Minerals Engineering 127 (2018) 178–184

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Minerals Engineering
journal homepage: www.elsevier.com/locate/mineng

On the role of nanobubbles in particle–bubble adhesion for the flotation of T

quartz and apatitic minerals
⁎
A.F. Rosa, J. Rubio
Laboratório de Tecnologia Mineral e Ambiental (LTM), Departamento de Engenharia de Minas, PPGE3M, Universidade Federal do Rio Grande do Sul, Setor 6-Av. Bento
Gonçalves, 9500, 91501-970 Porto Alegre, RS, Brazil

A R T I C LE I N FO A B S T R A C T

Keywords: This work evaluated the influence of nanobubbles (150–200 nm, mean diameter) on the visual adhesion of
Flotation microbubbles (70 μm mean diameter) and macrobubbles (1 mm mean diameter) onto selected mineral particles
Nanobubbles (quartz and apatite) and on the flotation of both minerals, at bench scale. The adhesion of bubbles to high purity
Microbubbles grains of quartz and apatite was monitored using a specially designed photographic technique. The results
Macrobubbles
showed that the highest adhesion of bubbles onto the mineral grains occurred only after “conditioning” with
Apatitic ore
Quartz
nanobubbles. The nanobubbles appear to adhere to hydrophobic surfaces and confined to the rough surfaces of
the grains, probably due to the dissipation of the free surface energy of the solids. As a result, the nanobubbles
appear to serve as nuclei for enhanced adhesion of micro and/or macrobubbles, assisting the flotation of both
minerals. In the case of quartz (D50 = 290 μm), the recovery increase was about 23% compared to a standard
test of flotation with macrobubbles only. Furthermore, flotation kinetics was rapid and quartz recovery, at the
first min, was double that obtained in the absence of nanobubbles. In the case of a fine apatitic ore
(35% < 37 μm particles), best results were obtained with a combination of nano, micro and macrobubbles, with
a 500–1000 g t−1 saponified soybean oil collector and a 300–600 g t−1 gelatinized corn starch depressant of iron
bearing minerals. The P2O5 recoveries increased about 9% compared to flotation with macrobubbles only, and
separation also occurred at a higher rate. The total recovered phosphate (4 min standard test) was obtained in
the first 1.5 min, after conditioning with nanobubbles, followed by injection of and microbubbles. Results va-
lidated the reported high potential for nanobubbles in “surface conditioning”, the first stage of mineral flotation
and were explained in terms of the solution and interfacial phenomena involved.

1. Introduction
Froth flotation is believed to be the most efficient and cost-effective
unit operation in mineral processing (Fuerstenauet al., 2007). Yet, se-
paration efficiency decreases for particles less than 37 µm and fall
sharply for the ultrafines fractions (< 13), due to the low probability of
bubble-particle capture (poor attachment). Yet, it has been reported
that fine particle recovery in flotation is enhanced by using micro-
bubbles (MBs - 30–100 μm diameter) and/or nanobubbles (NBs of
120–800 nm diameter) (Ahmed and Jameson, 1985; Ralston et al.,
1999; Gontijo et al., 2007, Azevedo et al., 2016a,b, Etchepare et al.,
2017, Oliveira et al., 2018).
Mechanisms involved while employing microbubbles are related to
a higher residence time for bubble-particle adhesion at the film-thin-
ning and disjoining pressure stage (Yoon, 2000; Ralston et al., 1999;
Rubio et al., 2003; Fuerstenau et al., 2007; Santana et al., 2012). Yet,
microbubbles do not have enough lifting power (carrying capacity) and
a combination with coarser bubbles appears to be essential; un-
fortunately, the practical use of a wide bubbles size distribution poses a
serious challenge to flotation machine manufacturers. This occurs
mainly because of bubbles interactions themselves, usually leading to
coalescence or engulfing of the fine bubbles by the coarser bubbles
(Yoon, 2000; Ralston et al., 1999; Azevedo et al., 2016a; Fuerstenau
et al., 2007).
Regarding nanobubbles in mineral flotation, recent studies reported
advantages regarding the enhancement of the contact angles after their
capture by particles, assisting the probability of flotation (and its rate)
by larger bubbles (> 1 mm) (Ahmadi et al., 2014; Calgaroto et al.,
2015; Fan and Tao, 2008; Fan et al., 2012; Sobhy and Tao, 2013,
Azevedo et al., 2016b). In other words, they would act as a conditioner

⁎
Corresponding author.
E-mail address: jrubio@ufrgs.br (J. Rubio).
URL: https://www.ufrgs.br/ltm (J. Rubio).

