Released this past November, the list is based on data collected from the Web of Science and highlights some of the world’s most influential scientific minds by naming the researchers whose publications over the previous decade have included a high number of Highly Cited Papers placing them among the top 1% most-cited.
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We wish to congratulate all of the researchers named and especially our authors on this amazing accomplishment! We are happy and proud to share in their success!
IntechOpen is proud to announce that 179 of our authors have made the Clarivate™ Highly Cited Researchers List for 2020, ranking them among the top 1% most-cited.
\n\n
Throughout the years, the list has named a total of 252 IntechOpen authors as Highly Cited. Of those researchers, 69 have been featured on the list multiple times.
\n\n\n\n
Released this past November, the list is based on data collected from the Web of Science and highlights some of the world’s most influential scientific minds by naming the researchers whose publications over the previous decade have included a high number of Highly Cited Papers placing them among the top 1% most-cited.
\n\n
We wish to congratulate all of the researchers named and especially our authors on this amazing accomplishment! We are happy and proud to share in their success!
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1. Introduction
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Optical coherence tomography (OCT) is a noninvasive imaging technique that has very important advantages in the diagnosis, treatment, and management of a variety of macular disorders [1]. Since its first use in the clinics, there has been continuous advancements in OCT technology, and current spectral-domain (SD) OCT, and swept-source (SS) OCTs demonstrate macular structures on a microscopic level further clarifying the pathophysiology of many diseases and enabling novel therapeutic options. OCT evaluation has become the routine imaging method for any vitreomacular disease in retinal evaluation of the patients in the clinics as well as the essential component in any study design regarding the treatment of retinal diseases. Recently, OCT has also been integrated into our operating rooms by supporting our decision-making during vitrectomy known as intraoperative OCT (iOCT).
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Epiretinal membrane (ERM), which has also been named as epimacular membrane, cellophane maculopathy, preretinal macular fibrosis, and surface-wrinkling retinopathy, is a disorder of the vitreomacular interface. It is a fibrocellular membrane lying on the inner surface of the retina, which can cause decreased vision and/or metamorphopsia. Epiretinal membranes are frequently seen in an aging eye, especially after posterior vitreous detachment (PVD), and its prevalence increases with increased age [2]. The mean age of ERM diagnosis is 65 years old, affecting both sexes equally [3]. The prevalence of ERM varies from 2.2 to 28.9% depending on the population being studied [4, 5]. The incidence of developing an ERM in the primary eye is 1.1% per year, whereas its incidence in the fellow eye is 2.7% per year. Bilaterality changes between 19 and 31% of the eyes, and mostly with asymmetric involvement.
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2. ERM classification
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Epiretinal membranes are classified as idiopathic, and secondary regarding their etiology. Idiopathic ERM is the most common form. Secondary ERMs are associated with posterior uveitis, retinal vascular occlusions, diabetic retinopathy, trauma, retinal tear or detachment, and their repair, argon laser photocoagulation, cataract surgery [6]. Other risk factors include age, PVD, and history of ERM in the fellow eye. Secondary ERMs tend to occur in younger patients [7]. Clinically, ERMs are classified as cellophane macular reflex or preretinal macular fibrosis according to their severity [8]. Cellophane macular reflex is an early form, including a thin transparent membrane overlying the macula usually clinically asymptomatic, whereas preretinal macular fibrosis is the later form with thickened and contracted membrane causing visual impairment in most eyes.
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3. ERM-pathogenesis
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The diagnosis of PVD, which is defined as separation between the posterior vitreous cortex and the internal limiting membrane (ILM) of the retina, has been described in up to 95% of cases of idiopathic ERM [9]. Residual cortical vitreous secondary to a PVD or anomalous PVD leading to vitreoschisis with only partial separation of the posterior hyaloid remain to be factors allowing proliferation of glial cells. Inflammation is a central component of disorders leading to secondary ERMs, with increased inflammatory mediators promoting fibrocellular growth. Retinal glial cells, hyalocytes, fibroblasts, myofibroblasts are the predominant cell types found in the ERMs. Retinal pigment epithelial cells, macrophages, T-, and, B-cells are identified in secondary ERMs [6]. Extracellular matrix production and remodeling are predominant. The extracellular matrix components that have been described in ERMs include collagen types I, II, III, IV, and VI, fibronectin, and laminin [10, 11, 12]. Extracellular fibrils are thin in cellophane macular reflex and are much thicker in preretinal macular fibrosis [10].
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4. ERM clinical findings
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Epiretinal membrane is relatively common especially after 60 years of age, and both sexes are equally affected. A careful history should be obtained to evaluate for secondary causes of ERMs. The patient more often presents without any symptoms diagnosed on a routine ophthalmological examination especially with very early and thin membranes. He can also present with the symptoms of metamorphopsia, blurred vision, monocular diplopia, and micropsia [13]. Contrast sensitivity is frequently decreased.
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In the ophtalmological examination, best corrected visual acuity (BCVA) is noted. Amsler grid test is also performed. On slit lamp examination lens status with any form of cataract is noted. Dilated fundus examination is performed. Careful examination of the macular area for any subtle membrane is important as it can easily be missed on routine examination. The presence of PVD is noted. Detailed examination of the peripheral retina for any missed retinal tear should be performed. The examination of the vitreous for any cells, and of retinal vessels for secondary causes should also be performed. The same examination should also be done for the fellow eye.
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Clinically, an ERM can be seen as a loss in the normal convex contour of the fovea, an abnormal reflectivity of the macular area, or as wrinkling on the macular area in fundoscopy. As cellophane macular reflex is a thin membrane without causing any distortions in the retina, it usually does not cause visual impairment, and usually observed as an incidental finding in routine fundus examination. More advanced ERMs classified as preretinal macular fibrosis can be easily seen as they are often opaque and whitish in color, obscuring the underlying retina (Figure 1). There may be traction, or tortuosity in the vessels in thick membranes sometimes with intraretinal hemorrhages, or exudates in severe cases. Macular edema can be observed. Preretinal macular fibrosis usually distorts the retina causing visual impairment in nearly 80% of cases [14]. ERMs can give an impression of a macular hole, when there is proliferation on both sides of the fovea, but a gap in the center which looks like a macular hole gives the name as a “pseudohole”. The best method to examine it is with a contact macular or a goniolens, though it may be difficult in a busy daily practice. ERMs can also be associated with lamellar macular holes or less commonly with macular holes. The usual course is slow progression over the years with VA decreasing to 0.1.
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Figure 1.
Epiretinal membrane. Color fundus image of the left eye showing grayish tissue over the macula obscuring the details of the underlying retina and causing tortuosity in the retinal vessels. The patient complains of blurred vision and metamorphopsia.
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5. ERM diagnostic tests
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5.1. Optical coherence tomography
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Despite the fact that ERM can be diagnosed clinically, OCT imaging has become a routine part of the vitreomacular surface examination. OCT has proven to be more sensitive than clinical examination for the diagnosis of numerous disorders of the vitreomacular interface, including ERM [15]. OCT imaging shows the macular area in cross section, and three dimensionally in high resolution, and is extremely helpful in detecting subtle, very thin membranes, associated findings as macular edema, traction on the macula, lamellar macular hole, changes in the contour and the thickness of the macula, or any other macular pathology. 3D OCT imaging can help to evaluate the degree of traction, identify points of attachment and of detachment of the ERM to the retina [16]. OCT not only shows clearly if a lamellar hole is present, but also helps the differential diagnosis of ERMs, macular holes, lamellar macular holes, pseudoholes, and macular edema. OCT evaluation of eyes with ERM has also a prognostic value. It is ideal to follow the patient with the same OCT device and through the same baseline point.
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5.1.1. OCT findings
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ERMs are observed as highly reflective layer on the retinal surface. ERMs in early stage are seen as thin hyperreflective line with normal foveal contour and retinal architecture (Figure 2a, b). Idiopathic ERMs mostly are globally adherent to the retina seen as hyperreflective band, but in some cases (20–25%), they are clearly separated from the retina with focal points of attachment (Figure 3a, b) [17]. Secondary ERMs are more frequently (50%) seen with focal attachments. ERM causes increase in central macular thickness. Usually there is diffuse retinal thickening without any cystic changes in cases with ERM. Especially, the retinal layers above the outer plexiform layers increase in thickness. Increased central macular thickness alone is not usually correlated with VA of the patient. Normal foveal contour is lost. The characteristic foveal depression is not seen (Figure 4a–c). Hyperreflectivity between ILM and inner plexiform layers is increased especially in longstanding ERMs, which is a typical finding (Figure 3b). This type of fibrosis generally produces traction in retinal layers, causing visual impairment. They may be associated with underlying corrugation of the retinal surface. The surface of the retina where the ERM is more pronounced has a distinctive saw-toothed appearance corresponding to retinal striae from ERM traction [18]. ERMs can also cause irregularities in retinal layers (Figure 4a). This feature is seen more frequently with partially attached ERMs. Also, slight elevation of photoreceptor layer above RPE layer has been described as “outer retinal defect”, which may be related with traction of retina (Figure 5a). Cystoid changes in the retina observed as hyporeflective round spaces are usually accompanying longstanding ERMs as a result of intraretinal traction in idiopathic ERMs. If cystoid retinal thickening is more dominant, vascular reasons of a secondary ERM should be kept in mind. Pseudohole formation is usually accompanied by globally attached membranes (Figure 6). There is abnormally steep and wide foveal pit contour. The retinal tissue at the base of the fovea is preserved differentiating it from a lamellar (Figure 7a) or a full-thickness macular hole, and ERM is seen as hyperreflective band on the macular surface.
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Figure 2.
(a) Infrared (IR) photography of an asymptomatic patient with visual acuity of 20/20, and a thin ERM observed in routine fundoscopy. IR imaging shows a pseudo hole image at the fovea with slight wrinkling of the retina. The retinal vasculature looks normal. (b) SD-OCT image of the same eye. A thin hyperreflective line is seen on the retina which is globally adherent. There is no increase in foveal thickness, with the foveal pit contour being steeper, and wider than usual indicating an early form of a pseudohole. The retinal layers are normal. The retinal tissue at the base of the fovea is intact unlike a lamellar hole.
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Figure 3.
