Mining, Metallurgy & Exploration

https://doi.org/10.1007/s42461-020-00247-0

REVIEW

A Critical Review on the Mineralogy and Processing

for High-Grade Quartz
Min Lin 1 & Ziyuan Liu 1 & Yan Wei 1 & Bin Liu 1 & Yu Meng 1 & Hang Qiu 1 & Shaomin Lei 2 & Xun Zhang 3 & Yubiao Li 2

Received: 25 February 2019 / Accepted: 9 June 2020

# Society for Mining, Metallurgy & Exploration Inc. 2020

Abstract
High-purity quartz (SiO2) is an important material widely used in many industries, including semiconductor technology, tele-
communication, and optics. The content and distribution of impurities in quartz significantly affect the processing methods. This
paper provides an insightful review on the processing of high-purity quartz, covering the analytical techniques, separation
methods, and the critical procedures used to assess the quality of quartz ore. More importantly, the critical review of the thermal
phase transition separation method for fine-grained mineral inclusions, micron-grade fluid inclusions, and lattice-bound trace
elements is notably opened for the first time. It is proposed that the research field as a monopolized industry would benefit by
expounding the critical problems that occur during the preparation of high-purity quartz.

Keywords High-purity quartz . Analysis technique . Fluid impurity . Lattice impurity

1 Introduction processing techniques due to their similar surface properties

High-purity quartz (HPQ, SiO2) is an important material wide-
ly used in semiconductor technologies, high temperature lamp
tubing, thin-film transistor-liquid crystal display (TFT-LCD),
telecommunications, and optics [1]. Common quartz ores
(vein quartz, quartz sandstone, etc.) inferior to crystal-grade
quartz have been used to prepare HPQ owing to the exhaus-
tion of high-grade quartz resources and a growing demand in
the modern technology industries [2, 3].
However, common quartz ores usually contain various
mineral and lattice impurities [4]. It is therefore necessary to
combine physical (e.g., magnetic and flotation separation) and
chemical (e.g., acid leaching) methods to remove these impu-
rities [3, 5, 6]. For instance, it is very difficult to separate trace
mica and feldspar from quartz ores by conventional
* Yubiao Li
Yubiao.Li@whut.edu.cn
1
Wuhan BOE Optoelectronics Technology Co., Ltd., Wuhan 430040,
People’s Republic of China
2
School of Resources and Environmental Engineering, Wuhan
University of Technology, Wuhan 430070, People’s Republic of
China
3
Jiangsu Kaida Quartz Co., Ltd., Xinyi 221400, People’s Republic of
China
[7, 8]. The non-metallic element H, as a widely distributed
impurity, exerts an extremely negative effect on the prepara-
tion of fused silica product [9–11]. Commonly, trace element
H is mainly from the widely distributed fluid inclusions and
Si–OH. However, the removal of H, especially those from
micro fluid inclusions and atomic micro-cluster, has not been
paid adequate attention [12, 13]. In addition to the non-
metallic elements (e.g., H, B, and P), certain amounts of me-
tallic elements, such as Al, Fe, Ti, Ca, Mg, K, Na, and Li, can
be found in quartz lattices [14–17]. Traditional procedures
consisting of combination methods unavoidably lead to high
cost and unreliable product quality. Hence, fluorides are often
used in the flotation and acid leaching processes to raise sep-
aration efficiency [18–20]. However, the fluorides released
into the waste water show significantly negative influence
on the surrounding environment [21, 22]. Therefore, a clean
strategy to produce HPQ is urgently required.
Thus far, many challenges remain regarding the character-
ization and high-efficiency separation of lattice impurities,
although various analysis and separation techniques for
lattice-bound trace elements in HPQ have been developed
[23, 24]. Hence, an insightful review covering analysis and
separation strategies concerning the mineral, fluid, and lattice
impurities to assist in producing HPQ is provided.