https://doi.org/10.1016/j.mineng.2018.08.020
Received 7 May 2018; Received in revised form 6 August 2018; Accepted 8 August 2018
Available online 20 August 2018
0892-6875/ © 2018 Elsevier Ltd. All rights reserved.
A.F. Rosa, J. Rubio
a b
Table 1
Conditions of bubbles-particles (apatite/quartz) interac-
tions. The adhesion of bubbles onto quartz was studied
under conditions 1, 2 and 3.
Condition Bubbles injected
1 MaBs
2 NBs
3 NBs + MaBs
4 MBs
5 NBs + MBs
6 MBs + MaBs
7 NBs + MBs + MaBs
Table 2
Flotation studies conditions at 28% w/w.
Conditions Reagents dosage [collector]a; [depressant]b (g·t−1)
1 1000; 600
2 500; 300
a
Fatty acid soap from soybean oil.
b
Gelatinized corn starch.
or as a “second collector,” because the nanobubbles do not rise (or
float) in water, nor do they have lifting power.
Furthermore, recent studies by our research group have revealed
two other phenomena:
i. Nanobubbles are able to aggregate particles (ultrafines) and im-
prove their floatability (Azevedo et al., 2016a; Etchepare et al., 2017,
Calgaroto et al., 2015). ii. Nanobubbles serve as nuclei (“seeds”) for the
adhesion of other bubbles, micro and macro (> 1 mm diameter)
(Azevedo et al., 2016b). The validation of this phenomenon and its
effect on the particle flotation of quartz and phosphate at laboratory
scale is the main theme of this work.
2. Experimental
2.1. Materials
Distilled water treated in a reverse-osmosis cartridge and modules
of ion-exchange resins and activated carbon was employed for the
particle-adhesion studies. The conductivity of the water was 3 µS cm−1;
had a surface tension of 72.5 ± 0.1 mN m−1 and an equilibrium pH of
5.5. For flotation tests, tap water from the city of Porto Alegre – South
Brazil was used. A sulfochromic solution and subsequent abundant
rinse with the treated water were used to remove possible organic
compounds from all glass materials. Hydrochloric and nitric acids,
ammonium metavanadate, ammonium molybdate and monosodium
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Minerals Engineering 127 (2018) 178–184
Fig. 1. Experimental setup for image ac-
3.3 quisition of the bubble-mineral particle in-
3.1 teractions; (a): (1) Compressed-air filter; (2)
Saturator vessel; (3) Flat glass cell; (4)
White-light source; (5) Stereomicroscope
coupled to a digital camera; (6) Monitor for
image reproduction. (b): Details of the flat
glass cell - (3.1) Mineral grain holder; (3.2)
Mineral particle; (3.3) Inlet for injection of
3.2 aqueous dispersion of NBs and deionized
3.4
water; (3.4) Inlet for injection of aqueous
dispersion of MBs; (3.5) Inlet for genera-
tion/injection of MaBs.
Source: Adapted from Azevedo et al.
3.5 (2016b).
phosphate were the reagents used for the quantitative determination of
P2O5.
High purity lumps of apatite (Ca5 (PO4)3(OH, F, Cl)) and quartz
(SiO2), both from southern Brazil, were used to investigate bubble-
mineral interactions. Samples of phosphate ore for the flotation studies
were collected from Tapira (Vale Fertilizers, South Brazil), from a feed
flotation circuit, after comminution, classification, low intensity mag-
netic separation, attrition and desliming stages. More than 98% of the
sample consisted of particles smaller than 200 # (75 μm), with 37% in
the 400 # fraction (37 μm). The mean diameter (D50) of the particles
was 55 μm, while the D80 was 100 μm. The average sample content was
8.4% P2O5. Quartz samples for flotation were prepared from rock
crystals from Lajeado (South Brazil). The quartz particles were frac-
tioned using Mesh Tyler sieves, and the particle-size distribution of each
fraction was measured in a Cilas 1064 laser particle size analyzer. A
−48 + 100# fraction was used in the flotation studies with a mean
diameter (D50) of 290 µm.
Fatty acid soap from soybean oil was used as the collector for
phosphate and gelatinized corn starch was used as gangue mineral
depressant. A 10% NaOH solution was used for pH adjustment. In the
quartz flotation studies, the collector was the commercial reagent
Flotigam EDA 3B (Clariant®), an alkyl ether monoamine.
2.2. Methods
2.2.1. Chemical analyses
The P2O5 content was determined by molecular absorption spec-
trophotometry based on the reaction of the phosphate with a solution
containing ammonium molybdate and ammonium metavanadate in an
acid medium.
2.2.2. Studies of quartz and apatite bubble-adhesion
The experimental setup, shown in Fig. 1, was a modified technique
previously reported by our group (Azevedo et al., 2016a) and consisted
of a system that allowed the injection of different types of bubbles into a
flat glass cell. The visualization was possible using a stereomicroscope
(Zeiss Stemi SV 11) and a digital camera (Sony NEX 3). A strip of graph
paper, as a size reference for measuring the size of the larger bubbles,
was attached at the bottom of the cell. Glass tubing (0.5 cm in diameter
and 15 cm in length) containing either quartz or apatite particles ad-
hered to its end was inserted into the cell through a hole at the top.
Additionally, the cell contained two more orifices for injecting the
bubbles.
Nanobubbles (NBs - mean diameter 150–200 nm) and microbubbles
(MBs - mean diameter 40 μm) were generated by the depressurization
of DI water, previously saturated with air at various saturation pres-
sures for 30 min (Psat; Psat = 2.5 bar for NBs and Psat = 4.0 bar for
A.F. Rosa, J. Rubio
Fig. 2. Micrographs of bubbles - apatite particle adhesion: (a) Only with MaBs; (b) with NBs + MaBs; (c) with MBs; (d) with MBs + MaBs; (e) with NBs + MBs; (f)
with NBs + MBs + MaBs.
MBs). The steel saturation vessel was equipped with an internal con-
tainer made of glass (40 cm high, 10 cm diameter, and 0.5 cm thickness;
0.7 L effective capacity). The concentration, mean size and size dis-
tribution of the NBs were measured in quadruplicate in a nanoparticle-
tracking analysis (NTA) instrument (NanoSight LM10 & NTA 2.0
Analytical Software, Malvern Instrument Ltd, Salisbury, UK) at room
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Minerals Engineering 127 (2018) 178–184
temperature. The microbubbles, were measured using the LTMBSizer
following the technique developed, in our group, by Rodrigues and
Rubio (2003).
The depressurization-cavitation stage was performed at a 2-mm
internal diameter needle valve (Globo 012-Santi®, São Paulo, Brazil)
and MBs and NBs were generated in a glass column, as described by
A.F. Rosa, J. Rubio Minerals Engineering 127 (2018) 178–184

