Correlation factors of virgin olive oil tocopherol content and a microclimate parameters (mean temperature and rainfall; Figures 1 and 2) in the period of olives’ intensive growth and ripening.
\r\n\t"
",isbn:null,printIsbn:null,pdfIsbn:null,doi:null,price:0,priceEur:null,priceUsd:null,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"cc796459268324e827219d1d904e4265",bookSignature:"Prof. Moulay Tahar Lamchich",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/7196.jpg",keywords:"Induction motor, smart motor, electrical vehicles, energy generation, drives, electromechanical, hybrid transportation, smart control, high efficiency motor, variable speed drives, power electronic, energy efficiency.",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:0,numberOfDimensionsCitations:0,numberOfTotalCitations:0,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"July 4th 2018",dateEndSecondStepPublish:"July 25th 2018",dateEndThirdStepPublish:"September 23rd 2018",dateEndFourthStepPublish:"December 12th 2018",dateEndFifthStepPublish:"February 10th 2019",remainingDaysToSecondStep:"3 years",secondStepPassed:!0,currentStepOfPublishingProcess:5,editedByType:null,kuFlag:!1,biosketch:null,coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"21932",title:"Prof.",name:"Moulay Tahar",middleName:null,surname:"Lamchich",slug:"moulay-tahar-lamchich",fullName:"Moulay Tahar Lamchich",profilePictureURL:"https://mts.intechopen.com/storage/users/21932/images/system/21932.png",biography:"Moulay Tahar Lamchich is a Professor at the Faculty of Sciences Semlalia at Marrakech (Morocco). 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Venkateswarlu",coverURL:"https://cdn.intechopen.com/books/images_new/371.jpg",editedByType:"Edited by",editors:[{id:"58592",title:"Dr.",name:"Arun",surname:"Shanker",slug:"arun-shanker",fullName:"Arun Shanker"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}},{type:"book",id:"878",title:"Phytochemicals",subtitle:"A Global Perspective of Their Role in Nutrition and Health",isOpenForSubmission:!1,hash:"ec77671f63975ef2d16192897deb6835",slug:"phytochemicals-a-global-perspective-of-their-role-in-nutrition-and-health",bookSignature:"Venketeshwer Rao",coverURL:"https://cdn.intechopen.com/books/images_new/878.jpg",editedByType:"Edited by",editors:[{id:"82663",title:"Dr.",name:"Venketeshwer",surname:"Rao",slug:"venketeshwer-rao",fullName:"Venketeshwer Rao"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}}]},chapter:{item:{type:"chapter",id:"52019",title:"Tocopherols: Chemical Structure, Bioactivity, and Variability in Croatian Virgin Olive Oils",doi:"10.5772/64658",slug:"tocopherols-chemical-structure-bioactivity-and-variability-in-croatian-virgin-olive-oils",body:'\nTocopherols are the natural antioxidants synthesized at various levels and in different combinations by all plant tissues. They are amphipathic molecules with the polar chromanol ring and hydrophobic saturated side chain. The general structure of tocopherols is shown in Figure 1. The four homologues, α-, β-, γ-, and δ-tocopherol, differ in the number and position of methyl groups in the aromatic ring [1].
\nTocopherol structures. The table indicates the number and position of methyl groups on the aromatic ring.
Tocopherols act as antioxidants by scavenging peroxy radicals of polyunsaturated fatty acids or by reacting with singlet oxygen and other reactive oxygen species (ROS). ROS quenching occurs by charge transfer mechanism. Termination of polyunsaturated fatty acids oxidation chain reactions is achieved by donation of a hydrogen atom from the hydroxyl group on the chromanol ring resulting in a “tocopherol radical“ formation. The tocopherol radicals are resonance stabilized within the chromanol ring and do not propagate the chain reactions or are rapidly recycled back to the corresponding tocopherol, allowing each tocopherol to participate in many peroxidation chain-breaking events. One tocopherol molecule can protect about 103–108 polyunsaturated fatty acids at low peroxide values [1, 2]. Tocopherol homologues possess different antioxidant activity as a result of their structural differences. The antioxidant activity of tocopherol homologues decreases in the order δ > β > γ > α in vitro, while in vivo, that is vitamin E activity, decreased in order α > β > γ > δ [3]. Although there is no significant difference in the absorption of tocopherols from the gastrointestinal tract, the highest vitamin E activity of α-tocopherol can be explained by its preferential retention and incorporation into lipoproteins by the hepatic α-tocopherol transfer protein, occurring in higher plasma and tissue level [1, 4].
\nThe main role of tocopherols is the protection of lipids from peroxidation. Therefore, they are abundantly found in plant-based food, but vegetable oils are considered to be the best source of tocopherol in nutrition [3]. Their content and composition mostly depend on the type of oil [2, 5]. Tocopherol content of virgin olive oils (VOOs) varies from 97 to 785 mg/kg. Despite differences in the concentration of total tocopherols that can be attributed to agronomical, geographical, and technological factors, α-tocopherol is the dominant homologue in virgin olive oils making more than 90% of total tocopherols. γ-Tocopherol is in virgin olive oils present in low amounts (<10%), and β-tocopherol is present only in trace amounts [6–8].
