An evaluation of the effects of microstructural characteristics and frost

heave on the remediation of saline-alkali soils in the Yellow River Delta,

China

Author names：Kesheng Li, Quanxin Li, Yuhan Geng, and Chuanxiao Liu

Author affiliations：College of Water Conservancy and Civil Engineering, Shandong Agricultural

University, Tai'an 271018, Shandong, China

*Corresponding author: Chuanxiao Liu: Email: lchuanx@163.com

Declarations：

Funding:

This work was supported by the National Natural Science Foundation of China [grant number 51574156] and

the Key Development Program for Research of Shandong Province [grant number 2018GNC110023].

Conflicts of interest/Competing interests:

The authors declare that they have no conflicts of interest.

Availability of data and material:

The data used to support the findings of this study are available from the corresponding author upon request.

This article has been accepted for publication and undergone full peer review but has not been
through the copyediting, typesetting, pagination and proofreading process which may lead to
differences between this version and the Version of Record. Please cite this article as doi:
10.1002/ldr.3801

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Abstract

In the Yellow River Delta of China, soil salinization is of serious concern from both agricultural and

environmental perspectives. In this study we investigated the microstructural characteristics of saline-alkali

soils in this region and explored the influence of frost heave on soil microstructure. Soil mineral composition,

pore distribution, particle arrangement, and pore characteristics were measured using X-ray diffraction (XRD),

mercury intrusion porosimetry (MIP), and scanning electron microscopy (SEM). Soil pore characteristics,

overall porosity, and unconfined compressive strength (UCS) were measured at water content of 10, 15, 20,

25% (w/w) before and after freezing at –10 ℃. The results showed that deterioration of soil physical properties

was largely caused by dense particle arrangement, high proportion of ultra-micropore-specific surface area,

and poor pore distribution, rather than mineral content or particle size distribution. The microstructure of

saline-alkali soil was greatly improved by frost heave with the overall porosity and UCS of frost heave-treated

soil samples significantly higher than for the control. Moreover, particle cementation decreased with

increasing soil water content. This study demonstrated that a combination of XRD, SEM, and MIP offers

accurate evaluation of the microstructural characteristics of saline-alkali soils, and frost heave may serve as an

economically sustainable and technically feasible method for saline-alkali soil amelioration in the Yellow

River Delta.

Keywords: saline-alkali soil; XRD; SEM; MIP; frost heave; Yellow River Delta

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1 Introduction

Soil salinization is one of the most significant global problems limiting agricultural production and

environmental construction. Salinized soil is present in more than 100 countries and regions, covering a total

area of 1 billion hectares (Qadir et al., 2006; Xia et al., 2019). Salinized soils are barren and unsuitable for

planting crops, severely restricting the development of agricultural production in several countries and have

considerable negative impacts on ecosystem health (Wang et al., 2017). The degradation of soil properties

results in low permeability, high bulk density, and dispersion of soil particles, which are the main factors that

limit the utilization of saline-alkali soil globally (Brinck & Frost, 2009; Ganjegunte et al., 2014; Qadir &

Schubert, 2002). Current remediation practices or management measures for saline-alkali land primarily

include irrigation, addition of sediments, chemical remediation, organic amendments, and planting

salt-tolerant species (Ahmad et al., 2013; Heng et al., 2018; Li et al., 2019; Oo et al., 2013; Srivastava et al.,

2014; Yang et al., 2018). At present, it is generally believed that an effective control measure is the addition of

gypsum and fly ash to saline-alkali soils (Murtaza et al., 2017; Temiz & Cayci, 2018); however, the associated

high costs and environmental pollution are issues of concern, particularly in developing countries (Pandey et

al., 2009).

China has approximately 340,000 km2 of saline-alkali soil, which accounts for about 25.20% of cultivated

land. These saline-alkali soils are distributed primarily in northern China, particularly in the Yellow River

Delta (Mao et al., 2016). Saline-alkali land accounts for 70% of the total area of the Yellow River Delta (Fan et

al., 2012; Yao & Yang, 2010). The remediation of saline-alkali land in the Yellow River Delta depends, for the

most part, on a hydraulic engineering approach; however, the lack of freshwater resources make such measures

gradually lose their efficacy. Although the application of crop residues is considered to be the most effective

saline-alkali land remediation practice in the region, its widespread adoption is currently limited by the lack of

sufficient crop residues and concerns regarding the spread of crop diseases (Mao et al., 2018). Consequently,

there is an urgent need to develop novel remediation practices that address all existing concerns.

