Biomass Conversion and Biorefinery

https://doi.org/10.1007/s13399-021-01880-5

ORIGINAL ARTICLE

Development and evaluation of biochar‑based secondary

and micronutrient enriched slow release nano‑fertilizer for reduced
nutrient losses
Shaon Kumar Das1,2   · Goutam Kumar Ghosh2

Received: 27 July 2021 / Revised: 9 August 2021 / Accepted: 14 August 2021

© The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature 2021

Abstract
Four diverse biochars were impregnated into secondary and micronutrient solutions to develop slow release nano-fertilizer via
a three-step synthesis process and to verify the appropriateness of biochar as a support material for nutrient release patterns
to crops on a slow release basis. The nano range (8.33–24.33 nm), such as the structure of the synthesized nano-fertilizer,
was confirmed by a transmission electron microscope. It exhibited a nearly neutral pH (5.94–6.61) with adequate percent-
ages of C, H, N, and O. The developed nano-fertilizer showed an excellent water absorbency character (32.46–45.76%) hav-
ing a lower density (0.731–0.762 g ­cm−3). It represented excellent swelling (4.15–4.61%) capacity with a lower salt index
(0.04–0.07) and equilibrium water content (68–74%). It also augmented the soil water retention (42.47–53.16%) capacity
than commercial compound fertilizer (22.43%) and soil (19.52%) after 45 days which is very desirable for supplying water
under water stress conditions. It demonstrated lower ­Ca+2, ­Mg+2, ­Zn+2, ­Fe+2/+3, and ­Na2O release than commercial fertilizer,
representing its low release behavior. The nutrient release pattern study depicted that after 90 days, the concentration of C­ a+2
+2 +2 +2 +2
released 87.4–90.7%, ­Mg 81.8–85.3%, ­Na 96.2–99.1%, ­Fe 2.8–5.2%, and ­Zn 0.5–1.6%. Thus, among the mineral
nutrients, the leaching capacity was highest for ­Na2O followed by ­Ca+2 > ­Mg+2 > ­Fe+2/+3 > ­Zn+2. Besides, among the four
diverse biochars, the pine needle biochar showed the best nutrient retention/sorption capacity followed by Lantana camara,
black gram, and maize stalk biochars for slow release of C­ a+2, ­Mg+2, ­Fe+2/+3, and N
­ a2O nutrients. But exceptionally, Lantana
+2
camara biochar showed significant ­Zn nutrient retention/sorption capacity followed by pine needle, black gram, and maize
stalk biochars. Thus, feedstock types also manipulated the nutrient release pattern of the secondary and micronutrient from
the developed nano-fertilizer. Hence, biochar-based nano-fertilizer has a greater possibility to decrease nutrient leaching,
enhance water retention, and thus augment plant nutrient and water use efficiencies.

Keywords  Biochar · Secondary and micronutrients · Nutrient losses · Slow release · Nano-fertilizer

1 Introduction controlled-release fertilizers show great potential [2]. For

Controlled-release fertilizers are able to release nutrients
slowly, which tries to synchronize nutrient demand during
crop growth and supply of nutrients [1]. Thus, to improve
fertilizer use efficiency and to alleviate environmental
problems due to fertilizer application and management, the
* Shaon Kumar Das
shaon.iari@gmail.com
1
ICAR Research Complex for NEH Region, Sikkim Centre,
Gangtok, Sikkim 737102, India
2
Palli Siksha Bhavana, Visva Bharati, Sriniketan, Birbhum,
West Bengal 731236, India
delivering the plant nutrients, biochar can be used as an
interesting support material [3]. A novel controlled-release
fertilizer can be developed using biochar and polyvinylpyr-
rolidone (PVP) as coating materials and a waterborne copol-
ymer of polyvinyl alcohol (PVA) to enhance the effective-
ness of PVA-coated fertilizers [4]. For slow and prolonged
plant nutrient release, the use of biochar as a nutrient carrier
can be used due to its porous microstructure and high surface
area [5]. The highly porous structure and surface area make
biochar develop a biochar-based fertilizer that could increase
nutrient bioavailability; reduce leaching; and accordingly
crop growth parameters, biomass, and crop production and
productivity. N- and P-laden biochar could behave as a slow
release fertilizer [6]. The addition of biochar can increase