2 Analytical Techniques
Many modern analytical techniques are widely applied in de-
termining the distribution and concentration of mineral phase
and fluid impurity in HPQ. Figure 1 shows the equipments
covering optics, acoustics, spectroscopy, and mass spectrom-
etry that are effective in characterizing mineral and fluid in-
clusions embedded in quartz [12, 25–28].
2.1 Mineral and Fluid Impurities
PM is widely applied in the mineralogy analysis of quartz ores
to investigate the type and distribution of impurities [3, 13,
29]. However, the gangue minerals can only be ascertained in
a semi-qualitative level by PM due to the birefringence char-
acteristics of different minerals [30]. In addition, an enormous
amount of time is consumed on locating the associated min-
erals within the quartz [8]. EMP equipped with PM shows
great advantages in the mineralogy analysis of quartz ores
because it saves locating time significantly. PM is used to
identify the type of gangue minerals, while the EMP is applied
to analyze the components of associated minerals by energy
dispersive spectroscopy (EDS) or wavelength dispersive spec-
troscopy (WDS), as well as the distribution characteristics
using the backscattered electron model [31–33]. Some non-
transparent minerals contained in quartz slices can be quickly
located by PM, and then analyzed by EMP. However, it is
difficult to efficiently distinguish similar transparent minerals,
including feldspar and mica, in quartz at the PL model.
Common EMP equipped with PM can only analyze quartz
slices at plane-PL model rather than the XPL model. At the
XPL model, transparent silicate minerals are quickly distin-
guished and located due to their bright interference colors.
Fig. 1 Recommended analysing techniques during process mineralogy of
quartz ore. XRD, X-ray diffraction; PM, polarizing microscopy; PL, po-
larized light; XPL, crossed and polarized light; EMP, electron micro-
probe; La-RS, laser Raman spectroscopy; D-ICP, decrepitation method-
inductively coupled plasma analysis; PY-GC/MS, pyrolysis gas
chromatograph/mass spectrometry; SEM-CL, scanning electron
Mining, Metallurgy & Exploration
Therefore, the analytical accuracy is raised from the semi-
qualitative level to qualitative level via combining
the advantages of PM and EMP. More importantly, the anal-
ysis efficiency can be greatly improved.
However, EMP is limited in analyzing the fluid inclusions
in quartz [34] mainly due to the permeation power (1–3 μm)
of the electron beam because most fluid inclusions range from
micrometers to tens of micrometers. In addition, many factors,
including the thickness of quartz slice, size, and location of
fluid inclusions, decrease the analytical accuracy of EMP on
fluid inclusions to qualitative and semi-quantitative levels
[34]. For instance, the fluid inclusions regularly distributed
on the surface of quartz slices cannot be analyzed by EMP.
Moreover, the fluid may be polluted during the polishing pro-
cess of the quartz slice.
In contrast, some other methods including LA-ICP-MS,
PIXE, and La-RS can be used as effective in situ analysis
methods for fluid inclusions in quartz. In contrast to LA-
ICP-MS and PIXE, the La-RS is not limited in analyzing
components of fluid inclusions greater than 50 μm [35, 36].
The La-RS is not only used to investigate small molecules
(CO2, N2, CH4, etc.) trapped in fluid inclusions but also to
distinguish anions (NO3−, CO32−, SO42−, etc.) at room tem-
perature and cations (Na+, K+, Ca2+, Mg2+, etc.) at low tem-
perature [37–39]. However, the contents of the anions and
cations in host quartz cannot be ascertained by the La-RS.
The acoustic decrepitation method is an important tech-
nique used to measure the decrepitation temperature of fluid
inclusions in opaque minerals. This method uses a sound re-
corder to record the decrepitation frequency of fluid inclusions
at different temperatures to ascertain the critical
activation temperature of the fluid impurities [12, 40].
However, previous research shows that fluid inclusions in
microscope-cathodoluminescence; AAS, atomic absorption spectrosco-
py; ICP-OES/MS: inductively coupled plasma-optical emission
spectroscopy/mass spectrometry; LA-ICP-MS, laser ablation-
inductively coupled plasma-mass spectrometry; Micro-FTIR, micro-
Fourier transform infrared spectroscopy; SIMS, secondary ion mass
spectroscopy
Mining, Metallurgy & Exploration
quartz can be obviously triggered by phase transformation at
approximately 573 °C [41]. Therefore, calcination at
600~700 °C is effective in removing fluid inclusions from
the superficial layer of quartz particle, but can only activate
the fluid inclusions from the interior of quartz particles, dif-
fusing to the closed fractures to re-equilibrate [12]. Thus, an
activation temperature of fluid inclusions in quartz can be
obtained by the acoustic decrepitation method, rather than
the critical temperature at which the fluid inclusions are re-
leased. Although the crepitation of fluid inclusions is recorded
to define the “decrepitation temperature” when the host min-
erals are calcined at 600~700 °C, this does not mean
that mineral salts such as NaCl [42] from fluid inclusions