The SD-OCT imaging of both eyes of a patient with a complaint of slight blurring in vision, but no metamorphopsia. The VA in both eyes are 20/32 with early nuclear sclerosis in both eyes. The patient has also drusen bilaterally. (a) RE; ERM is seen as a hyperreflective layer on the macula, and we can clearly see the separated areas of ERM from the retina. There is also associated corrugation of the underlying retinal surface prominent on the temporal side. Slight intraretinal traction can be seen, and the normal foveal depression is decreased. (b) LE; The similar appearance is seen. Hyperreflectivity between ILM and inner plexiform layers is also increased at the nasal side as a typical finding. (c) The central macular thickness map shows that the central foveal thickness is increased to 390 μ in RE, and to 394 μ in LE.
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Figure 4.
(a) SD-OCT imaging of a symptomatic eye with decreased VA of 0.3, and metamorphopsia shows increased central macular thickness with loss of foveal depression. Especially the inner retinal layers are increased in thickness with associated traction of the retina. The inner segment ellipsoid band and ELM can be seen undisrupted associated with better postoperative VA. The retinal surface is irregular due to ERM, and there is traction on the retinal vasculature at the temporal side of the fovea seen in IR photograph on the left. The 62-year-old male underwent 23 g pars plana vitrectomy with ERM and ILM peeling. (b) SD-OCT image at postoperative month 1 shows decreased central macular thickness with no traction of the retina. The retinal surface is smooth. The VA increased to 0.5. However, during follow-up, the VA decreased to 0.2 at postoperative month 10 due to nuclear cataract formation. Following phacoemulsification and IOL implantation, VA increased to 1.0. (c) SD-OCT image 3 months following lens surgery shows the intraretinal architecture is almost normal with normal retinal thickness and foveal depression is formed. The focal small depressions on the retinal surface of temporal side of the fovea are seen probably associated with ILM peeling. The VA is 1.0 with no symptoms.
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Figure 5.
(a) SD-OCT image of a 69-year-old male presenting with decreased vision, and metamorphopsia on the RE. The patient had an ERM with nuclear cataract. ERM is seen as a hyperreflective layer on the macula. The central macular thickness is increased to 398 μ with loss of normal contour of fovea. The ERM is partially attached. Also, there is slight elevation of photoreceptor layer above the RPE layer, which has been described as “outer retinal defect” at the center of the fovea. This feature may be related with traction of retina. The VA was 0.3. (b) The patient underwent combined lens surgery with ERM, and ILM peeling. At postoperative week 2, SD-OCT shows decreased macular thickness, with foveal depression appearing. The photoreceptor layer is still a bit irregular at the fovea. (c) Postoperative month 1, the VA increased to 1.0. Intraretinal architecture is getting better. (d) Postoperative month 3. The photoreceptor and ELM layers look normal and intact.
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Figure 6.
SD-OCT image of a patient shows an ERM as a thin hyperreflective layer on the macula on both sides of the fovea, but there is a gap in the foveal center. Foveal depression is steeper, giving the image of a pseudohole. There is no loss of outer retinal tissue at the base of the fovea.
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Figure 7.
(a) SD-OCT image of a 39-year-old female with an ERM and a lamellar macular hole (LMH) secondary to tractional retinal detachment. There is a hyperreflective layer of ERM on both sides of the fovea, retinal thickness is increased at the nasal side. There is loss of retinal inner layers at the temporal side of the fovea compatible with LMH. The outer layer is also decreased at the center, and disruption of the photoreceptor segment layer is noted. The retinal thickness is decreased due to atrophy at the temporal side of the fovea. The VA decreased to 0.6 during follow-up with symptoms of metamorphopsia. The patient underwent vitrectomy with ERM, and ILM peeling due to TRD, and vitreous hemorrhage from active vessels despite argon laser treatment. (b) At postoperative month 6, SD-OCT image demonstrates that LMH is closed. The retinal layers are better defined at the nasal side. Photoreceptor and ELM layers are continuous with no disruption. The VA increased to 1.0 with totally attached retina.
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There is still no internationally approved OCT-based classification system of ERMs. In one study, classification of idiopathic ERM based on the morphologic characteristics of the fovea has been proposed [19]. In another one, the anatomical structure of the vitreoretinal interface and the macula was studied and divided into two major groups according to the presence of PVD, and subdivided by the presence of contraction, edema, lamellar macular hole, and vitreomacular traction [20]. However, their clinical relevance is unclear.
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OCT imaging is also helpful for decision-making in the management of an ERM. If the membrane is thin showing near normal contour in OCT not associated with metamorphopsia or blurred vision clinically the patient is usually followed up with periodically checking for symptoms and with OCT. However, some clinically subtle ERMs are better observed with OCT for accompanying vitreomacular traction. These cases may be offered earlier surgery or at least followed up more closely for worsening of symptoms. On the other hand, with OCT imaging, we can assess the vitreoretinal interface in detail and note how diffuse or how tight is the adherence of the ERM and can decide to approach which site to start peeling of the ERM surgically. 3D OCT imaging can also be helpful in identifying any free edges of the ERM that may help in starting membrane peeling during surgery [16, 21]. A new report using en-face OCT scans and generating a map, which is called the GapMap, showing the elevated and attached areas between an ERM and the macula stated that this imaging can help surgeons detect elevated areas of ERM preoperatively to avoid excessive retinal contact during surgical manipulation [22]. They commented that in the future, such en-face gliosis reports may be incorporated into computer-assisted surgery systems installed in the operating microscope’s oculars, serving as a source of intraoperative guidance for surgeons to facilitate the removal of ERM with reduced trauma [23].
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OCT imaging also demonstrates all the layers of the retina, which is also important for the prognosis of the surgical outcome of an ERM removal. These features will be outlined below in “Surgical Prognosis” section.
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5.1.2. Intraoperative OCT
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OCT has become an essential imaging in guiding our clinical decision-making, and it has recently been adapted to use during surgery, known as intraoperative OCT (iOCT). Prospective studies performed have already shown the safety and feasibility of iOCT imaging [24, 25]. The most common posterior segment procedure was vitrectomy with membrane peeling, in 43% of which iOCT informed surgeon decision-making [24]. The following study, performed to evaluate a microscope-integrated iOCT system with a heads-up display, showed that iOCT data conflicted with the surgeon’s impression of membrane peel completeness in 19% of cases [25]. The surgeons reported that use of iOCT provided valuable feedback in 71% posterior-segment surgeries [26]. The author’s experience is also compatible with the findings of the studies that, iOCT can show residual membranes if any, unconnected areas between ERM and the retina, and confirm if ERM/ILM peel is completed during ERM surgery. Although iOCT is a nice instrument to supplement surgical assessment, it is not available in most ORs, is costly, and is apt to further advancements of the system in the future.
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5.2. Optical coherence tomography angiography
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Optical coherence tomography angiography (OCTA) is a new technology for imaging the microvasculature of the retina and choroid, using laser light reflectance of the surface of moving red blood cells to demonstrate vessels noninvasively. The vessels through different segmented areas of the eye can be imaged, and differences can be analyzed between scans. The image is segmented into four zones, namely, the superficial retinal plexus, the deep retinal plexus, the outer retina and the choriocapillaris. OCTA can show the changes in the retinal vasculature caused by macular traction of an ERM. OCTA can help to evaluate the depth and extent of foveal capillary distortion. Reduction in VA is found to be associated with this distortion [27]. Differences in foveal avascular area and decrease in parafoveal vascular density both in superficial and deep capillary plexus are also reported in the eyes following ERM surgery, and these changes were associated with worse postoperative VAs [28]. As more studies will be performed with OCTA imaging, more prognostic findings may be available for surgeons to help decision-making for removal of ERM as well as to determine visual prognosis.
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5.3. Fundus fluorescein angiography
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Fundus fluorescein angiography (FFA) is usually not necessary in routine evaluation of ERMs, but it is helpful in secondary ERMs following retinal vascular occlusions or inflammations to assess not only the macular area but also the peripheral retinal circulation. It can demonstrate leakage, traction on the vessels, ischemia, or secondary neovascularizations.
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6. ERM-management
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6.1. Indication for surgery
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Most thin ERMs are visually asymptomatic and can be followed up for a long time with periodical visits and with amsler card testing by the patient himself. In reported series regarding the natural evolution of an idiopathic ERM, it is reported that in a mean follow-up of 21 months, there was no significant change in mean VA of CRT or central volume of the macula [29]. The author’s experience is also similar, especially for the initial severity, thin membranes without major tractional components. In asymptomatic cases, the OCT may reveal thickened macula with loss of central depression, and a CRT of higher than 330 microns with a VA of 20/20. So, only thickened macula due to ERM, which is measured with OCT imaging, does not correlate with the complaints of the patients. The retinal distortions induced by ERM contraction are believed to be the primary reason for visual impairment in idiopathic ERM, which can easily be observed with OCT imaging.
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When indicated, the management of idiopathic ERMs is surgical. There are still no strict recommendations regarding the exact timing of the surgery. However, the most important indication is deciding the presence of visual complaints of the patients are related with ERMs, but not cataractous or refractive changes. As the mean age of patients with ERM is usually around their 70s, their lenses have frequently cataractous changes, which should be considered as a cause of blurred vision. On the other hand, the complaint of metamorhopsia is often more intolerable for the patient and is an indication for surgical removal of an ERM even though the visual acuity is high. If the tractional distortions in the retinal layers are not prominent, and the patient has cataract without any metamorphopsia, the patient can be offered a lens surgery first, and the ERM can be followed-up, informing the patient has a higher risk of having postoperative macular edema. On the other hand, if the surgical removal is indicated, a combined surgery of a pars plana vitrectomy and a lens surgery is usually preferred as cataractous changes usually increase fastly following PPV, necessitating a lens surgery soon after.
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6.2. Surgery
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Epiretinal membrane surgery involves a pars plana vitrectomy procedure with ERM peeling. Internal limiting membrane peeling (ILM) is usually performed to prevent secondary membrane formation. It is already reported that ILM peeling decreased secondary membrane formations significantly [30]. A meta-analysis reported that vitrectomy with ILM peeling resulted in better visual improvement in long-term follow-ups and lower ERM recurrence rates [31]. On the other hand, other meta analyses reports found that although additional ILM peeling could result in a significantly lower ERM recurrence rates, it does not significantly influence postoperative best-corrected VA and central macular thickness [32, 33]. The postoperative VA is not found to be different in two groups with or without ILM peeling in idiopathic ERMS in a prospective trial [34]. The author’s experience is also similar. In a prospective interventional case series, the efficacy and safety of combined peeling of ERM and ILM membranes with the single injection of mixture of tryphan blue and brilliant blue G dyes in eyes with idiopathic ERM was evaluated (Video). Seven (three pseudophakic and four phakic) eyes underwent vitrectomy and eight eyes had combined phacoemulsification and vitrectomy. Four phakic patients needed lens surgery with a mean of 10 months postoperatively. At postoperative month 6, the mean CMT decreased significantly from 502 ± 35 to 277 ± 43 μ. The mean VA significantly increased from 20/64 to 20/32 in all eyes with no recurrent ERM observed (Figure 8) [35].