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polymer film degradability due to the fact that biochar is
able to sorb soil microorganisms [7]. Biochar-modified
waterborne polyacrylate materials prolong the nutrient
release period and enhance the mechanical strength, thereby
exhibiting a huge potential to improve waterborne polymer-
coated controlled-release fertilizers [8]. Biochar has the
capability to improve plant nutrient use efficiency through
enhancement in soil nutrient retention and via slow release
of nutrients according to plant requirements in conjunction
with chemical fertilizers for a longer period of time [9]. The
potential of biochar as a carrier of plant nutrients is enor-
mous in addition to the provision of essential nutrients as
enriched biochar [10]. N- and P-laden biochar could behave
as a slow release fertilizer. The formation of biochar-based
releases of nitrogen fertilizer between the reaction of nitro-
gen and lignocellulosic matrices using a chemical reaction
was studied [11]. To increase the nutrient concentrations
in biochar, biochar-ammonium phosphate is considered an
efficient method as an uncoated slow release fertilizer [12].
An already published report suggests the incorporation of
biochar into the soil as a biofertilizer after modification such
as encapsulation, pelletization, and the addition of one or
more nutrients either by a direct mixing process [13]. Slow
release fertilizers were developed based on cotton stalk
biochar using N ­ H4+ absorption on biochar, and these slow
release fertilizers (SRFs) showed the lowest N-leaching loss,
and it was due to the fact that it had better water holding
capacity and slow release characteristics than other normal
biochar [14]. To sequester C for a longer time and enhance
soil fertility in the soil, the phosphate-laden biochar con-
tained valuable nutrients which can act as a slow release
fertilizer [15]. Biochar impregnated with different second-
ary and micronutrient materials was utilized to design and
develop slow release nano-fertilizers to alleviate losses of
nutrients and enhance crop productivity [16–20]. The objec-
tive of this research paper was to develop and evaluate four
diverse biochar (MSB (maize stalk biochar), BGB (black
gram biochar), LCB (Lantana camara biochar), and PNB
(pine needle biochar))-based secondary nutrient (calcium,
magnesium) and micronutrient (zinc, iron) enriched slow
release environmentally friendly nano-fertilizer utilizing
biochar’s highly porous structure and surface area character
which could be easily available to plants and soil on a slow
release basis. Perhaps this was the first attempt using biochar
as a nutrient impregnation carrier for slow release nano-fer-
tilizer preparation. Such a technique will definitely not only
facilitate in biomass waste decrease but also promote pollu-
tion avoidance by alteration of biomass waste into valuable
creation and resolution of mineral nutrient leaching compli-
cations of conventional fertilizers. The detailed objectives of
the study were (a) developing secondary and micronutrient
enriched nano-fertilizer using biochar as a carrier through
impregnation followed by physicochemical characterization
13
Biomass Conversion and Biorefinery
of nano-fertilizer and (b) cumulative concentrations of nutri-
ent release behavior of the developed nano-fertilizer as com-
pared with conventional chemical fertilizer.
2 Materials and methods
2.1 Biomass collection and biochar preparation
Maize stalk and black gram crop biomass was collected from
the ICAR-Sikkim Center Research Farm from previous crop
harvesting. Pine needle (tree) and Lantana camara (weed)
biomass was collected from a nearby farm area jungle. The
biomass was shredded to pieces of ≤ 6 in. and oven-dried at
70 °C followed by pyrolysis into a biochar production unit.
Charring of all the biomass (moisture level 5%) was carried
out in a portable charring kiln (28-in. length × 10-in. diam-
eter) developed by ICAR-Sikkim Center to keep the process
quick, low cost, and simple. Biomass was inserted into the
kiln, combusted at 600 °C (heating rate 10 °C ­min−1 and
holding temperature 4.0 h), and the temperature was main-
tained by an electrically operated manual switch connected
to the kiln. After preparation, the biochar was collected with
shovel/scoop, dried at 100 °C (24 h), pulverized to fine pow-
der, sieved through 0.2 mm, and used for the synthesis of
biochar-based secondary and micronutrient enriched slow
release nano-fertilizer. The morpho-mineralogical charac-
terization along with compositional heterogeneity of the
biochar produced at 600 °C was already published in our
previous work.
2.2 Chemicals and glassware
Different types of analytical grade calcium phosphate
­[ Ca3(PO4)2], magnesium sulfate ­(MgSO4, ­7 H 2O), zinc
sulfate ­(ZnSO4, ­7H2O), and sodium phosphate monobasic
­(NaH2PO4, ­2H2O) and ferrous chloride (­ FeCl2, ­4H2O) were
purchased from Sigma-Aldrich, New Delhi. The reagents
used for different analyses were of analytical grade (AR) and
were purchased from different repute companies in India.
The glasswares used in different experiments in this study
were of Borosil made.
2.3 Development of slow release biochar‑based
nano‑fertilizer
Preparation of the slow release nano-fertilizer based on bio-
char consists of three steps, viz., biochar carrier produc-
tion, impregnation of biochar carrier with Ca-Mg-Zn-Fe-Na
nutrient solution, and finally granulation technology. Nutri-
