Introduction:-
Light-emitting diodes (LEDs) have made an extensive contribution in
the modern era of lighting with their energy efficiency, high durability, and eco-friendliness.
Unlike conventional incandescent and fluorescent lighting, LEDs’ operation relies on
electroluminescence, where the electrical energy is directly converted into light, losing little
heat. Because of their high efficiency and fast development of materials and manufacturing
methods, LEDs have come to be the lighting choice for many cases of medium and large
lighting, such as general lighting, automotive headlights, displays, and medical equipment.
They can be widely adopted owing to superior durability and low power consumption relative
to conventional lighting sources and high brightness. LEDs developed in the early 20th
century, beyond that first century, have seen no significant development until the early 1960s
with the creation of practical semiconductor-based LEDs. In the 1990s, the invention of high-
brightness blue LEDs made it possible to create white LEDs from phosphor conversion. A
breakthrough, this allowed for an energy-efficient alternative to traditional sources of light.
LEDs are today leading the global lighting market, thanks to them being superior to others in
terms of performance, cost-effectiveness, and their application to most industries.
The LED industry is advancing rapidly, and with continuous research
undertaken on efficiency, longevity, and functionality. There are two such notable trends as
the integration of LEDs into smart and connected lighting systems. The IoT smart LEDs are
for automation, remote operation, and energy optimization of homes, offices, and public
spaces. The development of Micro-LED and Mini-LED displays is also becoming another
trend that holds much potential by reducing the screen’s brightness, contrast, and power
consumption. For the next generation of televisions, smartphones, and augmented reality
(AR) applications, these are very important advancements.
At the same time, human-centric lighting (HCL) is growing in
popularity, as the power of LED has increased to make the lighting imitate natural daylight
and assist with circadian rhythms. HCL systems change color temperature and intensity for
enhanced comfort, productivity, and well-being. In addition, there is an increasing use of UV-
C LEDs for disinfection and sterilization. Being able to inactivate bacteria and viruses, they
are perfectly suited for use in water purification, air filtration, and healthcare environments.
Development of phosphor materials has also been another key area of development, which
has increased the efficiency and color rendering of LEDs to the extent that they can be
utilized in ideal lighting solutions for high-quality.
The versatility and efficiency of the LEDs make them used for a large
number of applications. In general illumination, LEDs have almost completely displaced
incandescent and fluorescent bulbs for residential, commercial, and industrial lighting. LEDs
are used in the automotive industry for headlights, taillights as well as interior lighting,
because they are more visible and durable. The high-resolution display industry also utilizes
LED technology for televisions, smartphones, outdoor billboards, and others. LEDs are used
in medical applications in lighting, with surgery, phototherapy, and in diagnostic imaging
devices because of their highly precise illumination and heat generation. LED technology has
also been applied in agricultural applications such as controlling the lighting systems in
indoor farming as well as in greenhouse environments, helping to improve plant growth. At
the same time, LEDs are key components in optical communication systems, such as Li-Fi
(Light Fidelity), where light is used to transmit wireless data at very high (>1 Gbit/s)
bandwidths.
LED technology has continued to expand at a rapid pace in terms of its
innovations in the same order of magnitude, such that it has become an integral part of
modern life. Research and the development of LEDs will continuously rise in the upcoming
years, growing the LED innovation in lighting, display technologies, and communication
systems.
SrMgAl₁₀O₁₇ (SAM) is a widely and extensively studied aluminate-
based host material that is attractive for use as phosphors in lighting and display applications.
It is a β-alumina-type compound with a hexagonal crystal structure and space group
P6₃/mmc, consisting of spinel blocks and intermediate layers. The unique structure enables
cation substitution so that it is a useful host for luminescent materials. SAM's excellent
thermal and chemical stability makes it an ideal material for phosphor applications in its
applications of high power sources such as white light emitting diodes (WLEDs) and plasma
display panels (PDPs).
SrMgAl₁₀O₁₇ (SAM) can be doped with different activator ions (for
example Europium, Manganese, Chromium, and Cerium) to tailor its luminescent properties
for different applications. SAM doped with Mn²⁺ has green emission and can be used to
enhance the color rendering of lighting systems. Long-lasting phosphorescence makes it find
applications in display technologies, emergency lighting, and glow in the dark materials.
Nevertheless, SAM is known to emit deep red to far-red color emission with Cr³ ⁺ doping.