can be separated from the host mineral in the later washing
process.
Recent research [43] shows that the critical temperature,
which has instructive significance on separating fluid inclu-
sions from quartz, is obtained by the decrepitation-ICP anal-
ysis (D-ICP) method rather than the indirect acoustic decrep-
itation method. For the D-ICP, quartz sands calcined at differ-
ent temperatures were leached by ultrapure water, and then the
leach liquors were analyzed by ICP (OES or MS) to calculate
separation efficiencies of typical elements (Na, Ca, Mg, etc.)
occurred in the fluid inclusions of quartz. Research results
indicate that calcination at 900 °C, rather than 700 °C, is
supported to remove fluid inclusions from quartz effectively.
During the heating process from room temperature to 700 °C,
quartz phase transition can trigger the decrepitation of fluid
inclusions [12, 40]. Some fluid inclusions were not removed
from quartz because the fluid inclusions were only re-
equilibrated in the β-quartz stability field, giving a density loss
due to the α–β phase transition. The calcination temperature
of 900 °C is obtained by D-ICP technique according to the
optimal separation efficiency and can reflect the actual releas-
ing temperature of fluid inclusions. Therefore, both the cations
contents and critical temperature can be accurately ascertained
by the D-ICP technique.
However, the D-ICP method shows little effect for some
fluid inclusions (H2O-CO2/N2/SO2/SO3/CH4) not containing
mineral salts. Pyrolysis gas chromatograph/mass spectrometer
(PY-GC/MS) is commonly used to investigate the critical re-
lease temperature for these small molecules during calcina-
tion. The critical temperature is supported to be the releasing
temperature of fluid inclusions from quartz particles during
calcination as the small molecules are included in the quartz
fluid inclusions [44]. Similar to the D-ICP technique, the
method has directly instructive significances on separating
fluid inclusions from quartz.
Hence, the identification of the main mineral and fluid
impurities in common quartz ores, by combining advantages
of different analysis instruments including PM, EMP, La-RS,
D-ICP, and PY-GC/MS, can be explored in detail. More
importantly, the systematic research on process mineralogy
of HPQ shows great significance for quartz processing.
2.2 Lattice-Bound Trace Elements
Lattice-bound trace elements in quartz grains mainly includes
substitutional ions (Al3+, Fe3+, B3+, Ti4+, Ge4+, P5+) of Si4+
and interstitial ions (Li+, K+, Na+, H+, Fe2+) that act as charge
compensators for the substitutional ions Al3+, Fe3+, P5+, etc.
[45]. There are four theoretical configurations for these trace
elements bound in quartz lattice accepted by most researchers:
simple substitution (Ti4+ or Ge4+ = Si4+), coupled substitution
(Al3++P5+ = 2Si4+), silanol groups (4H+ = Si4+), and charge-
compensator substitution in the interstice of Si–O tetrahedron
(Al3++Li+ (Na+, K+) = Si4+; B3++H+ = Si4+; Fe3++K+ = Si4+)
[10, 46–48]. The existing studies support that the common
trace impurities occur in the form of the diamagnetic [AlO4/
M+]0 center (M+ = H+, Li+, Na+) in the Si–O interstitial posi-
tion of quartz [49–53]. In addition, other impurity centers in
quartz are possibly associated with substitutions between Si
and metal Ti, Ge, and Fe [49–53].
The variation of scanning electron microscope-
cathodoluminescence (SEM-CL) intensity are responsible for
structural defects, many of which are directly or indirectly
caused by the incorporation of trace elements in the quartz
lattice [54]. A previous study [55] shows that CL-
spectroscopy revealed five possible emission bands that are
important in quartz. Ultra-violet to blue luminescence between
330 and 400 nm reveals a relationship between CL intensity
and concentration of M+ (H+, Li+, Na+, K+) and Al as the
[AlO4|M+] defect center in quartz [56, 57]. Blue to bluish-
green luminescence at the 450 and 505 nm is supported to be
caused by self-trapped excitations and SiH-groups [58, 59].
However, a convincing correlation of these emission bands
with a distinct defect in the bulk crystal has not been found to
date. Greenish-yellow luminescence at 580 nm is assumed to be
caused by the enrichment of primary fluid inclusions and
patchy luminescence [60]. Brown to reddish luminescence be-
tween 630 and 650 nm is assigned to non-bridging oxygen hole
centers [61]. An additional band in the near infrared at 710 nm
is likely caused by the incorporation of Fe3+ [62].
Many impurity-related defects can be detected and modi-
fied by irradiation [55]. The common view is that the UV
emission at 395 nm seems to be affected by Al-defects, and
water-related defects may be partly responsible for emission at
650 nm. Previous research focused on establishing an effec-
tive relationship between CL-spectroscopy and lattice defects
to directly analyze trace elements occurred in natural quartz.
Although each defect may provide additional energy levels in
the band gap, a confidential assignment of distinct defects to
the emission bands remains difficult [55].
The LA-ICP-MS technique provides an effective method
to show the relations between concentration variations of trace