­ a+2-Mg+2-Zn+2-Fe+2/+3-Na2O was prepared
ent solution of C
by dissolving calcium phosphate [­ Ca3(PO4)2], magnesium
sulfate ­(MgSO4, ­7H2O), zinc sulfate ­(ZnSO4, ­7H2O), ferrous
Biomass Conversion and Biorefinery
chloride ­(FeCl2, ­4H2O), and sodium phosphate monobasic
­(NaH2PO4, ­2H2O) in deionized water. In a beaker, the bio-
char carrier (MSB, BGB, PNB, and LCB) was mixed prop-
erly with the already prepared secondary and micronutri-
ent nutrient solutions. The contents were stirred for a few
minutes and kept for 72 h at 25 ± 0.5 °C to allow maximum
adsorption of mineral nutrients into the porous structure of
four diverse biochars separately. A starch–PVA binder was
prepared by mixing starch (cassava starch/potato starch/
cornstarch) solution and PVA. The nutrient-impregnated
biochar was mixed with starch–PVA binder to achieve an
even coating and proper binding. The nutrient-impregnated
biochar binder mixture was then passed through a sieve with
small holes and then air-dried, ground, and stored for further
study.
2.4 Physicochemical analysis of nano‑fertilizer
The water absorbance, pH, C/N ratio, and electrical conduc-
tivity (EC) were determined following procedures developed
by the International Fertilizer Development Centre (IFDC).
The density of each biochar-based nano-fertilizer was
determined using the tapped method. Ultimate or elemental
analysis of biochar was done for the determination of the
percentage of C, H, N, and O by the Euro EA elemental
analyzer. The water absorbency was estimated by submerg-
ing 0.5 g (W1) of biochar-based nano-fertilizer in 10 mL
of deionized water followed by taking out the sample after
72 h and wiped properly. Then, their weights were again
measured (W2). The water absorbency was determined as
(W2 − W1) / W2 × 100.
2.5 Nano range particle size determination
The developed nano-sized biochar-based secondary and
micronutrient enriched slow release nano-fertilizer having
an average particle size < 100 nm was determined with a
transmission electron microscope (TEM). For analysis by
TEM, a 2.0-mg sample was mixed with 20 mL of 1-methyl-
2-pyrrolidone solvent followed by sonication at 53 kHz
(30 min) and then centrifuged at 1000 rpm (1 h). Then, the
C-film-coated Cu grid was generated in a vacuum evapora-
tor (JEOL.JEE-420). The supernatant was dropped onto the
C-film-coated grid. TEM was carried out with an electron
microscope (model no. JEM-1011, JEOL) to record different
black dots at 200 kV, and the digital images were processed.
Swelling ratio, salt index, and equilibrium water content
estimation.
At first, 0.5 g of four different biochars and biochar-based
nano-fertilizers was put in 100 mL of double distilled water
independently for 1 day to swell followed by filtration. Then,
swelling ratio and equilibrium water content (%) were meas-
ured as swelling ratio = (Ms − Md) / Md and equilibrium water
content = (Ms − Md) / Ms × 100, where Ms and Md are wet and
dry mass of biochar and biochar-based nano-fertilizer. For
the determination of the salt index, 0.5 g of biochar-based
nano-fertilizer and ­NaNO3 was submerged in 100 mL of
double distilled water in two different separate beakers. The
conductivity was determined by a Utech microprocessor-
based pH-EC-ion meter (1:10 sample: water suspensions)
after 1 day. The salt index was measured as a ratio of these
conductivities.
2.6 Determination of water retention
The synthesized four biochar-based secondary and micro-
nutrient enriched nano-fertilizers (1 g) along with control
and unamended soil were properly mixed with sandy loam
soil in a 500-mL beaker. Approximately 100-mL deionized
water was added gradually into it and measured its weight
(Mi). The experiment was carried out in triplicate, i.e., three
replications per sample. The entire beakers were kept in a
BOD incubator at 25 ± 1 °C. The beaker was withdrawn at 0,
1, 3, 7, 15, 20, 25, 30, and 45 days (Mi) from the incubator,
and their weights were taken again. Water retention of soil
was measured as Mf / Mi × 100.
2.7 Nutrient release studies
The nutrient release patterns of secondary and micronutri-
ent solution-impregnated biochar-based nano-fertilizer were
determined using the sequential leaching method. In brief,
5 g of biochar-based slow release nano-fertilizer was put
into self-sealing nylon bags followed by submergence into
a 100-mL double distilled water in a glass container. The
leachate fraction was brought together after 24 h. After that,
fresh 100-mL distilled water was added, and the leachate
was again collected after 3 days. It was repeated for differ-
ent days (7, 15, 22, 30, 45, 60, 75, and 90), and the slow
release pattern of nutrients was calculated. The leachate
was estimated for C ­ a+2, ­Mg+2, ­Zn+2, ­Fe+2/+3, and N
­ a2O.
A control was also maintained by using commercial inor-
ganic compound fertilizer (X). The micronutrients ­Zn+2 and
­Fe+2/+3 were estimated as per the method of Lindsay and
Norvell (DTPA-CaCl2-TEA method). Such an analysis was
done using atomic absorption spectroscopy (Thermo-Scien-
tific; iCE3000 series). ­Ca+2 and ­Mg+2 were determined by
complexometric titration rather than the flame photometry
method as the former method is more accurate and widely
used. The concentration of N ­ a2O was determined by the
flame photometry method.
2.8 Statistical analysis
All the data generated during the entire period of inves-
tigation was statistically analyzed using the “F” using
13
 Biomass Conversion and Biorefinery