\nTocopherols possess high antioxidative activity; this makes them important components in cardiovascular disease and cancer prevention [9, 10, 11]. Furthermore, tocopherols appear to act synergistically with other antioxidants [12]. This indicates that intake of tocopherol in the form of food like virgin olive oil, which is rich in other natural antioxidants such as biophenols and carotenes, might improve their efficiency.
\nConsidering the importance of tocopherols in daily nutrition and disease prevention, it is important to know and examine the influence of certain factors on their content and composition.
\nCultivars “Oblica” and “Leccino,” in three consecutive years (2010, 2011, and 2012), grown at two different locations in Dalmatia (Kaštela and Šestanovac), Croatia, were studied. The fruit samples were hand-harvested from the olive trees, at biweekly intervals, from the end of September till mid-November. An aliquot of 100 fruits was taken from each fruit sample to determine ripening index which is based on evaluation of the olive skin and pulp color [13]. The olive fruits were processed by centrifugal extraction using an Abencor laboratory oil mill (mc2, Ingenierias y Sistemas, Seville, Spain) within 24 h after the harvesting. Tocopherol content and composition were determined in all produced virgin olive oils using standard method (ISO 9936:2006) with normal-phase HPLC analysis. Total tocopherols were calculated as a sum of the concentration of the individual tocopherols. Results are given in milligrams of tocopherol per kg of oil.
\nIn order to study the effect of cultivar, year, growing area location, and fruit ripening index on the tocopherol content in olive oil samples, factorial ANOVA was performed (Fisher’s F-test), followed by Tukey”s honest significant difference (HSD) test. A significance level of p ≤ 0.05 was applied. The correlation coefficients (r) determined by Pearson correlation matrix were used to define the influence of climatic conditions during the year on the VOOs tocopherol content. The obtained data were analyzed using Statistica software version 11.0 (StatSoft, Inc., USA, 2012).
\nCroatia is a fringe growing area of olive trees cultivation. Selected growing area locations are from different olive growing subregions. Kaštela is located at 28 m above sea level and influenced by Mediterranean climate, while Šestanovac is located at 358 m influenced by continental climate in winter and the Mediterranean climate in summer period.
\nThe monthly mean values of temperature and rainfalls registered for studied years at selected locations were obtained from weather stations (Meteorological and Hydrological Service of Croatia) (Figures 2 and 3).
\nMicroclimate temperature parameters (°C) measured for two olive growing areas in the year 2010, 2011, and 2012.
Monthly rainfall (mm) for two olive growing areas in the year 2010, 2011, and 2012.
Year 2010 was recorded as the highest rainfall year and with lowest average daily air temperature (Figures 1 and 2). During olives intense growth and ripening (July-November), higher mean daily temperatures were recorded in 2012, compared to overall 3 years of research, while 2011 is the year with the lowest rainfall. Kaštela could be considered as the more drought affected and warmer growing area.
\nThe quality of virgin olive oil is influenced by several factors, but the olive cultivar stands out as the most important one [14]. The content of tocopherols in the virgin olive oils varies from 97 to 785 mg/kg [6–8], from 163 to 510 mg/kg in the Spanish oils [8], 98–370 mg/kg in the Greek oils [14], 97–403 mg/kg in oils from Turkey [6], 120–478 mg/kg in oils from Tunisia [15], and 138–298 mg/kg in the Portuguese oils [16].
\nTocopherol content of studied cultivars is presented in Figures 4–6. Cultivar shows a significant impact on the content of the α-, γ-, and total tocopherols. “Oblica” VOOs have a modest total tocopherol content, ranging from 186 to 442 mg/kg. Significantly higher total tocopherol content had varietal oils from “Leccino” with average value of 510 mg/kg (337–784 mg/kg). Higher total tocopherol content in “Leccino” VOOs also was recorded for several different cultivars in the study reported by Tura et al. [17] and Koprivnjak et al. [18]. In “Oblica” and “Leccino” VOO samples δ-tocopherol was not detected.
\nTotal tocopherol content (mg/kg) of “Oblica” and “Leccino” virgin olive oils during ripening at two different growing locations in three successive crop years. £Cultivar has a significant effect (p < 0.05); §year has a significant effect (p < 0.05); †growing location has a significant effect (p < 0.05); harvest period has a significant effect (p < 0.05). The means marked with different letters (within the same cultivation year), labeled with different letters, are significantly different (Tukey’s test, p < 0.05).
α-Tocopherol content (mg/kg) of “Oblica” and “Leccino” virgin olive oils during ripening at two different growing locations in three successive crop years. £Cultivar has a significant effect (p < 0.05); §year has a significant effect (p < 0.05); †growing location has a significant effect (p < 0.05); harvest period has a significant effect (p < 0.05). The means marked with different letters (within the same cultivation year), labeled with different letters, are significantly different (Tukey’s test, p < 0.05).