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 Since the beginning of the 21st century, there have been several studies regarding the effects of different

factors on the microstructure of non-saline-alkaline soil (mainly offshore clay, swamp soil and loess) (Ahmed

2015; Hashemi et al., 2015; Murmu et al., 2019; Perisic et al. 2019). Among these, there is a plethora of

scientific reports on the effects of additives on soil microstructure. Jha et al. (2016) analyzed the

microstructures of clay soils and investigated the deformation characteristics of lime-improved soil in terms of

expansibility, compressibility, and permeability. Yao et al. (2019) investigated the effect of nano-MgO on the

mechanical properties and microstructure of cement-stabilized soft soil. Their results showed that the addition

of nano-MgO increased the strength of soft soil and enhanced its microstructure. Furthermore, it also has been

demonstrated that the microstructure of soil can well explain its unique engineering properties. For example,

Liu et al. (2016) characterized the mineralogy, microstructure, and particle morphology of loess soil in the

Loess Plateau region of China, to elucidate the origin of its collapse behavior. Liu et al. (2014) investigated

relationships among the types of connections between particles in the soil skeleton and the mechanical

properties of saline soils with different salt contents. They found that there are three forms of soil particle

connections, namely, point contact, stacked contact, and salt crystal cementation, of which salt crystal

cementation was demonstrated to be an important factor affecting the mechanical strength-related properties of

saline soils. Thus, it has been known that the microstructure of soil has been increasingly used as a standard to

evaluate the properties of soil in the field of civil engineering (Al-Mukhtar et al., 2012; Cuisinier et al., 2011;

Frost et al., 2019; Oualmakran et al., 2016). It has been beneficial that scholars have recently shown a great

amount of interest in soil microstructure, in the field of agriculture. Some studies have shown that soil

hydraulic properties are determined by the soil microstructure, with the pore distribution, particle arrangement

and overall porosity significantly affecting the movement and storage of water in soil (Ajayi et al., 2016; Fei et

al., 2019; Vogel & Kretzschmar, 1996;). Therefore, we assume that the resulting deeper understanding of the

microstructure of saline-alkali soil will enable us to find a new approach to remediate these soils.

In recent years, scholars have carried out in-depth research on the frost heave effect of saline-alkali soils

and have obtained significant findings. Factors such as salinity and freeze-thaw times contribute to changes in

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the structure of the soil, resulting in corresponding changes in soil properties (Liu & Zhang, 2014; Jamshidi et

al., 2016; Tang & Yan, 2015;). Changes in soil microstructure that occur due to multiple freeze-thaw cycles

result in a decrease in the shear strength, modulus of elasticity, cohesion, and other shear properties of saline

soil (Han et al., 2018). A series of studies have found that the microstructures of certain soils significantly

affect their mechanical properties; thus, frost heaves can effectively change the structural characteristics of

these soils (Kochiieru et al., 2020). In addition, researchers have carried out a more in-depth study of frozen

soil (French 1986; French et al., 2007; Liu et al., 2020d). To date, no research has hitherto been conducted to

comprehensively characterize the microstructure of undisturbed saline-alkali soils, and the effect of frost heave,

in the Yellow River Delta, China. Therefore, we hypothesize that the remediation of saline-alkali soil in the

Yellow River Delta is closely related to its microstructure; and that the frost heave effect probably improves the

microstructure and remediates these barren soils.

This study serves as the first attempt in the Yellow River Delta to demonstrate that the poor soil

microstructure is the primary challenge in the remediation of saline-alkali soil and that the frost heave effect

can be used to ameliorate soil microstructure. Specifically, our objectives were: (i) to comprehensively

evaluate the microstructural characteristics of saline-alkali soil using XRD, SEM, and MIP, and investigate the

effects of microstructure on the physical properties of these soils in the Yellow River Delta; and (ii) to explore

the effects of frost heave for various values of water content on the microstructure and mechanical properties

of saline-alkali soils.

2 Materials and methods

2.1 Study area

The study area is located in Guangrao County, Dong-Ying City, Shandong Province, China, which is a

major industrial and agricultural area of the Yellow River Delta. The geographic coordinates lie between

118°36′–118°42′ east longitudes, and 37°18′–37°19′ north latitudes. The study area is located in a warm,

temperate, semi humid zone, with a continental monsoon climate, and is characterized by large seasonal

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variations of temperature, rainfall, wind, and evaporation. The annual average temperature is 12.8 ℃, ranging

from −22.3 ℃ to 41.9 ℃,and the average annualfrost-free period is 206 days. In addition to the topsoil (0−10

cm), there is only one freeze-thaw cycle within the year, for the other depths of soil investigated. The annual

average precipitation is 555.9 mm, 65% of which is between May and August. The annual evaporation is

1900.8 mm on average, with the maximum occurring in May and the minimum in January (Sun et al. 2018).

