Techniques of hybrid seed production.
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He is the Spanish delegate at the group of experts in wine microbiology and wine technology of the International Organisation of Vine and Wine (OIV). He is the author of more than 70 research articles, 3 books, 4 edited books, 6 special issues and 16 book chapters.",institutionString:"Technical University of Madrid",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"6",totalChapterViews:"0",totalEditedBooks:"3",institution:{name:"Technical University of Madrid",institutionURL:null,country:{name:"Spain"}}}],coeditorOne:{id:"186423",title:"Dr.",name:"Iris",middleName:null,surname:"Loira",slug:"iris-loira",fullName:"Iris Loira",profilePictureURL:"https://mts.intechopen.com/storage/users/186423/images/system/186423.jpg",biography:"Iris Loira is an assistant professor of Food Science and Technology at the Universidad Politécnica de Madrid (UPM), Spain. 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Vegetables can prevent several chronic diseases, including cancer [1]. But the successful production of vegetables depends on the first primary input that is the seed. Seeds are the consequences of sexual reproduction in the plant, and not all plants produce. Besides, the seeds are of tremendous organic and financial value. They have abundant protein, starch and oil reserves that assist during the early stages of development of a plant. These reserves are what make several portions of cereal and legumes main foods resources for any considerable proportion in the world’s inhabitants [2]. Vegetable seeds signify a crucial organ intended for the multiplication of vegetables. Seeds accumulate well-balanced free of charge amino acids, which stored inside the seed storage proteins (SSPs). The seed quality is determined by the kind of amino acids, specifically crucial amino acids [3].
Vegetables require two successive processes, namely pollination and fertilisation, to produce the seeds. Pollination refers to the transfer of pollen from the androecium (male flower part) to the gynoecium (female flower part). Generally, flowers contain two other parts, the sepals and petals, which may be helpful to attract pollinators, namely insects. It is not necessary for flowers to have all of these four structures mentioned. Flowers either may be complete, having all four or incomplete, not having all four parts. Likewise, flowers may be grouped into perfect and imperfect flowers [4]. There are two main types of pollination, namely, self and cross-pollination. Self-pollination refers to the deposition of pollen from the anther on the stigma located on the same plant (geitonogamy). It is the closest form of inbreeding which leads to homozygosity. Species having this type of pollination develop homozygous balance and do not exhibit significant inbreeding depression [5].
Whereas the transfer of pollen from the anther of one flower to the stigma of another flower on a different individual is called cross-pollination. It is the form of outbreeding which leads to heterozygosity. Outbreeder species develop heterozygous balance and exhibit significant inbreeding depression on selfing. In addition to these two types of pollination, there is one a different kind of pollination, often called cross-pollination, where cross-pollination often exceeds 5% and may reach 30%. Various mechanisms such as bisexuality, homogamy, cleistogamy and position of anthers promote self-pollination, whereas other mechanisms such as dicliny (namely monoecy and dioecy), dichogamy, heterostyly, herkogamy, self-incompatibility (namely sporophytic and gametophytic) and male sterility promote cross-pollination [6].
Nearly one-third of the current global population is suffering from some form of malnutrition. Moreover, with a constant rise in the world population the food demand tends to increase up to 60% [7]. Vegetables being shorter duration crops can play a crucial role in providing more food per unit of cultivated area [8]. Similarly, climate change is a result of human activities primarily related to the emission of greenhouse gases. It means that there must be a focus on vegetable production and lowering the per capita emissions of greenhouse gases [9]. Vegetables are sensitive to temperature fluctuations, and environmental stresses have also been found to affect the nutrient composition of vegetables [10].
Monoecious, that is, cucurbits have both male and female flowers on different branches of the same plant. Dioecious (like spinach) have male (staminate) and female (pistillate) flowers on separate plants. Generally, both of these monoecious and dioecious plants require cross-pollination. Pollen grain germinates and penetrates the style to reach the ovary and then fertilises the ovule. This fertilised ovule changes into seed and the surrounding ovary develops into the fruit [11]. There are different agents for pollination such as insects, wind and water, etc. Insects are main agents for pollination in vegetables; they visit flowers to collect pollen and nectar as food and transfer this pollen unknowingly to the stigma of other flowers on the same plants or different plants. In this review, we have tried to comply with the important aspects for the successful and mass production of healthy vegetable seeds [12].