γ-Tocopherol content (mg/kg) of “Oblica” and “Leccino” virgin olive oils during ripening at two different growing locations in three successive crop years. £Cultivar has a significant effect (p < 0.05); §year has a significant effect (p < 0.05); †growing location has a significant effect (p < 0.05); harvest period has a significant effect (p < 0.05). The means marked with different letters (within the same cultivation year), labeled with different letters, are significantly different (Tukey”s test, p < 0.05).
α-Tocopherol comprises more than 97% in all analyzed VOO samples (Figure 5). The γ-tocopherol content in “Leccino” oils ranged from 4 to 32 mg/kg (average 17 mg/kg), while the content in “Oblica” oils was significantly lower (Figure 6). Average concentration in “Oblica” oils was 7 mg/kg, and values ranged from traces to 14 mg/kg. The γ-tocopherol concentrations obtained in this study for both varieties are within the concentrations reported in different varietal virgin olive oils studies [16, 17, 19].
Production geographic area, marked by soil factors, altitude and latitude, and climatic conditions during the year, has a significant impact on the properties and chemical composition of virgin olive oils [7, 17, 20–23]. Studies of environmental factors impact on VOOs chemical composition have quite different results, due to the fact that all these factors together interact and as result varieties behave differently in different agroclimatic conditions.
\nMean temperature (°C) | \n|||||
---|---|---|---|---|---|
Parameter | \n|||||
\n | July | \nAugust | \nSeptember | \nOctober | \nNovember | \n
α-Tocopherol conc. | \n0,287* | \n0,252* | \n−0.021 | \n0,391* | \n0,302 | \n
γ-Tocopherol conc. | \n0,059 | \n0,044 | \n0,055 | \n0,114 | \n−0,068 | \n
Total tocopherol conc. | \n0,295* | \n0,244* | \n−0,037 | \n0,376* | \n0,293 | \n
Rainfall (mm) | \n|||||
α-Tocopherol conc. | \n−0,190 | \n−0,079 | \n0,015 | \n−0,217 | \n0,009 | \n
γ-Tocopherol conc. | \n−0,067 | \n0,252* | \n0,048 | \n−0,010 | \n−0,329 | \n
Total tocopherol conc. | \n−0,206* | \n−0,053 | \n0,030 | \n−0,206 | \n−0,002 | \n
Year and geographical production area significantly influenced the content of tocopherol in “Oblica” and “Leccino” VOOs (Figures 4 – 6). The correlation coefficients of rainfall and mean daily temperature during intense growth and ripening of olive fruit (July-November) with α-, γ-, and total tocopherol content were calculated and presented in Table 1. It is evident that the mean daily air temperatures have a significant impact on the α- and total tocopherol content. The highest average α- and total tocopherol content in “Oblica” and “Leccino” VOOs was recorded in year 2012, while in oils from year 2011, concentrations were the lowest of three studied years (α-tocopherol: “Oblica”: 302 mg/kg in year 2010, 264 mg/kg in year 2011, 319 mg/kg in year 2012; “Leccino”: 467 mg/kg in year 2010, 464 mg/kg in year 2011, 547 mg/kg in year 2012.) (Figure 5). A Spanish group of scientists [24] recorded lower tocopherol content in the year with the lowest average air temperature. For the lower α- and total tocopherol content in year 2011, a possible explanation lies in rainfall, due to the fact that tocopherols negatively correlate with rainfall in July (Figure 2 and Table 1). Results are in line with a Beltrán et al. [8] publication according to which the year has a very significant impact on the α- and total tocopherol content in “Picual”, “Frantoio”, and “Hojiblanca” VOOs, and the highest content was recorded in the year with the lowest rainfall. In the same study, the effect of the year on the γ-tocopherol was not recorded, contrary to our results on the “Oblica” and “Leccino” VOOs (Table 1). The γ-tocopherol positively correlates with the rainfall in August. In the year 2010, more rainfall and, as mentioned previously, the highest γ-tocopherol content in oils of the two investigated cultivars were recorded (Table 1 and Figure 6).
\nHigher α-, γ-, and total tocopherol content had “Oblica” and “Leccino” VOOs obtained from fruits harvested at the growing area of lower altitude (Figures 4 – 6). The correlation coefficient results are in accordance with the observation (Table 1) that oils from growing area of higher average temperatures synthesize more tocopherols. Similar results were published by Arslan et al. [6] and Aguilera et al. [22]. On the other hand, Tura et al. [17] report that the growing area had no effect on α-, β- and total tocopherol content and that only the γ-tocopherol content was influenced, with the highest content in oils of the highest altitude area.
\nThe fruit ripening is one of the most important factors that lead to changes in the chemical composition of virgin olive oil [25]. The knowledge of varietal oil characteristics, as well as changes that take place through fruit maturation, contributes to the higher quality of VOOs. The genetic composition directly affects the ripening; thus, in each cultivar, different changes in composition of the olive fruit and its virgin olive oils are confirmed [25].
\nA wide range of α-, γ-, and total tocopherol content was perceived during ripening of “Oblica” and “Leccino” VOOs (Figures 4 – 6). Analysis of variance showed a difference in tocopherol content of VOOs derived from olives harvested at different ripening stages.
