Mater. Res. Express 10 (2023) 035005 https://doi.org/10.

1088/2053-1591/acbf98

PAPER

Anhydrous MgCO3: Controllable synthesis of various morphology

OPEN ACCESS
based on hydrothermal carbonization
RECEIVED
30 September 2022
Yunhua Lu1 , Qiuyan Bi2,∗, Qingwei Zhang1 and Zhihao Wan2
REVISED 1
26 January 2023
School of Artificial Intelligence, Chongqing University of Technology, Chongqing, People’s Republic of China
2
School of Chemical Engineering, Qinghai University, Xining 810016, People’s Republic of China
ACCEPTED FOR PUBLICATION ∗
Author to whom any correspondence should be addressed.
27 February 2023
PUBLISHED
E-mail: bqy1110@163.com
10 March 2023
Keywords: anhydrous MgCO3, morphology control, hydrothermal carbonization
Supplementary material for this article is available online
Original content from this
work may be used under
the terms of the Creative
Commons Attribution 4.0
licence. Abstract
Any further distribution of A novel, simple and efficient anhydrous MgCO3 (AMC) synthesis method using ascorbic acid (ASA)
this work must maintain
attribution to the has been developed based on the hydrothermal carbonization. In this process, ASA acts as both a CO2
author(s) and the title of
the work, journal citation
source and a crystal modifier to regulate and control the crystallization of AMC. Furan derivatives,
and DOI. aldehydes and ketones from ascorbic acid play an unexpected role as a structure-directing agent. The
effect of pH values of ASA, reaction time and the concentrations and types of Mg2+ were systematically
investigated. Pure AMC with different morphology were successfully prepared.

1. Introduction

Magnesium carbonate is a class of materials, including anhydrous magnesite (MgCO3), nesquehonite

(MgCO3·3H2O), lansfordite (MgCO3·5H2O) and hydromagnesite (Mg5(CO3)4(OH)2·4H2O). So far, except
anhydrous MgCO3 (AMC), the latter three have been widely utilized in various industrial applications (e.g.,
pharmaceuticals, rubber industry, lithographing inks, and as precursors for other magnesium-based chemicals
[1]). Up to now, immense research interests have focused on the production of these hydrated magnesium
carbonate with various morphologies (e.g., needles [2], rods [3], flakes [4] and microspheres [5]) by
precipitation, carbonization or hydrothermal methods [6, 7]. Actually, AMC possess more advantages
compared with hydrated ones owing to their higher CO2 storage capability and thermodynamic stability. In
addition, since AMC inherently have characteristics such as good thermal absorption, excellent fire
extinguishing property via releasing a great deal of CO2 and pollution-free, they are the attractive candidates as a
new kind of inorganic flame retardant [8]. However, almost no ready-made AMC products with high quality
and purity are available in the current market. One of the major reasons is that it is difficult to be properly
prepared under mild conditions. Further, the natural mineral magnesite always accomplished with certain of
impurities like Fe2+ and Mn2+. Herein, it is urgent to explore the techniques for AMC synthesis.
However, only a few reports are correlated with the synthesis of AMC, which are typically prepared under
harsh conditions such as high CO2 partial pressure (∼10 MPa), high temperatures (>150 °C), and/or long
reaction time (>12h), with the products lacking size, morphology or structure homogeneity [9, 10]. Liang et al
[11] successfully synthesized the AMC under 3GPa and 800 °C for 1h based on the MgCO3·3H2O, whereas Lou
et al [12] prepared the single crystal of AMC under 500 °C for 20 h by mixing the MgCO3 powder, metallic
sodium and carbon tetrachloride,. Swanson et al [13] investigated the effect of seed particles on fabricating AMC
under 80 °C–150 °C and 3.0 MPa CO2 partial pressure. Moreover, only irregular shape and the rhombohedral
morphology with size between 1–30 um of AMC have been reported in these works. It is known that
multifunctional inorganic materials extensively applied in diverse fields usually possess well controlled
morphologies [14, 15], and the properties of particles are often associated with their shapes [16, 17]. Therefore, it
is crucial to design and fabricate inorganic materials with desirable shapes and sizes for practical applications. In
our previous study, three different morphologic AMC particles have been prepared and their effect on the