elements and their CL textures at a micron level using both
spot analyses and trace element maps [54, 63]. Combining
SEM-CL and LA-ICP-MS, confidential relationships of lat-
tice defects and the emission bands in quartz can be
ascertained in detail. As shown in Fig. 2, the SEM-CL image
of quartz (McLaughlin, CA epithermal deposit) combined
with LA-ICP-MS provides a clear message that the CL tex-
tures are affected by the distribution of trace elements bound
in quartz lattice. This supports that the concentration of metal
Al is positively correlated with trace Li, Na, K, and Cs, but
negatively correlated with Ga [54]. The boxed area in Fig. 2
shows the CL texture where the trace element maps were
obtained [54]. Unfortunately, LA-ICP-MS cannot be used to
analyze micro regions <50 μm and the trace element H due to
spot size and mass spectrometer ability. Some micron-, sub-
micron-, and nanometer-gangue minerals and fluid inclusions
may lead to a seriously negative impact on the distribution
analysis of trace elements occurred in quartz lattice. Hence,
accurate trace element analysis in quartz can be achieved by
further reducing the spot size of the laser and increasing its
ablation capacity.
In addition to the trace element distribution, the analysis for
the content of trace elements has attracted much attention
[64–66]. Spectroscopic methods, including AAS and ICP-
OES, show great advantages on the content analysis of main
trace elements (Al, P, S, Fe, Ti, Cu, etc.) in quartz. However,
massive detection errors are caused by mutual interferences of
different elements, especially for light or alkali metal elements
(e.g., B, Na, Mg, Ca, K). The ICP-MS technique can reliably
detect trace elements (Li ~ U) at the ppb level while reducing
the mutual interferences [65, 66]. However, the three detection
methods are only suitable for analyzing liquid samples, rather
than solid quartz. Solid quartz (bulk quartz or quartz sand) has
to be digested by strong acid (HF, HNO3, etc.) prior to anal-
ysis. The systematic error caused by the pollution from water
Fig. 2 SEM-CL image and LA-ICP-MS trace element maps of quartz from the McLaughlin, CA, epithermal deposit [54]
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and particles during the dissolution process is inescapable. A
pressure-tight dissolution method using ultrapure water and
chemical reagents [67] is suggested to deal with the solid
quartz sample because it can avoid the main water and particle
pollution. Compared with LA-ICP-MS, ICP-MS can provide
the content of all trace elements for the whole quartz sample,
rather than a micro-zone in quartz.
More attention should be paid to investigating the concen-
tration, occurrence, and separation method of trace element H
in quartz because of its negative effects on quartz wares [67].
In contrast to all analysis techniques mentioned above, micro-
FTIR is the only in situ technique to quantify H concentration
and occurrence [10, 11, 68]. However, there are four main
problems in the application of micro-FTIR in quartz mineral-
ogy. Firstly, other trace elements cannot be simultaneously
quantified [54]. Secondly, there are a number of complications
in data quantification [11, 54]. In addition, the resolution of
this technique is on the order of 50 μm [54, 68]. Moreover, it
requires special sample preparation and inclusion-free quartz
[54]. Fortunately, the detection accuracy of micro-FTIR has
been greatly improved with the development of more sophis-
ticated infrared generators and sensors. Another instrument
that can be used to map H distribution is the secondary ion
mass spectroscope (SIMS). The spatial resolution of SIMS is
intermediate between EMP and LA-ICP-MS, with a typical
spot size of 10–15 μm [17, 36, 54]. However, the main draw-
back of the SIMS technique is that no standards are available
to quantify quartz trace elements.
3 Separation Processes
Extensive research studies [69–73] suggest that trace lattice
elements, fine-grained minerals, and fluid inclusions occurred
in the interface and interior of quartz are difficult to remove by
Mining, Metallurgy & Exploration
conventional processing methods, hindering the preparation
of HPQ using high-grade quartz. The fine-grained impurities
are closely included in quartz grains so that they can only be
removed under exacting conditions. Although high tempera-
ture, high pressure, and HF have been used for further pro-
cessing of high-grade quartz [18, 74, 75], separation rates and
efficiencies of the impurities remain limited by the special
occurrences of fine-grained inclusion impurities. Moreover,
migration and separation mechanisms of trace elements bound
in quartz lattice are rarely reported. Therefore, it is necessary
to summarize the main obstacles of quartz processing to draw
more research attention to HPQ.
3.1 Mineral Impurities
3.1.1 Interface Impurities
Fine-grained gangue minerals occurred in the interface of
quartz grains, mainly including feldspar, mica and hematite,
can be efficiently separated by flotation, magnetic separation,
and conventional leaching processes when the mineral impu-
rities have been exposed or liberated by crushing and grind-
ing. Flotation and magnetic separation are commonly used to
process low-grade quartz ores, or as a pretreatment technique
to purify quartz because they show low selectivity on separat-
ing the fine-grained gangue minerals [7, 69, 76]. Chemical
leaching is an effective method to selectively remove mineral
impurities from quartz interfaces, and shows great advantages
on dissolving aluminosilicate minerals and surface irons from
intergrowth of quartz and the impurities. Fluoric or catalytic
pressure leaching is considered as one of the most effective
processes for some fine-grained impurities that are not liber-
ated during crushing and grinding processes, because these
methods can leach the impurities along the crystal interface
of quartz [29, 73, 77]. In addition, some thermal treatment
techniques, such as oxidizing calcination, are widely applied
in the primary processing of high-grade quartz with the pur-
pose of activating the inert mineral impurities. Using calcina-
tion, the mineral impurities not only can be exposed or liber-
ated from quartz grains but also transformed into active sub-
stances or structures to be efficiently dissolved during chem-
ical leaching.
3.1.2 Fine-Grained Mineral Inclusions
Fine-grained gangue minerals (especially mica, Fig. 3) includ-
ed in quartz grains are difficult to remove using common
chemical leaching. First, quartz samples are commonly
ground to specific sizes rather than small enough due to the
demands of downstream industries. Usually, the larger the
size, the higher the value of quartz sand. At the specific size,
liberation degrees of the fine-grained gangue minerals are se-
verely limited, resulting in low separation efficiencies [75,
78]. Although high-temperature calcination is used to build
migration channels of the fine-grained gangue minerals in
the micro-cracks, effects of conventional chemical leaching
processes are strictly controlled by the very tiny migration
channels providing important exchange opportunity for
leaching agents and impurity ions.
Leaching processes enhanced by microwave, ultrasonic,
thermal power, and pressure have been developed to efficient-
ly separate intractable fine-grained mineral impurities includ-
ed in quartz in recent years [80–84]. Among these techniques,
pressure leaching is the most widely used and effective tech-
nique for high-grade quartz processing. In general, quartz sand
is calcined at 700~900 °C, and then leached by fluoric solu-
tions or acid-NH4Cl solutions. The leaching agents are dif-
fused into the quartz interior along micro-cracks caused by
calcination. At the same time, mineral impurities are inten-
sively released at high temperature and pressure. The pressure
leaching process shows high selectivity on removing fine-
grained gangue minerals but retaining the major structure of
quartz particles (Fig. 4). Moreover, the tiny micro-cracks can
be further developed into relatively broad migration channels
during the pressure leaching. The broad migration channels
lead to a high exchange rate for the leaching agents and im-
purity ions.
3.2 Micron-Grade Fluid Inclusions
Micron-grade fluid inclusions (Fig. 5) can be removed by
high-temperature calcination, which commonly leads to a
high cost [13]. Some inorganic salts (NaCl, KCl, CaCl2,
etc.) occurred in fluid inclusions might react with active quartz
solution to form inert Si–O–Na, Si–O–K, and Si–O–Ca struc-
tures above 900 °C. Moreover, the micron-grade fluid inclu-
sions deep in the quartz grains are not released at the conven-
tional 700 °C of calcination. Previous studies indicate that the
phase transition of quartz could trigger the decrepitation of
fluid inclusions [12, 13, 40].
Phase transition between β-quartz and β-tridymite at
870 °C shows great significance in removing micron-grade
and nanometer-grade fluid inclusions because the activation
energy of releasing fluid inclusions is intensively reduced dur-
ing the phase transformation. Furthermore, the tiny fluid
inclusons hold sufficient energy to break the bonds of Si–O–
Si at 870 °C. More importantly, the iterative phase transition
between β-quartz and β-tridymite by controlling calcination
temperature can promote a series of decrepitations of the
micron-grade and nanometer-grade fluid inclusions. For some
aggregative fluid inclusions (Fig. 5(a)), high-temperature cal-
cination contributes to more migration channels. The impuri-
ties remaining in migration channels are further removed by
chemical leaching. The iterative phase transition also shows a
positive influence on separating asphalt inclusions in quartz
grains from sedimentary rock (Fig. 5(b)).