\nThe total tocopherol content in VOOs decrease with increase in the fruit ripening index from which the oil is produced (Figure 4). The average total tocopherol content reduction of about 30% in VOOs from unripe to ripe olives has the same trend as the α-tocopherol; this is expected since the α-tocopherol abudance in VOOs is around 95%. The results are in line with research reported by Matos et al. [16], Bengana et al. [25] and Beltrán et al. [8]. Depending on the olive fruit pigmentation, variations in the total tocopherol content in the “Chetoui” (138–496 mg/kg) and “Chemlali” (224–350 mg/kg) were also noted [15].
\nIn general, the α-tocopherol content decreases during ripening, although a decrease rate of the studied cultivars was not quite equal (Figure 5). Lower α-tocopherol content for 25% (Kaštela) and 35% (Šestanovac) in “Oblica” VOOs obtained from ripe olive fruits was recorded in comparison with initial content in oils from the unripe olive fruits. The loss of α-tocopherol is more pronounced in the “Leccino” VOOs of both locations. Decrease of the α-tocopherol through the ripening period has also been reported in other studies [8, 26–28].
\nThe γ-tocopherol content in “Oblica” VOOs decreases as the fruit ripening index increases, although decrease rate was not the same at both studied locations (Figure 6). A significant decrease of 70% as average value was recorded in the oils from the Kaštela, while in oils from Šestanovac, an increase in the γ-tocopherol content in oils from ripe olive fruits was observed. This is consistent with Beltrán et al. [8] who have also reported a similar trend for “Frantoio,” “Hojiblanca,” and “Picual” VOOs. γ-Tocopherol in “Leccino” VOOs was not clearly associated with the increase in olive fruit ripening index (Figure 6), what was also reported for virgin olive oils of several different cultivars [15, 16, 19].
\nVirgin olive oil after processing is a metastable mixture that can be consumed without refining [29]. From the commercial point of view, apart from major manufacturers and industrial producers who prefer filtered oils, there is an increasing interest of consumers for unfiltered oils which they consider as minimally processed [30]. Suspended substances (cellulose, hemicelluloses, pectin, proteins) can affect the quality by increasing triacylglycerols hydrolysis causing a free fatty acids increase. Therefore, filtration is the process of clarification aimed at a faster process during which the qualitative and quantitative changes in the composition of virgin olive oils may take place. In fact, there is a controversy and there are some confusing comments in relation to “cloudy“ and filtered oils.
\nIn the study of six different Spanish and Italian varietal VOOs by Fregapane et al. [31], filtration was not found to cause significant differences in the α-tocopherol content. A new filtration method based on the flow of an inert gas developed and patented by the University of Bologna and Sapio [32] had also no effect on the lipophilic phenols level [33].
\nThe overall quality of virgin olive oil decreases over the time as a consequence of oxidative and hydrolytic degradations which also cause the partial loss of other minor constituents having health-promoting effects. Consequently, VOOs is generally consumed within one year from its production [34–36]. As it was mentioned formerly, the main role of tocopherols is the protection of lipids from peroxidation, and according to Aparicio and Luna [37], their contribution accounts for around 11%. Thus, monitoring of tocopherol levels during its shelf life, it is needed.
\nThe degradation rate of the α-tocopherol content during storage under the store shelves conditions was reported by Psomiadou and Tsimidou [38]. Keepability test carried out on five VOOs in conventional storage at room temperature resulted in insignificant α-tocopherol losses in samples kept sealed [39]. On the other hand, in the same study, considerable α-tocopherol losses were observed in samples opened periodically within the period of two years storage as a result of renewal of oxygen supply. Rastrelli et al. [40] investigated storage conditions regarding availability of oxygen in the oil headspace and lighting. These authors reported the loss of tocopherols in VOO samples, stored 12 months in completely filled dark glass bottle, in range from 20 to 25%. Similarly rate of α-tocopherol losses was also reported in storage condition study [7], which is contrariwise almost total loss of α-tocopherol in “Arbequina” oils in same storage conditions (in darkness and at ambient temperature for 12 months) [41]. Under medium temperature at accelerated storage conditions (50°C, 36 weeks), the α-tocopherol loss was much more rapidly in oils stored in open bottles than in close bottles [42]. The research of VOOs storage conditions (room temperature, +4 and −20°C) influences on tocopherol content evidenced α-tocopherol content decreasing trend with storage time [7]. In same study, after 12 months storage, the highest loss of α-tocopherol was recorded in oils stored at room temperature, among which the oils obtained from unripe olives showed the greatest α-tocopherol stability. Storage at lower temperatures did not always delayed α-tocopherol consumption compared to room temperature.
\nAs it can be seen, different effect of storage conditions on tocopherol content and α-tocopherol degradation rate is shown through literature affecting the amount of tocopherol in oils within the period in which positive chemical and organoleptic properties remain preserved and VOOs are desirable to consume.
\nResearch work on the tocopherol content and composition variability in virgin olive oils of Croatian cultivar “Oblica” and Italian cultivar “Leccino” showed that the cultivar has a major influence on the tocopherol content and composition. Location also has an impact, which can be associated with a microclimate characteristic of the growing area.