© 2023 The Author(s). Published by IOP Publishing Ltd

Mater. Res. Express 10 (2023) 035005 Y Lu et al

Figure 1. The schematic of morphology control of anhydrous MgCO3.

properties of PVC have been investigated [18]. In order to extend their application, AMC particles with more
special morphologies are necessary to be developed. In the current study, preparation conditions are
systematically investigated, and the results demonstrated that uniform AMC with different morphology could
be obtained without additional additives and CO2 source under mild conditions. As shown in figure 1, different
AMC can be prepared by hydrothermal carbonization.

2. Experimental

2.1. Materials
L(+)-ascorbic acid, sodium hydroxide, magnesium sulphate (MgSO4) and magnesium chloride (MgCl2) were
purchased from Adamas Chemical Reagent Co., Ltd., (Shanghai, China). Deionized water was prepared in our
lab using a water purifier (RD0R0100, RephiLe Bioscience, Co., Ltd., Shanghai, China).

2.2. Preparation of anhydrous MgCO3

First, 7.5 g of L(+)-ascorbic acid was dissolved in 50 ml of deionized water, and then 5 mol l−1 NaOH was
utilized to adjust pH values before adding a certain of MgSO4 or MgCl2. Then the mixture was added into a
Teflon-lined autoclave and hydrothermally treated at 180 °C for several hours and the synthesis conditions for
AMC are summarized in table S1. Finally, the obtained solid products were separated by centrifugation, washed
several times with deionized water, and finally dried at 100 °C for 24 h.

3. Results and discussion

3.1. Effects of pH values

A series of AMC particles have been synthesized under different conditions, and the summary of conditions is
shown in table S1. To investigate the effect of pH values of ASA on the morphology of products, the experiments
were performed at 180 °C for 3 h. The results are shown in figure 2 for MgSO4 as Mg2+ source and figure 4 for
MgCl2 as Mg2+ source, respectively.
In figure 2, AMC particles show different morphologies at different pH values. When the pH value is
relatively low, the AMC are irregular blocks as shown in figures 2(A)–(C). A dramatic shape change occurs when
the pH value increases to 10.5, which produces string-like crystals with a length of 0.5–0.8 um accumulated by
small lamella (figure 2(D)). Remarkably, as the previous reported [18], well-defined monodisperse dumbbell-
like AMC with a length of 1.0–1.5 um assembled by small polyhedrons (figure 2(E)) are obtained when pH value
is 12.5. Further increasing the pH value to 13.5, the morphology of AMC shows like hydrangea consisting of
sheet-like structures with the diameters in the range of 0.8–1.0 um [18]. Figure 3 show the particle size
distribution of AMC, which is in accordance with the SEM results.
Similarly, the pH values of ASA exert substantial influence on the morphology of AMC particles obtained
from MgCl2 system as shown in figure 4. Spindle-like AMC with size in the range of 8.0–20.0 um (figure 4(a)) are
produced when the pH value is 5.5, whereas when the pH value reaches 7.0, crystals with spindle shape attach to
each other and form the irregular particles just as displayed in figure 4(b). At pH 8.5, microspheres assembled by
many polyhedrons (figure 4(c)) are produced. Obviously, the size of the crystals shows a tendency to decrease
with the increase of the pH in comparison between figures 4(a)–(c) and (d)–(f). In figure 4(d), AMC particles
with size between 0.5–1.0 um exhibit irregular shape. And rod-like AMC with rough surface (figure 4(e)) are
obtained when pH value increases to 12.5, while hydrangea-like AMC (figure 4(f)) similar to figure 2(F) are
produced under pH value of 13.5. Figure 5 show the particle size distribution of AMC, which is in agreement
with the SEM results.