the procedure of Gomez and Gomez [21]. LSD values at
P = 0.05 were used to determine the significance of the dif-
ference between the treatment means. This analysis was
done using the statistical package “STATISTICS.”
3 Results and discussion
3.1 Physicochemical characterization
of biochar‑based slow release nano‑fertilizer
The developed biochar-based slow release nano-fertilizer
was cylindrical in shape and granular in form, having an
average diameter of approximately 2 mm. Actually, granu-
lation is very necessary to assist the handling process and
also to compare with the commercial compound fertilizer
(X) [22–24]. Different physicochemical uniqueness (pH,
density, EC, water absorbance, C, H, N, O, and C/N ratio)
of biochar-based slow release nano-fertilizer are presented
in Table 1. Among the slow release nano-fertilizer, the pH
was high in MSB-SRF (6.61) followed by BGB-SRF (6.32),
LCB-SRF (6.08), PNB-SRF (5.94), and control (X). The
pH of the developed nano-fertilizer was very near to neutral
and roughly two units notably more (p = 0.05) as compared
with compound (X), which was moderately acidic [25]. The
more acidic character of “X” may be due to residual acid-
ity because H ­ 2SO4 and H
­ NO3 are probably utilized during
the production of commercial fertilizer [26, 27]. Similarly,
the density was highest in control (0.88 g ­cm−3) and lowest
in MSB-SRF (0.731 ­cm−3). The developed nano-fertilizer
showed lower densities as compared with commercial com-
pound fertilizer (X), indicating the intrinsic density vari-
ations between the biochar and nutrient carrier utilized in
fertilizers [25, 28, 29]. Actually, it is already known that
biochar shows a lower density, and therefore, the addition
of biochar in soil is mentioned to decrease the bulk density
of soil [30]. Thus, the continuous addition of biochar-based
slow release nano-fertilizer in soil may significantly decrease
the bulk density and increase water infiltration and water
retention [31]. Electrical conductivity was highest in PNB-
SRF (5.38 ds ­m−1) and lowest in control (2.83 ds ­m−1). The
electrical conductivity of the developed nano-fertilizer was
medium in range, and it supported the actuality of metal
salt/ metal inclusion into the nano-fertilizer structure [32].
Such sorption of salts helps to augment the bulk density.
The developed biochar-based nano-fertilizer showed a con-
siderably more (p = 0.005) EC as compared with “X,” and
it is considered as generally low. Such EC of both nano-
fertilizer and compound X depicted that they have the mod-
est influence to affect soil salinity and osmotic potential.
Water absorbance was maximum in MSB-SRF (45.76%)
followed by BGB-SRF (37.91%), LCB-SRF (35.53%), PNB-
SRF (32.46%), and control (0.537%). For any biodegradable
substance, the water absorbency character is very significant.
The results of this work revealed that biochar-based nano-
fertilizer showed higher water absorbency demonstrating the
capacity of biochar to absorb and retain water. Therefore, it
might contribute to enhance the slow release of secondary
and micronutrient properties [33]. The actual explanation
for such occurrence might be due to the networks formed
between the fertilizer, biochar particles, and binding agents
that reduced the water absorbency of the film. But the water
absorbency of “X” could not be calculated properly due
to the fact that it got disintegrated during its immersion in
water [34]. The C/N ratio was highest in LCB-SRF (14.82)
followed by PNB-SRF (14.02), MSB-SRF (13.53), BGB-
SRF (13.04), and control (1.02). Finally, the C, H, N, and
O% contents were also varied along with varying biochar
types. Previous results revealed that biochar has huge poten-
tial to store mineral nutrients via physio-sorption and/or
chemisorption [35]. Thus, such character of biochar may be
applied to utilize in the development of slow release nano-
fertilizer because it both guarantees nutrient availability for
a longer time to crops and enhances the quality of soil [36].
Comparative behavior of biochar and biochar-based slow
release nano-fertilizers is presented in Table 2. The swelling
ratio was maximum in MSB-SRF (4.61 g. g­ −1) followed by
BGB-SRF (4.42 g. ­g−1), LCB-SRF (4.36 g. ­g−1), and PNB-
SRF (4.15 g. g­ −1). The salt index also followed the same
trend, followed by the swelling ratio having a maximum in
MSB-SRF (0.07) and minimum in PNB-SRF (0.04). The
salt index actually estimates the possibility of the designed

