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221 

This work is licensed under a Creative Commons Attribution 4.0 International License 

 

   

 

 

 

*Corresponding Author: rashatariq46@gmail.com 

                      

 
  

 

 

Abstract  

    The main focus of research is on the nature of applications in the fields of science and 

technology, particularly nanotechnology. In this paper, a simple, non-toxic, inexpensive, and 

environmentally friendly green method was used to synthesize TiO2 nanoparticles using the 

extraction of portulacaria afra plant leaves and TiCl4 as a precursor. The synthesized titanium 

dioxide nanoparticles were characterized by scanning electron microscopy, atomic force 

microscopy, X-ray diffraction patterns, Fourier transform infrared spectroscopy, and Brunauer-

Emmett-Teller analysis. The SEM image of TiO2 nanoparticles showed a few spherical, non-

agglomerated particles. The average diameter of the nanoparticles, according to the surface 

topography of TiO2-NPs, is 70.24 nm. It was found that the average crystalline size was 18.9 nm 

by utilizing the Debye-Scherrer equation to calculate the size of the crystals. The vibrational 

mode of Ti-O-Ti exhibits a distinctive peak in the broad band centered at 578.64, 547.78, and 

514.99 cm-1, which denotes the development of metal-oxygen bonding, confirming the presence 

of TiO2-NPs. The specific surface of the synthesized particles was calculated using the Brunauer-

Emmett-Teller BET equation. 

Keywords: Green method, Portulacaria afra, Titanium dioxide nanoparticles,     synthesized, 

Nanotechnology.    

1. Introduction 

      Nanotechnology aims mainly to improve, develop, and utilize the unique properties of 

molecules at the nano level in order to enhance materials, instruments, and systems with 

fundamentally different properties. In all fields of science and technology, innovative ideas 

continued to be developed in the fields of medical technologies, sensor technology, energy 

resources, and environmental protection and preservation [1]. TiO2 is a semiconductor material 

with a large band gap that can be crystalline as rutile, anatase, or brookite. It is a great material 

for chemical sensors, solar cells, photocatalysis, dye-sensitized solar cells, microelectronics, 

doi.org/10.30526/36.4.3161 

Article history: Received 26 December 2022, Accepted 22 January 2023, Published in October 2023. 

 

Ibn Al-Haitham Journal for Pure and Applied Sciences 

Journal homepage: jih.uobaghdad.edu.iq 

 

Synthesis, Characterization and Surface Properties of Nano-TiO2 Using a Novel 

Leaf Extracts 

                    Rasha Tariq salim *  

Department of Chemistry, College of Science, 

University of Baghdad,Baghdad Iraq.  

 

Sarah.wathib@gmail.com 

 

 

 

       Dunya Edan AL-Mammar  

Department of Chemistry, College of Science, 

University of Baghdad,Baghdad Iraq. 

 

https://creativecommons.org/licenses/by/4.0/
mailto:rashatariq46@gmail.com
mailto:Sarah.wathib@gmail.com
mailto:rashatariq46@gmail.com
mailto:Dunya.almammar@gmail.com


IHJPAS. 36 (4) 2023 

222 
 

electrochemistry, and charge-spreading devices [2]. The anatase phase of TiO2 nanocrystals has 

recently attracted attention due to their intriguing features as compared to the bulk and because 

they are essential not just for applications but also from a fundamental standpoint [3]. TiO2-NPs 

can be synthesized chemically or physically using microwave [4], hydrothermal [5], solid state , 

solution route, sol gel [6], chemical phase breakdown vapor, solvothermal crystallization [7], co-

precipitation [8], ultrasonic irradiation, and biologically applicable green synthesis methods [9].  

Green synthesis is a simple process that utilizes a variety of biological agents, such as plants, 

bacteria, fungi, algae, and yeast, with no dangerous products [10]. Due to its low cost, simple 

technique, and scalability for large-scale production, green synthesis has greater advantages over 

physical and chemical processes. With this technique, expensive equipment, hazardous 

chemicals, high temperatures, and high pressure are not necessary [11].  As a result, plant and 

herbal extracts are more desirable due to the easier and more cost-effective process and the 

inclusion of compounds such as flavonoids, terpenoids, and polysaccharides [12]. The creation 

of environmentally safe nanoparticles with a variety of natural features, great stability, and 

suitable dimensions can be achieved through a one-step green reduction method called nano-TiO2 

biosynthesis for the production of biological nanoparticles [13]. TiO2-NPs are created from a 

variety of plants, including the Jatropha curcas plant [14], the glycosmis cochinchinensis plant 

[15], the Syzygium cumini plant [16], the Moringa oleifera plant [17], the Psidium guajava plant 

[18], and the Aloe vera plant [11].  