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Figure 2. SEM images of AMC with different morphology obtained under varying pH values: (A) pH = 5.5, (B) pH = 7.0, (C) pH =
8.5, (D) pH = 10.5, (E) pH = 12.5, (F) pH = 13.5 and the inset is at a higher magnification. Reaction conditions: T = 180 °C, c
(MgSO4) = 1.0 mol l−1 and t = 3 h.

Figure 3. Particle size distribution of AMC obtained under varying pH values: (A) pH = 5.5, (B) pH = 7.0, (C) pH = 8.5, (D) pH =
10.5, (E) pH = 12.5, (F) pH = 13.5. Reaction conditions: T = 180 °C, c(MgSO4) = 1.0 mol l−1 and t = 3 h.

Corresponding XRD patterns of AMC in the presence of varying pH values are shown in figures 6(A) and (B).
All products are identified as pure AMC both using MgSO4 and MgCl2 as magnesium source on condition that
the pH values are higher than or equal to 7.0. Moreover, the pH value is higher, the crystallization peak is
stronger, indicating the crystallinity is better.
When the pH value of ASA is relatively low („7.0), HCO− 3 is the major ion in the system while CO 3
2−
–2
mainly exists in the high pH conditions [17]. Consequently, only limited Mg and CO3 can combine with
2+

each other to form MgCO3 particles, and then they will aggregate to meet the rule of lowest energy and grow

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Figure 4. SEM images of AMC with different morphology obtained under varying pH values: (A) pH = 5.5, (B) pH = 7.0, (C) pH =
8.5, (D) pH = 10.5, (E) pH = 12.5, (F) pH = 13.5 and the inset is at a higher magnification. Reaction conditions: T = 180 °C, c
(MgCl2) = 1.0 mol l−1 and t = 3 h.

Figure 5. Particle size distribution of AMC obtained under varying pH values: (A) pH = 5.5, (B) pH = 7.0, (C) pH = 8.5, (D) pH =
10.5, (E) pH = 12.5, (F) pH = 13.5. Reaction conditions: T = 180 °C, c(MgCl2) = 1.0 mol l−1 and t = 3 h.

in size to form stable phase (figures 2(A)–(B) and 4(a)–(b)). At the high pH condition, the quick dissolution
of CO2 results in a high supersaturation, which leads to a rapid formation of small MgCO3 precipitates [17].
Because of the high surface energy of these small MgCO3 particles, they prefer to aggregate together to form
irregular polyhedron via specific hydrogen bonding and favorable adsorption interactions [19, 20]. Then
under the driving of crystal facet selective adsorption and similar orientation attachment modes [21], these
irregular polyhedrons can further assemble into different morphological MgCO3 as shown in figures 2(C)–
(F) and 4(c)–(f). In other words, organic molecules (furan derivatives, aldehydes and ketones decomposed
from ASA) can adhere to the surface of small MgCO3 particles via electrostatic interaction and then lead to

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Figure 6. XRD patterns of AMC in the presence of varying pH values. Reaction conditions: (A) T = 180 °C, c(MgSO4) = 1.0 mol l−1
and t = 3h; (B) T = 180 °C, c(MgCl2) = 1.0 mol l−1 and t = 3h.

Figure 7. SEM images of AMC with different morphology obtained with varying MgSO4 concentration (mol l)−1: (A) c = 0.6, (B)
c = 1.0, (C) c = 1.4, (D) c = 2.2 and the inset is at a higher magnification. Reaction conditions: T = 180 °C, t=3h and pH = 12.5.

the reduction of surface energy and the inhibition of the growth of surfaces in this direction, and finally
contributes to the formation of various morphologies.