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Figure 8.
(a) SD-OCT image of a 73-year-old female presented with visual blurring and metamorphopsia with a VA of 0.6 shows a tightly adherent hyperreflective layer of ERM on the macula. The central retinal thickness is increased with traction on the fovea causing intraretinal cystic changes seen as hyporeflective spaces in the inner retina. The outer retinal layers are intact. The symptomatic patient underwent vitrectomy with ERM and ILM peeling. (b) SD-OCT at postoperative month 1 shows normal retinal architecture with normal retinal thickness. There is small depression on the superior side. The patient’s metamorphopsia decreased with a VA of 1.0. (c) SD-OCT image at postoperative year 5 is the same with no recurrent ERM observed during 5 years of follow-up.
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ILM peeling maneuver should be performed cautiously to avoid secondary complications as a retinal hole formation, traumatic defects in the macular area, as well as phototoxicity. The surgery itself has the possible complications of a PPV, such as retinal tear and detachment, endophthalmitis, loss of ganglion cells, and others, which must be discussed with the patient.
\n
\n
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6.3. Surgical prognosis
\n
Following ERM removal increase in VA of two or more lines in 60–85% of cases 6–12 months postoperatively with around 50% gaining a VA of 20/50 or better [36]. The mean preoperative and postoperative VA has been reported to be 20/110 and 20/55 [37]. This data were a meta-analysis of three studies reporting surgical results following small incision pars plana vitrectomy, in which the recurrence of ERM was around 1% [37]. Those with worse VA preoperatively gain more lines postoperatively. However, the eyes with higher preoperative VA tend to have a higher postoperative VA [38, 39, 40]. Poor preoperative VA, and long duration of symptoms are poor prognostic factors [36, 38, 39]. Visual acuity improves in 1–6 months postoperatively. However, VA improvement can continue to increase following 1–2 years of surgery. Successful surgical intervention is associated with both decreased central foveal thickness (CFT) and improved VA [30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42]. However, central macular thickness is not necessarily correlated with postoperative VA [4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43]. Although CFT may be useful for evaluating the impact of ERM on baseline VA, it is probably not useful for predicting postoperative VA [6]. The preoperative OCT characteristics are more important. Intact preoperative inner segment ellipsoid (ISe) band is associated with a better postoperative VA than a disrupted preoperative ISe band in both idiopathic and secondary ERMs [38, 41, 42, 43, 44, 45, 46, 47, 48, 49]. The longer photoreceptor outer segment (PROS) length is also reported to be a good prognostic factor for the postoperative VA [39, 42]. It has also been shown that the integrity of outer photoreceptor cell layer as well as of ELM is related with better postoperative VA [50]. Postoperative increase in contrast sensitivity is associated with the thickness of outer retinal layer [44]. The preoperative degree of metamorphopsia was also found to be a prognostic factor for the postoperative degree of metamorphopsia, suggesting that surgery for ERM should be performed before development of severe metamorphopsia [39].
\n
\n
\n
\n
7. Conclusion
\n
In conclusion, OCT provides a very detailed information of all the retinal layers, and the vitreomacular interface. Epiretinal membranes are a frequent clinical finding in an aging eye, and sometimes result in decreased vision, and/or metamorphopsia. OCT, as a noninvasive, fast imaging system of the macula being more sensitive than the clinical examination has become the routine evaluation of ERMs. OCT imaging is used to diagnose, differentiate, manage, and follow ERMs. It also gives valuable information regarding the visual prognosis of the operated eye. Intact and continuous preoperative inner segment ellipsoid band, the longer photoreceptor outer segment, and the integrity of ELM are reported to be good prognostic signs. On the other hand, preoperative three-dimensional OCT evaluation of an ERM can also help the surgeons to identify any free edges of the ERM that may help in starting membrane peeling with reduced trauma. Lastly, OCT has recently been integrated into our operating rooms as intraoperative OCT and may support our decision-making during vitrectomy.
\n
\n\n',keywords:"central macular thickness, external limiting membrane idiopathicepiretinal membrane, internal limiting membrane, lamellar macular hole, optical coherence tomography, OCT, pars plana vitrectomy, photoreceptor, posterior vitreous detachment, pseudohole, secondary epiretinal membrane",chapterPDFUrl:"https://cdn.intechopen.com/pdfs/62880.pdf",chapterXML:"https://mts.intechopen.com/source/xml/62880.xml",downloadPdfUrl:"/chapter/pdf-download/62880",previewPdfUrl:"/chapter/pdf-preview/62880",totalDownloads:521,totalViews:238,totalCrossrefCites:0,totalDimensionsCites:1,hasAltmetrics:0,dateSubmitted:"February 8th 2018",dateReviewed:"June 26th 2018",datePrePublished:null,datePublished:"September 19th 2018",dateFinished:null,readingETA:"0",abstract:"Epiretinal membranes (ERM) are frequently seen in an aging eye, especially after posterior vitreous detachment, and can cause decreased vision, and/or metamorphopsia. Not all of the ERMs detected in routine ophthalmological examination are indicated to be removed with surgery. Optical coherence tomography (OCT) examination reveals the microanatomy of all the retinal layers and enables the vitreoretinal surgeon to make decision to follow-up or to perform a vitrectomy to peel the ERM. OCT imaging clearly shows all the tractions on the retina and the intraretinal layers; and can have a prognostic value for the surgery. OCT imaging is also very valuable in the differential diagnosis of pseudoholes with macular and lameller holes; much better than the clinical examination. It is a routine part of the detailed retinal examination of an eye with an ERM. This chapter covers OCT findings in ERMs, and examples of cases with ERMs indicated for surgery of follow-up will be shown, explaining the clinical results of the cases.",reviewType:"peer-reviewed",bibtexUrl:"/chapter/bibtex/62880",risUrl:"/chapter/ris/62880",book:{slug:"oct-applications-in-ophthalmology"},signatures:"Nur Acar",authors:[{id:"244973",title:"Prof.",name:"Nur",middleName:null,surname:"Acar",fullName:"Nur Acar",slug:"nur-acar",email:"nuracarr@gmail.com",position:null,institution:null}],sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_2",title:"2. ERM classification",level:"1"},{id:"sec_3",title:"3. ERM-pathogenesis",level:"1"},{id:"sec_4",title:"4. ERM clinical findings",level:"1"},{id:"sec_5",title:"5. ERM diagnostic tests",level:"1"},{id:"sec_5_2",title:"5.1. Optical coherence tomography",level:"2"},{id:"sec_5_3",title:"5.1.1. OCT findings",level:"3"},{id:"sec_6_3",title:"5.1.2. Intraoperative OCT",level:"3"},{id:"sec_8_2",title:"5.2. Optical coherence tomography angiography",level:"2"},{id:"sec_9_2",title:"5.3. Fundus fluorescein angiography",level:"2"},{id:"sec_11",title:"6. ERM-management",level:"1"},{id:"sec_11_2",title:"6.1. Indication for surgery",level:"2"},{id:"sec_12_2",title:"6.2. Surgery",level:"2"},{id:"sec_13_2",title:"6.3. Surgical prognosis",level:"2"},{id:"sec_15",title:"7. Conclusion",level:"1"}],chapterReferences:[{id:"B1",body:'Huang D, Swanson EA, Lin CP, et al. Optical coherence tomography. Science. 1991;254:1178-1181\n'},{id:"B2",body:'Aung KZ, Makeyeva G, Adams MK, et al. The prevalence and risk factors of epiretinal membranes: The Melbourne Collaborative Cohort Study. Retina. 2013;33(5):1026-1034\n'},{id:"B3",body:'Fraser-Bell S, Guzowski M, Rochtchina E, et al. Five-year cumulative incidence and progression of epiretinal membranes: The Blue Mountains Eye Study. Ophthalmology. 2003;110(1):34-40\n'},{id:"B4",body:'You Q, Xu L, Jonas JB. 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Journal of Ophthalmology. 2015;2015:838646;1-7. DOI: 10.1155/2015/838646\n'},{id:"B23",body:'Kreatsoulas J. Enhancing retinal surgery with augmented reality technology. Retina Today. 2011;6(3):18\n'},{id:"B24",body:'Ehlers JP, Dupps WJ, Kaiser PK, et al. The prospective intraoperative and perioperative ophthalmic imaging with optical coherence tomography (PIONEER) study: 2-year results. American Journal of Ophthalmology. 2014;158:999-1007\n'},{id:"B25",body:'Ehlers JP, Goshe J, Dupps WJ, et al. Determination of feasibility and utility of microscope-integrated optical coherence tomography during ophthalmic surgery: The DISCOVER study RESCAN results. JAMA Ophthalmology. 2015;133:1124-1132\n'},{id:"B26",body:'Ehlers JP, Tao YK, Farsiu S, et al. Integration of a spectral domain optical coherence tomography system into a surgical microscope for intraoperative imaging. Investigative Ophthalmology & Visual Science. 2011;52:3153-3159\n'},{id:"B27",body:'Nelis P, Alten F, Clemens C, Heiduschka P, Eter N. Quantification of changes in foveal capillary architecture caused by idiopathic epiretinal membrane using OCT angiography. Graefe\'s Archive for Clinical and Experimental Ophthalmology. 2017;255(7):1319-1324\n'},{id:"B28",body:'Kim YJ, Kim S, Lee JY, Kim JG, Yoon YH. Macular capillary plexuses after epiretinal membrane surgery: An optical coherence tomography angiography study. The British Journal of Ophthalmology. 2017. DOI: 10.1136/bjophthalmol-2017-311188. pii: bjophthalmol-2017-311188\n'},{id:"B29",body:'Hejsek L, Stepanov A, Dohnalova A, Rehakova T, Jiraskova N. The natural evolution of idiophatic epimacular membrane. Biomedical Papers of the Medical Faculty of the University Palacky, Olomouc, Czech Republic. 2017;161(1):100-106\n'},{id:"B30",body:'Sandali O, El Sanharawi M, Basli E, et al. Epiretinal membrane recurrence: Incidence, characteristics, evolution, and preventive and risk factors. Retina. 2013;33(10):2032-2038\n'},{id:"B31",body:'Chang WC, Lin C, Lee CH, Sung TL, Tung TH, Liu JH. Vitrectomy with or without internal limiting membrane peeling for idiopathic epiretinal membrane: A meta-analysis. PLoS One. 2017;12(6):e0179105\n'},{id:"B32",body:'Fang XL, Tong Y, Zhou YL, Zhao PQ, Wang ZY. Internal limiting membrane peeling or not: A systematic review and meta-analysis of idiopathic macular pucker surgery. The British Journal of Ophthalmology. 