The Dependence of Boron Concentration in Diamond Electrode for Ciprofloxacin Electrochemical Sensor Application

At a Glance

Metadata	Details
Publication Date	2023-06-08
Journal	Indonesian Journal of Chemistry
Authors	Ilmi Nur Indriani Savitri, Prastika Krisma Jiwanti, Ilmanda Zalzabhila Danistya Putri, Irkham Irkham, Yasuaki Einaga
Institutions	Indian Institute of Technology Roorkee, Padjadjaran University
Citations	6
Analysis	Full AI Review Included

Technical Documentation & Analysis: High-Performance BDD Electrodes for Electrochemical Sensing

Reference Paper: The Dependence of Boron Concentration in Diamond Electrode for Ciprofloxacin Electrochemical Sensor Application

Executive Summary

This study validates the critical role of precise boron doping in MPCVD diamond for high-sensitivity electrochemical sensor applications, directly aligning with 6CCVD’s core material expertise.

Material Validation: Microwave Plasma-Assisted Chemical Vapor Deposition (MPCVD) Boron-Doped Diamond (BDD) electrodes were successfully utilized as highly effective electrochemical sensors for Ciprofloxacin (CIP) detection.
Doping Optimization: The research definitively proves that higher boron concentration (1% B/C ratio) significantly improves sensor performance, achieving superior electrochemical reactivity and signal response.
Ultra-Low Detection Limit: The 1% BDD electrode achieved an ultra-low Limit of Detection (LOD) of 0.17 µM, demonstrating high sensitivity suitable for detecting trace antibiotic residues in complex matrices.
High Material Purity: Raman spectroscopy confirmed the high quality of the MPCVD films, verifying the absence of sp² carbon impurities, which is essential for stable, low-background current electroanalysis.
Robust Performance: The developed BDD sensor method showed excellent precision (%RSD < 3.23%) and high accuracy (%Recovery 85-110%) when analyzing real-world samples (pharmaceuticals, wastewater, and milk).
Strategic Insight: The findings provide crucial data for engineers designing next-generation quinolone antibiotic detection devices, emphasizing the necessity of tightly controlled, heavy boron doping.

Technical Specifications

The following hard data points were extracted from the research, highlighting the performance metrics achieved using optimized BDD electrodes.

Parameter	Value	Unit	Context
Deposition Method	MPCVD	N/A	Microwave Plasma-Assisted CVD
Substrate Material	Silicon Wafer (111)	N/A	Base for BDD film growth
Optimal Boron Concentration	1.0	% (B/C ratio)	Highest sensitivity achieved
Limit of Detection (LOD)	0.17	µM	Best result (1% BDD)
Limit of Quantitation (LOQ)	0.59	µM	Best result (1% BDD)
Linear Concentration Range	30-100	µM	Ciprofloxacin detection
Signal/Background (S/B) Ratio	16.90	N/A	Highest performance (1% BDD)
Sensitivity (1% BDD)	0.379	µM/µA	Slope of calibration curve
Potential Window (CV)	-2.5 to 2.5	V	Measured in 0.1 M H₂SO₄
Electrochemical Technique	SWV	N/A	Square Wave Voltammetry
Electrode Diameter	0.5	cm	Working electrode dimension
%Recovery Range	85-110	%	Accuracy in real samples

Key Methodologies

The following steps outline the critical parameters used in the synthesis and characterization of the BDD electrodes:

BDD Synthesis: Boron-Doped Diamond films were deposited on Si (111) wafers using a commercial Microwave Plasma-Assisted Chemical Vapor Deposition (MPCVD) system (CORNES Technology Corp, Model AX6500X).
Deposition Parameters: A fixed deposition time of 6 hours was used for all samples.
Doping Control: Three distinct BDD electrodes were prepared by controlling the ratio of boron and carbon sources to achieve nominal boron concentrations of 0.1%, 0.5%, and 1.0% (B/C ratio).
Structural Characterization: Raman spectroscopy (532 nm excitation) was performed at room temperature to confirm the presence of high-quality sp³ diamond (peaks near 1331 cm^-1) and verify the absence of sp² carbon impurities (no peaks near 1500 cm^-1).
Electrochemical Pretreatment: Prior to sensing, electrodes were electrochemically pretreated using Cyclic Voltammetry (CV) for 40 cycles in an aqueous solution of 0.1 M H₂SO₄, scanning a wide potential range from -2.5 V to 2.5 V.
Sensing Conditions: Electrochemical measurements were conducted using a three-electrode cell setup (BDD working, Ag/AgCl reference, Pt mesh counter) utilizing Square Wave Voltammetry (SWV) in 0.1 M Phosphate Buffered Saline (PBS) at the optimal pH of 7.