2.2 Experimental materials

Micro test samples for microstructure analyses were collected from wastelands at distances of 5, 18, 20,

25, 28, and 30km from the Bohai Sea, designated as locations S1, S2, S3, S4, S5, and S6, respectively (Figure

1). It can be seen from Table 1 that the salt content at S1 is as high as 18.66 g kg-1 , which is much higher than

that at other locations. This implies that the saline-alkali soil at this location has not been effectively controlled

or is difficult to control. Hence, a frost heave experiment was conducted on the soil at location S1. In view of

the World Reference Base for Soil Resources (IUSS Working Group WRB, 2007), these barren soils are

customarily classified as “saline-alkali soils”, with an electrical conductivity (EC)>0.5 dS m-1 and pH>8.5

(Table 1). The deterioration of soil properties in this region is due to the excessive accumulation of salt,

especially leading to the buildup of Na+, in the soil (Mao et al. 2016). The soil saturated hydraulic conductivity

in this area is only (1.85–5.36) ×10-5 cm s-1 (Table 1), which is classified as being extremely micro-permeable

soil.

The composition of the soil is 5.47–12.43% clay, 33.35–65.30% silt, and 22.27–61.18% sand, with

particle sizes of < 0.002 mm, 0.002–0.02 mm and >0.02 mm, respectively (Table 1). The soil texture is sandy

loam (S1) and silty loam (S2–S6), according to the international standard for soil texture classification. Table 1

also lists other basic physicochemical properties of the soil in this area.

2.3 Sample preparation

2.3.1 Microscopic experiment

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 The soil samples were dried at 105 ℃, crushed, and passed through a 75 μm sieve forX-ray diffractometer

(XRD) analysis. Undisturbed soil samples were cut into cuboids measuring 8 mm × 8 mm × 15 mm, and

grooves with a prefabricated depth of approximately 1 mm were cut into the middle of the samples for a

scanning electron microscopy (SEM) analysis. The same soil samples were cut also into cuboids measuring 5

mm × 5 mm × 10 mm for a mercury intrusion porosimetry (MIP) analysis. Subsequently, each sample was

freeze-dried immediately for 48 h at – 80 °C, following the experimental procedure proposed by Delage (Dalla

et al., 2019), and was subjected to both MIP and SEM tests thereafter.

2.3.2 Freezing experiments

The samples for freezing tests were obtained from the wasteland 5 km away from the Bohai Sea (i.e.,

location S1). The topsoil is removed from the samples since the surface soil is exposed to air, and disrupted by

the natural environment and human factors. Hence, the sampling depth for this study was determined to be

40–50 cm. The soil container used for the experiments was an opaque PVC cylinder, with an inner diameter of

50 mm and a height of 120 mm. To avoid the effects of extrusion on the physical and mechanical properties of

the soil, the PVC cylinder was coated with Vaseline and inserted into the soil to a certain depth. The moisture

content of the sample was changed by the drying method and the water film transfer method, to obtain the

samples with different moisture content, at 10% (W10), 15% (W15), 20% (W20), and 25% (W25). Triplicates

of each moisture content sample were prepared.

2.4 Testing methods

The experimental procedure included measurements by XRD, SEM, and MIP, and freezing tests

including polarizing microscope (PM) and unconfined compressive strength (UCS) tests. The experimental

methodology, techniques, and devices adopted in this study are described in the following paragraphs.

2.4.1 X-ray diffractometer

An XRD was used to quantify the minerals of saline-alkali soil used for the tests, using the TD-3500

X-ray diffractometer (Dandong Tongda Technology Co., Ltd., Dandong City, China). The test conditions were

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as follows: the target was Cu(Kα1), the wavelength was 1.54 × 10-10 m, the excitation voltage and current were

40 kV and 30 mA, respectively, the scanning range was 5–60°, the step width was 0.02°, and the scanning

speed was 2° min-1 .

2.4.2 Scanning electron microscopy

The freeze-dried SEM samples were fractured along the centrally created grooves, and the soil particles

on the surface were gently removed using suction balls. The sections with smoother surfaces were selected for

the SEM analyses. The spatial allocation of pores and particles in the saline-alkali soil was directly observed at

a micro-scale by SEM, including the pore characteristics, particle morphology, and particle connection forms.

The SEM device used was the Quanta250 scanning electron microscope (FEI Company, US).

2.4.3 Mercury intrusion porosimetry

In the present study, we measured soil porosity and pore size distribution using MIP. Compared with

traditional methods, the pore size distribution of soil was obtained directly from the MIP analysis, and the

measured pore diameters range from 7nm to 350 μm. It is also possible to use the MIP analysis to determine

other important characteristic parameters, such as total porosity, permeability, compressibility, fractal

dimension, and pore tortuosity.

The freeze-dried MIP samples required no additional treatment and were ready to use for the mercury

intrusion analysis. The pore radius was obtained from the intrusion pressure using Washburn's equation (1),

thereby enabling a plot of the pore volume–pore diameter curve and pore specific surface area–pore diameter

curve to illustrate the percentages of different pore sizes.

2σ cos θ
p= − (1)
r

where p is the applied pressure, σ is the coefficient of surface tension of the immersed liquid, θ is the

contact angle between the liquid and solid materials, and r is the cylindrical pore radius. The values of σ and θ

used in this study were 0.485 N m-1 and 140°, respectively (Tatar et al., 2018; Wyrzykowski et al., 2014).