Crops can be classified into three categories depending upon the mode of pollination, that is, naturally self-pollinated, naturally cross-pollinated and both self and cross-pollinated crops. Naturally self-pollinated: In such plants, same floral structure or different flowers on same plant houses both pollen and embryo sac. Examples are tomato (Solanum lycopersicum L.), lettuce (Lactuca sativa L.), parsnip (Pastinaca sativa L.), peas (Pisum sativum L.), dwarf bean (Phaseolus vulgaris L.) (Table 1).
Crops | Techniques used for hybrid seed production |
---|---|
Onion | *S and T type-cytoplasmic male sterility (CMS) with natural pollination |
Carrot | Brown anther and *petaloid sterility-cytoplasmic male sterility (CMS) with natural pollination |
Cole crops and radish | Oguro type-cytoplasmic male sterility (CMS) and *Sporophytic self-incompatibility (SSI) with natural pollination |
Cucurbits | Genetic male sterility mainly in muskmelon and *hand emasculation with natural (pinching and use PGR for staminate flower) or hand pollination |
Pepper | *Genetic male sterility with hand pollination or natural pollination |
Tomato and Brinjal | *Hand emasculation and hand pollination |
Techniques of hybrid seed production.
Commercial use of techniques in hybrid seed production.
Naturally cross-pollinated: in cross-pollinated plants, male and female flowers are present on different plants. While in some cases, the stigma may not be receptive at the time of pollen availability. For example, cabbage (Brassica oleracea var. capitata L.), cauliflower (Brassica oleracea var. botrytis L.), onion (Allium cepa L.), broccoli (Brassica oleracea var. italic L.), carrot (Daucas carota L.), radish (Raphanus sativus L.), pumpkin (Cucurbita moschata Duchesne), squash (Cucurbita pepo L.), beet (Beta vulgaris L.), muskmelon (Cucumis melo L.), cucumber (Cucumis sativus L.). Other cucurbits (bitter gourd, bottle gourd, ridge gourd, sponge gourd, snake gourd, pointedgourd, ash gourd, etc.), amaranths.
Both self and cross-pollinated: Plants are primarily self-pollinated, but cross-pollination occurs to varying extents. Examples include brinjal (Solanum melongena L.), okra (Abelmoschus esculentus (L.) Moench), chilli (Capsicum annuum L.), sweet pepper (Capsicum spp.). After landing on stigma, pollen grains germinate and grow down the style of the flower, and this process is called fertilisation. Sperms of the pollen unite with ovules in the ovary which leads to seed production. In the event of pollen incompatibility, a fully pollinated flower does not get fertilised. Some plants are capable of producing fruit without fertilisation and seed production, and such species are called parthenocarpic [13, 14].
Among the different pollination agents like wind, birds, insects, gravity, water and mammals, the most important are insects. Insects contribute 80–85% of the pollination, out of which a hefty proportion of 75–80% is attributable to honey bees. Because of their body characteristics and behaviour patterns, solitary bees, bumblebees and honey bees constitute the largest group of pollinators. Pollination by insects is indispensable for improvement of plant and yield characteristics like seed set, quality of produce, early flowering, oil content, rubber content, pyrethrin content, etc. Managed pollination of crops by honey bees is a surest and most effective way of increasing yield and quality of the produce. Honey bees enhance productivity of crops through cross-pollination along with additional income through production of honey and beeswax, etc. Honey bees and other cross-pollinating agencies like bats, small mammals, birds, etc. owing to its body modifications to pick pollen, floral fidelity, efficiently communication among the colony members and their adaptability to different climates [15]. Cross-pollination results in hybrid vigour, thus improving the quality as well as quantity of the produce which is a boon for vegetable seed production (Table 2).