Table 1  Physicochemical Treatments pH Density (g c­ m−3) EC (ds ­m−1) Water %C %H %N %O C/N ratio

analysis of diverse biochar- absorbance
based slow release nano- (%)
fertilizer
Control (X) 4.91 0.889 2.83 0.53 31.56 2.03 10.00 16.34 1.02
MSB-SRF 6.61 0.731 3.57 45.76 67.43 4.28 11.39 13.56 13.53
BGB-SRF 6.32 0.753 3.45 37.91 62.26 2.91 11.42 12.91 13.04
PNB-SRF 5.94 0.742 5.38 32.46 70.37 3.89 10.97 14.07 14.02
LCB-SRF 6.08 0.762 3.26 35.53 76.13 3.41 11.01 10.72 14.82

X, commercial compound fertilizer; EC, electrical conductivity; % C, % carbon; % H, % hydrogen; % N, %

nitrogen; % O, % oxygen

13
Biomass Conversion and Biorefinery

Table 2  Comparative behavior of biochar and biochar-based slow pores than those in biochar alone [42]. The biochar-based
release nano-fertilizer nano-fertilizer porous structure appears to lock several salt
Treatments Swelling ratio Salt index Equilibrium crystals most probably of Ca, Mg, Zn, Fe, and Na [43].
(g. ­g−1) water content
(%) 3.2 Water retention properties of biochar‑based
MSB 3.72 0.04 65 nano‑fertilizer
BGB 3.53 0.03 63
PNB 3.26 0.01 59 The mean water retention of soil with biochar-based slow
LCB 3.47 0.02 60 release nano-fertilizer, control, and unamended soil is pre-
MSB-SRF 4.61 0.07 74 sented in Table 3. The water retention of the synthesized
BGB-SRF 4.42 0.06 72 nano-fertilizer decreased with an increase in time. After
PNB-SRF 4.15 0.04 68 45 days of study, results revealed that the mean water reten-
LCB-SRF 4.36 0.05 70 tion was maximum in MSB-SRF (53.16%), followed by
BGB-SRF (49.56%), LCB-SRF (46.43%), and PNB-SRF
(42.47%) and minimum in control (27.43) followed by
biochar-based nano-fertilizer to cause crop injury. More unamended soil (19.52). The maximum water retention of
numerical salt index values of any nano-fertilizer are recog- MSB-SRF may be due to the large porous structure of MSB
nized to damage crops and therefore result in less economic biochar as compared with the other three biochars. Thus,
yield. During the comparison with an acceptable tolerable water retention was largely dependent on the porous struc-
limit of the salt index, i.e., 2 mmhos ­cc−1 (in terms of con- ture and pore volume of the respective biochar [44]. By and
ductivity; reference to ­NaNO3 taken as 100), the salt index large water retention reduces with time lapse. The reten-
of biochar-based nano-fertilizer was very low (0.04–0.07 tion of water of any substances in earth assists to provide
mmhos ­cc−1) in this research which makes it appropriate water to soil and afterward to crops [45]. Superior water
for soil and crop utilization and accordingly sustainable retention capacities were monitored for the nano-fertilizer-
environment and agriculture [37]. Finally, the equilibrium amended soil as compared with control treatment, depicting
water content was higher in MSB-SRF (74%) followed by that such soils can efficiently gain additional water to crops
BGB-SRF (72%), LCB-SRF (70%), and PNB-SRF (68%). and delay the onset of water stress [46]. Such helpful influ-
Interestingly, the swelling ratio, salt index, and equilibrium ence of biochar-based nano-fertilizer on soil water retention
water content were lower in all the four biochars alone than in collaboration with its near-neutral pH is predominantly
biochar-based nano-fertilizer [38]. The salt index, water significant for sandy coarse soils [47].
absorbency, and equilibrium water content were slightly
increased in nano-fertilizer as compared with biochar alone. 3.3 Formation of nano‑sized biochar‑based
As a general rule, biochar has a highly porous morphology fertilizer composite
[39] which may be physically sorbed water molecules to be
later released on crops and soil in dry arid locations [40]. Transmission electron microscopy (TEM) analysis of bio-
In our earlier study, it was found that all the four diverse char-based nano-fertilizer was performed for particle size,
biochars showed coarse and highly porous morphology [41]. size distribution, and morphology. The TEM images of four
Such a wide-ranging porous structure confers the diverse different biochar-based nano-fertilizers confirm the for-
biochar with the capability to have room for visitor nutrient mation of nano-sized material, having an average particle
ions such as ­Ca+2, ­Mg+2, ­Zn+2, ­Fe+2/+3, and ­Na2O. Following size of less than 100 nm (Fig. 1). In MSB-based nano-ferti-
impregnation, the synthesized and developed nano-fertilizer lizer, the particle size was in the range of 22.81–24.33 nm.
represented aggregates on an asymmetrical plane with tiny In LCB-based nano-fertilizer, the particle size was

Table 3  Mean water retention Treatments Water retention (%) at different days

of soil with biochar-based slow
release nano-fertilizer, control, 0 1 3 7 15 20 25 30 45
and unamended soil
Control (X) 98.75 95.56 92.56 81.71 64.29 56.54 51.79 42.03 22.43
MSB-SRF 98.67 98.03 96.63 87.71 77.53 71.168 64.84 58.43 53.16
BGB-SRF 98.86 97.93 96.01 86.6 75.84 69.12 62.43 55.68 49.56
PNB-SRF 98.72 97.01 95.79 85.23 73.17 65.63 58.09 50.55 42.47
LCB-SRF 98.84 97.24 95.91 85.99 74.66 67.58 60.51 53.42 46.43
Unamended soil 95.93 92.12 90.95 79.04 65.43 54.93 48.43 35.42 19.52