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 With reference to Shear’s pore size division theory (Shear et al. 1993) and considering the pore-size

characteristics of saline-alkali soils in the Yellow River Delta, we divided the pore sizes of saline-alkali soils in

this region into five categories (Table 2). An MIP analysis of these samples was performed with the PM-33-18

fully automatic mercury intrusion analyzer (Conta Instruments Company, US).

2.4.4 Freezing tests

Prepared soil samples with different values of water content were observed at 400x magnification using

an Xpv-900e polarizing microscope (PM) (Shanghai Rectangular Optical Instrument Co., Ltd., Shang-Hai

City, China), and 100 original surface images of each of the unfrozen soil samples were obtained.

Subsequently, these soil samples were transported to the low-temperature preservation laboratory of Shandong

Agricultural University. The temperature of the freezing laboratory was reduced to –10 ℃ within 20 min of the

samples reaching the laboratory, and maintained at −10 ℃for 24 h.The frozen soil samples were then observed

at 400x magnification using an Xpv-900e PM, and 100 surface images of each of the soil samples under frost

heave were thus observed in the frozen soil laboratory. Finally, the unconfined compressive strength of each

group of soil samples after freezing was measured using YYW-II Strain Controlled Unconfined Compressive

Strength Tester (Tianjian Instrument Manufacturing Co., Ltd., Cang-Zhou City, China). To ensure that the

sample does not melt during the freezing test, the observation and mechanical testing of all samples were

carried out in the cryopreservation laboratory of Shandong Agricultural University.

The images from the PM were processed by Photoshop software and imported to Image-J software to

obtain binary images and to calculate the porosity as the ratio of the white area to the total area. The porosity

calculation principle is shown in Figure 2, in which the white area represents void spaces and the black area

represents soil particles. Using Image-J software to calculate the ratio of the white area to the total area, the soil

porosity is obtained. Since 100 images of each sample were randomly collected on a cutting plane, according

to probability, the porosity calculated by processing these images would be the key parameter to characterize

the pore characteristics of the plane.

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3 Results

3.1 Quantitative analysis of the mineral phase

Table 3 presents the proportions of minerals in saline-alkali soils at different positions on a horizontal

plane in the Yellow River Delta, China. As the samples obtained advance from coast to inland, the proportion

of minerals in saline-alkali soil does not show an obvious trend; the mineral compositions of these soils at

different positions remain the same, although the proportion of each mineral is slightly different. The

proportion of primary minerals in local saline-alkali soil is much higher than that of clay minerals, and the

degree of weathering of these soils is relatively low. The primary minerals characterizing saline-alkali soils in

these areas include quartz, calcite, orthoclase, and albite. Quartz is predominant, accounting for 44.15–64.26%

of the total mineral composition, followed by albite and calcite. Clay minerals include illite, kaolinite, and

chlorite. Illite is predominant, accounting for 5.72–12.48% of the total soil mineral content, whereas kaolinite

and chlorite are present in relatively small amounts, together accounting for less than 5% of the total soil

minerals content.

3.2 Qualitative analysis of microstructure characteristics

Figure 3 shows a series of SEM micrographs of saline-alkali soils at different horizontal positions in the

Yellow River Delta, China. It can be seen from these images that saline-alkali soil in this area is divided into

two categories, soil from location S1 is in one category, and soil from locations S2–S6 are in the other category,

which is consistent with the results of particle size analysis. The skeleton particles of saline-alkali soil from the

S1 category are large, with a diameter of 10–25 μm, and are arranged as a closely inlaid "brick wall", resulting

in the low porosity and poor permeability of these soils. Most of the pores in saline-alkali soils are

intergranular pores, below which are large particles, with no communication between the pores. The shapes of

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saline-alkali soil particles are mainly regular strip-like, semicircular and circular, and the contact mode of

particles is mainly face-to-face inlay.

Inter-particle spaces of saline-alkali soil from the S2–S6 category are filled with a large amount of debris,

forming a typical cemented structure. The shapes of these saline-alkali soil particles are mainly flake and flat

with an elevated orientation, and the contact mode of the particles is mainly in the form of indirect surface

contact. Only when the SEM images are magnified to 10000 times are the micron-scale pores visible. Although

there are differences in the micro-characteristics of saline-alkali soil of different textures, it is not difficult to

detect, from the SEM images, the dense microstructures that make it arduous and time-consuming to remediate

the soils in the Yellow River Delta.

3.3 Quantitative analysis of pore characteristics

Tables 4 and 5 present the results of the MIP analysis, which was conducted to determine the total volume

and total specific surface area of the pores, and the average proportions of the specific surface area and volume

of the different pore types.