Crop | Pollination type | Mechanism |
---|---|---|
Solanaceae | ||
Tomato (Solanum lycopersicum) | Self | Bisexual, stigmas surrounded by anthers |
Eggplant (S. melongena) | Self | Bisexual, stigmas surrounded by anthers |
Potato (S. tuberosum) | Self | Bisexual, hypogynous |
Peppers (Capsicum annuum) | Self | Bisexual, hypogynous |
Cucurbitaceae | ||
Bottle gourd (Lagenaria siceraria) | Cross | Monoecious |
Watermelon (Citrullus lanatus) | Cross | Monoecious |
Cucumber (Cucumis sativa) | Cross | Monoecious |
Gherkin (C. anguria) | Cross | Monoecious |
Muskmelon (C. melo) | Cross | Monoecious |
Snake gourd (Trichosanthes cucumerina) | Cross | Monoecious |
yellow-flowered gourd (Cucurbita pepo ovifera) | Cross | Monoecious |
zucchini (C. pepo) | Cross | Monoecious |
Cole crops | ||
Brussels sprouts (Brassica oleracea var. gemmifera) | Cross | Sporophytic self-incompatibility |
Cabbage (B. oleracea var. capitata) | Cross | Sporophytic self-incompatibility |
Cauliflower (B. oleracea var. botrytis) | Cross | Sporophytic self-incompatibility |
Kale (B. oleracea var. sabellica) | Cross | Sporophytic self-incompatibility |
Broccoli (B. oleracea var. italica) | Cross | Sporophytic self-incompatibility |
Turnip (B. rapa subsp. Rapa) | Cross | Sporophytic self-incompatibility |
Fabaceae | ||
Common Bean (Phaseolus vulgaris) | Self | Self-fertilisation before opening the flowers (Cleistogamous) |
Faba bean (Vicia faba) | Partial cross pollination | Partly cleistogamous |
Lima bean (P. lunatus) | Self | Cleistogamous flower structure |
Chickpea (Cicer arietinum L.) | Self | Cleistogamous flower structure and stigmas surrounded by anthers |
Cowpea (Vigna unguiculata) | Self | Cleistogamous flower structure |
Fenugreek (Trigonella foenum-graecum) | Self | Cleistogamous flower structure |
sweet pea (Lathyrus odoratus) | Self | Cleistogamous flower structure and stigmas surrounded by anthers |
Pea (Pisum sativum) | Self | Cleistogamous flower structure and stigmas surrounded by anthers |
Soybean (Glycine max) | Self | Cleistogamous flower structure and stigmas surrounded by anthers |
Different kind of pollination mechanisms in the vegetable crops.
Inadequate pollination has been a major constraint to the potential returns of vegetables. Different insect pollinators have been identified in various vegetable crops, which increased the seed yield by increasing the pollination. Vinícius-Silva et al. [16] found fifteen floral visitors with Exomalopsis analis being the most representative in tomato crop. They also reported the presence of the other two effective pollinators, namely Apis mellifera and Trigona spinipes in tomato crop. Shah et al. [17] observed the highest population of honey bees among all tracked pollinators in cucumber and showed that insect pollination in cucumber acts as additional input in enhancing the yield [18].
Similarly, the highest weight of fruits, number of seeds per fruit, fruit size and TGW was achieved in honey bee pollination compared to others. Azmi et al. [19] observed heavier, longer and larger fruits in cucumber when pollinated by stingless bee (Heterotrigona itama) and hand compared to those produced from pollination without H. itama. Rouf et al. [20] reported an increase of 45.46 and 23.17% in seed yield of cauliflower plants pollinated by honey bee over plants grown inside net without bees and open pollination, respectively. Further, they showed that maximum yield attributes of seed could be achieved if planned bee pollination and central curd cutting employed together.
For the first time in 1968, Donald introduced the concept of ideotype in plant breeding. Later in 1976, the concepts of isolation, competition and crop ideotypes were proposed by Donald and Hamblin [21].
Manipulation of plant architecture of tomato may provide increased fruit yield resulting in increased seed yield. Suarma et al. [22] suggested emphasising on traits such as fruit yield (q/ha), plant height, average fruit weight for ideotype construction in tomato. Direct selection for these traits, having high heritability and genetic advance, may yield expected genetic up-gradation of a genotype. Sarlikioti et al. [23] suggested a new plant ideotype for optimization of light absorption and canopy photosynthesis in tomato. This new ideotype with more spacious canopy architecture due to long internodes and long and narrow leaves led to an increase in crop photosynthesis of up to 10%. Recently, Zsögön et al. [24] suggested that vital monogenic traits whose physiology has been revealed thoroughly can be molecularly tailored using genome editing techniques to achieve the target ideotype for elite cultivars of tomato. They also proposed that wild relatives or progenitors harbouring polygenic traits of interest could be de novo domesticated by manipulating monogenic yield-related characters through these techniques to get ‘model type’ plants which would perform expectedly in a defined environment. It has been suggested that shifting of crop plants from annuals to perennials may provide an additional advantage in seed yield. Eggplant ideotypes characterised by a radical change in plant architecture, with an arborescent or shrubby habit and perennial instead of annual fruit set using somatic hybridization [25, 26, 27].