In this research, Portulacaria afra (PA) was used to synthesize TiO2-NPs. (PA) is a succulent plant 

that is native to South Africa and can live in different regions of the world, including Iraq. (PA) 

is commonly found in semi-arid regions. This plant has small, succulent leaves and is in the form 

of a tall or small woody tree. The height of this plant can reach 2–5 meters. This plant contains 

bioactive substances such as alkaloids, amino acids, flavonoids, terpenoids, and other phenolic 

intermediates that may act as effective reducing agents for the bioreduction of metals into 

nanoparticles (NPs), which in turn have a variety of biological applications [19].  

2. Materials and Methods 

2.1. Materials  

    Titanium tetrachloride TiCl4, 99.0% was purchased from CDH, Portulacaria afra leaves 

collected from a local garden in Baghdad, Iraq. 

2.2. Methods   

2.2.1. Biosynthesis of TiO2-NPs by Portulacaria afra (PA) 

   In this method, TiO2-NPs were synthesized using the aqueous extract of (PA) plant leaves. (PA) 

leaves were removed from the original plant, thoroughly cleaned with tap water to eliminate 

impurities, then rinsed with distilled water and chopped into little pieces. 25 g of chopped plant 

leaves were added to 100 mL of boiled distilled water and heated for two hours continuously at 

90 oC.  

The plant extract was filtered using a Whatman No. 1 filter solution. For the synthesis of titanium 

dioxide nanoparticles, 2.8 mL of titanium tetrachloride as an aprecursor was added to 100 mL of 

distilled water and shaken well. (PA) leaf extract was added to the titanium tetrachloride solution 

gradually with continuous stirring. The mixture was continually stirred for 4 hours. Titanium 



IHJPAS. 36 (4) 2023 

223 
 

dioxide nanoparticles were synthesized during this process, and they were separated by drying 

the precipitate for a day at room temperature. Then it was heated in an electric oven for one hour. 

The precipitate was dried for 24 hours at 100 oC. Then the precipitate was calcined at 500 oC for 

4 hours continuously [11]. After that, the precipitate was often washed with distilled water to get 

rid of the impurities. To obtain titanium dioxide nanoparticles as a white precipitate, the 

precipitate was dried and heated at 700 oC for one hour. Finally, a laboratory mill ground the 

precipitate and stored it for characterization and application. Figure 1 shows the steps of TiO2-

NPs preparation from (PA) plant. 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Figure 1. Steps of TiO2-NPs preparation by (PA) plant. 

2.2.2. Characterization of TiO2-NPs 

      For chemical, structural, physical, and morphological evaluations, TiO2 NPs were 

characterized. Analyses of the morphology of nano-TiO2 were done using scanning electron 

microscopy (FESEM-EDS, MIRA III, TESCAN, and Czech). The physical assessment was done 

using atomic force microscopy (AFM 2022, Nanosurf, and Switzerland). Structural assessment 

of the nanoparticles was characterized using X-ray diffraction XRD (PW1730, Philips, and 

Holland). Chemical assessment was carried out using Shimadzu IR-Affinity-1 Japan. Brunauer-

Emmett and Teller surface area analyzer type BELSORP MINI II, BEL, Japan, was applied to 

estimate the specific surface area, average pore volume, and pore size distribution [20] .These 

measurements were used to describe the topography and examine the characteristics of a material 

at the nanoscale. 



IHJPAS. 36 (4) 2023 

224 
 

3. Results and Discussion  

3.1. Scanning Electron Microscopy (SEM) 

    SEM measurements were used to obtain the images of samples using the technique of scanning 

electron microscopy to explore the surface features, porosity morphology [21], and crystalline 

structure [22]. It can be seen from Figure 2 that the sample showed excellent crystallinity. The 

particle size of TiO2-NPs was 47.580 nm, which was calculated using IMAGE J software. The 

SEM image of TiO2 nanoparticles revealed that TiO2 has a nanosheet-like structure on its surface 

and is porous [23]. The SEM image showed that the TiO2 nanoparticles had clumped together 

and took an irregular shape, which was obtained at a magnification of 500 nm. There were a few 

non-clumping particles that were spherical in shape. So, it can infer that the phytochemicals of 

Portulacaria afra leaf extract coat the surface of TiO2 nanoparticles, inhibiting their accumulation 

[15].  

