Available online at http://ijcpe.uobaghdad.edu.iq and www.iasj.net 

Iraqi Journal of Chemical and Petroleum 
 Engineering  

Vol.23 No.4 (December 2022) 25 – 32 
EISSN: 2618-0707, PISSN: 1997-4884 

 

Corresponding Author:  Name: Hasan Ali Abbood , Email: hasan.abbood1607m@coeng.uobaghdad.edu.iq  

IJCPE is licensed under a Creative Commons Attribution-NonCommercial 4.0 International License. 

 

Enhance the Properties of Lignosulfonate Mud by Adding 

Nanoparticles of Aluminum Oxide and Iron Oxide 

 
Hasan Ali Abbood and Ibtehal Kareem Shakir 

 
Chemical Engineering Department/College of Engineering/University of Baghdad/Baghdad, Iraq 

 

Abstract 
 

   Oil well drilling fluid rheology, lubricity, swelling, and fluid loss control are all critical factors to take into account before 

beginning the hole's construction. Drilling fluids can be made smoother, more cost-effective, and more efficient by investigating and 

evaluating the effects of various nanoparticles including aluminum oxide (Al2O3) and iron oxide (Fe2O3) on their performance. A 

drilling fluid's performance can be assessed by comparing its baseline characteristics to those of nanoparticle (NPs) enhanced fluids. 

It was found that the drilling mud contained NPs in concentrations of 0,0.25, 0. 5, 0.75 and 1 g. According to the results, when 

drilling fluid was used without NPs, the coefficient of fraction (CoF) was 44%, when added Al2O3 NP and Fe2O3 NP at 0.75g 

reduced CoF by 31% and 33% respectively. When Al2O3 and Fe2O3 NPs were used, particularly at a concentration of 1g, the amount 

of mud filtration decreased from 13.5ml to 9.3 ml and 8.5 ml respectively. Additional improvements rheological properties as well as 

swelling when Fe2O3NPs and Al2O3 NPs were added at 1g. Overall, it was found that adding NPs to the Lignosulfonate-WBM at a 

concentration of 1g can improve rheological, swelling, and filtration properties as well as lubrication at 0.75g. 

      
Keywords: drilling mud; nanoparticles; lubrication; rheological; swelling. 
 

Received on 20/05/2022, Accepted on 19/07/2022, Published on 30/12/2022 

 
https://doi.org/10.31699/IJCPE.2022.4.4  

 
1- Introduction 
 

   Extracting oil and gas from the ground begins with 

drilling. Developing this operation to its full potential will 

help boost output. Drilling mud is essential to achieving 

this goal. Water, oil, synthetic, and pneumatic (air-based) 

drilling fluids are just a few of the many types of drilling 

fluids available. The most widely used fluid is water. 

About 80% of all wells are drilled with them because they 

are less expensive than oil or synthetic-based fluids [1]. 

To maximize oil recovery and shorten the time it takes to 

reach first oil, drilling fluids are an absolute necessity. 

Drilling fluids can be likened to blood in the human body 

because they are used in the drilling process to remove 

rock. Similarly, to how the kidneys and lungs remove 

waste from the body via the blood, the mud pump 

removes drilling cuttings from the bottom and transports 

them through drilling fluid to clean the mud before it is 

used again [2]. Drilling muds are used to prevent reservoir 

fluids from entering the wellbore by providing hydrostatic 

pressure [3], reduce contact forces and torque between the 

drill string and wellbore [4], reduce the filtration rate [5], 

and transport drilling waste to the surface for cooling 

purposes [6]. 

   When it comes to the construction and completion of a 

well, drilling mud is an essential consideration. Any 

drilling operation's success is directly related to the 

quality and efficiency of its fluid mix, as well as its cost 

and environmental impact. Pipe sticking and mud loss are 

two problems that can arise as a result of poor drilling 

fluid design. Poor mud design can lead to other problems, 

such as bit balling and borehole collapse [7]. 

   In recent years, nanotechnology has been used to 

improve the properties of NPs. This is because 

Nanomaterials' ability to improve fluid performance 

depends on their size and shape, which is determined by 

their ability to interact with mud components. Some of the 

functions of drilling fluid, such as preventing drill 

cuttings and minimizing formation damage and stabilizing 

the wellbore. Nanomaterials can be added to drilling 

fluids to perform any of these functions [8]. Drilling fluid 

problems can be solved by utilizing NPs with unusual 

characteristics, such as high thermal conductivity and a 

large surface area. A few of the most important 

advantages of using nanoparticles in drilling fluids are 

their reduced fluid loss and mud cake, as well as their 

ability to remove hazardous materials and enhance heat 

transfer, lubrication, and rheological properties such as 

viscosity [9]. 