13

Fig. 1  Transmission electron
microscope images indicat-
ing formation of nano-sized
composite
10.97–12.15 nm. In PNB-based nano-fertilizer, the particle
size was 8.33–12.82 nm, and in BGB-based nano-fertilizer,
it was 9.01–15.67 nm, underlying porous carbon matrix.
The TEM image also depicted normal globular-shaped par-
ticles and slim particle size distribution in the developed
nano-fertilizer, providing a promise about the possibility of
a protocol to result in particles with less distribution in par-
ticle size [48, 49]. During the magnification process, some
black dots with a nano range (≤ 100 nm) particle size of
different biochar-based nano-fertilizers on the graphene-like
surfaces were seen, and these black dots were of crystalline
stripes [50]. The presence of crystalline stripes on black dots
proved that the nano range such as sheets was haphazardly
arranged in a turbostratic state [51]. As carbon is domi-
nant in biochar-based nano-fertilizer, thus the black dots
resembled graphene-like structures [52]. The TEM analysis
showed that the particle size was significantly influenced
by feedstock type [53]. The slightly gray fraction of all the
four biochar-based nano-fertilizer was attributed to aromatic
clusters having extremely twisted and disordered structures
which showed that they have disordered stacking [54].
3.4 Cumulative secondary nutrient release pattern
SEM–EDX analyses from our previous study revealed
that biochars were highly porous, which contributed to
its capability to adjust nutrient ions to develop a slow
release nano-fertilizer [55]. The sequential leaching tech-
nique utilized in this research describes mainly for easily
13
Biomass Conversion and Biorefinery
available water-soluble nutrients, except comparatively
strongly sorbed fractions [56]. For acting as slow release
character of nano-fertilizer, different mechanisms act con-
currently to account for the sorption of solutes into the
biochar, and they are co-precipitation, ligand/complexa-
tion exchange, ion exchange on charged biochar surfaces,
electrostatic forces/van der Waals, pore diffusion, and
π-cation communications between the solute ions and bio-
char aromatic rings [57, 58]. Furthermore, the utilization
of starch–PVA as a binding agent might improve the slow
release performance of biochar-based nano-fertilizer [59].
Cumulative concentrations of calcium ­(Ca+2) released from
biochar-based slow release nano-fertilizer at different days
of leaching event are presented in Fig. 2. The calcium con-
centrations in leachates were 0.53, 2.18, 4.07, 7.62, 11.16,
14.71, and 21.8 mg ­L−1 at 0, 7, 15, 30, 60, and 90 days,
respectively, in the control (X) sample. The calcium con-
centrations in leachates were 0.41, 1.64, 3.05, 5.7, 11.0, and
16.3 mg ­L−1 at 0, 7, 15, 30, 60, and 90 days, respectively,
in MSB-SRF. The calcium concentrations in leachates were
0.39, 1.54, 2.85, 5.32, 10.26, and 15.20 mg ­L−1 at 0, 7, 15,
30, 60, and 90 days, respectively, in BGB-SRF. The calcium
concentrations in leachates were 0.40, 1.31, 2.35, 4.30, 8.20,
and 12.1 mg L ­ −1 at 0, 7, 15, 30, 60, and 90 days, respec-
tively, in PNB-SRF. The calcium concentrations in leachates
were 0.38, 1.49, 2.76, 5.15, 9.92, and 14.7 mg L ­ −1 at 0, 7,
15, 30, 60, and 90 days, respectively, in LCB-SRF. Thus, the
calcium leachate was maximum in MSB-SRF nano-fertilizer
and minimum in PNB-SRF nano-fertilizer as compared to
Biomass Conversion and Biorefinery

Fig. 2  Cumulative concentra- 90
tions of calcium released from LCB-SRF
biochar-based slow release 80 PNB-SRF

Calcium in leachates (mg L-1)

nano-fertilizer at different days
BGB-SRF
of leaching event 70
MSB-SRF
60 Control (X)
50
40
30
20
10
0
0 1 3 7 15 22 30 45 60 75 90
Different days

control. Thus, in conclusion, biochar-based slow release
nano-fertilizer significantly reduced calcium leaching in
the soil column. Cumulative concentrations of magnesium
­(Mg+2) released from biochar-based slow release nano-
fertilizer at different days of leaching event are presented
in Fig. 3. The magnesium concentrations in leachates were
0.84, 2.99, 5.45, 10.06, 19.28, and 28.5 mg ­L−1 at 0, 7, 15,
30, 60, and 90 days, respectively, in the control (X) sample.
The magnesium concentrations in leachates were 0.73, 2.10,
3.67, 6.62, 12.51, and 18.4 mg ­L−1 at 0, 7, 15, 30, 60, and
90 days, respectively, in MSB-SRF. The magnesium concen-
trations in leachates were 0.71, 2.02, 3.52, 6.34, 11.97, and
17.6 mg ­L−1 at 0, 7, 15, 30, 60, and 90 days, respectively,
in BGB-SRF. The magnesium concentrations in leachates
were 0.75, 1.79, 2.99, 5.23, 9.71, and 14.2 mg L ­ −1 at 0, 7,
15, 30, 60, and 90 days, respectively, in PNB-SRF. The mag-
nesium concentrations in leachates were 0.72, 1.94, 3.35,
5.98, 11.24, and 16.5 mg ­L−1 at 0, 7, 15, 30, 60, and 90 days,
respectively, in LCB-SRF. Thus, the magnesium leachate
was maximum in MSB-SRF nano-fertilizer and minimum
in PNB-SRF nano-fertilizer as compared to control. Thus,
in conclusion, biochar-based slow release nano-fertilizer sig-
nificantly reduced magnesium leaching in the soil column
[60]. The findings of the research facilitated to interpret the
slow release performance of particular secondary nutrients
which then support the selection of appropriate fertilizer
for plants [61]. Biochar is able to sorb mineral nutrients
due to its highly porous structure, large surface area, and
physiochemical bonding which guarantees decreased nutri-
ent leaching and thus assisting increased crop development