 

 

 

 

 

 

Figure 2. SEM image for TiO2-NPs. 

3.2. Atomic Force Microscopy (AFM)  

      AFM analysis is used to measure the important properties such as surface morphology with 

probes at nanometer scales [24]. The average diameter of prepared TiO2-NPs is 70.24 nm. 

Through these results, it was observed that the sample that was synthesized by Green Biology 

produced a particle with a small size distribution. Figures 3a, b show the typical surface obtained 

from the AFM image and the granularity cumulating distribution for the TiO2 sample. 

 

 

 

 

 

 

Figure 3 (a, b). View of AFM image and granularity cumulating distribution chart of TiO2-NPs. 

 

a 

60 80 100 120 140 160 180 200 220 240 nm

0

13

26

Mean diameter b 



IHJPAS. 36 (4) 2023 

225 
 

3.3. X-Ray Diffraction (XRD) 

     Figure 4 shows a polycrystalline structure of mixed anatase and rutile phases, which is how 

the crystalline structure of the synthesized TiO2-NPs was explained by XRD patterns. The 

dominant Anatase phase angles 2θ= 25.5795°, 37.1949°, 38.0553°, 38.7313°, 48.2265°, 

55.2019°, 62.8841°, 69.0913°, 70.5356°, 75.1449°  correspond to crystalline planes (101), (103), 

(004), (112), (200), (211), (204), (116), (220),  and (215), respectively, according to the standard 

card No. 96-152-6932. The diffraction peaks for the identified Rutile phase appeared at 27.6076°, 

36.2423°, 41.5277°, 54.3108°, and 56.7998° corresponding to crystalline planes (110), (101), 

(111), (211), and (220), respectively, according to standard card No. 96-900-4142. The dhkl value 

was calculated using Bragg law [25]: 

n λ = 2 dhkl sin θ                   (1) 

whereas the Debye-Scherrer equation was used to determine the value D [26]: 

D = 
K λ

β Cosθ
                                (2)  

Where D: crystallite size, K: constant Scherrer, λ: is the monochromatic wavelength of X-ray= 

0.154061 nm, θ: diffraction angle, and β: full width at half maximum (FWHM) in rad. Table 1 

shows the X-ray peak parameters of TiO2-NPs. The average crystalline size is 18.9 nm. 

 

 

Figure 4. XRD pattern for TiO2-NPs. 

 

 

 

 

 



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226 
 

Table 1. XRD results for TiO2-NPs. 

2θ (Deg.) FWHM (Deg.) dhkl (Å) D (nm) Phase 

25.6218 0.3876 3.4740 21.0 AnataseTiO2 

27.7385 0.3279 3.2135 25.0 RutileTiO2 

36.3842 0.3876 2.4673 21.6 RutileTiO2 

37.2487 0.4472 2.4120 18.8 AnataseTiO2 

38.1133 0.4472 2.3592 18.8 AnataseTiO2 

38.8884 0.4174 2.3140 20.2 AnataseTiO2 

41.6312 0.4771 2.1677 17.8 RutileTiO2 

44.3739 0.4770 2.0398 18.0 RutileTiO2 

48.3986 0.4770 1.8792 18.3 AnataseTiO2 

54.2419 0.4770 1.6897 18.7 RutileTiO2 

54.6891 0.3875 1.6770 23.1 AnataseTiO2 

55.4940 0.4472 1.6545 20.1 AnataseTiO2 

56.8952 0.4472 1.6171 20.2 RutileTiO2 

63.1261 0.5367 1.4716 17.4 AnataseTiO2 

64.4080 0.5068 1.4454 18.5 RutileTiO2 

69.2973 0.6261 1.3549 15.4 AnataseTiO2 

70.6687 0.6559 1.3319 14.9 AnataseTiO2 

75.3790 0.5665 1.2599 17.7 AnataseTiO2 

76.3330 0.7752 1.2465 13.0 AnataseTiO2 

 