\nThe cultivation year, climate characteristics of temperature and rainfall, has significant impact on the variation of the tocopherol content. The amount of rainfall in July correlated negatively with the total tocopherol content, and the highest content was recorded in the year with the lowest rainfall. Both cultivars have gained an average higher α-, γ-, and total tocopherol content at a warmer and of low altitude location. The fruit ripening stage has a significant impact on the composition of the tocopherols and primarily α-tocopherol. The clear decrease in α-tocopherol content as ripening progresses was observed.
\nThe authors acknowledge the Ministry of Science, Education and Sports of the Republic of Croatia (Project No: 091-091 0468 0364) for financial support.
\nThe significance of nanostructuring techniques has increased with the progress of scaling down devices to nanometer order in accordance with Moore’s law [1]. The realization of three-dimensional (3D)-architected nanostructures, that is, the transformation from novel two-dimensional (2D) film-based planar devices to 3D complex and multifunctional nanodevices, is of crucial importance to future electronic applications [2, 3], the so-called More Moore. So far, various nanofabrication techniques have been proposed and developed with different levels of success. In many cases, materials grown on substrates are affected by substrate structural characteristics such as shape, roughness, and dimensionality. Three-dimensional patterned substrates prepared by a conventional lithographic method can be used to form 3D nanostructures. Although considerable attention has been devoted to controlling the size, shape, and positioning in research on 3D patterning, little attention has been focused on the atomic ordering of arbitrarily oriented surfaces on 3D patterned substrates. The realization of perfect surfaces on 3D structures is required to produce high-quality samples. Since material growth starts on a surface, the surface condition clearly determines the structural and physical properties of the grown material.
Although techniques for studying 2D surfaces, namely, surface science, have been intensively developed and established, little attention has been devoted to controlling the atomic ordering and structures of side-surfaces on 3D architectures. Fabrication techniques for 3D nanoscale structures that are promising for 3D integrated circuits have been individually developed from surface science.
The subject of study should be changed from 2D planar surfaces to 3D assembly surfaces to enable atomically ordered nanofabrication on vertical side-surfaces and/or tilted facet-surfaces in 3D space (Figure 1). For this purpose, a simple and accurate structure evaluation technique is required. Currently, scanning electron microscopy (SEM) is widely used for the observation of 3D nanostructures. However, SEM cannot be used to evaluate structures involving atomic ordering. On the other hand, transmission electron microscopy (TEM) is a powerful technique for examining the atomic structure of 3D nanomaterials, but it is destructive and not convenient. An alternative technique is a diffraction method. Reflection high-energy electron diffraction (RHEED) enables the examination of surface properties such as atomic ordering, surface roughness (flatness), and surface homogeneity [4]. Low-energy electron diffraction (LEED) is also a conventional and nondestructive surface observation technique [5]. To apply these techniques to 3D structured samples with various oriented surfaces, instead of 2D planar samples, an appropriate alignment of the incident electron beam considering the configuration in 3D space is indispensable [6, 7, 8, 9].
Concept of our approach toward realizing atomically ordered 3D structures.
In this chapter, we first show how to obtain and evaluate RHEED and LEED patterns from 3D structured samples by explaining the principle of diffraction. Then, we demonstrate creating and evaluating atomically ordered side- and facet-surface structures of 3D silicon nano-architectures. Finally, we discuss novel structures that have been constructed on 3D patterned Si to form 3D interconnected structures and their physical properties.
Electron diffraction is one of the most powerful tools for investigating crystalline structures, particularly nanomaterials and material surfaces owing to their larger atomic scattering cross sections
Schematics of (a)–(c) 1D, (d) and (e) 2D, and (f) and (g) 3D crystals: real space structures (a), (d), and (f) and corresponding reciprocal space structures (b), (c), (e), and (g). 1D, 2D, and 3D crystals show reciprocal lattice planes, reciprocal lattice rods, and reciprocal lattice points, respectively.
For instance, an ideal one-dimensional (1D) material with lattice constant
A 2D material with lattice constants
From diffraction patterns (e.g., diffraction rings or spots) projected on a detection screen, the original reciprocal structure pattern (e.g., reciprocal lattice planes, rods, or points) in a 3D RSM can be regenerated by changing the incident angle of the electron beam to the crystalline material (i.e., the direction of
Schematic of relationship between diffraction spots and reciprocal lattice points intersecting with a partial Ewald sphere in 3D RSM, for 3D crystal.
(a) and (b) RHEED patterns of α-FeSi2110001∥ Si001110 at azimuth angles ϕ = 0° and 45°, respectively. Ep is 15.0 keV (k0= 62.7 Å−1). (c) Top view and (d) and (e) side views of the 3D RSM regenerated from a series of RHEED patterns. In (a) and (b), diffraction spots indicated by orange and red arrows are assigned to reciprocal lattice points of 3D α-FeSi2 nanocrystals and reciprocal lattice rods of a 2D Si001 substrate surface, respectively. Reciprocal lattice rods [e.g., 00 and 01] lie on Laue zones (e.g., L0 and L1). DB denotes the direct beam position. a0∗=2π/a0≈2π/3.84Å−1 is the reciprocal lattice unit length of Si0011×1.