The pores of coastal saline-alkali soil (S1) are mainly small pores (2 ≤ d < 10 μm) and micropores (0.1 ≤

d < 2 μm), accounting for 30.51% and 49.34% of the total pore volume, respectively, where d is the pore

diameter. By comparison, the pores of saline-alkali soil far away from the Bohai Sea (S2–S6) are mainly

micropores (0.1 ≤ d <2 μm) and ultra-micropores (d < 0.1 μm), accounting for 89% and 37% of the total pore

volume, respectively. Macropores (d ≥ 20 μm) in the soil are the main conduits for water and salt, and the

proportion of macropores in local saline-alkali soil is only 5.95–8.43%. The specific surface area of pores in

saline-alkali soil is mainly contributed by ultra-micropores (d < 0.1 μm), followed by micropores (2 ≤ d <10

μm), accounting for 80.433–88.988% and 10.9044–17.5780% of the total specific surface area of the pores,

respectively.

Figure 4 shows the overall porosity of saline-alkali soil at different horizontal positions in the Yellow

River Delta, China. It is seen that the overall porosity does not change significantly from the coast to the

hinterland, and the minimum and maximum overall porosity are 24.88% (S6) and 35.32% (S5), respectively.

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3.4 Frost heave effect as an approach for remediation of saline-alkali soils

In comparison to soil before freezing, all freezing treatments at the S1 location for different moisture

content soil samples, resulted in an increase in porosity and unconfined compressive strength (Figure 5). The

soil porosity was 33.25% before freezing, while after freezing, the porosity of saline-alkali soil increased by

4.72% for W10, 6.32% for W15, 8.00% for W20, and 13.15% for W25. The unconfined compressive strength

was 163.900 kPa for control (CK), 288.279 kPa for W10, 363.894 kPa for W15, 477.316 kPa for W20, and

669.9864 kPa for W25. Compared with CK, the increase in unconfined compressive strength for W10, W15,

W20, and W25 was significant (p<0.05), accounting for an increase of about 75.89–308.78%.

Figures 6a and 6b show comparisons of the microstructures of saline-alkali soil before and after freezing.

From the polarizing microscope (PM) images before freezing, the saline-alkali soil particles are found to be

arranged in a staggered pattern, with the particles being closely interspersed and densely distributed, and with

mainly small intergranular pores. Figure 6b indicates that the soil specimen is looser after freezing, and that

there are more large pores. The pores in these images appear to be more than 50μm, which facilitates the

transport of water and salt in the soil. During the freezing process, ice crystals are formed in these pores of soil,

which increase the unconfined compressive strength of soil. The results of these PM images are consistent with

the results of macro mechanical tests. This further proves that the macro behavior of saline-alkali soil depends

on its microstructure.

4 Discussions

4.1 Mineral composition of saline-alkali soil based on XRD

Soil particle size distribution, texture, and mineral composition are the most fundamental physical

properties of soil, which control the uptake of water and nutrients, and oxygen exchange in plants (Letey, 1985).

Our study data shows that the proportions of clay (particle size<0.002 mm) and clay minerals in saline-alkali

soil are 5.47–12.43% and 7.00–19.04%, respectively (Table 1 and Table 3), indicating that the mineral

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composition and particle size distribution of these soils are not primary factors contributing to the poor

permeability of these soils. Our results were similar to the analysis of saline-alkali soil microstructure of

different land-use types in the Yellow River Delta by Liu et al. (2020a). However, a study found that the low

permeability of saline-alkali soil in the Yellow River Delta is mainly due to the large amount of clay particles,

and added Yellow River sediment to change the particle size distribution to remediate the saline-alkali soil

(Mao et al., 2016 and 2018). The possible reason for the discrepancy in the results is that we are concerned with

the microstructure of the soil rather than the macro behavior, and our sampling location is close to the Yellow

River and the Bohai Sea.

4.2 Microscopic characteristics and pore size distributions of saline-alkali soil based on SEM and

MIP

The physical and chemical properties of soil depend largely on its microstructure, including pore

distribution, particle arrangement, and pore characteristics (Cotecchia & Chandler 2000; Fang et al., 2013;

Oualmakran et al., 2016). It also can be seen from the SEM images (Figure 3) that the structure of the

saline-alkali soil in the Yellow River Delta is dense, the pores are poorly developed, and the lack of

connectivity of soil pores. The pores in the soil serve as conduits for the movement of water and salt, and soil

porosity is the most important physical property that affects the permeability of soil (Strudley et al., 2008). In

the present study, we found the overall porosity of saline-alkali soil in the Yellow River Delta being only

24.88–35.32% (Figure 4), and the proportion of macropores in the soil is only 5.95–8.43% (Table 4). It makes

the saturated hydraulic conductivity of local saline-alkali soil to be (1.85–5.36) ×10-5 cm/s (Table 1). The lower

saturated hydraulic conductivity of soil, as described above, makes it relatively difficult for water and salt to

infiltrate the soil profile after precipitation or irrigation, which causes surface runoff and accelerates the loss of

soil nutrients. Moreover, a low porosity and dense soil structure provides channels enabling the rise of shallow

underground water. Therefore, due to evaporation, soil capillary action causes salt to move from deeper soil

layers to the surface layer along with the rising underground water. The salt is retained at the soil surface after

the water evaporates, which negatively affects the growth of plants.