Fig. 3  Cumulative concentra-
tions of magnesium released 100 LCB-SRF
from biochar-based slow release PNB-SRF
Magnesium in leachates (mg L-1)

90
nano-fertilizer at different days BGB-SRF
of leaching event 80
MSB-SRF
70 Control (X)
60
50
40
30
20
10
0
0 1 3 7 15 22 30 45 60 75 90
Different days

13

[62]. Such a concrete basis supports biochar utilization to
accelerate soil health and augmenting crop growth [63].
The nutrient release from the diverse biochar-based slow
release nano-fertilizers may be manipulated largely through
the size of pore size, level of adsorption, and ion binding
capabilities. It was understandable that the nutrient release
(i.e., ­Mg2+ and ­Ca2+) was unhurried at the starting point of
study which progressed quickly to a nearly constant value
at the end of the experiment [64, 65]. Such type of nutrient
release character is very similar to the nutrient utilization
blueprint of crops which need lesser uptake near the begin-
ning stages (germination), and after that, a fixed supply of
nutrients (development stage) is needed to achieve more
crop growth and yield [66, 67]. Such tendency realized in
this study may be helpful to provide nutrients constantly
to crops as per their demand and reduces nutrient leaching
while judging against any commercial fertilizers [68, 69].
3.5 Cumulative micronutrient released pattern
Cumulative concentrations of zinc ­(Zn+2) released from
biochar-based slow release nano-fertilizer at different days
of leaching event are presented in Fig. 4. The zinc concen-
trations in leachates were 7.3, 83.8, 171.2, 335.2, 663.1,
and 991 mg L ­ −1 at 0, 7, 15, 30, 60, and 90 days, respec-
tively, in the control (X) sample. The zinc concentra-
tions in leachates were 5.2, 59.9, 122.5, 239.8, 474.4, and
709 mg ­L−1 at 0, 7, 15, 30, 60, and 90 days, respectively,
in MSB-SRF. The zinc concentrations in leachates were
4.8, 55.2, 112.8, 220.8, 436.9, and 653 mg ­L−1 at 0, 7, 15,
30, 60, and 90 days, respectively, in BGB-SRF. The zinc
concentrations in leachates were 5.1, 51.9, 105.4, 205.7,
406.3, and 607 mg ­L−1 at 0, 7, 15, 30, 60, and 90 days,
respectively, in PNB-SRF. The zinc concentrations in
leachates were 4.9, 46.6, 94.4, 183.9, 362.9, and 542 mg
Fig. 4  Cumulative concentra-
tions of zinc released from
biochar-based slow release
nano-fertilizer at different days
of leaching event
Zinc in leachates (mg L-1)
13
Biomass Conversion and Biorefinery
­ −1 at 0, 7, 15, 30, 60, and 90 days, respectively, in LCB-
L
SRF. Thus, the zinc leachate was maximum in MSB-SRF
nano-fertilizer and minimum in LCB-SRF nano-fertilizer
as compared to control. Thus, in conclusion, biochar-
based slow release nano-fertilizer significantly reduced
zinc leaching in the soil column. Cumulative concentra-
tions of iron ­(Fe+2/+3) released from biochar-based slow
release nano-fertilizer at different days of leaching event
are presented in Fig. 5. The iron concentrations in lea-
chates were 1.8, 8.1, 15.4, 29.1, 56.4, and 83.7 mg ­L−1 at
0, 7, 15, 30, 60, and 90 days, respectively, in the control
(X) sample. The iron concentrations in leachates were 1.2,
59., 11.4, 16.1, 21.6, 42.0, and 62.4 mg L ­ −1 at 0, 7, 15,
30, 60, and 90 days, respectively, in MSB-SRF. The iron
concentrations in leachates were 1.2, 5.5, 10.6, 20.0, 38.8,
and 57.6 mg ­L−1 at 0, 7, 15, 30, 60, and 90 days, respec-
tively, in BGB-SRF. The iron concentrations in leachates
were 1.1, 4.6, 8.5, 11.9, 15.8, 30.5, 37.9, and 45.3 mg ­L−1
at 0, 7, 15, 30, 60, and 90 days, respectively, in PNB-
SRF. The iron concentrations in leachates were 1.1, 4.9,
9.2, 17.2, 33.3, and 49.5 mg ­L−1 at 0, 7, 15, 30, 60, and
90 days, respectively, in LCB-SRF. Thus, the iron leachate
was maximum in MSB-SRF nano-fertilizer and minimum
in PNB-SRF nano-fertilizer as compared to control. Thus,
in conclusion, biochar-based slow release nano-fertilizer
significantly reduced iron leaching in the soil column. The
micronutrient (Zn and Fe) release prototypes indicated that
biochar-based nano-fertilizer released these nutrients very
slowly, steadily, and constantly [70–72]. The starch–PVA
binding material and four diverse biochar configurations
assisted to deliver captured Zn and Fe, which were either
discovered in the biochar porous structure or act together
with various surface functional groups [73]. Such sequen-
tial release technique utilized in this research investiga-
tion also largely extracts water-soluble nutrients and does
4000 LCB-SRF
PNB-SRF
3500
BGB-SRF
3000 MSB-SRF
Control (X)
2500
2000
1500
1000
500
0
0 1 3 7 15 22 30 45 60 75 90
Different days
Biomass Conversion and Biorefinery