In Figure 4(a) and (b), there are also diffraction spots on arcs indicated by red arrows. These spots are often observed under a glancing condition of an electron beam nearly parallel to a substrate surface in RHEED with a primary energy Ep of typically 10–15 keV. The conversion of the spots generates reciprocal lattice rods perpendicular to the substrate surface in a 3D RSM, as indicated by red arrows in Figure 4(c)–(e). The existence of spots on arcs or reciprocal lattice rods implies that the surface perpendicular to the rods is atomically well-ordered; in this case, it implies the formation of a well-defined clean Si
The width of a reciprocal lattice rod is finite (full width at half maximum
Schematics of 2D diffraction spots and reciprocal lattice rods of (a) substrate surface and (b) side-surface of 3D fabricated material. In both cases, diffraction spots are elongated in the surface normal direction.
One of the advantages of RHEED is its ability to observe atomically ordered surfaces in any direction, as described later in Sections 3.2 and 4. RHEED has been used to investigate crystalline structures on planar substrate surfaces. Recently, for 3D fabricated materials, the authors have demonstrated that not only substrate surfaces but also surfaces inclined from or perpendicular to a substrate plane exhibit atomically ordered structures where surface spots elongated along directions inclined from or perpendicular to the substrate normal direction appear in RHEED patterns (Figure 5(b)) [6, 7, 9]. We emphasize that a simple surface property of 3D fabricated materials, that is, a surface direction, can be confirmed by the elongation of surface spots.
Low-energy electron diffraction (LEED) with a typical Ep of 50–100 eV focuses the interference caused by the backward scattering of an electron incident to an atom, while RHEED focuses the interference caused by forward scattering. Both LEED and RHEED are sensitive to surface structures. A LEED pattern at the normal incidence corresponds to a top view of reciprocal lattice rods intersecting with an Ewald sphere from the surface normal direction. The diffraction spots move to the
The authors demonstrated the creation of atomically ordered side- and facet-surfaces owing to the arbitrary selection of planes (Figure 6). Atomically reconstructed Si
(a)–(c) Schematic relationship among flat surface, vertical side-surfaces, and tilted facet-surfaces.
The 3D architected Si samples with arbitrary faces discussed here were produced on commercial mirror-polished Si substrates by the following dry and wet etching procedures. All processes were performed at room temperature (RT). First, a line mask pattern was drawn using a photoresist. To produce the vertical side-surfaces (Figure 7(a)–(c)), Si was etched in an inductive coupled plasma (ICP)-reactive ion etching system (RIE-400iPB, Samco). The process parameters were an ICP source power of 300 W, a bias power of 10 W, and a working pressure of 4 Pa. Mixture gases of 10 sccm SF6, 5 sccm O2, and 200 sccm Ar were used in the etching cycle, and 40 sccm C4F8, 5 sccm O2, and 200 sccm Ar were used in the passivation process [6, 7, 8, 9]. Depending on dry RIE conditions, various curved structures from trapezoid to triangle shapes were obtained. When we produced tilted facet-surfaces (Figure 7(d) and (e)), the optimized conditions for a triangle-like shape were a flow rate of 51 sccm, a pressure of 4.0 Pa, and a bias power of 60 W using an RIE system (RIE-10 NR, Samco) with SF6 gas [9].
(a) Photograph of a 3D patterned Si110 substrate consisting of 111 vertical side-surfaces. (b) Top and (c) cross-sectional SEM images of a patterned area. (d) Cross-sectional and (e) top SEM images of a sample with tilted 111 facet-surfaces.
After dry etching, wet etching was performed to reduce the side- and facet-surface roughnesses. The base solution used in the wet process removes the damage and contaminants [19, 20, 21], and flash annealing promotes reconstruction through the sublimation of the contaminants [22]. Unoptimized conditions never led to reconstructed patterns on side- or facet-surfaces. In this process, the etching recipe was optimized by considering the plane-dependent etching properties [23]. A
RHEED patterns were obtained at RT using an electron beam with an Ep of 15 keV and a diameter of ∼0.5 mm. Au advantage of the RHEED technique is the accessibility of various 3D surfaces; that is, the diffraction pattern consists of all diffractions from the substantial crystal surfaces in 3D space. Actually, the selection of the incident e-beam direction enables the identification of 3D surface structures. In this study, the direction of the incident electrons was defined by the glancing angle
Schematic of the diffraction from the top- and side-surfaces of a 3D patterned Si110 substrate. The control of the incident electron beam direction defined by θ and ϕ enables the observable faces in the 3D space to be selected.
Figure 9(b)–(d) show typical filtered RHEED patterns obtained from 3D Si with a vertical
(a) Dependence of observable conditions (orange) in the RHEED pattern on the polarity of θ and ϕ. (b)–(d) RHEED patterns from 3D Si with 111 vertical side-surfaces observed at (b) θ = 0.0° and ϕ = +1.9°, (c) θ = +0.3° and ϕ = −1.6°, and (d) θ = +0.3° and ϕ = +1.1°. Insets schematically show the relationship between the incident electron beam and the observable surfaces in 3D space.