Plant architecture of muskmelon has also been manipulated to get increased fruit yield. Two different plant ideotypes have been proposed to get increase fruit set in muskmelon: “bush” or “birdnest” type possessing multilateral branches of the same length and bearing uniform sized fruits near the centre of plants and short internodes types having indeterminate growth behaviour and shorter internodes which can be planted at higher densities [28].
Manipulation of the architecture of plants to achieve high seed production has been accomplished in various fabaceous species such as common bean, broad bean and pea; and also in the underexploited species of this family [29, 30].
Isaacs et al. [31] employed participatory plant breeding approach and together with farmers, identified specific traits that constitute a bean ideotype: adaptation, restricted height, columnar plant structure, even distribution of pods, fewer leaves, and earlier maturity. Plants with this ideotype produced good seed yield and were suitable for maize-bean cropping systems. Polania et al. [32] 2017 evaluated 36 bean genotypes to test the relationships between shoot traits and root traits under drought conditions. They identified two ideotypes related to efficient water use: water savers having a shallower root system and water spenders presenting more in-depth root system. Both showed greater root vigour under drought stress and produced high grain yield. Recently, Bodner et al. [33] identified ideotypes, having higher average yield, taller structure, more pods per node and longer flowering duration, suitable for Northern Europe. They considered Baltic landraces as promising ideotypes for increased V. faba yields in Nordic target environments as well as the other workers [34].
Since all vegetables are angiosperms, so a standard procedure of fertilisation, seed set and development is followed in all vegetables with few modifications. We are presenting here a general mechanism of fertilisation, seed set and development. At the time of fertilisation, protective coats, known as integuments and a central tissue called nucellus are present in the angiosperm ovule. If we see the structure of ovule, clear differentiation of these two integuments and nucellus can be found in the region of the micropyle, it is a minute pore in the integuments through which, the pollen tube enters the nucellus and move towards egg cell and polar nuclei. A stalk, funicle, attaches the ovule to the wall of the ovary. In general, megaspore mother cell inside the nucellus once divides meiotically and then divides mitotically three times to produce embryo sac or female gametophyte, a haploid eight-nucleate, seven-celled structure which comprises of one egg cell, two synergids, three antipodal and two polar nuclei. Although among angiosperms, the female gametophyte has a variety of forms, it may not necessarily encompass all these seven cells. On the other hand, inside the anther, microspore mother cell first divides meiotically and then mitotically to produce pollen grain or microgametophyte, which comprises two sperm cells enclosed with one vegetative cell [35].
These two female and male gametophytes play essential roles in the reproductive process of angiosperm. Sexual reproduction starts with the transmission of male gametophyte or pollen grain from anther to the carpel’s stigma. Subsequently, pollen grain begins to germinate on stigma and a pollen tube carrying two sperm cells is formed, which penetrates the style. Growth and development of pollen tube is controlled by vegetative nucleus which disintegrates after serving its duty. Pollen tube enters into the embryo sac through micropyle, in general, and releases two male gametes. One male gamete fertilises the egg cell, called syngamy, and the second male gamete fuses with the central cell or polar nuclei [36]. Since two successive fertilisations take place, the procedure is known as double fertilisation. The zygote is formed after uniting of one sperm cell with egg cell, and this zygote gives rise to seed’s embryo which is the starting of the sporophyte generation. Following fertilisation, central cell’s polar nuclei produce seed’s endosperm, which is the nutrition source for developing embryo. These two embryos and endosperm encompass the central portion of the seed. Two synergids and three antipodal, remaining five nuclei, do not play any further role in seed development. For the development of viable seed, successful fertilisation of egg cell and the central cell is necessary [37]. All seeds mostly contain an embryo, a protective cover-seed coat and a reserve of food materials or any other specified tissue such as perisperm. Occasionally, polyembryony condition refers to development of more than one embryo in a single seed, may also be observed in some families such as Solanaceae and Amaryllidaceae families.