Fig. 3 Fine-grained mica
inclusions in quartz grain: (a)
secondary electron image, (b) Al
distribution [79]
The fluid and mineral impurities can be effectively re-
moved by combining high-temperature calcination with pres-
sure leaching. Iterative heat shock at high temperature pro-
motes decrepitation of micron-grade fluid inclusions and
phase transforms of gangue minerals from the crystal state to
amorphous state. Commonly, fluid inclusions and layer sili-
cate minerals in quartz ores show great thermal expansion
performances during the high-temperature calcination, which
usually lead to abundant micro-fractures. Meanwhile, the
micro-fractures formed during high-temperature calcination
provide important migration channels for the impurities re-
maining in quartz particles. Moreover, the pressure leaching
process commonly shows 98% or higher efficiency in remov-
ing mica/feldspar from quartz ores, obviously better than the
flotation processes [73]. Although the application of pressure
leaching is limited in high-grade quartz processing due to its
high cost, the process shows a very strong ability to purify the
quartz ores in which the fine-grain gangue minerals are closely
included. Compared with conventional leaching processes,
pressure leaching consumed less chemical agents but remov-
ing more impurities. Lin et al. [3, 78] introduced NH4Cl into
the pressure leaching of hydrothermal quartz and expressed a
novel opinion which suggests that NH4+ can further reduce
agent consumption by its hydrolysis triggered by high temper-
ature and Si–O− structure. It should be noted that more
Fig. 4 Secondary electron images of quartz particle containing inclusion impurities after fluoric pressure leaching
Mining, Metallurgy & Exploration
efficient and stable liquid catalytic agents (e.g., NH4Cl) during
the pressure leaching requires more attention to intensively
reduce agent consumption and increase separation efficiency.
3.3 Trace Lattice Elements
Trace elements bound in quartz lattice are the most intractable
impurities because the advanced hot chlorination process can
only selectively remove alkali metal impurities [9, 23, 67, 73].
Lin et al. [67] analyzed the reasons for the low removal effi-
ciency by investigating five possible substitutions (Fig. 6) in
α-quartz based on density function theory. The results support
that low removal rates of Al3+ and Ti4+ are mainly caused by
lower lattice energies relative to the original Si–O–Si structure
because the two elements are strictly limited inside the Si–O
structure. However, alkali metal ions, including Li+, Na+, and
K+, act predominantly as charge compensators for the trivalent
substitutional ions Al3+ and Fe3+ and can be efficiently re-
moved by hot chlorination due to relatively weak limitation
of the Si–O–Si structure. Non-metal elements H, B, and P can
also be efficiently removed by oxidizing calcination due to
their unstable oxidation states at high temperature.
Separation of alkali metal elements (M+) from solid quartz
phase by the hot chlorination process is mainly based on the
ion exchange of M+ and H+. The H+ can be easily diffused into
Mining, Metallurgy & Exploration