The photosynthesis efficiency in agriculture is aided by artificial lighting by SAM: Cr³⁺
phosphors, which are key for absorbing the red and far red wavelengths. SAM doped with
Ce³⁺ gives very efficient blue luminescence with good thermal and chemical stability. Thus,
it is a promising candidate in solid-state lighting, backlight display, and high-performance
optical applications. SAM shows versatility as a phosphor host to develop advanced lighting
and display technologies that are important to both consumer electronics and specialized
applications, such as horticultural lighting and long persistence phosphors.
Instrumentation:-
Analytical balances: Usually, ceramic laboratory balances are quite heavy, however, you
will be able to quantify the object's mass exactly. In scientific settings, the analytical balances
that are used most widely tend to have a readability of up to 0.0001 grams. As you can
imagine, the balance is very sensitive because it provides such precise measurements. In
order to protect the analytical balances from the outside factors that may disturb the balance
accuracy, draft shields are incorporated into analytical balances.
Magnetic stirrer: A commonly used laboratory device is the magnetic stirrer, which has a
rotating magnet or a stationary electromagnet to generate a rotating magnetic field. This field
provides a stir bar immersed in a liquid to spin rapidly, so it can provide efficient stirring or
mixing of a solution.
Beaker: A beaker is a Cylindrical container with a flat bottom, used in a laboratory. Most
beakers have spouts, otherwise known as beaks, that are so small, they are able to pour from.
However, they are usually made from glass (borosilicate glass). Beakers come in various
sizes and are used to hold liquid or solid samples. They may be used as containers for
chemical reactions.
China dish: A China dish, also known as an evaporating dish, is a type of glazed porcelain
vessel available in many different sizes. It is thick, gives great insulation, and can endure high
temperatures. For laboratory uses, it is commonly used for the burning of solutions and
evaporation processes.
Vertical furnace: High-temperature vertical furnace is a specific heating device employed
for combustion synthesis, material processing, as well as high-temperature reactions. It is
intended to operate at elevated temperatures up to 1600°C, depending on the application, but
is generally between 500°C and 1600°C.
Muffle furnace: High temperature treatment, above 500°C, is employed in the muffle
furnace for the removal of volatiles, improvement of crystallinity, and stability of the
material. The ash-like product is then ground and heated at 900°C for 12-16 hours to aid
phase formation and impurity removal.
Synthesis Methods:-
The synthesis of extremely pure substances, which are then analyzed and
characterized in a well-equipped physics lab that can go to over 1600°C, is all necessary in a
highly controlled chemical laboratory. The above classifies the purity of materials in terms of
ore (1%), technically pure (90%), chemically pure (99.9%), reagent grade (99.99%),
spectroscopically pure (99.999%), luminescence pure (99.9999%), and completely pure
(100%).
There are different ways of synthesizing phosphors, and each synthetic
method is chosen on the basis of the purpose of their use. It is difficult to create a single-
phase powder of many phosphor compositions that comprise more than four elements. The
synthesis process has significant effects on the resulting atomic structure, composition,
microstructure, defects and interfaces of these materials, and the luminescence properties,
which depend on all these properties are in turn dependent upon the thermodynamics and
kinetics of the synthesis process. Commonly used synthesis methods are solid state reactions,
sol-gel Pechini methods, co-precipitation, solvothermal methods, microwave assisted
techniques, sonochemical synthesis, combustion synthesis, etc. Among these particular
reaction methods, solid state reactions and solvothermal methods are particularly flexible
methods to synthesize all types of compounds.
Combustion Method:
The Combustion method is a wet chemical technique, and thus there is
no need for further calcinations of the sample and other repeated heating, resulting in a cost-
effective and energy-efficient process. It is an exothermic reaction that releases both heat and
light and produces the multi-constituent oxides rapidly. Solid state synthesis is usually
followed by this method, which gives products that are more chemically uniform, having
fewer impurities and a higher surface area than solid state synthesis.
It requires fuel and oxidizer, and metal nitrates are used as oxidizer and
urea the fuel. A highly exothermic reaction can be ignited by having the metal nitrates mixed
with fuel (such as urea or glycine) and aqueous solution and heated below 500°C, producing
a flame. This reaction occurs at temperatures in excess of 1200°C and lasts only a brief
period of less than ten minutes. Nanocrystalline powders can then be produced with a short
duration at high temperatures, giving superficially agglomerated, weaker, somewhat
submicron particles, but easily ground to finer powders. The proper balance of the fuel and
oxidizer is important to get the most heat produced during synthesis.