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 Additionally, some earlier studies have also shown that the surfaces of soil pores provide favorable

locations for the attachment of salts, thereby posing challenges in the restoration of saline-alkali soil (Liu et al.,

2020b). In this study, we found that the contribution of ultra-micropores to the specific surface area accounts

for as much as 80.433–88.988% of the total surface area (Table 5). Since it is difficult for water to pass through

the ultra-micropores in the soil and clear the soil of salt, it results in lowering the hydraulic conductivity and

hence the accumulation of salt in these pores, that in turn, seriously affects the growth of crops. These results

indicate that the poor microstructure of the saline-alkali soil in the Yellow River Delta, including the low

porosity and macroporosity, the close arrangement of soil particles, and the high proportion of the total specific

surface area of the pores in the micropore group are the primary factors leading to the poor physical properties

of the local saline-alkali soil.

Pore size distributions are usually obtained indirectly from soil water characteristic curves obtained using

suction devices, and the measured pore sizes are typically more than 20 μm (Amer et al., 2009; Bayat et al.,

2019; Wang et al., 2020; Yi et al., 2020). In this study, we obtained the pore size distribution curves from an

MIP analysis, and the measured pore diameters reached a minimum value of 7nm. In the investigation of

macropores, it was found that the results obtained from the MIP analysis were consistent with those obtained

from soil water characteristic curves. However, the total porosity obtained from the MIP analysis is higher than

that obtained from soil water characteristic curves. The reason for this difference is that the ranges of pore

diameters obtained by the two methods are not consistent, with the range of pore diameters obtained from the

MIP analysis being larger.

4.3 Analysis of the mechanism of microstructure degradation of saline-alkali soil

The current literature supports the theory that the interaction between excessive Na+ and clay particles in

soil is the cause of poor physical properties of clay soil (Gill et al., 2009; Brinck & Frost., 2009; Ganjegunte et

al., 2014). Studies have shown that the clay content of soil is in the range of 5.47–12.43% and that micro and

super micro pores account for 57.87–89.25% of soil pores. The mechanism of degradation of the physical

properties of soil proposed by the above researchers does not explain the phenomenon of soil microstructure

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degradation observed in this study. The degradation of sand microstructure in this study should be traced to its

formation. The sand studied in the current research is a type of water deposited loess. The soil in this area

originates from the Loess Plateau. After being transported by the Yellow River, large particles of soil are

deposited in the upper, middle, and lower reaches of the Yellow River and the loess deposited in the river delta

has finer particles and larger bulk density. This mechanism of deposition of soil in the Yellow River Delta

leads to the degradation of soil microstructure, thereby worsening the physical properties of the soil.

4.4 Effect of frost heaving on the unconfined compressive strength of saline-alkali soil

As a soil layer freezes, its pore water migrates from unfrozen areas toward subzero areas, where the pore

water crystallizes into pore ice (and sometimes ice lenses appear), resulting in severe frost heave and

performance deterioration in soil engineering applications (Kozlowski & Nartowska, 2013; Simonsen &

Isacsson, 2001; Xu et al., 2019; Zhou et al., 2018). Although freeze-thaw cycles lead to the deterioration of soil

mechanical properties, the strength of soil can be significantly improved when frozen. Our data support this

conclusion, and when the soil is frozen, the unconfined compressive strength of saline-alkali soil in the Yellow

River Delta is significantly increased (Figure 5). This study examines seasonal soil freezing in the Yellow

River Delta, where the soil is generally frozen in winter (November–April). During this season, the strength of

saline-alkali soil is greatly improved, and the soil can be used for water conservancy measures in the

high-strength state, with effective reinforcements placed before the melting of saline-alkali soil in spring.

Although frost heave has disastrous consequences for the civil engineering industry, it can be beneficial for the

remediation of saline-alkali land.

4.5 Effect of frost heaving on the microstructure and porosity of saline-alkali soil

From the analysis of the microstructure of the saline-alkali soil in the Yellow River Delta, we assume that

local saline-alkali soil is characterized by low porosity, dense particle arrangement, and reduced hydraulic

conductivity. Jayawardane & Chan (1994) and Xia et al. (2019) emphasized that the key objectives for

remediation of saline-alkali soil were to increase the number and proportion of soil macropores and to improve

the saturated hydraulic conductivity of the soil. In this study, we found that the frost heave effect significantly

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improved the soil pore structure including decreasing the bond between soil particles, increasing the number

and proportion of effective pores, increasing the void ratio, and promoting soil water migration. It has been

previously stated in the literature that the size of soil micropores decreases due to the migration of pore water

during freezing, while the size of larger pores increases due to ice lens formation and expansion (Liu et al,

2020c). In the present study (Figure 5), we also found that the overall porosity of saline-alkali soil greatly

increased before and after frost heave at –10 ℃, and the soil moisture content was conducive to the increase of

porosity. Through soil amendment methods including the addition of gypsum, fly ash and biochar, the

improvement of large porosity and drainage characteristics may be one of the most significant effects of saline

soil improvement (Luna et al, 2018; Nan et al., 2016; Sahin et al., 2011). Our experimental results confirm, in

general, that the beneficial effect of frost heave on the porosity of saline-alkali soil is consistent with that of the

remediation measures mentioned in these studies. However, from an economic point of view, compared with

other measures, using soil frost heave to improve porosity might be more beneficial for agriculture, especially

in developing countries.