3.4. Fourier Transform Infrared Spectroscopy (FTIR) 

   FTIR spectra provide specific data about the chemical bonding and molecular structures of 

organic compounds and a limited number of inorganic materials. It is useful for the identification 

of unknown compounds when patterns of IR spectra are available. FTIR spectra were recorded 

over a wavelength range between 400 and 4000 cm-1. Figure 5 shows the FTIR spectrum of TiO2-

NPs. In this Figure, a wide absorption band at 3421.72 cm-1 is caused by the surface adsorbed 

moisture of the synthetic TiO2-NPs straining the O-H bond. The weak absorption bands at 

2380.16 and 2312.65 cm-1 could be caused by the C=O bond stretching generated by carbon 

dioxide that was adsorbed to the NPs surface .The O-H bending of water molecules was adsorbed 

on the particle surface, resulting in the absorption band appearing at 1627.92 cm-1. The vibrational 

mode of Ti-O-Ti exhibits a distinctive peak in the broad band centered at 578.64, 547.78, and 

514.99 cm-1, which denotes the development of metal-oxygen bonding  [27]. The peak at 2879.72, 

2831.50 cm-1 confirmed the presence of secondary amines, and the peak at 1643.35 cm−1 was 

caused by the O-H bending vibration of adsorbed water molecules on the surface of TiO2 which 

may play a significant role in photocatalytic activity. Strong peaks at 1546.91, 1531.48, and 

1517.98 cm-1 indicate aliphatic nitro compounds with stretching of N-O [15].The peaks 1394.53, 

1342.46, and 1319.31 cm−1 related to aliphatic amine-containing and C-N-stretched amines [28]. 

Table 2 shows the FTIR spectrum data for TiO2-NPs. 

 

 



IHJPAS. 36 (4) 2023 

227 
 

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Figure 5. FTIR spectrum of TiO2-NPs. 

 

 

Table 2. FTIR spectrum data for TiO2-NPs. 



IHJPAS. 36 (4) 2023 

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3.5. BET analysis  

  The characteristic and adsorption capacity of the synthesized TiO2-NPs could be predicted from 

the surface area and porosity information obtained from the BET equation [29]. The specific 

surface area was calculated from the BET equation and found to be 14.741 m2/g, as shown in 

Figure 6. The total pore volume and mean pore diameter were found to be equal to 0.1191 cm3/g 

and 32.304 nm, respectively. The N2 gas adsorption/desorption isotherm for TiO2-NPs is 

presented in Figure 7. This figure shows the presence of a cylindrical pore in this sample with a 

narrow distribution of uniform pores [30]. 

 

 

 

 

 

Figure 6. BET plot for N2 gas adsorption isotherm at 77 K for TiO2-NPs. 

0

0.06

0.12

0.18

0 0.25 0.5
p/p0

p
/V

(p
0
-p

)



IHJPAS. 36 (4) 2023 

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Figure 7. Nitrogen gas adsorption/desorption isotherm for TiO2-NPs. 

4. Conclusion 

    The environmentally friendly technique for producing TiO2-NPs from PA plant extract 

compared to other preparation methods could be a promising technology because it uses no 

hazardous chemicals and is environmentally benign. SEM, AFM, XRD, FTIR, and BET are 

among the diagnostic methods used to describe the prepared particles. A few spherical, non-

agglomerated particles could be seen in the SEM image of TiO2 nanoparticles. When the surface 

topography of TiO2-NPs was studied, an average diameter of 70.24 nm was observed. Through 

the use of Debye Scherrer, the crystallite size was calculated. The crystalline size was 18.9 nm 

on average. The presence of TiO2-NPs is confirmed by the vibrational mode of Ti-O-Ti, which 

displays a characteristic peak in the broad band centered at 578.64, 547.78, and 514.99 cm-1. This 

peak indicates the development of metal-oxygen bonding. According to BET analysis, the 

specific surface area was 14.741 m2 / g and the total pore volume was 0.1191 cm3 / g. 

Titanium dioxide nanoparticles, especially those prepared by green methods, have many unique 

features and characteristics that enable them to be used to treat environmental pollution problems. 

For future work, it is recommended: 

1. Study the use of the green synthesized TiO2-NPs to get rid of other contaminants from 

the environment, such as heavy metals. 

2. Study the possibility of using these prepared nanomaterials in medical 

 

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