The Sr(1-x)MgAl10O17:REx (RE=Mn, Ce, Cr) phosphors were synthesized
by the Solution Combustion method. In this process, the starting materials taken were
Strontium nitrate anhydrous [Sr(NO3)2] (98%), Magnesium nitrate hexahydrate
[Mg(NO3)2.6H2O] (98%), and Aluminium nitrate nonahydrate [Al(NO3).9H2O] (98.5%). Then
weighted quantities of each were dissolved in DDW using magnetic stirrer. Then the rare
earth dopants, all in nitrate form, were added individually to the above solution. After that,
Urea was added as a fuel and stirred continuously using a magnetic stirrer to obtain a
homogeneous mixture. The prepared solution was then transferred to a preheated vertical
furnace maintained at 550 °C. The combustion reaction occurred within a few minutes,
giving fluffy, voluminous powder. The obtained powders were collected, ground gently, and
then annealed at 900 °C for 12 to 18 hours. Thus, the final product Sr 1-xRExMgAl10O17 is
obtained .
Characterization Technique:-
Photoluminescence (PL) Spectroscopy Analysis
It is known that photoluminescence (PL) spectroscopy is a powerful
analytical technique focusing on the emission of light after the materials absorb photons of
light. The use of this method results in an abundance of data which gives valuable electronic
structure information for a vast variety of materials from semiconductor or organic surfaces.
Researchers can study how the light emitted depends on such properties as energy levels, the
dynamics of recombination, and the presence of defects by analysing the light emitted.
Principle of Photoluminescence Spectroscopy:
For PL spectroscopy, the photoexcitation is the fundamental principle. If
a material is exposed to a light source such as a laser or UV lamp, photons are absorbed by
electrons, and they are promoted to excited states. Two principal radiative processes then
occur due to this excitation: fluorescence and phosphorescence. In fluorescence, the excited
electrons return almost instantly to their ground states and emit light almost instantaneously.
However, phosphorescence involves the electrons taking part in this delayed emission
process wherein they transition from a triplet state and subsequently demote back to their
equilibrium state.
Working of Photoluminescence Spectroscopy:
PL spectroscopy typically consists of several steps:
Excitation: Usually, a monochromatic light source like UV or visible laser is used to excite
the sample, and electrons of the sample are excited.
Emission: Excited electrons eventually drop back down to lower energy states by emitting
energy in the form of photons, and that is what constitutes the emitted light.
Detection: Light is collected and analyzed by means of a spectrometer. PL spectrum peaks
are produced by plotting the intensity of emitted light vs their wavelength, from which the
electronic structure and properties of the material can be inferred by the energy levels of the
material.
Because the material's intrinsic characteristics are not altered in this
technique, it is particularly suitable for the analysis of surfaces and interfaces without
affecting the material.
XRD:
XRD is a widely used analytical technique used to analyze materials
elemental structure. If the sample is crystalline, X-rays will be scattered by the atoms in the
crystal when shot through it. The scattering of the X-rays at specific angles depends on the
wavelength of the X-rays and the separation between the atomic planes in the crystal. By
recording these angles and intensities of these diffracted X-rays, that is, diffraction patterns,
we determine how the material is arranged, its unit cell size, and what phases are present.
Peak Position: The position of a peak in an XRD pattern indicates the electron spacing from
the diffracted lattice planes when the diffracted X-rays meet Bragg's Law.
Peak Intensity: The intensity of a peak is a measure of the number and distribution of the
scattering centres in the material. High electron density is indicated by sharp peaks, but the
overall electron density cannot be estimated from them.
Peak Width: This gives information on crystallite size, lattice strain and defects. For
instance, broad peaks mean smaller crystallites and thus higher strain or more defects.
Peak Shape: Peak shape depends upon the instrumental broadening, crystallite size, strain
and defects. If there are deviations from a symmetric shape, this might indicate some
structural issues caused by crystal imperfections, or phase mixing.
SEM:
The Scanning Electron Microscope (SEM) is a key material science and
nanotechnology instrumentation throughout the technique it is employed in, for making high
resolution articles of surfaces. SEM is different from the optical microscope, as it uses a fine
focused beam of electrons with their corresponding advantages: greater resolution and depth
of field. The ability to visualize surface structures at the nanometer scale makes SEM
particularly valuable for many applications: biological studies, materials analysis, and others.