Underlying molecular mechanisms of seed set and development in angiosperms is becoming clear rapidly with the advancements of various omics studies such as genomics, transcriptomics and proteomics etc. and genetic transformation techniques. These mechanisms are generally conserved across all the angiosperms and may also be operated in vegetables. Various studies have been conducted in vegetables such as tomato (and cucumber to explore the underlying molecular mechanism of seed set and fruit set) [38]. In 2016, isolated and characterised two allelic mutants, twisted seed1-1 (tws1-1) and tws1-2 of a single copy gene (TWS1). This gene encodes a small protein of 81 amino acids which regulates embryonic development and accumulation of storage compounds in the seed [39].
This gene is specifically conserved among angiosperms and can be cloned from vegetables to explore its function in seed development in vegetables. The importance of AN3-MINI3 gene cascade in seed embryo development. Their regulatory model provided a deep insight into the seed mass regulation, which may be further explored to increase seed yields of vegetables [40]. Role of mitochondrial reactive oxygen species homeostasis in gametophyte and seed development has also been highlighted in angiosperms. It was reported that the effect of the mutation in AtHEMN1 gene which encodes for coproporphyrinogen III oxidase. They showed adverse effects of Athemn1 mutant alleles on gametophytic and seed development. Adverse effects included the development of nonviable pollen and embryo sacs with unfused polar nuclei, defects in endosperm development due to abnormal differentiation of the central cell and arresting of embryo development at the globular stage [41].
To ensure successful sexual plant reproduction, fruit set or transformation of flowers to fruits is very critical. Role of hormones (i.e. auxin and gibberellins) in controlling fruit set after pollination and fertilisation have been well understood. It was shown that the role of microRNA-based (microRNA159/GAMYB1 and −2 pathway) regulation ovary development and fruit set in tomato. They initiated fruit set by modulating auxin and gibberellin responses using SlGAMYBs. On the other hand, proteins such as TIR1-like proteins have also been shown to have essential roles in auxin-mediated fruit development processes. Two TIR1-like genes have been identified in cucumber and designated as CsTIR1 and CsAFB2 [42]. Xu et al. [43] used tomato as a model plant to investigate the effects of these two genes on fruit/seed set. They highlighted the crucial role of the miR393/TIR1 component in fruit/seed set and concluded that post-transcriptional regulation of these two genes mediated by miR393 is vital for fruit set initiation in both cucumber and tomato. The different stages of seed development and the structure of a dicot seed is presented in Figure 1.
Different stages of seed development.
Peterson (1958) first reported the cytoplasmic genetic male sterility (CGMS) in chilli in an introduction of C. annuum from India (PI-164835) and found its instability under fluctuating conditions, particularly temperatures and natural cross-pollination. Genetic male sterility in chilli well exploited on a commercial scale in hybrid seed production. Male sterile plants easy to identify in the field at a comparatively early stage. Nearly 20 genes governed genetic male sterility. The ms-10 gene is linked with taller plant height, erect growth and dark purple anther. MS-12 (ms-509/ms-10) and ms-3 genes are commercially utilised in India and Hungry, respectively [44].
Tomato crop has different types of male sterility identified, but presently commercial hybrid seed production in tomato and brinjal possible with manual emasculation and hand pollination and it is economically viable and dominates in the seed industry. Though, the availability of different sterility methods can be used to avoid selfing and optimise crossing resulted in reducing the cost of hybrid seed production [45].
To exploit heterosis in cucurbits the essential requirement is heterotic combination potential of crops from flower size to pollination and fruit set resulted in proper seed setting to economic feasibility. The cucurbit vegetables have a more substantial size of male and female flowers and allow following other systems of pollination control strategies. The hand emasculation with hand and natural pollination mechanism used in hybrid seed production in bottle gourd, pumpkin, squash, cucumber, muskmelon and bitter gourd with specific planting ratio. Genetic male sterility mainly uses in muskmelon, and most of the genetic male-sterile mutants in cucurbits are monogenic recessive. There are many types of male sterility identified in cucurbits, but commercial exploitation is still lacking. Gynoceious lines based on genetic male sterility (GMS) stability gene and use of different plant growth regulators are also useful in hybrid seed production of cucurbits with sex modification [46].