Fig. 5 Micron-grade fluid

inclusions and organic matter in a
quartz sandstone

(a) aggregative fluid inclusions (b) asphalt included in quartz grain

(XPL) (PL)

quartz lattice due to its minor radius when alkali metal ele-
ments are removed from quartz grains [73]. Efficient chlori-
nating agents, including NaCl and KCl, have been used to
purify high-grade quartz based on an effective exchange be-
tween K+ (Na+) and Al3+ (Fe3+, Ti4+) [24, 67]. The crystal
structure of quartz can be intensively destroyed by cations,
promoting a rapid phase transition from α-quartz to β-quartz
or cristobalite. The phase transition can also lead to abundant
crystal defects in the form of a mesoporous and active inter-
face, which provides a possible position for phase separation.
The cations (K+ or Na+) from chlorinating agents can be re-
moved by chlorine or hydrogen chloride gas to achieve a
comprehensive removal of alkali metal elements and structure
impurities. It should be noted that the dosages of NaCl and

(Si=Al+Li) (2Si=Al+P) (Si=B+H)

(Si=4H) (Si=Ti)
Fig. 6 Simulation images of five substitutions in α-quartz [67]
 Mining, Metallurgy & Exploration

Table 1 Main literature related to

quartz analysis and processing Classification Author and year Research field

Quartz analysis XRD [1, 6, 9] Quartz deposit

PM [3, 13, 29] Quartz mineralogy
EMP [31–33] Quartz mineralogy and processing
La-Rs [35, 36] Fluid inclusions in quartz
D-ICP [12, 13, 40–43] Fluid inclusions in quartz
PY-GC/MS [44] Fluid inclusions in quartz
SEM-CL [45, 53] Trace elements distribution
AAS [64] Trace elements content
ICP-OES/MS [65, 66] Trace elements content
La-ICP-MS [54, 63] Trace elements distribution
Micro-FTIR [10, 11, 68] Trace elements distribution
SIMS [54] Trace elements distribution
Quartz processing Magnetic separation [29] Fe-bearing impurities separation
Flotation [7, 69, 76] Silicate mineral separation
Oxidizing calcination [12, 13, 40] Fluid inclusion separation
Chemical leaching [29, 73, 77] Interface impurities separation
Enhanced leaching [80–84] Fine-grained mineral inclusion separation
Decrepitation [12, 13, 40] Micron-grade fluid inclusion separation
Hot chlorination process [9, 23, 73] Trace lattice element separation