3.2. Effects of Mg2+ concentration

As shown in figure 7, the morphology and the size of the products are affected by the MgSO4 concentration.
When the concentration is 0.6 mol l−1, monodisperse corncob-like AMC with the length of 0.8–1.2 um
(figure 7(A)) are obtained. However, when the concentration increases to 1.0 mol l−1, crystals display dumbbell
shape as described before in figure 2(E). Furthermore, short rod-like AMC assembled by small lamella are
produced under concentration of 1.4 mol l−1. Increasing the concentration to 2.2 mol l−1, homogeneous cubes
accumulated by layers are observed in figure 7(D) [18]. The particle size distribution of AMC is shown in
figure 8.
Figure 9 shows the influence of MgCl2 concentration on the morphology of AMC, clearly, which is not as
remarkable as that of MgSO4. In comparison among figures 9(a)–(d), all crystals exhibit rod-like shape with

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Figure 8. Particle size distribution of AMC obtained with varying MgSO4 concentration (mol l): (A) c = 0.6, (B) c = 1.0, (C) c = 1.4,
(D) c = 2.2. Reaction conditions: T = 180 °C, t = 3h and pH = 12.5.

Figure 9. SEM images of AMC with different morphologies obtained with varying MgCl2 concentration (mol l)−1: (a) c = 0.6, (b)
c = 1.0, (c) c = 1.4, (d) c = 2.2 and the inset is at a higher magnification. Reaction conditions: T = 180 °C, t = 3h and pH = 12.5.

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Figure 10. Particle size distribution of AMC obtained with varying MgCl2 concentration (mol l)−1: (a) c = 0.6, (b) c = 1.0, (c) c = 1.4,
(d) c = 2.2. Reaction conditions: T = 180 °C, t = 3h and pH = 12.5.

Figure 11. XRD patterns of AMC in the presence of varying(A) MgSO4 and (B) MgCl2 concentration. Reaction conditions: T = 180
°C, pH = 12.5 and t = 3h.

rough surface. The particle size distribution of AMC is shown in figure 10, which is as observed as the SEM
results.
XRD results of all products prepared in the presence of varying Mg2+ concentrations are shown in
figures 11(A) and (B), indicating the Mg2+ concentration place no impact on the crystal phase of AMC.
In comparison between figures 7 and 9, it can be seen that under the same reaction conditions, AMC
prepared in MgSO4 and MgCl2 system almost shows different morphologies, which is mainly associated with
influence of Cl− and SO2− 4 on the interaction with crystal face [22]. On the other hand, when the concentration
of Mg2+ is same, the concentration of Cl− in the MgCl2 system is twice higher than SO2− 4 in the MgSO4 system.
−
The large number of Cl might put obstacles on the collision between organic molecules (aldehydes, ketones
and furan derivatives) decomposed from ASA and MgCO3 crystals, resulting in the limited shape-controlled
effect. Obviously, the concentrations of Mg2+ also can significantly modify the morphology of AMC especially

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Figure 12. SEM images of AMC with different morphology obtained under varying reaction time (h): (A) t = 2, (B) t = 3, (C) t = 6, (D)
t = 9 and the inset is at a higher magnification. Reaction conditions: T = 180 °C, c(MgSO4) = 1.0 mol l−1 and pH = 12.5.

for MgSO4 system. The higher the concentration of Mg2+ in the reaction system, the greater collision
frequencies among different ions and formation of more aggregates. With this reaction, organic molecules
absorbed on aggregates will reduce their surface energy, which is conducive to the further aggregation and
mineralization into different morphology.

3.3. Effects of reaction time

Figures 12 and 14 show the SEM images of AMC synthesized at 1.0 mol lmol l−1 and 180 °C for 2 h, 3 h, 6 h and 9
h. According to the SEM images, corncob-like AMC, as the major phase, are observed with a mixture of a few
dumbbell-like particles in figure 12(A). As the reaction time extends to 3 h, complete dumbbell-like AMC
(figure 12(B)) are obtained; however, when the reaction time further extends to 6h and 9h, the shape of AMC
changes into double-hemisphere. The corresponding XRD results are shown in figure 16(A), indicating that all
products are pure AMC. Figure 13 shows the corresponding particle size distribution, which is consistent with
the SEM results.
Figure 14 shows the impact of reaction time on the morphology of AMC based on the MgCl2 as magnesium
source. When the reaction time is 2 h, there is just some uniform blocks. And the corresponding XRD pattern
shown in figure 10(B) indicates that these particles are mainly Mg3O(CO3)2. When the reaction time extends to
3, 6 and 9 h, the morphology of products shows like short rod and the longer the reaction time is, the smoother
the surface of the crystals is as shown in figures 12(b)–(d). Also, the XRD results (figure 16(B)) demonstrate that
when the reaction time is longer than 2 h, pure AMC can be prepared. Corresponding particle size distribution is
shown in figure 15.
The reaction time plays an active role in regulating the morphology of AMC. When the reaction time is in the
range of 2–3 h, crystals possess rough surfaces and 0nonequilibrium shapes as shown in figures 12(A)–(B) and
14(a)–(b). With the reaction time extending, these crystals have the possibility to rearrange into a more stable
phase. In comparison between the AMC obtained at 6 h and 9 h both for MgSO4 and MgCl2 system, similar
morphology and size are observed, indicating they are the stable phase in that conditions.

