Modified MAX Phase Synthesis for Environmentally Stable and Highly Conductive Ti₃C₂ MXene
MXenes are a family of two-dimensional (2D) transition-metal carbides, nitrides, and carbonitrides. They have attracted major attention because of their excellent electrical conductivity, tunable surface chemistry, high mechanical strength, and ability to disperse easily in water. These properties make MXenes ideal for applications such as:
energy storage (batteries, supercapacitors)
EMI shielding
sensors
composites
biomedical technologies
catalysis
Among all MXenes, Ti₃C₂Tₓ is the most widely used and studied. It has some of the highest conductivity reported for solution-processed 2D materials, making it important for future electronic, energy, and composite technologies.
However, one of the biggest limitations of Ti₃C₂Tₓ, and MXenes generally, is that they oxidize quickly, especially when stored as water-based suspensions. Even freshly made Ti₃C₂Tₓ typically lasts:
1–2 weeks in water
sometimes only a few days for some compositions
even as powders, they degrade over time
Oxidation leads to loss of conductivity, structural breakdown, formation of TiO₂, and complete loss of MXene performance.
This study focuses on solving that problem.
2. What the Researchers Discovered
The researchers found a surprisingly simple and effective way to dramatically increase the stability of Ti₃C₂ MXene:
They added extra aluminum during MAX phase synthesis.
This modified synthesis produces a better MAX precursor called Al-Ti₃AlC₂, which leads to:
MXene flakes with far fewer defects
much more ordered MAX crystal structure
smoother MXene edges
significantly reduced vacancy defects
higher flake quality
outstanding oxidation resistance
As a result, Ti₃C₂Tₓ MXene produced from Al-Ti₃AlC₂ (called Al-Ti₃C₂) has:
over 10 months of shelf life in water (versus 1–2 weeks normally)
much higher conductivity (up to 20,000 S/cm)
oxidation starts 100–150 °C later than normal Ti₃C₂
stronger thermochemical stability
extremely clean, defect-free flake edges
This is a breakthrough that can allow MXenes to finally be used reliably and commercially.
3. Why Adding Extra Aluminum Helps
Traditionally, MAX phases (the precursors of MXenes) are made using precise stoichiometric ratios. Scientists previously assumed that phase-pure MAX would produce the best MXene.
However, this study overturns that assumption.
When you add extra aluminum (Al) during the MAX synthesis:
a molten aluminum phase forms during high-temperature sintering
molten Al increases diffusion rates of atoms
this helps Ti, C, and Al atoms arrange in a more ordered structure
the final MAX grains have better crystallinity and fewer defects
Even though the extra Al introduces intermetallic impurities, those impurities can be easily washed away with HCl.
The end result is a higher quality MAX crystal, and therefore, a higher quality MXene after etching.
4. Characterization of the Modified MAX (Al-Ti₃AlC₂)
4.1 XRD Analysis
The X-ray diffraction showed:
initial impurities like TiAl₃
but after HCl washing, these impurities disappear
the MAX phase peaks remain, indicating a purified structure
4.2 Raman Spectroscopy
Raman data revealed:
slight shifts in vibrational modes
broader Al-related vibrational peaks
signals that the Al layer environment has changed
evidence for improved structural ordering
4.3 SEM Imaging
SEM images showed:
large, clean, well-formed hexagonal grains
smooth surfaces
better grain geometry than conventional MAX
These observations confirm that the molten Al improved the grain formation.
5. Producing MXene from the Modified MAX: Al-Ti₃C₂
After washing the MAX, the authors etched it using HF/HCl and delaminated it using LiCl, following standard MXene protocols.
The resulting MXene flakes:
kept the clean hexagonal shape of the MAX
had smoother edges compared to conventional Ti₃C₂
showed fewer defects and pinholes
had cleaner basal planes
were highly dispersible in water
TEM images clearly showed that the Al-Ti₃C₂ flakes have dramatically reduced defects, particularly at the edges.
This is a major reason for the improved stability.
6. Record-Breaking Conductivity
Typically, Ti₃C₂Tₓ MXene films have conductivities between 8,000 and 15,000 S/cm.
But films made from Al-Ti₃C₂ reached:
> 20,000 S/cm — the highest conductivity ever reported for solution-processed 2D materials.