2017;101(11):1535-1541\n'},{id:"B33",body:'Azuma K, Ueta T, Eguchi S, Aihara M. Effects of internal limiting membrane peeling combined with removal of idiopathic epiretinal membrane: A systematic review of literature and meta-analysis. Retina. 2017;37(10):1813-1819\n'},{id:"B34",body:'Tranos P, Koukoula S, Charteris DG, Perganda G, Vakalis A, Asteriadis S, Georgalas I, Petrou P. The role of internal limiting membrane peeling in epiretinal membrane surgery: A randomised controlled trial. The British Journal of Ophthalmology. 2017;101(6):719-724\n'},{id:"B35",body:'Acar N. Combined peeling of epiretinal and internal limiting membranes with the single injection of membraneblue-dual® in eyes with idiopathic ERM. In: Proceedings of 13th Annual Meeting of European Vitreo Retinal Society; Rhodes, Greece; 2013\n'},{id:"B36",body:'Wong JG, Sachdev N, Beaumont PE, Chang AA. Visual outcomes following vitrectomy and peeling of epiretinal membrane. Clinical & Experimental Ophthalmology. 2005;33(4):373-378\n'},{id:"B37",body:'Gupta OP, Brown GC, Brown MM. A value-based medicine cost-utility analysis of idiopathic epiretinal membrane surgery. American Journal of Ophthalmology. 2008;145(5):923-928\n'},{id:"B38",body:'Kinoshita T, Imaizumi H, Okushiba U, Miyamoto H, Ogino T, Mitamura Y. Time course of changes in metamorphopsia, visual acuity, and OCT parameters after successful epiretinal membrane surgery. Investigative Ophthalmology & Visual Science. 2012;53(7):3592-3597\n'},{id:"B39",body:'Kinoshita T, Imaizumi H, Miyamoto H, Katome T, Semba K, Mitamura Y. Two-year results of metamorphopsia, visual acuity, and optical coherence tomographic parameters after epiretinal membrane surgery. Graefe\'s Archive for Clinical and Experimental Ophthalmology. 2016;254(6):1041-1049\n'},{id:"B40",body:'Rahman R, Stephenson J. Early surgery for epiretinal membrane preserves more vision for patients. Eye (London, England). 2014;28(4):410-414\n'},{id:"B41",body:'Mitamura Y, Hirano K, Baba T, Yamamoto S. Correlation of visual recovery with presence of photoreceptor inner/outer segment junction in optical coherence images after epiretinal membrane surgery. The British Journal of Ophthalmology. 2009;93(2):171-175\n'},{id:"B42",body:'Jeon S, Jung B, Lee WK. Long-term prognostic factors for visual improvement after epiretinal membrane removal. Retina. 2018 May 14. DOI: 10.1097/IAE.0000000000002211\n'},{id:"B43",body:'Shimozono M, Oishi A, Hata M, Matsuki T, Ito S, Ishida K, Kurimoto Y. The significance of cone outer segment tips as a prognostic factor in epiretinal membrane surgery. American Journal of Ophthalmology. 2012;153(4):698-704\n'},{id:"B44",body:'Sugiura Y, Okamoto F, Okamoto Y, Hiraoka T, Oshika T. Contrast sensitivity and foveal microstructure following vitrectomy for epiretinal membrane. Investigative Ophthalmology & Visual Science. 2014;55(11):7594-7600\n'},{id:"B45",body:'Inoue M, Morita S, Watanabe Y, et al. Preoperative inner segment/outer segment junction in spectral-domain optical coherence tomography as a prognostic factor in epiretinal membrane surgery. Retina. 2011;31(7):1366-1372\n'},{id:"B46",body:'Itoh Y, Inoue M, Rii T, Hirota K, Hirakata A. Correlation between foveal cone outer segment tips line and visual recovery after epiretinal membrane surgery. Investigative Ophthalmology & Visual Science. 2013;54(12):7302-7308\n'},{id:"B47",body:'Kim JH, Kang SW, Kong MG, Ha HS. Assessment of retinal layers and visual rehabilitation after epiretinal membrane removal. Graefe\'s Archive for Clinical and Experimental Ophthalmology. 2013;251(4):1055-1064\n'},{id:"B48",body:'Cobos E, Arias L, Ruiz-Moreno J, et al. Preoperative study of the inner segment/outer segment junction of photoreceptors by spectral-domain optical coherence tomography as a prognostic factor in patients with epiretinal membranes. Clinical Ophthalmology. 2013;7:1467-1470\n'},{id:"B49",body:'Kim HJ, Kang JW, Chung H, Kim HC. Correlation of foveal photoreceptor integrity with visual outcome in idiopathic epiretinal membrane. Current Eye Research. 2014;39(6):626-633\n'},{id:"B50",body:'Theodossiadis PG, Theodossiadis GP, Charonis A, Emfietzoglou I, Grigoropoulos VG, Liarakos VS. The photoreceptor layer as a prognostic factor for visual acuity in the secondary epiretinal membrane after retinal detachment surgery: Imaging analysis by spectral-domain optical coherence tomography. American Journal of Ophthalmology. 2011;151(6):973-980\n'}],footnotes:[],contributors:[{corresp:"yes",contributorFullName:"Nur Acar",address:"nuracarr@gmail.com",affiliation:'
School of Medicine, Acıbadem Mehmet Ali Aydınlar University, Maslak Hospital, Sarıyer, Istanbul, Turkey
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Ispa, Javier Mateo and Francisco Javier Ascaso",authors:[null]},{id:"66639",title:"Swept-Source Optical Coherence Tomography and Optical Coherence Tomography Angiography in Selected Posterior Uveitides",slug:"swept-source-optical-coherence-tomography-and-optical-coherence-tomography-angiography-in-selected-p",signatures:"Magdy Moussa and Mahmoud Leila",authors:[{id:"242399",title:"Prof.",name:"Magdy",middleName:null,surname:"Moussa",fullName:"Magdy Moussa",slug:"magdy-moussa"},{id:"257712",title:"Dr.",name:"Mahmoud",middleName:null,surname:"Leila",fullName:"Mahmoud Leila",slug:"mahmoud-leila"}]},{id:"67418",title:"Role of Optical Coherence Tomography in the Evaluation and Management of Glaucoma",slug:"role-of-optical-coherence-tomography-in-the-evaluation-and-management-of-glaucoma",signatures:"Baswati Sahoo and Julie Pegu",authors:[null]}]}]},onlineFirst:{chapter:{type:"chapter",id:"70161",title:"Stoichiometric and Nonstoichiometric Compounds",doi:"10.5772/intechopen.89402",slug:"stoichiometric-and-nonstoichiometric-compounds",body:'
1. Introduction
In solid-state chemistry, the study of compound has been expanded to the crystal structure level. The law of definite proportions, the law of constant composition, and the law of conservation of mass state that a chemical compound always contains exactly the same proportion of elements by mass. All chemical compounds obeying these laws are called as stoichiometric compounds. While nonstoichiometric compounds are the chemical compounds deviated from stoichiometry, namely their elemental composition cannot be represented by a ratio of well-defined natural numbers, and therefore violate the law of definite proportions, hence a nonstoichiometric compound is a type of special solid-state compound with definite structure and thermodynamic characteristics, which differs from its stoichiometric counterpart and a mixture. Due to defect structure in a continuous manner, these compounds are different with stoichiometric compounds. Beside some unusual information on solid-state chemistry, stability, and dynamics can be explore through their structure and characteristic. These nonstoichiometric compounds exhibit different properties such as conductivity, magnetism, catalytic nature, color, and other unique solid-state properties, which have important technological applications.
Experimental and calculated results demonstrate that the migration of anion and cation vacancies and the formation of insulating vacancy clusters near the vicinity of the interface are the fundamental switching mechanism [1]. The enhancement in photoconduction under below-band gap light illumination is attributed to the transition from defect levels (e.g., oxygen vacancies) [2]. The unique properties are determined by their solid phase composition, thermodynamic properties, and crystal defect structure. These properties depend upon the structure and phase of the crystal; hence, the unit cell parameter plays an important role in nonstoichiometric compound, which varies in a definite manner. The microscopic structural and macroscopic thermodynamical properties also vary with phase and unit cell parameters. The X-ray diffraction study reveals that as the composition of the nonstoichiometric compound changes, the cell parameter and other property continuously changes, which is different from crystalline stoichiometric compound. Hence, X-ray diffraction and chemical analysis are important tools to investigate the nonstoichiometry [2]. The lattice defect can be analyzed by their different properties [2]. Hence, nonstoichiometry plays very important role in the solid compounds of transition metals and becoming a challenge and new opportunity in chemistry. Therefore, study of the nonstoichiometric compounds has become an interesting field in solid-state chemistry and defect chemistry.
There are significant structural changes that are seen in nonstoichiometric compounds. The phase of matter changes as external conditions such as pressure, temperature, or chemical composition are varied. Due to sudden change in these external thermodynamical conditions, the crystalline structure also changes. Thus, an abrupt change in thermodynamical conditions, such as specific volume, entropy, or specific heat, also changes the derivatives of free energy. Therefore, these parameters can be used as a helpful indicator of phase transitions. The abrupt changes can identify them as driven by a pseudo phase transition that is a result of a sharp switch of predominant defect species [3]. The defect that is introduced by sudden change in conditions, changes the physical properties of a material. It is quite different from the abrupt variation in physical properties that arises from symmetry or ordering change in a conventional phase transition. Therefore, according to the conventional classification, a defective state of a material cannot be labeled as a distinct physical phase compared with the perfect one.
In this chapter, we tried to understand the effect of change in stoichiometry of nickel oxide compound. We have prepared the samples of nickel oxide with thermal decomposition method. The samples were analyzed by different characterized methods and found to nonstoichiometric. The effect of nonstiochiometry on oxidation state, bonding between oxygen and nickel, magnetic property, specific heat, and structural property were studied.