Principle of Scanning Electron Microscope (SEM)
The basis of SEM is on the interaction between electrons and the
specimen’s surface. This technique produces a number of signals such as secondary electrons,
backscattered electrons, and the X-rays. In this case, these signals allow the sample
topography, composition, and other physical properties to be determined. Secondary electrons
that are emitted are principally used to form images of the sample surface morphology, with
backscattered electrons giving elemental composition information on the sample.
Working of Scanning Electron Microscope (SEM) :
The working mechanism of an SEM involves several key components:
Sample Preparation: Electronic Imaging methods require samples to be prepared in a
manner, usually to a thickness of 100–300 nm, which is then covered in a thin layer of
conductive material at the surface (typically gold) with good adhesion to ensure the minimum
charging of the sample. The preparation helps to reduce charge buildup on the surface during
the examination.
Electron Source: The source that emits electrons can be a tungsten filament or a field
emission gun. It is this source that beams electrons through a series of electromagnetic lenses
to produce the beam used.
Scanning Process: The focused electron beam is raster pattern scanned across the sample.
Electrons emitted as secondary and backscattered electrons are produced as they pass through
or hit the sample.
Detection and Imaging: Detectors, including a secondary electron detector (SED) for
topographical, and a backscattered electron detector (BSD) for compositional information,
collect the electron emissions. The data is then processed and the sample is displayed on a
monitor for real time analysis of the sample.
These employable elements available in combination in SEM make it an
imperative tool in numerous scientific and industrial fields to bring necessary knowledge as
to material properties and behaviour's at the microscopic levels.
FTIR:
Fourier Transform Infrared Spectroscopy (FTIR) is a well-known
analytical technique for the characterization of materials using the vibrational spectra. It
works according to infrared light, which investigates the absorptive characteristics of various
substances and indicates the molecular composition and structure. FTIR is a technique of
choice in many fields such as chemistry, biology, materials science and environmental studies
due its high sensitivity and the ability to analyse solid, liquid and gas samples.
Principle of FTIR:
The principle of FTIR spectroscopy is basic, namely, the molecular
vibration of a sample interacting with infrared light. Infrared radiation is a type of light
energy that, when a sample is exposed to, certain frequencies will be absorbed, which
encourages molecular bonds to vibrate. These vibrations are specific to certain functional
groups in the molecule at which distinctive absorption peaks occur. The factor determining
the analysis is the relationship between the frequency of the absorbed light and the energy
necessary to sustain these vibrational states.
Working Mechanism of FTIR:
FTIR operates through several key steps:
IR Source and Sample Interaction: The infrared source exposes the sample to a broad
spectrum of light. This radiation, which the sample absorbs, depends on its molecular
composition, absorbs specific wavelengths of the sample.
Interferometer: In FTIR, an interferometer is used instead of a conventional
monochromator, as in this, the light beam is split into two paths before recombining.
Constructive and destructive interference patterns are obtained that give rise to an
interferogram due to the difference in path length between these beams.
Fourier Transform: Basically, the Fourier transform of the recorded interferogram gives the
intensity of the light as a function of time. This data is a time domain data and thus, it is
converted into a Mathematical form known as the Fourier Transform, which converts said
data into a frequency spectrum and shows the specific wavelengths absorbed by the sample.
Spectrum Analysis: The absorption peaks originating from the vibrational modes of
functional groups in the sample are displayed in it. These peaks can be analyzed to give
molecular structure and functional group identification, thus providing qualitative and
quantitative analysis.
The combination of these principles and technology defines FTIR as a
very useful tool in many research and industrial operations for unravelling the detailed
composition and properties of materials.
Future scope:
Future prospects of SrMgAl10O17 (SAM) doped with Mn2+, Ce3+, and
Cr3+ for LED phosphors are promising in multiple end applications. In addition to enhancing
color rendering and thermal stability, Eu2+ degrades the output color of the LED
semiconductor. The narrow-band emissions of Mn2+ are also attractive for energy-efficient
lighting and for giving customized input spectra. As an efficient blue emitter, Ce3+ is
becoming a promising blue emitter that can be used for optimizing solid-state lighting
solutions. Advanced imaging and sensing technologies are dependent on Cr3+ ions for their
broadband near-infrared emission, which, if quenched thermally, is known to have minimal
influence. Overall, research and development in these dopants is ongoing and providing new
possibilities for energy-efficient high-performance LED lighting technologies for commercial
lighting to high-end sensor systems, thus heralding a new period in the LED market.