Fig. 5  Cumulative concentra-
tions of iron released from 350 LCB-SRF
biochar-based slow release PNB-SRF
nano-fertilizer at different days 300
BGB-SRF

Iron in leachates (mg L-1)

of leaching event
250 MSB-SRF
Control (X)
200

150

100

50

0
0 1 3 7 15 22 30 45 60 75 90
Different days

not allow the comparatively substantial sorbed fraction
[74]. The concentration of Zn and Fe released from the
biochar-based nano-fertilizer was reasonable quantities of
such ions [75]. Such observable fact may clarify the influ-
ence of starch–PVA binding substances, which performed
as a barricade and blocked water from penetrating the crop
and dissolving the nutrients [76–79]. Usually, the Zn and
Fe release prototypes offered in this work verify the slow
release performance of biochar-based nano-fertilizer in
contrast with commercial fertilizers [80]. Cumulative con-
centrations of sodium (Na) released from biochar-based
slow release nano-fertilizer at different days of leaching
event are presented in Fig. 6. The sodium concentrations
in leachates were 0.5, 1.7, 2.9, 5.4, 10.2, and 15.1 mg L ­ −1
at 0, 7, 15, 30, 60, and 90 days, respectively, in the control
(X) sample. The sodium concentrations in leachates were
0.3, 1.2, 2.3, 4.3, 8.2, and 12.2 mg L ­ −1 at 0, 7, 15, 30,
60, and 90 days, respectively, in MSB-SRF. The sodium
concentrations in leachates were 0.3, 0.6, 2.1, 2.9, 3.9,
7.5, and 11.1  mg L ­ −1 at 0, 7, 15, 30, 60, and 90  days,
respectively, in BGB-SRF. The sodium concentrations in
leachates were 0.2, 0.5, 1.7, 3.2, 6.2, and 9.3 mg L ­ −1 at
0, 7, 15, 30, 60, and 90 days, respectively, in PNB-SRF.
The sodium concentrations in leachates were 0.3, 1.1, 2.0,
3.8, 7.2, and 10.7 mg ­L−1 at 0, 7, 15, 30, 60, and 90 days,
respectively, in LCB-SRF. Thus, the sodium leachate was
maximum in MSB-SRF nano-fertilizer and minimum in
PNB-SRF nano-fertilizer as compared to control. Thus,
in conclusion, biochar-based slow release nano-fertilizer
significantly reduced sodium leaching in the soil column.

Fig. 6  Cumulative concentra-
70
tions of sodium released from LCB-SRF
biochar-based slow release
60 PNB-SRF
Sodium in leachates (mg L-1)

nano-fertilizer at different days

of leaching event BGB-SRF
50 MSB-SRF
Control (X)
40

30

20

10

0
0 1 3 7 15 22 30 45 60 75 90
Different days

13

4 Conclusion
The diverse biochar-based secondary and micronutrient
enriched slow release nano-fertilizer as a nutrient carrier
was designed and developed using a very simple and cost-
effective three-step synthesis mechanism. The valoriza-
tion of crop biomass via design and synthesis of biochar-
based slow release nano-fertilizer form a win–win strategy
by reducing the environmental and public health hazards
related to indecent biomass dumping, whereas concurrently
creating significant value chain chances via the provision
of agrochemicals. The nano-fertilizer cannot only provide
nutrients for a longer time but also enhance the water reten-
tion capacity of the soil, mitigating environmental issues and
land contamination which arise due to nutrient leaching and
volatilization from commercial-grade fertilizers. The nano-
fertilizer had notably decreased the Ca, Mg, Zn, Fe, and Na
release patterns and increased soil water retention capacity
as compared with commercial compound fertilizer. Such
developed secondary and micronutrient-based slow release
nano-fertilizers have various possible niche functions such
as environmental remediation, agriculture, and horticulture
crop production. The nano-fertilizer significantly has low
nutrient loss through leaching and runoff, more plant nutri-
ent use efficiency, and therefore negligible influences on
ground and surface water quality. The plant mineral nutrient
impregnation technology into biochar particles is believed to
be a huge appropriate technique to decrease nutrient release.
Hence, the biochar-based slow release nano-fertilizer addi-
tion into field soil may be treated as an environmental and
eco-friendly sustainable technology. The nano-fertilizers
may have hopeful functions to be a high-quality decision to
mitigate mineral nutrient losses in the environment. There-
fore, a developed biochar-based nano-fertilizer is believed
to be an ecofriendly material and viable for sustainable
agriculture.
Acknowledgements  The author Shaon Kumar Das is thankful to the
Director-ICAR Research Complex for NEH Region, Umiam, Megha-
laya, India, and the Department of Soil Science and Agricultural Chem-
istry, Palli Siksha Bhavana, Visva Bharati, Shantiniketan, India, for
providing necessary funds and facilities during the entire period of
the research work.
Declarations  21. Das SK, Roy A, Barman H (2016) Fungi toxic efficiency of some
Competing interests  The authors declare no competing interests.
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13

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