3.4. Possible crystallization process

In this study, the pH value of ASA, types and concentrations of Mg2+ and the reaction time act as crucial roles in
regulating and controlling the morphologies of the AMC particles. In this process (figure 17), CO2 from the ASA
−
can be converted into CO2− 3 by OH , and then the remaining organic molecules (aldehydes, ketones and furan

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Figure 13. Particle size distribution of AMC obtained under varying reaction time (h): (A) t = 2, (B) t = 3, (C) t = 6, (D) t = 9. Reaction
conditions: T = 180 °C, c(MgSO4) = 1.0 mol l−1 and pH = 12.5.

Figure 14. SEM images of AMC with different morphology obtained under varying reaction time (h): (a) t = 2, (b) t = 3, (c) t = 6, (d)
t = 9 and the inset is at a higher magnification. Reaction conditions: T = 180 °C, c(MgCl2) = 1.0 mol l−1 and pH = 12.5.

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Figure 15. Particle size distribution of AMC obtained under varying reaction time (h): (a) t = 2, (b) t = 3, (c) t = 6, (d) t = 9. Reaction
conditions: T = 180 °C, c(MgCl2) = 1.0 mol lmol l−1 and pH = 12.5.

Figure 16. XRD patterns of AMC in varying reaction time. Reaction conditions: (A) T = 180 °C, pH = 12.5 and c(MgSO4) = 1.0 mol
l−1; (B) T = 180 °C, pH = 12.5 and c(MgCl2) = 1.0 mol l−1

derivatives) decomposed from ASA can sequester Mg2+ due to the high local concentration of Mg2+, resulting in
the reduction of the collision frequency among different ions but also the formation of small MgCO3 aggregates.
Simultaneously, these organic molecules serve as agglomerant or structure-directing agent to arrange MgCO3
aggregates to assemble into different morphological MgCO3 particles [23].

4. Conclusion

In this study, a novel, green, and economical MgCO3 synthesis method was developed based on hydrothermal
carbonization approach, in which ASA served as both the CO2 source and the crystal modifier. Then the effect of
reaction time, pH values of ASA and the concentrations and types of Mg2+ were systematically investigated, and

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Figure 17. The Schematic illustration of different structure of AMC.

the resulting products were fully characterized. Pure anhydrous MgCO3 with different morphologies can be
obtained under different conditions. Significantly, this method provides the possibility to realize the industrial
production of anhydrous MgCO3 by using different available magnesium source.

Acknowledgments

This research is financially supported by the Foundation from Qinghai Science and Technology Department
(2021-ZJ-939Q), Scientific Research Foundation of Chongqing University of Technology (2020ZDZ026), the
National Nature Science Foundation of China (U22A20434), NSFC Cultivation Program of Chongqing
University of Technology (2021PYZ30), Thousand Talents Program of Qinghai Province, Scientific Research
Fund of Young Teachers in Qinghai University (2020-QGY-6).

Data availability statement

The reseach is still not finishe. The data cannot be made publicly available upon publication because they are
owned by a third party and the terms of use prevent public distribution. The data that support the findings of this
study are available upon reasonable request from the authors.

ORCID iDs

Yunhua Lu https://orcid.org/0000-0003-1879-215X

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