plasma at 500 °C for 10 min, resulting in self-organized Au nanodroplets acting as the etching mask.
Plasma Etching: Reactive Ion Etching (RIE) was performed using a capacitive coupled plasma system (Phantom III).
Etching Parameters: O₂/CF₄ gas mixture (60/3 sccm), 150 mTorr pressure, and 150 W RF power for 6 min.
Mask Removal: Residual Au nanodroplets were removed using a standard wet chemical etch (HNO₃ : HCl at 1:3 n/n).

6CCVD Solutions & Capabilities

This research highlights the critical role of highly doped, structured diamond films in next-generation electrochemical devices. 6CCVD is uniquely positioned to supply the foundational materials and custom processing required to replicate and advance this work.

Applicable Materials

To achieve the high conductivity and structural control demonstrated in this paper, 6CCVD recommends the following materials from our catalog:

6CCVD Material	Description & Application Match	Customization Potential
Heavy Boron-Doped PCD (BDD)	Required for high electrochemical activity and low resistivity (matching the 300,000+ ppm B/C ratios). Available in thicknesses from 0.1 µm up to 500 µm.	Custom resistivity tuning (Ω-cm) is standard.
Ultra-Nanocrystalline Diamond (UNCD)	Suitable for replicating the BUNCDp structure, offering high grain boundary density for enhanced surface area and doping uniformity.	Available on various substrates (e.g., Si, Al₂O₃, Mo) up to 125mm diameter.
Polished PCD Wafers	For applications requiring precise lithography or RIE uniformity, 6CCVD offers inch-size PCD polished to Ra < 5nm.	Ensures optimal adhesion and pattern transfer for subsequent nanostructuring steps.

Customization Potential

The fabrication process relied heavily on precise metalization and compatibility with plasma etching. 6CCVD offers comprehensive in-house services to streamline the research and development cycle:

Custom Metalization: We offer internal deposition of the required masking materials, including Au, Ti, Pt, and Pd, eliminating the need for external processing steps. We can deposit the 8 nm Au layer or multi-layer stacks (e.g., Ti/Pt/Au) directly onto the BDD film.
Custom Dimensions: While the paper did not specify size, 6CCVD can provide custom plates and wafers up to 125mm (PCD) or custom-cut SCD pieces, ensuring scalability for pilot production or large-area research.
Thick Substrates: For robust electrode designs, 6CCVD can supply thick diamond substrates (up to 10mm) for mechanical stability or heat dissipation.
RIE Compatibility: Our MPCVD films are grown under highly controlled conditions, ensuring low defect density and high purity, which is essential for uniform and repeatable Reactive Ion Etching (RIE) processes.

Engineering Support

6CCVD’s in-house PhD team specializes in the material science of diamond growth and processing. We can assist clients replicating or extending this research on Electrochemical Supercapacitors by providing:

Doping Optimization: Consultation on selecting the optimal B/C ratio and film morphology (microcrystalline vs. nanocrystalline) to maximize specific capacitance and cycle life.
Process Integration: Guidance on integrating 6CCVD materials into existing RIE or lithography workflows, including recommendations for plasma chemistries and mask materials.
Global Logistics: Global shipping is available (DDU default, DDP available) to ensure rapid delivery of custom materials worldwide.

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

View Original Abstract

Correction for ‘Vertically aligned boron-doped diamond nanostructures as highly efficient electrodes for electrochemical supercapacitors’ by Shradha Suman et al. , J. Mater. Chem. A , 2024, https://doi.org/10.1039/D3TA07728D.

Tech Support

Original Source

DOI: https://doi.org/10.1039/d4ta90146k