Let us analyze the curious RHEED patterns in more detail. In Figure 9(c) (
One can see the characteristic
Figure 10 shows the LEED patterns observed from the figured
LEED patterns for 3D Si sample with a wider 1¯11 side-surface at different incident angles of the electron beam with Ep = 80 eV: (a) normal incidence to the Si1¯11 side-surface and (b) ∼37° tilted from the normal direction. The relationship between the incident beam and the sample and the simulated LEED patterns are shown in the upper and lower right, respectively.
The LEED patterns are in good agreement with those simulated by considering the crystal orientation and electron beam (i.e., the cross sections of the reciprocal lattice rods and an Ewald sphere [22]) shown in the lower-right panels of Figure 10. It is possible to identify diffraction spots on Laue zones of both
Figure 11(a) shows a typical filtered RHEED pattern obtained from 3D Si with
(a) RHEED pattern from the 3D Si sample with vertical 100 side-surfaces at θ = +0.4° and ϕ = −1.2°. The inset shows the relationship between the incident electron beam and the 3D surfaces. (b) Schematics of the 2D reciprocal lattices on 1002×1 reconstruction (left) and simulated RHEED pattern from the 100 surfaces at θ = +0.4° and ϕ = −1.2°.
We can see that the diffraction spots on the left side are slightly elongated in the horizontal direction, which is a characteristic of a RHEED pattern from a side-surface [6]. The diffractions from the top-/bottom-surfaces disappeared and those from the left-side surface remained when we changed
The left part of Figure 11(b) shows the reciprocal lattice of the Si
Finally, the RHEED pattern from the vertical
(a) RHEED pattern from the 110 vertical sample observed at θ = +0.4° and ϕ = +1.1° with eye guides of Laue zone. Schematics of 2D reciprocal lattices on (b) Si1002×1 and (c) Si01¯116×2, corresponding to the top/bottom and right-side surfaces, respectively, as shown in (d).
The weak spots in the arcs from the DB in the upper right, some of which are indicated by blue arcs, can be assigned to the Laue zone in the
Figure 13(a) shows a typical filtered RHEED pattern obtained from the
(a) RHEED pattern for the 111 facet sample at θ = +0.7° and ϕ = +2.7°. The pattern consists of a 111¯7×7 pattern tilted ∼36° in the counterclockwise direction (yellow circles) and a faint 16×2 pattern (cyan circles). (b) Simulated RHEED pattern (left) reflecting geometric relationship (bottom right). The upper right figure represents the corresponding 2D reciprocal lattice normal to the facet direction.
Figure 13(b) shows a simulated RHEED pattern from the
The creation and observation methods for well-defined surfaces enable the epitaxial growth of an arbitrary geometry, a key technique for nanoconstruction in 3D space [26, 27, 28, 29, 30, 31]. Therefore, our established methodology contributes to the realization of well-ordered 3D nanofabrication, where the material stacking direction can be perfectly switched between the out-of-plane and in-plane directions. Novel 3D nanostructures are also expected to help unveil the underlying 3D surface science phenomena. Finally, two demonstrations utilizing a 3D architected Si platform are shown.
Atomically well-defined side-surfaces on a substrate can make an enormous contribution to nanofabrication [26, 27, 28, 29, 30, 31]. To demonstrate the applicability of material growth on such side-surfaces, we produced Si
Figure 14(a) and (b) show typical RHEED patterns obtained from the left-side and right-side surfaces, respectively. We can confirm
RHEED patterns obtained from (a) Si1¯11-Ag left-side surface and (b) Si11¯1¯-Fe right-side surface annealed at 773 K in UHV. Spots in the L0 Laue zone indicated by orange arrows correspond to the 3×3 reciprocal lattice rods in (a), and spots indicated by orange arrows correspond to the 2 × 2 superstructure in (b). Cross-sectional TEM images of (c) Ag-deposited and (d) Fe-deposited side-surfaces at RT.
Figure 14(c) and (d) show cross-sectional TEM images of the 0.4-nm-thick Fe layer deposited on the
Our results clearly show that a coherently grown (ultra) thin film was realized on the vertical side-surface with the growth alternating between the out-of-plane and in-plane directions. The siliciding reaction can be controlled on the side-surfaces. Therefore, highly developed thin-film formation techniques are applicable for the vertical side-surface of 3D patterned substrates, and the material stacking direction can be perfectly switched between the out-of-plane and in-plane directions.
Three-dimensional integrated circuits, which contain multiple layers of active devices, have the potential to dramatically enhance chip performance, functionality, and device packing density. Recent 3D structured field-effect transistors (FETs) have surfaces with different orientations; for instance, a fin-type tri-gate structure has one top-surface and two side-surfaces [35, 36].