4.6 Effect of frost heaving on salt discharge in saline-alkali soil

The cohesive force between particles of natural saline-alkali soil is very weak and is easily destroyed by

internal stress, with the resulting plastic deformation being permanent and irreversible. Water in the soil seeps

into different types of pores with incrementally varying moisture content. When this occurs, the volume of

some of the pores in the soil increases under the action of frost heaving. Thus, the frost heave effect causes a

redistribution of the pore sizes in soil. When the water in soil freezes, the pore volumes increase, but the

developed pores are not restored to their original volumes even after the saline-alkali soil thaws, which is the

main reason for the effectiveness of salt-discharge in engineering structures.

Previous studies have shown that there is a positive correlation between soil porosity and permeability

(Miranda et al., 2018; Fei et al., 2019; Ming et al., 2020). In this study, we found that under the action of frost

heaving, the porosity of soil gradually increases with an increase in the water content. Therefore, increasing

soil moisture content improves soil permeability and accelerates soil salt discharge, which results in a

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significant improvement in crop growth. On average, the temperature in the Yellow River Delta in winter is

about –10 ℃. Saline-alkali soil in the Yellow River Delta is in the typical littoral zone, where the climate results

in periodical frozen-heaving effects on its structures. In the winter, the freezing depth of soil in this area ranges

from 50cm to 65cm. The freezing depth of soil is greater than that of the tillage layer, hence the microstructure

and physical properties of the tillage layer were substantially improved by the effects of frost heave. Based on

the above analysis and existing research, we suggest that local agricultural workers increase the soil moisture

content using burettes, in the idle farmland in winter; for winter wheat, this process can be used to maintain as

high a moisture content as possible under normal growth conditions.

To effectively remediate saline-alkali soils, we performed a comprehensive analysis of the

micro-characteristics of Yellow River Delta saline-alkali soils at different positions on a horizontal plane,

based on a combination of analytical approaches, namely XRD, MIP, and SEM. While our results indicate that

the microstructure of the saline-alkali soil in this region is associated with the deterioration of soil physical

properties, there are limitations to this study. An MIP is a technical method of testing the pore distribution of

saline-alkali soil, but the needed high pressure to determine the pore structure may destroy the soil structure.

Moreover, the hypothesis that the frost heave effect significantly ameliorates the microstructural

characteristics of saline-alkali soil was confirmed in this study; however, the differences in the effects of frost

heave on the microstructural remediation of soils of different textures have not been studied. In practice,

interesting possibilities exist for similar experiments using real growing crops and a series of soil conditions.

Furthermore, there is room to consider the effects of different freezing temperatures and freeze-thaw cycles on

soil water, salt movement, and soil physical properties, and analyzing its internal mechanisms from a

micro-scale perspective.

5 Conclusions

In the Yellow River Delta, the proportion of clay minerals and clay (particle size< 0.002 mm) in the soil is

low; thus, it is probably not a primary factor contributing to the deterioration of soil physical properties.

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Interestingly, in this study, we found that the pores of saline-alkali soil are mainly composed of impermeable

pores, with very low-porosity and close arrangement of particles, showing that the poor microstructure of

saline-alkali soil is the primary impediment to long-term remediation.

Site-specific remediation practices include the incorporation of organic and chemical amendments that

significantly improve saline-alkali soil physical properties, but this study has demonstrated that the effects of

soil microstructure on physical properties are influenced considerably by frost heaving. The results of the

experiments conducted in this study show that after low-temperature treatments, the overall porosity and

unconfined compressive strength of saline-alkali soil increased by 75.89–308.78% and 75.89–308.78%

respectively. We, therefore, suggest increasing soil water content through irrigation in winter to enhance the

frost heave effect of soils.

To the best of our knowledge, this is the first study to undertake such an extensive and systematic

characterization of salinized soil microstructure in the Yellow River Delta. Moreover, our proposed beneficial

use of the frost heave effect has been proven to be effective for the amelioration of saline-alkali soils. Future

work should be directed at extending this investigation to field experiments, to compare the mechanisms of

soil-water-salt dynamics and the structural characteristics of saline-alkali soils with varying freezing

temperatures and irrigation rates.