This improvement comes from:
fewer defects
better flake alignment
improved crystallinity
smoother edge geometry
This makes Al-Ti₃C₂ one of the most electrically conductive 2D materials available today.
7. Dramatically Improved Oxidation Stability
7.1 TGA Data
Thermogravimetric analysis showed:
conventional Ti₃C₂ oxidizes early and rapidly
Al-Ti₃C₂ resists oxidation 150 °C longer
Al-Ti₃C₂ powder oxidizes much more slowly
delaminated Al-Ti₃C₂ films resist oxidation up to 450 °C, much higher than usual
Why this matters
MXene was previously unusable in environments above 200 °C.
Now, applications like:
high-temperature electronics
sensors near engines
hybrid composites
thermal devices
can become feasible.
8. Extraordinary Long-Term Shelf Stability
The most remarkable result is that Al-Ti₃C₂ solutions remain stable for more than 10 months at room temperature with minimal protection.
Normal Ti₃C₂ lasts:
1–2 weeks, even under careful storage
sometimes only a few days for M₂C phases
How the samples were stored
Degassed with argon
Put into sealed vials
Stored in a drawer at room temperature
No freezer, no antioxidant additives, no special handling
UV-Vis tracking
Over 10 months:
concentration barely changed
spectral red-shift was minimal
optical features remained stable
no significant degradation appeared until after ~6 months
even after 10 months, almost no TiO₂ particles were detected
Conductivity after aging
Films made from:
4-month-old solution → >10,000 S/cm
6-month-old solution → >6,000 S/cm
10-month-old solution → still showed low oxidation and minimal pinholes
This performance is unprecedented.
9. Why Al-Ti₃C₂ Is So Much More Stable
The researchers propose several reasons:
9.1 Fewer defects
Traditional MAX synthesis introduces vacancies:
Al monovacancies (VAl)
Al divacancies
divacancies involving Al and C
These turn into defects in MXene after etching.
But adding extra Al reduces these vacancies, leading to:
better Ti:C stoichiometry
fewer weak spots
stronger MXene lattice
improved resistance to hydrolysis and oxidation
9.2 Cleaner edges
Oxidation begins at edges and defects.
The improved MXene has:
smoother edges
no rough protrusions
fewer pinholes
fewer reactive sites
9.3 Lower oxygen content in MAX
XPS showed reduced oxygen in the MAX, which means:
fewer oxycarbides
less initial oxidation
cleaner Ti–C bonding
higher quality flakes
Together, these features make Al-Ti₃C₂ inherently more stable.
10. Implications for MXene Production
This study fundamentally changes how scientists view MAX synthesis:
Before:
MAX phase purity was thought to be the most important factor.
Now:
Crystal ordering
Stoichiometry
Defect density
Bond uniformity
are much more important.
Adding excess Al might initially seem counterproductive because it introduces impurities.
However:
those impurities are removable
the improved structural ordering remains
the resulting MXene is dramatically better
This will likely reshape future MXene synthesis protocols.
11. Industrial and Commercial Impact
The improvements in MXene stability and conductivity make large-scale applications far more realistic:
1. Energy storage devices
MXene electrodes that stay stable for months instead of days.
2. Conductive inks
Long-lasting suspensions that can be shipped globally without degrading.
3. EMI shielding coatings
More durable films for aerospace and telecom applications.
4. High-temperature electronics
MXenes that withstand >400 °C.
5. Sensors
More reliable environmental and chemical sensors.
6. Composites
Better reinforcement for metals, polymers, and ceramics.
This study could accelerate MXene commercialization by several years.
12. Conclusion
This groundbreaking research shows that:
Modifying the MAX phase synthesis by adding excess aluminum dramatically enhances the structural quality of Ti₃AlC₂.
The resulting MXene (Al-Ti₃C₂) has far better stability, much higher conductivity, and greater resistance to oxidation.
Al-Ti₃C₂ MXene remains stable for over 10 months, a record for aqueous MXene suspensions.
Conductivity can reach 20,000 S/cm, the highest for any solution-processed 2D material.
Oxidation resistance increases by more than 150 °C.
This work will enable MXenes to transition from laboratory research materials into reliable industrial materials.
Overall, the study provides a major step forward toward making MXenes practical for real-world technologies.