6CCVD Solutions & Capabilities

The successful implementation of high-performance electrochemical sensors relies entirely on the quality and precise control of the BDD material. 6CCVD is uniquely positioned to supply and enhance the materials required to replicate and advance this research.

Applicable Materials for Electrochemical Sensors

The research confirms that high boron concentration is paramount for achieving metal-like conductivity and superior sensitivity. 6CCVD recommends the following materials:

Heavy Boron-Doped Polycrystalline Diamond (PCD): Ideal for large-area electrochemical applications requiring high conductivity (approaching 10²⁰ B atoms/cm³ or 1% B/C ratio equivalent). Our PCD offers exceptional uniformity and stability, crucial for reproducible sensor arrays.
Boron-Doped Single Crystal Diamond (SCD): For applications demanding the highest structural purity and lowest background current, our SCD material provides unparalleled control over defect density and doping profile, ensuring maximum electrochemical window stability.
Custom Doping Profiles: 6CCVD specializes in tailoring boron doping levels across the entire range (from lightly doped insulating to heavily doped metal-like) to meet specific conductivity requirements, allowing researchers to explore B/C ratios beyond the 1% tested in this study.

Customization Potential & Manufacturing Scale

The paper utilized small (0.5 cm diameter) electrodes cut from Si wafers. 6CCVD offers the capability to scale and customize these components for commercial or advanced research purposes:

Requirement from Paper	6CCVD Capability & Advantage
Small Diameter Electrodes	Precision Laser Cutting: We provide custom laser cutting services to achieve precise electrode geometries and dimensions (e.g., 0.5 cm diameter) from larger wafers.
BDD on Substrates	Large-Area Deposition: We offer BDD films on substrates up to 125mm in diameter (PCD), enabling the fabrication of high-throughput sensor arrays or larger working electrodes.
Electrode Contacts	Internal Metalization Services: We provide robust electrical contact layers (Au, Pt, Ti, W, Cu) directly deposited onto the BDD surface, ensuring low-resistance contacts necessary for reliable voltammetry measurements.
Film Thickness	Thickness Control: We supply BDD films with precise thickness control, ranging from 0.1 µm to 500 µm, allowing optimization for specific electrochemical mass transport kinetics.
Surface Finish	Ultra-Smooth Polishing: Our polishing services achieve surface roughness (Ra) < 5nm for inch-size PCD, minimizing surface defects that can contribute to background current noise.

Engineering Support

The optimization of the B/C ratio, as demonstrated in this paper, is a complex material science challenge. 6CCVD provides comprehensive support:

Doping Optimization Consultation: Our in-house PhD team specializes in MPCVD diamond growth and can assist researchers in selecting the optimal doping concentration and profile to maximize sensitivity and minimize LOD for similar quinolone antibiotic detection projects.
Electrochemical Expertise: We offer technical guidance on material selection for specific electroanalytical techniques (CV, SWV, DPV) and complex matrix analysis (wastewater, biological fluids).
Global Logistics: We ensure reliable, global shipping (DDU default, DDP available) of sensitive diamond materials, supporting international research collaborations.

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

View Original Abstract

This study investigates the effects of boron concentration on boron-doped diamond (BDD) electrodes for electrochemical sensors of ciprofloxacin. The effects of boron concentration, scan rate, and pH of BDD electrodes with boron concentrations of 0.1, 0.5, and 1% were examined to determine the optimal conditions. Furthermore, square wave voltammetry (SWV) in phosphate buffer pH 7 was used to analyze the electrochemical behavior of ciprofloxacin. The results revealed a linear calibration curve in the concentration range of 30-100 μM with a recovery of 85-110%. Meanwhile, BDD electrode with the highest boron concentration in this experiment (1%) showed a very low limit of detection of 0.17 μM, meaning that 1% BDD gave a highly sensitive and significant measurement result for the electrochemical sensor of ciprofloxacin. With the results given, this study provides new insights for controlling boron concentrations in diamond electrodes for the electrochemical sensors of quinolone antibiotics.

Tech Support

Original Source

DOI: https://doi.org/10.22146/ijc.82135