2. Classification and point defect formation in nonstoichiometric compounds
The compounds with uniform physical phase in which unit cell parameters vary with its composition in a continuous manner are nonstoichiometric. The free energy of such compounds is function of composition and temperature of the system. The chemical potential depends on the composition of solid, and due to microscopic and macroscopic characteristics, the structural and thermodynamical property changes. Different parameters of crystallography cell, obtained by X-ray diffraction analysis, change due to nonstoichiometry. This parameter continuously varies with its composition [3].
Element composition is the main criteria to classify the nonstoichiometric compounds. These compounds exist only in the condensed state. Transition metal oxides are generally nonstoichiometric, some nitrides and sulfides also comes under such category [4, 5, 6]. Most nonstoichiometric compounds have compositions that are close to those of stoichiometric compounds and can be expressed by formulas such as WO3−x, Co1−xO, Zn1+xO, and Ni1−xO, in which x is a positive quantity much smaller than 1. In the first case, an oxygen vacancy would be formed, and in some cases, there is metallic deficiency that is seen. Due to deviation from stoichiometric composition, it would result in the formation of some lattice imperfections. Hence, in some nonstoichiometric compounds, there are anionic vacancies and in some, there are cationic vacancies. These vacancies are formed due to defects in the lattice structures of crystalline substances, such as the absence of ions from sites that would normally be occupied. The crystallographic point defects are the main defects in which interstitial atoms and vacancies resulting from excess or deficiency of a component element. Point defects are an important cause of formation of the nonstoichiometric compounds. There are two main point defects in nonstoichiometric compounds namely Frenkel defect and Schottky defect. The Frenkel defect explains a defect in the molecule, where an atom or ion (normally, the cation) leaves its own lattice site vacant and instead occupies a normally vacant site, while the Schottky defect forms when vacancies are created when oppositely charged ions leave their lattice sites. Formation of theses vacancies in stoichiometric system helps in maintaining an overall neutral charge in the ionic solid. These created vacancies are filled by the movement of surrounding atoms, due to which new vacancies are formed. The formation of defects in the crystal will lead to a decrease in the density of the crystal or metal. This can be understood by Figure 1.
Figure 1.
Schottky and Frenkel defects.
3. Nonstoichiometry in nickel oxide
Nickel oxide is an antiferromagnetic [7] and Mott-Hubbard insulator [7]. Nickel oxide (NiO) has been among some of the transition metal oxide, which is most thoroughly studied by the researchers. It can be easily synthesized and is very low in preparation cost, the nature of this material is such that it has low toxicity and it is environmental friendly. These properties of nickel oxide attracted considerable interest of the researchers. Due to its versatility, nickel oxide is useful in number of applications, such as transparent conductive film [8], chemical sensors [9], and resistive random access memory [10]. The positive electrode in batteries [11] and in quantum dot light emitting devices as a hole transport layer [12] are some of the very latest and important applications of nickel oxide material. The condition of synthesis of the material plays very important role in the applications. If the condition of sample preparation changes, then the oxygen content of the sample also changes, and NiO of different stoichiometry (Ni1−δO) can be obtained. In such samples, the composition ratios between nickel and oxygen are not exactly 1:1. Because of excess oxygen and vacancies on Ni site, nickel oxide thus becomes a p-type metal-deficit semiconductor [8]. The findings of investigations done by authors suggest that Ni vacancy is the most dominant point defect present in the system, rather than oxygen interstitial [13, 14]. The distribution of vacancy over a particular volume is an important issue. Due to difference in the nature of surface and bulk, the defect formation and hence distribution of vacancy will be different. The charge transport in NiO, as in other transition metal oxides, is of the thermally activated hopping type, and electron holes are localized at cation lattice sites. The nature of defect clusters and complexes in metal-deficit NiO, as well as the role of specific impurities, influence remarkably the different characteristic properties of nonstoichiometric NiO. This specific vacancy distribution has its strong effect on the overall electrical [15], optical [16], and thermal [17] properties, depending strongly on its stoichiometry.
The main reason for changes in properties could be the excess oxygen present in the samples. This excess oxygen also changes the oxidation state of nickel, which produces a vacancy at the metal side to produce cation vacant nickel oxide. As the temperature of sintering of precursor increases, the excess of oxygen decreases. Due to increase in the excess of oxygen, densities of nickel oxide and activation energy of electrical conductivity decrease, but the lattice parameter of such samples is unaffected [18]. The diffusion of vacancies to the crystal surface is the main reason for the decrease in vacancies [19].
NiO adopts the NaCl structure, with octahedral Ni(II) and O2− sites. The conceptually simple structure is commonly known as the rock salt structure. Like many other binary metal oxides, the nonstoichiometry is accompanied by a color change, with the stoichiometrically correct NiO being green and the nonstoichiometric NiO being black. Bulk material of NiO has a cubical crystal structure, and it shows antiferromagnetic behavior below Neel temperature, and above it, the structure is transformed into a cubic one with paramagnetic behavior [20]. The change in the particle size is attributed to the excess oxygen present in nonstoichiometric nickel oxide. Scientist suggested that due to the change in oxygen content of the sample, the complexity of the disordered arrangement, volume distribution, and random orientation of the magnetization vector changes; hence, thermal, optical, electrical, magnetic, and many other properties of sample change. Due to the change in the particle size of antiferromagnetic materials sintered at different temperatures, the surface to volume ratio becomes sufficiently large. Because of their large surface area, the existing uncompensated spins give a nonzero net magnetic moment.
4. Synthesis of nonstoichiometric nickel oxide
Preparation of compound plays an important role in its characteristic properties. Nonstoichiometric compounds, whose composition and structure are known, are very important as they have unique optical, electrical, magnetic, thermal, and mechanical properties. The selection of precursor for design and tailoring the materials of different stoichiometry for desirable performance is of great interest. By means of effective and precise control of the composition, defect, and structure, the nonstoichiometry can be created. Depending on the conditions of preparation, the sintering temperature, in particular, NiO samples of various surface areas, colors, and degrees of nonstoichiometry can be prepared. Nickel oxide can easily be prepared via several methods, including chemical route, evaporation [12], sputtering [8], chemical deposition [21], oxidation of nickel [22], sol-gel method [23], and thermal decomposition [24]. Thermal decomposition method is a typical powder preparation method, which is simple, low-cost, and fast endothermic process.
Nonstoichiometric nickel oxide was obtained by thermal decomposition of nickel nitrate hexahydrate [25]. Typically, about 5 g Ni(NO3)2.6H2O was decomposed thermally in open air for 3 hours at 400°C to produce nickel oxide sample with a particular content of oxygen (Ni1−δO). The product thus obtained was pure and contains no other mixture. This exothermic reaction is noncatalytic and does not require any other substance to initiate the reaction. The output material obtained by breaking down the precursor is nickel oxide and gaseous parts, which are escaped from the system freely. The decomposition mechanism of this process takes the minimum time-temperature condition. This sample was denoted as NiO400. Similarly, seven other samples were prepared at 500, 600, 700, 800, 900, 1000, and 1100°C. They were denoted NiO500, NiO600, NiO700, NiO800, NiO900, NiO1000, and NiO1100, respectively.
5. Characterization of nonstoichiometric nickel oxide
The study of compositions, substance phase, and defect are main parameters to characterize nonstoichiometric compounds. The effect of nonstoichiometry on composition, structure, and other properties is studied while characterizing these types of solids. These properties highly depend on the defects in the crystal. In the present study, composition can be determined by means of chemical analysis by iodometric titration, which was corroborated by thermo-gravimetric analysis (TGA). Phase and structure can be examined through X-ray diffraction, XPS analyses, and relationship of the composition, structure, and properties can be detected using FTIR, magnetic measurement, and specific heat measurement. So, we can categorically confirm that the nickel oxide is a nonstoichiometric compound rather than a stoichiometric compound. Furthermore, this FTIR also confirms the bonding of oxygen with metal ions, and shift in the FTIR peaks indicates change in stoichiometry of the as prepared samples.
Oxidation sate along with chemical nature and binding state were analyzed by X-ray Photoelectron Spectroscopy (XPS). This method is a surface analytical method, hence all the properties that change with composition were studied by this method. The behavior of transition temperature with change in stoichiometry was studied by temperature dependence of magnetic susceptibility (c) and heat capacity (Cp).
5.1 Structure determination of nonstoichiometric nickel oxide
To confirm the phase structure of polycrystalline powder sample, X-ray diffraction technique is one of the most important methods. This method can be used for the determination of the phase structure and unit cell parameters. The XRD measurements of the nonstoichiometric nickel oxide samples are conducted with the help of Bruker D8 Advance X-ray diffractometer. Cu Kα radiation (0.154 nm) is used for the analysis, and measurements were done in the angle ranging 10–90°. Silicon strip technology is used to detect the scattered X-ray radiations.
XRD analysis was employed to investigate the crystallinity and purity of the solid product obtained by thermal conversion in air of the polycrystalline compounds. Figure 2 shows XRD patterns of Ni1−δO samples, NiO400, NiO500, NiO700, NiO1100 and NiO600, NiO800, NiO900, and NiO1000. XRD peaks match well with the standard XRD of with no other impurity peaks, showing that these samples were of a single phase in nature in each of them. The XRD data show the presence of the characteristic peaks for NiO at 2θ in the range of 10–90°, in accordance with JCPDF File 47-1049. The lattice parameters were obtained from the following relationship analytically: sin2θ = C (h2 + k2 + l2), where C = λ2/4a2. The results of the X-ray structural analysis are given in Table 1.
Figure 2.
X-ray diffraction patterns of different nonstoichiometric samples.
Intensity (%)
2θ
Sin2 θ
h2 + k2+l2
C
(hkl)
a(Å)
a¯(Å)
61.69
37.279
0.1022
3
0.034
(111)
4.1772
4.1775
100
43.472
0.1365
4
0.034
(200)
4.1727
44.83
62.901
0.2722
8
0.034
(220)
4.1772
15.68
75.416
0.3741
11
0.034
(311)
4.1772
Table 1.
Crystallographic data using analytical analysis for NiO samples.
On comparing peaks obtained in X-ray analysis with standard JCPDF File 47-1049, we conclude that the precursor salt is transformed to NiO. Hence, data from analytical and structural analysis corroborate with the experimental data. This indicates that the NiO obtained by thermal conversion in air of the poly-nuclear coordination compounds is face-centered-cubic phase, also known as the bunsenite structure (lattice constant a of cubic unit cell, 0.4177 nm). Phase of the NiO prepared by thermal decomposition method is stable, as no other peaks were seen in the structural analysis.