KCl applied in quartz processing must be strictly limited. In
addition, the H+ remaining in quartz sand can be removed by
calcining quartz in a pure O2 atmosphere.
Owing to the cationic pollution of NaCl and KCl, HPQ
researchers are once again attracted to the dangerous hot chlo-
rination process (using chlorine or hydrogen chloride gas).
However, the contradiction between diffusion rate and reac-
tion rate of lattice impurities at 1200~1500 °C has become an
unavoidable issue. Moreover, they are also two important in-
dexes that reflecting the separation effects of lattice impurities
during conventional hot chlorination process of quartz. On the
basis of the mature hot chlorination process, how to signifi-
cantly reduce reaction time and increase removal efficiencies
of lattice Al and Fe become the focus.
In the conventional hot chlorination process, quartz
sand is ordinarily heated to temperatures of
1000~1200 °C in a chlorine or hydrogen chloride gas
atmosphere [9, 23, 73]. The main trace metallic ele-
ments (e.g., Al3+, Fe3+, Ti3+, and Ti4+) bound in quartz
lattice diffuse to the surface/interface of quartz grains
and then react with Cl− to be removed as low-boiling
chlorides [73, 85]. The chemical reaction is strictly lim-
ited by the low diffusion rate of metallic elements to
surface/interface because the binding ability of the
s i l i c o n - o x y t e t r a h e d r o n r e m a in s g re a t e v e n a t
1000~1200 °C [67]. At higher temperature
(1200~1500 °C), solid quartz sand would evidently melt
to form a solid solution, which intensively increases the
bulk density of quartz particles due to reduced total
porosity [86]. The solid solution loses a lot of interfaces
where lattice impurities would react with Cl−, although
the metallic elements have been activated. The chlorina-
tion rate is actually lower at higher temperature. Hence,
the contradiction between the diffusion rate and reaction
rate of lattice impurities in quartz is the most critical
problem that urgently needs to be solved.
The application of adequate thermal phase transition of
quartz to increase diffusion rates of lattice elements is novel
and effective in solving the contradictory situation. The β-
quartz at 820 °C is rapidly heated to temperatures of 920 °C
to form β-tridymite, then rapidly cooled down to temperature
of 820 °C. The heating procedure (820~920 °C) is repeated
tens times to achieve iterative phase transitions between β-
quartz and β-tridymite. Although β-quartz and β-tridymite
belong to the hexagonal system, β-quartz of the hexagonal
bipyramid is transformed into β-tridymite of the hexagonal
plate and then transformed back to the β-quartz. During this
repeated phase transition process, trace elements bound in
quartz lattice are continuously activated with the iterative
break and recovery of some special Si–O bonds. The special
phase transition leads to a direct and continuous external dif-
fusion of the lattice impurities from quartz. Activation ener-
gies of the lattice impurities are significantly reduced by reg-
ular breaking of Si–O bonds during the phase transition of
quartz. Rapid phase transition can also leads to abundant crys-
tal defects that result in an obvious change in density and
Mining, Metallurgy & Exploration

Table 2 Advantages and application of analytical techniques in quartz processing

Analytical Advantages used in quartz field Application in quartz processing

techniques

XRD Suited for analyzing gangue minerals (>5 vol%), not unstructured or organic impurities Crystal impurities with high
contents
PM Judge or speculate the type and distribution of impurities semi-qualitatively Semi-qualitative analysis &
impurities location
EMP Judge or identify impurities types qualitatively Mineral and fluid inclusion
La-Rs identification
D-ICP Analyze decrepitation temperature and components of fluid inclusions Fluid inclusions analysis
PY-GC/MS
SEM-CL Judge impurities types qualitatively and analyze distribution trace elements in crystal quartz Impurity identification and trace
element distribution
AAS Analyze contents of impurity elements quantitatively Impurity content (analysis
sensitivity: ppm ~ ppb)
ICP-OES/MS Impurity content analysis (analysis
sensitivity: ppm ~ ppt)
La-ICP-MS Judge or identify the type and distribution of impurity elements qualitatively, and analyze Trace element analysis in
contents of impurity elements quantitatively micro-zone (analysis sensitivity:
ppm ~ ppt)
Micro-FTIR In situ technique to quantify H concentration and occurrence H concentration in micro-zone
SIMS Mapping H distribution H distribution

provide a more activated crystal interface for surface enrich-
ment and phase separation of lattice impurities.
A chlorine or hydrogen chloride gas atmosphere is com-
monly used in conjunction with the thermal phase transition to
duly remove metallic elements enriched in the surface/
interface of quartz grains. Another method is to use
hydrofluoric acid or phosphoric acid solutions, rather than
dangerous chlorine or hydrogen chloride gas, to purify ther-
mally activated quartz sand. Elevated temperature and pres-
sure are very necessary in the leaching process because many
lattice elements are enriched around crystal interfaces. The
processing technique of quartz sand using hot phosphoric acid
has been focused on in recent years due to its low cost, high
efficiency, and “green” property [87–89].
In summary, the hot chlorination process using a chlorine
or hydrogen chloride gas atmosphere can only provide favor-
able separation conditions rather than activation conditions.
Major structural lattice elements, including Al, Fe, and Ti,
are strictly bound in quartz because diffusion rates of the
structural lattice elements remain slow at 1000~1200 °C. By
contrast, alkali metal elements, as charge compensators, can
be easily activated and removed because they are only bound
by the weak electrovalent bonds. Compared with the hot chlo-
rination process, the KCl-doping calcination can activate
structural lattice elements effectively during the phase transi-
tion of quartz. Regrettably the KCl-doping calcination process
commonly leads to cationic pollution. Distinguished from the
two processes, the thermal phase transition-chlorination/pres-
sure leaching processes can intensively activate the intractable