Fig. 3. Micrographs of bubbles - quartz particle adhesion: (a) Only with MaBs; (b) with NBs + MaBs.

Table 3
Flotation of apatitic ore: P2O5 recoveries and grades at different conditions. SD = standard deviation.
Condition [Collector]; [Depressant] (g·t−1) Distribution of bubbles used P2O5 Recovery (%) SD P2O5 Content (%) SD

1 1000; 600 MaBs 87.2 0.9 16.9 0.3

NBs + MaBs 88.3 2.9 16.2 1.2
MBs + MaBs 91.8 1.9 16.2 1.0
NBs + MBs + MaBs 96.1 2.9 15.0 0.4

2 500; 300 MaBs 78.3 1.9 26.3 2.6

NBs + MaBs 76.1 0.7 26.4 0.1
MBs + MaBs 84.7 0.2 21.6 0.7
NBs + MBs + MaBs 86.5 2.0 25.0 0.5

Fig. 4. Apatitic ore flotation studies: P2O5 recovery as a function of time in the STD (MaBs) tests and with combinations of different sized bubbles (NBs + MaBs,
MBs + MaBs, NBs + MBs + MaBs); pH 9.5. (a) Condition 1–28% solids; [collector] = 1000 g t−1; [depressant] = 600 g t−1; (b) Condition 2–28% solids; [col-
lector] = 500 g t−1; [depressant] = 300 g t−1. For standard deviations, see Table 3.