   The use of Nano sized particles as an additive agent in 

drilling fluid formulations has been the subject of several 

experimental studies. Table 1 reports a summary of NP 

behaviors on drilling fluids. 

   The goal of this experiment is to examine the 

performance of water-based Nano muds containing Al2O3 

NPs and Fe2O3 NPs and compare them to Lignosulfonate 

water-based muds (WBM). A series of lab tests were used 

to conduct this evaluation. 

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H. A. Abbood and I. K. Shakir / Iraqi Journal of Chemical and Petroleum Engineering 23,4 (2022) 25 - 32 

 

 

26 

 

Table 1. Summary of Nanoparticle Behaviors on Drilling 

Fluids 
Nanoparticle 

types 
Outcomes References 

Sio2                                      

proved the rheological and fluid 

loss properties. 

improved the shale inhibition. 
significant reduction in filtration . 

[10] 
[11] 

[12] 

laponite Enhancement of thermal stability. [13] 

TiO2 
improves the thermal stability and 
rheological properties. 

[14] 

α-MnO2 minimizing the filtration loss. [15] 

ZnO 

improved the rheological 
behaviors and provided better  

filtration control. 

[16] 

Al2O3 

Improved the effective thermal 
conductivity. 

improve the rheological 

properties. 

[17] 

[18] 

Fe2O3 

Developments rheological and 

fluid loss properties. 

improved filter cake and fluid 
loss.  

[19] 

[20] 

 

2- Experimental Work 
 

2.1. Characterization of the materials 
 

   Al2O3 and Fe2O3 are two of the most widely used NPs 

because of their heat transfer properties and low cost. For 

this study, Fe2O3 and Al2O3 NPs were chosen as a result. 

Nanjing Nano Technology and Sky Spring NPs, 

respectively, served as the suppliers of Al2O3 and Fe2O3. 

Nanoparticle properties are listed in Table 2 and Table 3. 

Al2O3 and Fe2O3 NP morphology is shown in Fig. 1 and 

Fig. 2 TEM and SEM images, respectively. 
 

Table 2. Physical Properties of Fe2O3 NPs 
Properties  Typical value 

Purity 99.9% 

Appearance black powder 

Size 20-30 nm 

Ash >0.2 wt.% 

 

Table 3. Physical Properties of Al2O3 NPs 
 

 

 

 

 

 

 

 

Fig. 1. TEM Images of AL2O3NPs 

 
Fig. 2. SEM Images of Fe2O3NPs 

 

2.2. Methodology 

 

   The drilling fluid utilized in this study is Ferro Chrome 

Lignosulphonate (FCL), which is commonly employed in 

southern Iraqi oil fields. This mud is simple and quick to 

prepare. According to API standards, bentonite fluid 

should be prehydrated by mixing 20 grams of sodium 

bentonite with 350 milliliters of fresh water for at least 20 

minutes using a Hamilton Beach Mixer and letting it sit 

for 16 hours. Then, add 0.5 g of caustic soda to improve 

the performance of lignosulphonate and raise the PH 

values. Also 1g of soda ash is used to remove the calcium 

ion and improve the properties of calcium bentonite. 

Lignosulfonate is used to deflocculate and control the 

rheology of 1g of bentonite. The mixture is then mixed 

for 20 minutes using a Hamilton Beach Mixer under 

laboratory conditions, where the concentrations of Al2O3 

and Fe2O3 NPs range from 0 to 1g. The fluid is then 

placed in an ultrasonic bath for 15 minutes to ensure that 

the Nano particles are evenly distributed throughout the 

fluid and experimental work flowchart as showing in Fig. 

3. 
 

 
Fig. 3. Experimental Work Flowchart 

Properties  Typical value 

Purity 99.9% 

Appearance White powder 

 Size 20 nm 

Ash >0.2 wt.% 



H. A. Abbood and I. K. Shakir / Iraqi Journal of Chemical and Petroleum Engineering 23,4 (2022) 25 - 32 

 

 

27 

 

2.3. Rheological Testing 
 

   Plastic viscosity, gel strength, filter cake thickness and 

filtrate loss were some of the rheological properties 

studied for the prepared muds. Mud viscosity and gel 

strength (10 sec and 10 min) were measured using a Van-

G meter. The API standard was used to measure the 

parameters of plastic viscosity (PV) and yield point (YP). 

The Van-G meter was used to determine the PV and yield 

point values at both 300RPM and 600RPM motor speeds. 

The filter cake was evaluated, and the filtration loss was 

calculated in a filter press with the help of this tool. Filter 

press pressurized cells contain a pressurized filter 

medium. 