Further, Sherrer formula: L = kλ/βcos(θ) is used to calculate the mean crystallite size of the NiO sample where L is the crystallite size, k is the Sherrer constant, usually taken as 0.89, λ is the wavelength of the X-ray radiation (0.154056 nm for Cu Kα), and β is the full width at half maximum (FWHM) of diffraction peak measured at 2θ.
The deduced values of crystallite size of the analyzed NiO samples are reported in Table 2, which indicates that as the sintering temperature of precursor increases the crystallite size of NiO changes.
Compounds
a (Å)
V (Å3)
Rf factor
Bregg’s R-factor
Rp
Rwp
Re
χ2
L (nm)
NiO (400°C)
4.176
72.82
2.39
3.94
24
16.7
14.9
1.26
240
NiO (500°C)
4.174
72.74
4.44
4.33
29
19.6
16.7
1.38
290
NiO (700°C)
4.172
72.64
4.04
4.51
22
15.8
13.3
1.16
350
NiO (1100°C)
4170
27.58
20.4
31.7
56
37.4
22.3
2.67
460
Table 2.
Rietveld parameters of different NiO samples.
XRD patterns were profile-refined using the Full-Prof software package (http://www-llb.cea.fr/fullweb/). Figure 3 gives the representative Rietveld profile fit for NiO400 and NiO700 samples along with different patterns obtained by using Fm3m (225) space group. The XRD analysis indicates that samples of nickel oxide have only one face-centered-cubic (fcc) phase. Table 2 gives the parameters of samples found in the characterization. XRD study reveals all the peaks of NiO that are present, and the calculation indicates unit cell volume changes with stoichiometry.
Figure 3.
Rietveld profile fit for NiO400 and NiO700 samples.
5.2 Stoichiometry and defect analysis of nickel oxide
In nonstoichiometric compounds, there exist defects in the lattice structures of crystalline substances. As there are no absolute defect-free crystals at T > 0 K, hence these defects are related to nonstoichiometry. To determine oxygen content, that is, change in vacancy of nickel oxide formed by thermal decomposition method, the redox iodometric titration is the suitable method. For iodometric titration, standardized sodium thiosulfate and potassium iodide solution were used as a titrant and titrand, and starch solution is used as an endpoint indicator. The result obtained from iodometric titration was matched by the results of thermo-gravimetric analysis (TGA). The TGA system with the top of the line METTLER TOLEDO ultra-micro balance with unique built-in calibration weights ensures an accuracy of 0.1 mg was used.
For iodometric titrations, 0.0025 g sample was dissolved in KI and HCl solution. The concentration of KI was 0.1 mol−1 and concentration of HCl was ca. 0.1 mol−1, titration was carried out using sodium thiosulfate (2.023 × 10−3 mol−1) as a titrant. The starch solution was added prior to the end-point being reached as it acts as indicator. Table 1 shows the results of excess oxygen in NiO samples obtained by iodometric titration. The oxygen content of the samples indicates that the ratio of oxygen concentration to nickel concentration is greater than 1 for those samples, which were prepared below 700°C, and as the temperature increases above 700°C, the O/Ni ratio becomes nearly equal to 1.
The result of iodometric titration indicates that, on sintering, the precursor below 700°C nickel oxide having different oxygen contents can be prepared. As the sintering temperature is raised above 700°C, the excess oxygen present in the samples evolved, and the sample becomes stoichiometric. It can also be inferred from the above results that the oxidation state of nickel ions is also affected by sintering temperature. This titration also gives the amount of Ni3+ present in the samples, and hence the percentage of excess oxygen can also be determined. This can be obtained by considering that two Ni3+ ions correspond to three ions of O2−.
The excess oxygen content of the samples was also calculated by TGA. The TGA analysis was performed in the inert atmosphere, in which the change in weight of a sample was analyzed with respect to temperature. TGA characterizes the materials according to its compositions. For our samples, by obtaining the weight loss with respect to increase in temperature, the weight of the excess oxygen is determined directly. Figure 4a gives the information about the thermogravimetric (TG) curve and its differential curve for NiO400 sample. Between 200 and 300°C, the sudden change in the mass of the sample is observed, and this indicates the amount of excess oxygen released in the heating process. This change in weight can also be associated with the desorption of oxygen from sample, which confirms nonstoichiometry. The other peak seen in the curve can be associated by the evaporation of the physically bound water. Hence, this change in the weight does not have any contribution to the estimation of excess oxygen.
Figure 4.
TGA curves of nonstoichiometric Ni1−δO samples for (a) NiO400, (b) NiO500, (c) NiO700, and (d) NiO1100; heating rate of 5°C per min. The curves indicate the change in oxygen content of different samples as the sintering temperature increases.
Unlike NiO400 TG and DGA curves for three more samples, that is, NiO500, NiO700, and NiO1100 were plotted and shown in Figure 4b–d. It is clear from the graphs that the loss in weight decreases as the sintering temperature for sample preparation increases. The change in mass for NiO500 sample is less than that of NiO400 sample and is negligible for the sample prepared above 700°C. The change in weight of samples directly indicates about excess oxygen present in the sample, which can be directly obtained from above TG curves and is shown in Table 3. Comparing the calculated excess oxygen in these nonstoichiometric samples by two different methods, it is understood that both results are similar to each other.
Excess oxygen calculated from iodometric titration and TGA.
% excess oxygen calculated for NiO400 sample prepared in presence of oxygen.
We have also prepared another sample of nickel oxide at 400°C, and the main difference is that this sample was prepared in the presence of oxygen. This sample is synthesized to understand the essential feature of excess oxygen in these nonstoichiometric samples. Figure 5 shows the TG and DGA curves of this sample. The curves shown in Figure 4a and in Figure 5 are almost similar. Hence, the samples of NiO400 prepared in air and in oxygen atmosphere are identical to each other. The weight of excess oxygen of sample prepared in presence of oxygen is slightly less as compared to NiO400 sample, which was prepared in air. The difference in loss of weight percentage is calculated, and the values are reported in Table 3. Hence from iodometric and TGA analysis, it can be understood that due to rearrangement of atoms at high temperature, the defects of atoms get heals up and the sample that was nonstoichiometric at low temperature becomes stoichiometric. This is due to change in oxidation state with respect to change in temperature of sintering of precursor.
Figure 5.
TGA curve of NiO400 prepared in oxygen atmosphere.
5.3 FTIR study of nonstoichiometric nickel oxide
FTIR spectroscopic study of Ni1−δO samples provides valuable information about the phase composition and the way in which oxygen is bonded to metal ions. Figure 6a–d show infrared (IR) transmission spectra of NiO400, NiO500, NiO700, and NiO1100 samples having different stoichiometry in the range between 400 and 4000 cm−1. We observed a prominent peak in spectrum between 440 and 460 cm−1. The slight shift in this peak for different samples is observed. This shift in the peak is noticed for all those samples that were sintered below 700°C. The reason of such peak shift can be attributed to stoichiometry of the samples. The observation of such peak in the long wavelength region, analogous to previous reports [26], could be assigned to the Ni–O stretching vibration mode, and the shifting is an indication of the nonstoichiometry present in these samples. In fact, in this long wavelength transverse optical mode, in which the sublattice of Ni2+ ions moves 180° opposite to the sublattice of O2− ions for bulk NiO has been reported to lie between 390 and 405 cm−1 [27].
Figure 6.
FTIR of nonstoichiometric Ni1_dO samples for (a) NiO400, (b) NiO500, (c) NiO700, and (d) NiO1100.
Some more peaks at 1032, 1383, and 1612 cm−1 in nonstoichiometric samples sintered below 700°C are seen prominently, which indicates the presence of hydroxide ions, nitrate ions, and some organic compounds. It is instructive to mention that the thermal analysis evidently identifies that the Ni(NO3)2.6H2O was decomposed completely to NiO at temperatures higher than 600°C [28]. The samples that are sintered till 600°C may contain some organic molecules. Further, some of the bands found to be disappeared as the decomposition temperature increases as TGA data indict that at higher sintering temperature excess oxygen decreases [28]. Some carbon impurities are also present in the spectra, indicated by 2924 and 3456 cm−1 peaks in the spectrum. Hence, FTIR data shown in Figure 6a–d, TGA data shown in Figure 4a–d, and iodometric analysis data are corroborating each other and indicate that the samples are nonstoichiometric in nature. Analyzing the data obtained by the vacancy model, the concentration of hole in nickel oxide indicates that there is deficiency of metal in Ni1−δO. Cationic vacancies of nickel in NiO are formed at nickel side due to the presence of excess oxygen. These vacancies can be ionized to create Ni3+ ions via the following reaction:
2NiNix+12O2→2NiNi+OOx+VNi′′E1
one ionized nickel vacancy (VNi′′) and two Ni3+ ions (NiNi.) will produce when two Ni2+ ions (NiNix) will react with oxygen to produce in the NiO crystal. The holes are donated by each created Ni3+ ion, which also alters the conductive NiO. The results of iodometric titration, TGA, and FTIR analyses indicate that nonstoichiometric nickel oxide is nickel-deficient. Hence, nonstoichiometric nickel oxide behaves as p-type semiconductor because according to Eq. (1), we argue that an increase in number of nickel hole concentration increases as Ni3+ ions increase.
The majority of defects in nonstoichiometric nickel oxide is electron holes, which creates the vacancies. The vacancy model crated by holes is confirmed by a Seebeck coefficient [29], electrical conductivity [30], and other measurements. The kinetic measurements of the rate of oxidation of nickel metal to nickel oxide are also given by vacancy model [31]. The physical and chemical properties of nonstoichiometric nickel oxide are altered by the defect processes, and hence excess oxygen becomes prominent role player in such crystals.
By calculating inter atomic potentials, the energies of defect formation, migration, and substitution can be calculated by the atomistic simulation [32]. In the present case, the potential describing interionic interactions is represented by ionic pair-wise potentials of the form Eq. (2) Here, the first term represents long-range Coulomb, the second term corresponds to Hafemeister and Flygare form of short-range repulsive energies [33], and Van der Waals multipole are represented by third and fourth terms, respectively.