181
A.F. Rosa, J. Rubio
Fig. 5. Flotation studies of the fraction -48 + 100 # of quartz in a mechanical
cell: Recovery as a function of time in tests with MaBs and with NBs + MaBs.
Conditions: pH 6.2; 12% w/w solids; impeller speed = 1000 rpm; air
flow = 6 L min−1; amine concentration = 0.5 mg g−1.
Calgaroto et al. (2014). The MBs were separated from the NBs after
5 min of rising and the microbubbles abandoning the glass column, as
in Calgaroto et al. (2015). The macrobubbles were formed by flowing
compressed air through a micro porous filter (Fig. 1b, item 3.5) and
sized by microscopy.
During the studies, conditioning with nanobubbles was carried out
with the mineral grains by contact for 3 min before the injection of the
other bubbles (Table 1).
2.2.3. Flotation of the apatitic ore
The studies were conducted with the combined injection of NBs,
MBs and MaBs, compared to standard tests (STD) where only MaBs
were used. The combinations of the types of bubble distributions
evaluated were: (i) NBs + MaBs; (ii) MBs + MaBs; (iii)
NBs + MBs + MaBs. A factorial experiment evaluated two concentra-
tions of reagents (Table 2), totaling 8 trials (in duplicate). The bubbles
were generated by the methods discussed above.
STD flotation studies using MaBs
Fig. 6. Graphical representation of main mechanisms involved in the flotation assisted by nanobubbles. Modified from Pourkarimi et al. (2017) and Xiong (2014).
182
Minerals Engineering 127 (2018) 178–184
The tests were performed in a mechanical cell, Darma-Denver,
model D12 (2 L), with pulps containing 28% (w/w), under agitation
(1000 rpm) for 4 min. Reagent conditioning was performed in the same
flotation cell. The pulp, at 60% solids (w/w) and pH 9.5, was condi-
tioned for 5 min with the depressant and 1 min with the collector at
1000 rpm. Flotation was started with the injection of air (5–7 L min−1)
and collection was done using a hand scraper, obtaining three con-
centrates (0–1.5 min, 1.5–3.0 min; 3.0–4.0 min). The volume in the cell
was kept constant with the injection of water (pH 9.5). Concentrates
and tailings were filtered, dried and prepared for chemical analyses.
Studies of flotation with injection of nano and macrobubbles
Tests with NBs were performed following the procedure of the STD
test, but an aqueous dispersion of NBs was used, rather than tap water.
Studies of flotation with injection of micro and macrobubbles
These tests were similar to the STD, but with MBs injection via a
hose connected from the discharge valve of the saturator vessel, used to
generate MBs, to the side entrance of the flotation cell. 400 mL of the
volume of the adjusting water for solids concentration was replaced
with an aqueous dispersion of MBs. In addition, another 4 injections of
100 mL each, were performed at the following times: 0.5; 1.0; 2.0 and
3.0 min.
Studies of flotation with injection of nano, micro and macro-
bubbles
In these studies, the water for pulp preparation, conditioning, di-
lution and cell level control were replaced by aqueous dispersions of
NBs. MBs were injected according to the conditions described in the
previous item.
2.2.4. Flotation of quartz
Standard flotation tests were conducted similarly to those described
for phosphate flotation studies. However, the pulp contained 12% so-
lids, pH was kept at 6.2, the quartz conditioning time with Flotigam
EDA 3B (0.5 mg g−1 quartz) was 2 min and the air injection into the cell
was 6 L min−1. Studies of flotation (in duplicate) with injections of
nano and macrobubbles were performed accordingly
3. Results and discussion
3.1. Studies of bubbles-apatite/quartz interactions
Figs. 2 and 3 show micrographs of bubbles attaching to particles of
A.F. Rosa, J. Rubio
apatite and quartz, respectively. As expected, there was no adhesion of
the macrobubbles on apatite or quartz particles in deionized water. This
is related to the short residence time of the bubbles at the collision-
adhesion stage (necessary for water film displacement) and also due to
the lack of attraction forces between hydrophobic bubbles and hydro-
philic particles.
After the interaction between apatite or quartz grains and nano-
bubbles, although adhered, the photographic technique cannot (as ex-
pected) visualize them in the microscope. However, the population of
macrobubbles increased greatly after conditioning both minerals with
nano and microbubbles. This enhancement reinforces the role of na-
nobubbles as “activators” or “collectors” of particles in flotation (Fan
and Tao, 2008; Fan et al., 2010a,b,c,d; Fan et al., 2012; Azevedo et al.,
2016a,b). These adhesions of bubbles were probably proceed by long-
range interactions and formation of bubble-particle bridges (Krasowska
et al., 2007; Nguyen et al., 2003).
Results also showed that the combination of NBs + MBs + MaBs
provided the highest bubble capture by the apatite grain, while that of
NBs + MaBs was responsible for the increase of bubbles adhered to
quartz. This large population of bubbles should contribute to increase
the probability of flotation since the density of bubble-particle ag-
gregates should decrease considerably. In addition, the roughness of
apatite and quartz grains, because of their surface cavities, porous
surfaces and etching, appear to allow micro and nano sized bubble
entrainment/entrapment, inside the holes of the surfaces, probably as a
result of the high superficial free energy. The micrographs in Fig. 2 also