   To A nitrogen gas cylinder was connected to the filter 

press equipment in order to raise the cell pressure to 100 

psi. It took about 30 minutes for each of the tests, and 

there were two of them. afterwards, the cell was 

disassembled and the mud thrown away. To avoid 

damaging the mud cake, be sure to take your time and be 

cautious when removing the components from the cake. 

The cake was gently scrubbed to remove any remaining 

mud before serving. As a final step, the filter cake 

thickness was measured and recorded in 1/32-inch 

increments. To be clear, all tests were performed at 27 °C. 

Equations are used to calculate (PV) and (YP) [29]: 

 

PV= 𝜃600 − 𝜃300                                                (1) 
 

YP=𝜃300 − 𝑃𝑉                                                 (2) 
 

   Whereas Φ600 = Dial reading at 600 RPM, and Φ300 = 

Dial reading at 300 RPM. 

 

2.4. Lubricity 

 

   Extreme pressure/lubricity testers were used to measure 

CoF for the lubricity test. Drill string and wellbore are 

analogous in that they are made of metal to metal. It was 

possible to calculate lubricity with this formula [23]: 

 

COF = 
Torque reading

100
                                                         (3) 

 

100=
150 inch−Ibs torque wrench reading 

1.5 inch torque shaft lever arm 
                                       (4) 

 
CF =

Meter reading for water (standerd)

meter reading obtained in water calbration 
                                (5) 

 

CoF =
(Meter reading for water )(CF)

100
                                            (6) 

 
   Whereas, CoF = Coefficient of fraction, and CF= 
Coefficient factor. 

 

2.5. Shale Swelling Testing  

 

   Drilling mud compatibility with the wellbore should be 

determined before operations begin. The interaction of the 

shale with the drilling muds is the method to test the 

shale's compatibility with the swelling process. In this 

studies, we used a compactor cell to create shale plugs for 

a swelling analysis. Swelling test procedure for shale is 

provided [11]. 

 

3- Results and Discussion 
 

3.1. Properties of Rheology 

 

A. Plastic viscosity 

 

   Due to the difficulty of pumping drilling fluid with a 

high PV, drillers avoid using it for drilling operations. 

Drilling fluid density, on the other hand, is directly related 

to mud viscosity and should be considered when 

designing a drilling fluid. For this reason, lower mud 

viscosity results in less dense water due to a reduction in 

hydrostatic pressure, which isn't always a good thing [22]. 

The PV of Lignosulfonate-WBM was found to be only 7 

cP. As shown in Fig. 4, The addition of NPs to 

Lignosulfonate - WBM generally increased the PV. 

However, the PV amounts at various concentrations of 

each NP type vary (from 0 to 1 g) was different. In 

addition, 1 g of Al2O3 NPs was added to increase the 

amount of PV to 8 cP. The Al2O3 NPs are dispersed 

throughout the fluid uniformly; the mud's viscosity may 

rise due to an increase in interlayer friction [19]. We were 

able to achieve 8 cP of PV by mixing in 0. 5 g Fe2O3 NPs 

with the base mud. When the concentration was increased 

to 0.5 g, the PV remained constant at 8 cP before 

increasing to 9 cP at the 1 g concentration point. 

 

 
Fig. 4. NPs Concentration Affects by Plastic Viscosity 

(cp) 

 

B. Yield Point 

 

   Mud-cutting capacity can be determined by taking into 

account the YP value, which is an important factor make 

it easier to transport heavier cutting [8]. We found that 
based Lignosulfonate -WBM had a yield point of 9 

lb/100ft2. It is shown in that NPs affect the yield point of 

linosulfonate -WBMs in Fig. 5, At different NP 

concentrations, the YP of WBM with linosulfonate -

WBM shows different results. The YP of Al2O3 NP 

Lignosulfonate -WBM increases at all concentrations. At 



H. A. Abbood and I. K. Shakir / Iraqi Journal of Chemical and Petroleum Engineering 23,4 (2022) 25 - 32 

 

 

28 

 

a concentration of 1 g of Al2O3 NP Lignosulfonate-WBM, 

the maximum YP was 55 lb/100 ft2. Yield point values 

risen sharply for Fe2O3 NPs, reaching 38 lb/100 ft
2 at 1g. 

Since Al2O3 NPs have a higher surface-to-volume ratio at 

1 g, they will interact more strongly with the base fluid 

around them, leading to a higher YP [25]. 