Table 3 Conceptual flow

diagram of quartz processing Flow diagram Impurity Product grade

(1) Mining Washing Clay mineral, etc. –

(2) Crushing Desliming Clay mineral, etc. 90~99%

(3) Grinding Screening Gangue mineral liberation –
(4) Magnetic separation Flotation 1. Fe-bearing impurities 99~99.99%
2. Silicate mineral
(5) Oxidizing calcination Decrepitation Fluid inclusion –
(6) Chemical leaching Enhanced leaching 1. Interface impurities 99.99%
2. Fine-grained mineral inclusion
(7) Hot chlorination process Lattice impurities >99.999%

structural lattice elements, including Al, Fe, and Ti, to surface/
interface of quartz grains by reducing activation energy and
effectively remove them by solid/gas or solid/liquid
separations.
4 Quartz Processing Summary
4.1 Critical Literature about High-Grade Quartz
Processing
From Sects. 2 and 3 in this article, some of the main
literature related to quartz analysis and processing are
summarized in Table 1. In addition, the advantages
and application of analytical techniques in quartz pro-
cessing are shown in Table 2. It is proposed that, by
integrating the analysis methods and processing process-
es of quartz, the research field as a monopolized indus-
try would benefit.
4.2 Conceptual Flow Diagram of Quartz Processing
Traditionally, some retreatment processes are used to purify
quartz ore, such as crushing and washing (desliming). After
the retreatment processes, quartz ore can be ground to appro-
priate size according to the product market. On the basis of
mineralogical analysis, a conceptual flow diagram of quartz
processing is shown below (Table 3).
4.3 Actual Production of High Grade Quartz
Common procedures of quartz processing mainly include
crushing, grinding, screening, desliming, high-intensity mag-
netic separation, reverse flotation, chemical leaching, wash-
ing, drying, oxidizing calcination, hot chlorination, and pack-
ing [73, 77, 90]. However, several issues seriously hinder the
development of the HPQ industry. First of all, the commercial
process of HPQ is easily polluted by particles and liquid from
the environment and equipment. In general, quartz processing
after desliming is only allowed to proceed in clean working
rooms at the electronic industry level. The pollution can be
reduced by regular cleaning, personnel training, equipment
cleaning, air filtration, and air current control. Moreover,
chemical agents used in flotation, leaching, and calcination
unavoidably contain some metallic elements that may reduce
the quality of quartz sand dramatically [79]. Hence, washing
and drying are always the last two but most important proce-
dures assuring the quality of quartz sand products.
Meanwhile, ultrapure water is the most conventional detergent
in washing and must be ensured to meet the standard of
18.2 MΩ cm. Besides counter-current washing, ultrasonic
and microwave can be applied as enhanced methods in the
washing procedure to improve washing efficiency [79, 90].
Mining, Metallurgy & Exploration
Quartz sand after washing can be dried by air, vacuum, and
heating dehydrations. Air dehydration is commonly used to
dry rough concentrate of quartz sand because this method is
high in dehydration efficiency and low in cost, although the air
must still be filtrated to remove possible impurities. Vacuum
and heating dehydrations are used to remove water and agents
remaining in quartz concentrate avoiding particle pollution. In
summary, the HPQ can only be produced by combining in-
dustrial engineering and management systems perfectly.
5 Conclusions
This paper provides an insightful review on HPQ processing,
focusing on summarizing the analysis techniques of mineral,
fluid, and lattice impurities, their advantages and disadvan-
tages, and providing recommended analysis methods in min-
eralogy. In addition, the dissecting techniques and mecha-
nisms of separating impurities from quartz interfaces and in-
clusions were discussed. Moreover, this paper emphasizes the
importance of quartz assurance in HPQ manufacturing. It is
proposed that the research field as a monopolized industry
would benefit by expounding the critical problems that occur
during the preparation of HPQ.
Acknowledgements Financial support was provided by the National
Natural Science Foundation of China (51974215, 51774223, 51604205).
Compliance with Ethical Standards
Conflict of Interest The authors declare that they have no conflict of
interest.
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