E2
The symbols: cij and dij are the Van der Waals coefficients, and βij is the Pauling coefficient, respectively. Zm is the modified ionic charge and parametrically includes the Coulomb screening effect, while b and r are short-range parameters. Thus, the effective interionic potential contains only three free parameters (Zm, b, and r), which can be determined from the crystal properties [34]. The short-range potential parameters assigned to each ion-ion interaction were derived by empirical fitting to observed structural properties. In the context of the Columbic term, integral ionic charges are presumed, that is, 2+ for Ni and 2− for O, which enables a straight forward definition of hole states as Ni3+ or O−. The deduced potential parameters are listed in Table 4 for all the samples. It is clear from the calculated parameters as the sintering temperature of precursor increases, the nature of ordering in systems in which ions occupy sites on a face-centered-cubic (fcc) lattice changes and the nearest-neighbor (NN) and next-nearest neighbor (NNN) exchange interactions also get altered. This happens in such a manner that the structure of NiO undergoes a week cubic-to-rhombohedral distortion as a result of the magnetostriction effect in the presence of excess oxygen in the samples [35]. The NN and NNN exchange interactions and the antiferromagnetic (AFM) structure of NiO are altered due to the presence of excess oxygen in the samples. Since the radius of Ni3+ ions is smaller than that of Ni2+. The Ni3+-O2− bond distance will be short for those samples whose oxygen content is higher. In due course, interatomic potential parameters and bond length change as the sintering temperature changes, the magnetic ordering transition temperature is expected to change as we will discuss in later sections.
Samples
b (10−12 erg)
P (Å)
F (eV)
NiO400
39.51
0.388
39.592
NiO500
39.46
0.388
39.602
NiO600
39.40
0.388
39.612
NiO700
39.38
0.388
39.623
NiO800
39.40
0.388
39.612
NiO900
39.41
0.388
39.612
NiO1000
39.57
0.388
39.518
NiO1100
39.41
0.388
39.612
Table 4.
Interatomic potential parameter of nickel oxide sintered at different temperatures as discussed in Eq. (2).
5.4 XPS studies of nonstoichiometric nickel oxide
The chemical properties and stoichiometry of nickel oxide were studied by XPS analysis. For NiO500 and NiO700, XPS spectra of Ni (2p) core level are shown in Figure 7a and b, while the XPS spectra for NiO400 and NiO1100 are shown in Figure 8.
Figure 7.
High-resolution XPS spectra of the Ni (2p) core levels of the Ni oxides decomposed at a temperature of (a) 500°C and (b) 700°C. The XPS spectra were decomposed using Voigt peak function fittings.
Figure 8.
High-resolution XPS spectra of the Ni (2p) core levels of the Ni oxides decomposed at a temperature of (a) 400°C and (b) 700°C. The XPS spectra were decomposed using Voigt peak function fittings.
In both the spectra, distinct peaks for different binding energies can be observed clearly along with the double peak features. These double peak features represented for the Ni (2p) core levels are observed in all samples. Voigt peak fitting function is used to analyze the double peak features of Ni(2p3/2) and Ni(2p1/2). These peaks were fitted within the Shirley background. The binding energy of 853.7 (±0.2), 855.5 (±0.2), 860.6 (±0.2), 865.9 (±0.2), 871.4 (±0.2), 873.3 (±0.2), 877.9 (±0.2), and 880.7 (±0.2) eV represented by a, a′, b, b′, c, c′, d, and d′ are associated with all eight peaks, which are perfectly fit. The peaks marked as a, a′, c, and c′, represent core levels of Ni2+(2p3/2), Ni3+(2p3/2), Ni2+(2p1/2), and Ni3+(2p1/2), respectively. The decomposed shake-up satellite peaks (marked as b, b′, d, and d′) were observed at ∼7.1(±0.2) or 10.2(±0.2) eV and ∼6.3(±0.3) or ∼7.1(±0.2) eV higher in binding energy than that of Ni2+(2p3/2), Ni3+(2p3/2), Ni2+(2p1/2), and Ni3+(2p1/2) peaks, respectively. The magnetic chemical state of Ni2+ and Ni3+ ions can be associated with the double peak features of Ni(2p). The consecutive shake-up satellite peaks also give information of the same [36]. The positions of the XPS peaks obtained in different nonstoichiometric samples are analogs to previous studies [37]. The O(1 s) XPS spectra of the samples obtained were similar to each other. Figure 8 shows the O(1 s) spectra Voigt peak fitting function within the Shirley background. The binding energy of 529.3 and 531.1 eV with FWHM of 1.2 and 1.7 eV are clearly observed in the figure for oxygen spectra. Hence, two peaks are clearly obtained for O(1 s) spectra. The lower binding energy peak observed at 529.3 eV corresponds to the O(1 s) core level of O2− anions associated with Ni-O chemical bonding. However, higher binding energy peak observed at 531.1 represents the surface contamination or presence of hydroxyl (−OH) groups [37].
The close analysis of decomposed XPS spectrum revealed that the intensity of the peaks assigned to core levels of Ni3+(2p3/2) and Ni3+(2p1/2) is larger than that of core levels Ni2+(2p3/2) and Ni2+(2p1/2) at decomposition temperature of 400 and 500°C. However, the intensity of the peaks of Ni2+(2p3/2) and Ni2+(2p1/2) core levels has increased than that of the peaks of Ni3+(2p3/2) and Ni3+(2p1/2) core levels after the decomposition temperature of 700°C and is continued to increase for the temperature of 1100°C. The intensity ratio obtained for the peaks of the Ni2+(2p3/2) and Ni3+(2p3/2) core levels (i.e., Ni2+/Ni3+) has increased from 0.85 (±0.03) to 1.23 (±0.03) with an increase in the temperature from 400 to 1100°C.
It is evident that for the samples prepared at 500 and 700°C have more prominent variation of intensity, and hence the Ni2+ and Ni3+ are more easily bifurcated at these temperatures because the conversion of Ni3+ ions into Ni2+ ions is fast. And the binding energy difference (ΔE) of 17.7 (±0.1) eV between the Ni(2p3/2) and Ni(2p1/2) peaks is very close to that of 17.8 eV for oxidized Ni and significantly larger than that of 17.2 eV for metallic Ni [38]. Hence, all the nickel is converted into oxide form, and there is no nickel present in the metal form. This can be confirmed by XPS investigation that the nonstoichiometric NiO400 contains Ni3+ ions in higher quantity as compared to NiO1000. The XPS analysis also corroborates with our TGA analysis for nonstoichiometric nickel oxide. Hence, the oxygen content of the samples can be controlled by controlling the temperature of preparation of samples. Hence, nonstoichiometry in nickel oxide can be created by controlling temperature of preparation.
5.5 Magnetic properties measurements of nonstoichiometric nickel oxide
The magnetic characterization of nonstoichiometric samples was performed to obtain the magnetic susceptibility (χ). These measurements were done for selected samples of NiO400 and NiO1100. Temperature-dependent magnetic susceptibility (χ) is shown in Figure 9. This measurement was performed at an applied magnetic field of 7 Tesla. Both zero-field-cooled (ZFC) and field-cooled (FC) conditions were employed to measure the susceptibility (χ) of nonstoichiometric nickel oxide samples. We observed a reversible behavior with negligible hysteresis of χ for different stoichiometry. It is interesting to describe that sample shows paramagnetic (PM) to antiferromagnetic (AFM) transition. This transition is observed at the Néel temperature TN. But the transition temperature at which transition takes place is different in both the samples. The values are 480 and 530 K for NiO400 and NiO1100 samples, respectively. TN and the absolute value of χ for NiO400 sample are lower than that of NiO1100 sample. However, PM to AFM transition width appears to be broader for the NiO1100 sample. This can be understood as TN changes with stoichiometry, which could be attributed to the effect of the partial destruction of Ni2+–O–Ni3+ exchange interaction network because of the reduction of the oxygen vacancies and the weakening of Ni2+–O–Ni3+ interaction arising from the decrease of the bandwidth of, for example, electrons due to the change in Ni–O bond length and Ni–O–Ni bond angle [39].
Figure 9.
Magnetization for ZFC and FC curves of nonstoichiometric Ni1−δO samples for NiO400 and NiO1100 in 7 T applied field as a function of temperature.
5.6 Specific heat measurement
Figure 10 shows the change in specific heat with respect to temperature of nonstoichiometric NiO. The irregularity or the change in specific heat for different samples is found in the vicinity of TN. This shows that AFM ordering of these samples is affected by oxygen content of the samples. A shift in anomaly is probed as the stoichiometry of sample changes. Change in heat capacity of different samples, due to stoichiometry, also alters the transition temperature. Hence, as the sintering temperature increases, TN will change and finally attain a fixed value. It is observed from the heat capacity graph that the transition temperature for NiO500, NiO700, and NiO1100 samples are 510, 519, and 525 K, respectively. It is understood that due to excess oxygen in the different ratios in NiO400 and NiO500 samples, change in specific heat anomaly is observed. Further, the observed transition temperature reaches to 525 K as reported for stoichiometric NiO [40]. An irregular behavior in Cp at TN is due to Ni-spin ordering as suggested by Néel [41] wherein due to the thermal agitation spin-lattice of the particle could reverse coherently and randomly.
Figure 10.
The temperature variation of specific capacity of nickel oxide samples sintered at different temperatures. Curve shows shifting in TN due to different oxygen contents of the samples.
Consequently, the net moment of uncompensated surface spins would fluctuate accordingly and in turn, significant downshift the TN in samples due to both the change of magnetic ions as well as their disorder. Probably due to change in excess oxygen, magnetic inhomogeneity in nonstoichiometric samples increases, and Néel temperatures eventually shift.
6. Conclusion
The samples of different oxygen contents of nickel oxide were synthesized by thermal decomposition method. The structure of these samples was characterized by X-ray diffraction spectroscopy, and full-proof refinement was used for indexing. The nonstoichiometry of these samples was recognized by iodometric titration and thermogravimetric analysis. Both these techniques give the excess oxygen content of samples, which was found to be similar. Different phases of nickel oxide were confirmed by the FTIR studies. The shift in FTIR pattern indicates about the nonstoichiometry of samples. The change in stoichiometry of sample is also responsible for the defect creation in the samples, as XPS results indicate that nickel vacancy can be created in samples with varying sintering temperatures. Those samples that were sintered at low temperature have high defect as compared to sample sintered at high temperature. The ZFC and FC curves are nearly identical to each other but the susceptibility changes with stoichiometry. The observed specific heat anomaly in the vicinity of TN is associated with the magnetic ordering, indicating a gradual transformation between two magnetic phases, and the observed TN shifted toward lower temperatures as excess oxygen content increases. The shifting of Néel temperature is presumably due to magnetic inhomogeneity arising from the excess oxygen in samples.