 

 
Fig. 5. NPs Concentration Affects the Yield Point 

 
C. Gel Strength 

 
   The gel strength of the drilling fluids   must be 

maintained at a relatively high level in order to suspend 

and transport cuttings in horizontal wells. Reduced WBM 

circulation circulating pressure loss also contributes to 

improved drilling efficiency [26]. It is a standard. Under 

static conditions, the electrochemical forces in the fluid 

determine the gel strength. Fig. 6 and Fig. 7, the influence 

of NPs at various concentrations on GS is demonstrated at 

10 s and 10 min, respectively. Base mud gel strength was 

determined to be 7 and 12 lb/100 ft2 for 10 sec and 10 

min, respectively, in the initial test. The addition of Al2O3 

NPs ranging from 0.25 to 1 g increased the 

Lignosulfonate - WBM gel strength values in both tests 

(10 sec and 10 min). A concentration of 1 g Al2O3 NPs 

produced a Lignosulfonate-WBM 10 sec gel strength of 

53 lb/100 ft2 and a 10 min gel strength of 58 lb/100 ft2. In 

the presence of Fe2O3 NPs, the 10 sec and 10-min gel 

strength values increased by addition NPs from 0.25 to 

1g. Fe2O3 NPs, on the other hand, increased the 10 sec 

and 10 min gel strength values to 40 and 50 lb/100 ft2 

respectively. The high gelling characteristics of the fluid 

may necessitate a high starting torque, which must be 

justified by investigating the fluid's shear thinning 

behavior. The absence of numerous and serious drilling 

issues can only be ensured by using a high-strength gel 

[27]. Finally, the gelling properties of Al2O3 NPs at 1g 

concentration are superior to those of Fe2O3 NPs, due to 

the electrostatic force between Al2O3NPs, which links 

their cases with base fluids to create a rigid structure, this 

happens [18]. 

 

 
Fig. 6. NPs Concentration Effects on Gel Strength over a 

10-sec 

 

 
Fig. 7. NPs Concentration Effects on Gel Strength over a 

10-min 

 

3.2. Loss of filtering 

 

   Wellbore plugging, formation expansion, and wellbore 

instability and collapse can all be caused by fluid outflow 

into the formation. Differential pressure adhesion, caused 

by cake buildup on the wellbore wall, increases the risk of 

drilling tool damage [28]. In order to prevent drilling fluid 

from escaping and entering a formation, NPs can be used 

to obstruct the pore space [7]. Fig. 8, shows the fluid loss 

behavior of Lignosulfonete-WBM with varying NP 

concentrations. The Lignosulfonete-WBM lost 13.5 mL 

of fluid after 30 minutes. The fluid loss volume was 

reduced to 9.3 mL after incorporating Al2O3 NPs into the 

WBM at a concentration of 1 g. In general, Al2O3 NPs are 

a good additive for lowering the filter loss of 

Lignosulfonete-WBM. The addition of 1g of Fe2O3 NPs 

reduced the lignosulfonete-WBM filter losses to 8.6 mL. 

Base mud fluid loss can be reduced by using 1g of 

Fe2O3NPs. However, Fe2O3 NPs are a better choice for 

reducing fluid loss, this finding concur well with [9]. 

 

 



H. A. Abbood and I. K. Shakir / Iraqi Journal of Chemical and Petroleum Engineering 23,4 (2022) 25 - 32 

 

 

29 

 

 
Fig. 8. NPs Concentration Affects the Filtrate (ml) 

 
3.3. Lubricity and NPs concentration 

 
   A lot of heat and friction is generated during drilling 

operations at the bit and the drill string/wellbore interface. 

In addition, when the drill string is rotating, the friction 

that occurs between the wellbore and the drill string can 

generate a significant amount of torque and drag [29]. It is 

one of the primary functions of drilling fluid to lubricate 

the drill string as it progresses through the well. To 

determine a surface's coefficient of friction, you must first 

determine how much traction there is between the two 

objects [23]. Fig. 9, a small amount of nanoparticles in the 

drilling fluid reduced CoF slightly, according to the 

results of this study. Using base mud, we were able to 

increase torque by about 44%. In contrast, the addition of 

Fe2O3 and Al2O3 NPs led to a Torque reduction of 33% 

and 31%, respectively, at a concentration of 0.75 g. 

Similar to Fe2O3 NPs, Al2O3 NPs above 0.75 g caused 

35% and 37% increase in COF, respectively.  WBM 

lignosulfonete crushes under rotation and forms angulated 

forms, resulting in higher CoF values than Fe2O3 and 

Al2O3 NPs. NPs reduce the CoF by creating a slippery 

layer between the drill string and the borehole. 