show a rapid growth of microbubbles due to the mass transfer of re-
sidual dissolved air leading to coalescence of the bubbles, in agreement
with the conceptual model of formation and growth of MBs proposed by
Rykaart and Haarhoff (1995) and also reported by Oliveira et al.
(2014).
3.2. Apatitic ore flotation studies
Table 3 summarizes the results of phosphate flotation with different
combinations of bubble sizes.
Table 3 shows that the combined use of bubbles in apatitic ore
flotation increased the P2O5 recovery under practically all conditions
when compared to STD tests. Results are in agreement with the bubble-
particle adhesion study. Best results depended on the distributions of
the type of bubble employed. The combined use of NBs + MBs + MaBs,
in this order was the condition that guaranteed the best separation
parameters, especially P2O5 recoveries.
Moreover, using half of the reagent concentration, P2O5 recovery
achieved with the combination of the three types of bubbles (86.5% -
condition 2) was only 0.7 percentage points lower than that obtained in
the STD test with the full concentration of reagents (87.2%) in condi-
tion 1. This fact confirms the role of nanobubbles in the conditioning
stage and flotation of apatite ores with reduction of the conventional
collector concentrations required, as reported in others studies (Fan
et al., 2010c; Sobhy and Tao, 2013; Ahmadi et al., 2014). Regarding the
kinetic flotation data, Fig. 4 shows that, with the combinations of
bubbles and at the optimal collector concentration, the maximum P2O5
recoveries were obtained within the first 1.5 min, whereas in the STD
(only macrobubbles) these recoveries were reached only after 4 min of
flotation.
Fan et al. (2010c) obtained similar results in phosphate column
flotation studies, where in addition to conventional bubbles generated
with a static mixer, the nanobubbles generated in a cavitation tube
were injected. In all ore fractions, the P2O5 recoveries in the presence of
nanobubbles were higher than in the absence of these bubbles.
Results for the kinetics of phosphate ore flotation validate the re-
sults of rapid bubble attachment observed in the photographic study
and the recoveries obtained during the first minute and a half were
higher than the standard test. Moreover, the presence of nanobubbles,
allowed a higher recovery of fine fractions (37% of feed was less than
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Minerals Engineering 127 (2018) 178–184
37 μm).
3.3. Bench quartz flotation studies
Studies showed that after conditioning with nanobubbles, higher
flotation recoveries than those with the standard (∼23%) were ob-
tained. More, similar to flotation in the apatitic ore, the quartz con-
ditioning with nanobubbles increased about two times the mass re-
covered in the standard, with only macrobubbles (Fig. 5).
The results of the present work reinforce the theory of “surface
conditioning” provided by nanobubbles, causing better (and rapid)
adhesion of coarser bubbles, highly improving flotation recoveries and
kinetics. Moreover, before flotation, the finest particle fraction appears
to aggregate and trap nanobubbles inside these aggregates. All these
mechanisms are illustrated in Fig. 6.
Summarizing, the role of nanobubbles appears to be significant for
mineral flotation. As nanobubbles have far-reaching application in
mineral and environmental science, a thorough understanding and
mastery of the stability, interfacial properties and potential applications
of nanobubbles is the premise of future research. Nowadays, there ap-
pear to be reliable technologies to generate nanobubbles at a high rate
with sustainability, a great challenge that might facilitate the industrial
use of nanobubbles in flotation (Azevedo et al., 2016a,b; Etchepare
et al., 2017, Oliveira et al., 2018). Another topic deserving attention is
the understanding the best point for the injection of the nanobubbles;
grinding, classification or conditioning stages appear to be other pos-
sibilities.
4. Conclusions
The technique of bubble visualization of surfaces of apatite and
quartz grains showed nucleation and growth of microbubbles (70 μm
mean diameter) and an increase of the population of macrobubbles
(1 mm mean diameter) but only after conditioning with nanobubbles
(150–200 nm, mean diameter). This study validated the theory of
“surface conditioning” whereby bulk nanobubbles appear to attach
rapidly at pulverized mineral surfaces mainly if they are hydrophobic
surfaces. Herein, the nanobubbles enhanced the attachment of larger
bubbles and, as a result, increased flotation recovery and process ki-
netics. Accordingly, almost 95% P2O5 recovery was reached at the first
1.5 min, 9% higher than the maximum flotation in the standard tests, at
4 min. Quartz conditioned with nanobubbles increased flotation re-
coveries by approximately 23% when compared to the standard test. In
the first min, the recovery of the quartz particles was about twice that
obtained in the standard. It is believed that the nanobubbles have good
potential in mineral flotation.
Acknowledgements
The authors would like to thank all the Brazilian Institutes sup-
porting this research, namely CNPq and UFRGS. Special thanks to Vale
Fertilizers in Tapira for providing the phosphatic ore sample, to
Professor Frank Heinrich for the minerals samples and to all students at
our laboratory and the friendly atmosphere.
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