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Tables

Table 1 Basic physicochemical properties of the saline-alkali soils used in this study

Distance from the ocean (km)

Soil property
5 18 20 25 28 30

Bulk density (g cm-3 ) 1.66 1.70 1.79 1.72 1.60 1.85

pH 9.56 9.31 8.89 8.72 8.55 8.93

Electrical conductivity (dS m-1 ) 6.81 1.14 0.37 0.71 0.53 0.51

Soluble salt (g kg-1 ) 18.66 3.11 2.05 1.90 1.79 1.50

Saturated hydraulic conductivity (10-5 cm s-1 ) 4.98 3.32 2.01 3.10 5.36 1.89

Organic matter (g kg−1 ) 18.83 16.67 18.20 14.78 14.53 15.01

< 0.002 mm 5.47 7.72 8.89 10.30 12.43 11.12

Soil particle distribution
0.002–0.02 mm 33.35 48.88 51.70 60.80 65.30 56.50
(%)
>0.02 mm 61.18 43.40 39.41 28.90 22.27 32.38

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Table 2. Classification of pore types in the saline-alkali soils of the Yellow River Delta, China.

Pore type Pore diameter (d) range (μm) Pore composition

Macropore d ≥ 20 Inter-granular pores and parts of intra-granular pores

Mesopore 10 ≤ d < 20 Intra-granular pores

Small pore 2 ≤ d < 10 Intra-granular pores and parts of inter-particle pores

Micropore 0.1 ≤ d < 2 Inter-particle pores

Ultra-micropore d < 0.1 Intra-particle pores

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 Table 3. Proportions of minerals in saline-alkali soil at different distances from the ocean in the Yellow River

Delta, China.

Distance from the ocean (km)

Mineral (%)
5 18 20 25 28 30

Quartz 58.15 52.10 64.26 52.68 58.91 44.15

Calcite 10.18 17.16 10.58 21.08 13.73 19.15

Primary mineral
Orthoclase 6.07 3.94 6.89 3.82 4.24 7.14

Albite 16.44 12.06 9.27 9.83 9.08 19.36

Illite 7.38 10.89 5.90 9.18 10.48 5.72

Clay mineral Kaolinite 0.22 0.18 0.30 0.12 0.29 1.57

Chlorite 1.56 3.67 2.80 3.29 3.27 2.91

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Table 4. Volume ratios (%) of different ranges of pore diameters of saline-alkali soil of the study area in the

Yellow River Delta, China.

Distance from the ocean (km)

Pore diameter (μm)
5 18 20 25 28 30

d≥20 8.43 7.17 8.37 7.49 5.95 6.38

10≤d<20 3.19 3.34 1.31 2.05 2.82 2.16

2≤d<10 30.51 4.32 3.27 2.18 1.98 4.39

0.1≤d<2 49.34 44.01 56.26 47.28 43.13 47.81

d<0.1 8.53 41.16 30.79 41.00 46.12 39.26

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Table 5. Surface area ratios (%) of different ranges of pore diameters of saline-alkali soil of the study area in

the Yellow River Delta, China.

Distance from the ocean (km)

Pore diameter (μm)
5 18 20 25 28 30

d≥20 0.0410 0.0091 0.0112 0.0066 0.0176 0.0071

10≤d<20 0.0520 0.0145 0.0062 0.0083 0.0127 0.0092

2≤d<10 1.8960 0.0694 0.0697 0.0286 0.0280 0.0913

0.1≤d<2 17.5780 11.1205 15.5080 14.3541 12.7383 10.9044

d<0.1 80.4330 88.7865 84.4050 85.6024 87.2033 88.9880

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 Page 29 of 34 Land Degradation & Development

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Figure 1 Location map of the Yellow River Delta and the sampling site.
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14 Figure 2 Original and binary images of a saline-alkali soil sample from the Yellow River Delta, China.
15 (a) Original image; (b) Binary image; (c) Original image; (d) Binary image.
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 Page 31 of 34 Land Degradation & Development

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22 Figure 3 Scanning electron microscopy (SEM) images at 1000x magnification of saline-alkali soil samples
23 from the Yellow River Delta region, China, collected at different distances from the ocean: (a) 5km; (b) 18
km; (c) 20 km; (d) 25 km; (e) 28km; (f) 30km.
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 Land Degradation & Development Page 32 of 34

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33 Figure 4 Overall porosity of saline-alkali soil in the Yellow River Delta, China, at different distances from the
34 ocean. (S1) 5km; (S2) 18 km; (S3) 20 km; (S4) 25 km; (S5) 28km; (S6) 30km.
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21 Figure 5 Comparison of the porosity (a) and unconfined compressive strength (b) of a saline-alkali soil
22 sample (S1) before and after freezing in the Yellow River Delta, China. Error bars represent the standard
deviation. Mean values labeled with the same letter were not significantly different at α = 0.05.
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 Land Degradation & Development Page 34 of 34

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20 Figure 6 Comparison of microstructure images, before and after freezing, of saline-alkali soil samples (at
21 location S1) from the Yellow River Delta, China. (a) Before freezing; (b) After freezing
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