 

 
Fig. 9. Friction of Coefficient (COF) Depends on the 

Concentration of NPs in the Fluid 

 

 

 

3.4. Swelling Behavior and Nanoparticle Effects 

 

   By far and away the most common result of freshwater 

intrusion is the alteration of clay minerals. When clays in 

the rock matrix are hydrated and swelled by water, they 

can become dispersed and cause particle plugging. The 

clay mineral smectite or montmorillonite is the most 

important one for swelling. Interlayer adsorption of water 

has the capability of expanding this clay up to a 10-fold 

range. This depends on the cation in the interlayer [30]. 

WBM with the NPs. Because of the synergetic properties 

of NPs, to expand, it means that the bentonite in the NPs 

system absorbed less water, resulting in less clay swelling 

and increased shale strength [24]. Fig. 10, show the 

expansion quantity meter results for the sodium bentonite 

shale, using four different drilling fluids, including fresh 

water, Al2O3 NPs, Fe2O3 NPs, and Lignosulfonete-WBM. 

After 15 hours in fresh water, the bentonite had grown by 

15% and the Lignosulfonete-WBM had grown by 13%. 

Al2O3-NP-treated Lignosulfonete-WBM grew by less 

than 7% after 16 hours of exposure to these systems. 

Finally, the addition of Fe2O3 NPs reduces swelling to 8% 

due to NPs' ability to plug Nano pores in clay, preventing 

shale swelling. As a result, Al2O3 NPs are the most 

effective additive for reducing Lignosulfonete-WBM 

swelling [11]. 

 

 
Fig. 10. Shale Interacted with Liginosulfonate-WBM 

/Al2O3, Fe2O3 NPs and Compared with Basic Muds 
 

4- Conclusion 
 

   Shale plug immersed in Al2O3 NPs mud shows less 

erosion and cracking along the boundary and at the center 

of the shale plug compared to basic mud, However, Al2O3 
NPs mud system shows good shale inhibition compared 

to Fe2O3 NPs mud system. Overall, the results showed 

that the addition of Al2O3and Fe2O3 NPs to the basic mud 

system improved shale inhibition and rheological 

properties. API and LPLT filtrate volumes were 

minimized by using Al2O3and Fe2O3 NPs. Minimizing 

CoF with Al2O3and Fe2O3 NPs. However, further studies 

are required to investigate the effect of Al2O3and Fe2O3 

NPs at higher concentrations over shale swelling and 

rheological behavior of the muds. 

 

 

 

 



H. A. Abbood and I. K. Shakir / Iraqi Journal of Chemical and Petroleum Engineering 23,4 (2022) 25 - 32 

 

 

30 

 

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بإضافة نانو أوكسيد االلمنيوم  Lignosulfonete Mud)تحسين خواص طين الحفر )

 واوكسيد الحديد
 

 حسن علي عبود و ابتهال كريم شاكر
 

 قسم الهندسة الكيمياوية/كلية الهندسة/جامعة بغداد
 

 الخالصة
 

لها النفطية ك لجدار البئر، والتحكم في الترشيح لسائل حفر االباران الخواص االنسيابية، والتزييت، واالنتفاخ    
، خواص مهمة يجب مراعاتها قبل البدء بعملية حفر البئر النفطي. حيث يمكن جعل تلك السوائل أكثر سالسة

 ك يمكنفعالية واقل كلفة من خالل إضافات مواد نانوية والتي تعرف بأوكسيد االلمنيوم واوكسيد الحديد. وكذل
ة، تقييم أداء تلك السائل من خالل مقارنة خصائصه األساسية مع تلك الخصائص المحسنة باإلضافات النانوي

دون سائل الحفر بغم(. وفقًا للنتائج، وجد ان 1.و0.25,0.5,0.75حيث تكون تلك اإلضافات بتراكيز مختلفة )
غم  0.75ز كسيد الحديد( وبتركياللمنيوم واو ، بينما مع النانو )اوكسيد ا%44النانو يمتلك معامل احتكاك بنسبة 

على التوالي. وكذلك استطاع النانو )اوكسيد االلمنيوم واوكسيد  %33و %31معامل االحتكاك بنسبة  قل
تفاخ على التوالي. وكذلك تم تحسين الخواص االنسيابية وتقليل االن %37و %30الحديد( تقليل الراشح بنسبة 

 غم استطاع تحسين1ك النانو. الخالصة، ان استخدام النانو وخاصة عن تركيز غم من تل1وخاصة عند تركيز 
 غم. 0.75الخواص االنسيابية والترشيح واالنتفاخ باإلضافة الى التزييت عند تركيز 

 
  ، التزييت، الترشيح، االنتفاخ.حبيبات نانوية، طين الحفر :ةلادالكلمات ال