The electric connection between metal wires on these surfaces—that is, the wiring interconnects at sharp edges of top- and side-surfaces—is one of the issues in the development of 3D devices. Although the conductivity in metal wires on isolated 2D planar or side-surfaces has been well discussed, there are no reports on the metal conductivity of interconnections between 3D surfaces with different orientations, probably owing to the difficulty in measuring the intrinsic conductivity in 3D angular interconnects, which is mainly caused by diffuse scattering on rough surfaces [37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48]. One of the most outstanding factors contributing to the conductivity in the 3D angular interconnects is the facet-edge, which is a boundary of two surfaces with different crystalline orientations. To extract an intrinsic conductive property for metal wires interconnected at facet-edges, atomically flat surfaces in 3D structured substrates are required for the evaluation of the 3D interconnect resistivity by eliminating extra factors, such as roughness. To elucidate the impact of the 3D geometric effect on the conductive property, angularly interconnected Au wires with two configurations, crossing over and parallel to the facet-edges, were produced on atomically flat facet
Figure 15(a) shows a typical cross-sectional SEM image of a
(a) Typical SEM image for a facet sample on which a 10-nm-thick Au layer was deposited. (b) Current vs. voltage curves of Au wires with the channel area (W×L) of 2×100 and 5×100 μm2 at 100 K in the parallel (red) and perpendicular (blue) configurations (insets). The upper left inset shows a schematic of the Au film on the Si111 facet sample. The Au film is assumed to consist of bottom-surface (B), facet-surface (F), top facet-edge (TE), and bottom facet-edge (BE) regions with resistivity of RB, RF, RTE, and RBE, respectively.
The simplified resistance ratio, defined as the inverse of the current ratio at a fixed voltage, was 3–10 for the measured wire widths. Note that the dimensions (cross section and length) and crystallinity of the Au film were almost the same in the parallel and perpendicular configurations. Thus, the significant anisotropic resistance in these configurations is ascribed to the properties of the geometric shapes of the Au wires, that is, 3D angular interconnects. Indeed, the perpendicular wires have more facet-edges than the parallel wires; the perpendicular channel crossed over 11 top and 23 bottom facet-edges, while the parallel channel crossed over one top and two bottom facet-edges for a wire width of 5
Au wires on the 3D facet structure can be separated into four regions: flat bottom-surface, flat facet-surface, convex top facet-edge, and concave bottom facet-edge regions with resistances of RB, RF, RTE, and RBE, respectively, as shown in the inset of Figure 15(b). The geometries of crystal grain boundaries in the polycrystalline Au wire may increase the electrical resistance [49]. The aggregation of crystal grain boundaries in the interconnect region, leading to the reduction in effective cross-sectional area, was attributed to the large
We found that the conductivity passing through the interconnects is sensitive to the alignment of the facet-edges in the electric path, and the series configuration showed a 3–10-fold larger resistance than the parallel configuration, which originated from the increased resistivity across the facet-edges by a factor of ∼30–180, as calculated from the circuit model. This work provides a fundamental understanding of the impact of the 3D angular interconnects of a metal wire on electric transport and guidelines for the comprehensive investigation of the intrinsic interconnect transport properties on 3D structures, which is expected to produce critical benefits in the semiconductor industry.
This chapter demonstrated the creation and evaluation of atomically ordered side-surfaces and inclined facet-surfaces in nanofabricated 3D Si architectures toward the realization of sequentially 3D integrated and stacked devices for More Moore [3]. Atomically flat and well-ordered 3D structured surfaces play an important role in creating high-performance films on arbitrarily oriented 3D surfaces, similar to films grown on ordinary planar substrates. We emphasized that electron diffraction techniques such as RHEED and LEED are convenient for evaluating atomically ordered 3D surfaces, while conventional SEM has no atomic resolution. The points for recognizing 3D surfaces in diffraction patterns were explained along the basic concept of diffraction in reciprocal space; the intersection of reciprocal lattice rods with an Ewald sphere led to diffraction spots on arcs, and the spots elongate in the surface normal direction.
By diffraction, we evaluated several systems with side- or facet-surfaces of Si
The authors appreciate Dr. Shohei Takemoto, Dr. Haoyu Yang, Prof. Hiroshi Daimon, and Prof. Hidekazu Tanaka for their contribution to these studies. We also thank Ms. Saeko Tonda, Ms. Michiko Sakuma, Mr. Shoichi Sakakihara, and Mr. Takeshi Ishibashi for their helpful support in the fabrication of 3D Si samples and Ms. Liliany N. Pamasi and Mr. Ken Maetani for their support in the diffraction measurement of Si samples. This work was partially supported by Adaptable and Seamless Technology Transfer Program through target-driven R&D (A-STEP) from the Japan Science and Technology Agency (JST) (No. JPMJTM19CM), Japan Society for the Promotion of Science (JSPS) Grant-in-Aid for Scientific Research B (Nos. 18H01871 and 20H02483), the Nanotechnology Platform Project (Nanotechnology Open Facilities in Osaka University, Nos. F-16-OS-0012 and F-16-OS-0016), and the Research Program of “Dynamic Alliance for Open Innovation Bridging Human, Environment and Materials” in “Network Joint Research Center for Materials and Devices” (No. 20203017).
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