Acknowledgments
The authors would like to thank Dr. A. M. Awasti, Dr. Mukul Gupta, and Dr. V. Ganesan, Centre Director, UGC-DAE-CSR, Indore, India for providing heat capacity measurements and XRD facilities. Financial support from the Science and Engineering Research Board (SERB), the Department of Science and Technology (DST), New Delhi, and the Madhya Pradesh Council of Science and Technology (MPCST), Bhopal (NK) are gratefully acknowledged.
Conflict of interest
The authors declare that there are no conflicts of interest.
\n',keywords:"nonstoichiometry, defect study, nickel oxide, thermo-gravimetrical analysis, iodometric titrations",chapterPDFUrl:"https://cdn.intechopen.com/pdfs/70161.pdf",chapterXML:"https://mts.intechopen.com/source/xml/70161.xml",downloadPdfUrl:"/chapter/pdf-download/70161",previewPdfUrl:"/chapter/pdf-preview/70161",totalDownloads:467,totalViews:0,totalCrossrefCites:0,dateSubmitted:"February 21st 2019",dateReviewed:"August 28th 2019",datePrePublished:"November 22nd 2019",datePublished:"November 4th 2020",dateFinished:null,readingETA:"0",abstract:"This chapter gives a general overview of synthesis and recent development of nickel oxide as a nonstoichiometric compound. We establish the synthesis chemistry of nickel oxide as a nonstoichiometric material, and hence successively introduce definitions and classifications of nonstoichiometric compounds as well as their point defects. The samples of nonstoichiometric nickel oxide are synthesized by thermal decomposition method. The nonstoichiometry of samples was then studied chemically by iodometric titration, and the results are further corroborated by excess oxygen obtained from the thermo-gravimetric analysis (TGA). X-ray diffraction (XRD) and Fourier transformed infrared (FTIR) techniques are used to analyze structural phase of nonstoichiometric nickel oxide. The change in oxidation state of nickel was studied by X-ray photoelectron spectroscopy (XPS) analysis. The shift in antiferromagnetic ordering and transition temperature due to nonstoichiometry is studied by magnetic and specific heat capacity analysis.",reviewType:"peer-reviewed",bibtexUrl:"/chapter/bibtex/70161",risUrl:"/chapter/ris/70161",signatures:"Paras Dubey and Netram Kaurav",book:{id:"7760",title:"Structure Processing Properties Relationships in Stoichiometric and Nonstoichiometric Oxides",subtitle:null,fullTitle:"Structure Processing Properties Relationships in Stoichiometric and Nonstoichiometric Oxides",slug:"structure-processing-properties-relationships-in-stoichiometric-and-nonstoichiometric-oxides",publishedDate:"November 4th 2020",bookSignature:"Speranta Tanasescu",coverURL:"https://cdn.intechopen.com/books/images_new/7760.jpg",licenceType:"CC BY 3.0",editedByType:"Edited by",editors:[{id:"24934",title:"Dr.",name:"Speranta",middleName:null,surname:"Tanasescu",slug:"speranta-tanasescu",fullName:"Speranta Tanasescu"}],productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"}},authors:[{id:"277555",title:"Dr.",name:"Netram",middleName:null,surname:"Kaurav",fullName:"Netram Kaurav",slug:"netram-kaurav",email:"netramkaurav@yahoo.co.uk",position:null,institution:null},{id:"299545",title:"Mr.",name:"Paras",middleName:null,surname:"Dubey",fullName:"Paras Dubey",slug:"paras-dubey",email:"parasdubey.74@gmail.com",position:null,institution:null}],sections:[{id:"sec_1",title:"1. Introduction",level:"1"},{id:"sec_2",title:"2. Classification and point defect formation in nonstoichiometric compounds",level:"1"},{id:"sec_3",title:"3. Nonstoichiometry in nickel oxide",level:"1"},{id:"sec_4",title:"4. Synthesis of nonstoichiometric nickel oxide",level:"1"},{id:"sec_5",title:"5. Characterization of nonstoichiometric nickel oxide",level:"1"},{id:"sec_5_2",title:"5.1 Structure determination of nonstoichiometric nickel oxide",level:"2"},{id:"sec_6_2",title:"5.2 Stoichiometry and defect analysis of nickel oxide",level:"2"},{id:"sec_7_2",title:"5.3 FTIR study of nonstoichiometric nickel oxide",level:"2"},{id:"sec_8_2",title:"5.4 XPS studies of nonstoichiometric nickel oxide",level:"2"},{id:"sec_9_2",title:"5.5 Magnetic properties measurements of nonstoichiometric nickel oxide",level:"2"},{id:"sec_10_2",title:"5.6 Specific heat measurement",level:"2"},{id:"sec_12",title:"6. 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Far-infrared reflection spectra, optical and dielectric constants, and lattice vibrations of some fluoride crystals. Bulletin of the Chemical Society of Japan. 1971;44:3014-3020. DOI: 10.1246/bcsj.44.3014'},{id:"B28",body:'Moore WJ. Seven Solid States. W. A. WA, USA: Benjamin, Inc; 1967'},{id:"B29",body:'Bosman AJ, Daal HJ, Van GF, Knuvers GF. Hall effect between 300° K and 1100° K in NiO. Physics Letters. 1965;19:372-373. DOI: 10.1016/0031-9163(65)90901-7'},{id:"B30",body:'Osburn CM, Vest RW. Defect structure and electrical properties of NiO—I. high temperature. Journal of Physics and Chemistry of Solids. 1971;32:1331-1342. DOI: 10.1016/S0022-3697(71)80191-9'},{id:"B31",body:'Fueki K, Wegner JB. Studies of the oxidation of nickel in the temperature range of 900° to 1400°C. Journal of the Electrochemical Society. 1965;112:384-388. DOI: 10.1149/1.2423553'},{id:"B32",body:'Catlow CRA. Computer simulation studies of transport in solids. Annual Review of Materials Science. 1986;16:517-548. DOI: 10.1146/annurev.ms.16.080186.002505'},{id:"B33",body:'Hafemeister DW, Flygare WH. Outer-Shell overlap integrals as a function of distance for halogen—Halogen, halogen—Alkali, and alkali—Alkali ions in the alkali halide lattices. The Journal of Chemical Physics. 1965;43:795. DOI: 10.1063/1.1696846'},{id:"B34",body:'Kaurav N. High-pressure phase transformation and elastic behavior of XC (X = Si, Ge, Sn and Pt) compounds. Physica Scripta. 2013;88:015604-015609. DOI: 10.1088/0031-8949/88/01/015604'},{id:"B35",body:'Mironova-Ulmane N, Skvortsova V, Kuzmin A. Magnetic ion exchange interactions in NiO-MgO solid solutions. Physics of the Solid State. 2005;47:1516-1522. DOI: 10.1134/1.2014504'},{id:"B36",body:'Shaikh JS, Pawar RC, Devan RS, Ma YR, Salvi PP, Kolekar SS, et al. Synthesis and characterization of Ru doped CuO thin films for supercapacitor based on Bronsted acidic ionic liquid. Electrochimica Acta. 2011;56:2127-2134. DOI: 10.1016/j.electacta.2010.11.046'},{id:"B37",body:'Wagner CD, Riggs WM, Davis LE, Moulder JF, Muilenberg GE. Handbook of X-Ray Photoelectron Spectroscopy. Minnesota: Perkin-Elmer Corporation; 1979. DOI: 10.1002/sia.740030412'},{id:"B38",body:'Devan RS, Lin C-L, Gao S-Y, Cheng C-L, Liou Y, Ma Y-R. Room-temperature wide-range photoluminescence and semiconducting characteristics of two-dimensional pure metallic Zn nanoplates. RSC Advances. 2012;2:2123-2127. DOI: 10.1039/C2RA00972B'},{id:"B39",body:'Lenglet M, Hochu F, Durr J, Tuilier MH. Investigation of the chemical bonding in 3d8 nickel(II) charge transfer insulators (NiO, oxidic spinels) from ligand-field spectroscopy, Ni 2p XPS and X-ray absorption spectroscopy. Solid State Communications. 1997;104:793-798. DOI: 10.1016/S0038-1098(97)00273-1'},{id:"B40",body:'Hutchings MT, Samuelsen EJ. Measurement of spin-wave dispersion in NiO by inelastic neutron scattering and its relation to magnetic properties. Physical Review B. 1972;6:3447-3456. DOI: 10.1103/PhysRevB.6.3447'},{id:"B41",body:'N’eel L. Superposition de l’antiferromagnétisme et du superparamagnétisme dans un grain très fin. Comptes Rendus de l’Académie des Sciences. 1961;252:4075-4079'}],footnotes:[],contributors:[{corresp:null,contributorFullName:"Paras Dubey",address:null,affiliation:'
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The Open Access Publishing Fee (OAPF) is payable only after your full chapter, monograph or Compacts monograph is accepted for publication.
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1,400 GBP Chapter - Edited Volume
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4,000 GBP Compacts Monograph - Short Form
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XML Typesetting and pagination - web (PDF, HTML) and print files preparation
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Discoverability - electronic citation and linking via DOI
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Permanent and unrestricted online access to your work
What isn't covered by the Open Access Publishing Fee?
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If your manuscript:
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Exceeds 20 pages (for chapters in Edited Volumes), an additional fee of 40 GBP per page will be required
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If a manuscript requires Heavy Editing or Language Polishing, this will incur additional fees.
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Your Author Service Manager will inform you of any items not covered by the OAPF and provide exact information regarding those additional costs before proceeding.
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Open Access Funding
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To explore funding opportunities and learn more about how you can finance your IntechOpen publication, go to our Open Access Funding page. IntechOpen offers expert assistance to all of its Authors. We can support you in approaching funding bodies and institutions in relation to publishing fees by providing information about compliance with the Open Access policies of your funder or institution. We can also assist with communicating the benefits of Open Access in order to support and strengthen your funding request and provide personal guidance through your application process. You can contact us at oapf@intechopen.com for further details or assistance.
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For Authors who are still unable to obtain funding from their institutions or research funding bodies for individual projects, IntechOpen does offer the possibility of applying for a Waiver to offset some or all processing feed. Details regarding our Waiver Policy can be found here.
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Indexing and listing across major repositories, see details ...
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