Cole crops and some root crops are a significant group of vegetables in the brassica family, and they are cabbage, cauliflower, broccoli, turnip and radish. GMS, CGMS and self-incompatibility (SI) are important pollination mechanism available in Brassica family to get a higher percent of heterosis in crops. In which, self-incompatibility (Sporophytic self-incompatibility) system is most useful in hybridisation program. But, CGMS method also developed with some self-pollination occurrence [47]. In cole vegetables, sterile cytoplasm (CMS system) derived from B. nigra through interspecific hybridisation between B. nigra and B. oleracea var. italica and Ogura type CMS also identified and reported in cultivar Japanese radish of Raphanus sativus. First, introgression of this sterility cytoplasm to Brassica oleraceae genome through repeated backcrosses with broccoli. Some plant physiological problems were found in Ogura based CMS lines of broccoli, cauliflower, cabbage, Brussels sprout and it has been solved using protoplast fusion, and this technique is also used in transfer Ogura cytoplasm from broccoli into cabbage [48].
Cytoplasmic male sterility in carrot can occur in two morphologically (brown anther and petaloid) distinct phenotypes. The brown anther male sterility was first discovered in the cultivar Tendersweet, and this is, characterised by shrivelled, yellow-to-brown anthers with no pollen. It is a homeotic mutation. This is established as the white petaloidy or green petaloidy. It is stable male sterility across a wide range of environments as compared to brown anther type. Seed yield of the brown-anther CMS are generally higher because of petaloid sterility shows less frequent deterioration to male fertility [49].
Male sterility in onion, first reported in the progenies of an onion cultivar Italian Red plants and is controlled by the combination of a cytoplasmic factor “S” together with a recessive nuclear restorer locus in its homozygous form (ms) and “T”-cytoplasm has been reported. Onion (Allium cepa L.) hybrid seed production has been produce in all over the world through CGMS-based systems in which mostly hybrids are derived from S-cytoplasm because of its stability in various environments [50, 51].
Self-incompatibility can be a widespread phenomenon in vegetable crops that forestalls inbreeding and encourages outcrossing. The response of self-incompatibility is genetically managed by several multi-allelic loci and depends on many intricate interactions among the self-incompatible pollen and pistil combinations. It is genetically regulated phenomena that function as a barrier to self-pollination in the big selection of vegetable crops like cabbage, cauliflower, tomato and many others. Self-incompatibility can be a critical system by which crops avert self-fertilisation and keep a broad genetic range. Self-incompatibility is considered to present in 30–50% of flowering plant species [52]. Many SI programs have now been discovered. In all situations, incompatible (self-) pollen is considered by a distinct system usually genetically managed that brings about inhibition on the pollen while in the stigma or on the pistil. Using SI in F1 hybrid generation has key gain over other approaches. Usage of Self-incompatibility in cole crops for hybrid seed generation is commercialised due to the availability of a robust mechanism/method to create large-scale F1 seeds employing picked parental strains is undoubtedly a critical issue, which in the long run establishes the professional viability on the hybrid varieties [53].
Self-incompatibility is classified as namely gametophytic and sporophytic. In gametophytic technique self-incompatibility response of pollen and stigma is decided with the genotype of the female plant on which pollens are developed (e.g. tomato) even though in sporophytic technique, pollen phenotype (self-incompatibility response) is identified with the genotype on the female plant on which pollens are developed (e.g. cole greens). In Brassicaceae, sporophytic self-incompatibility (SSI) has been ideally characterised and productively used for that growth of commercial hybrids. Using SI in F1 hybrid generation has key gain over other approaches; equivalent portions of seed on the two inbred strains can be blended jointly for demonstrating, along with the total crop is harvested for seed. For hybrid seed generation, equally the parental inbreds need to have two diverse S alleles for sturdy self-incompatibility in the event of one cross hybrid. Among the cole greens like cabbage, cauliflower, broccoli and many others, sporophytic self-incompatibility system is currently being used for the hybrid seed generation at many spots in India [54]. Usually in cauliflower self-incompatibility is weak, and its response is broken at substantial temperature. Self-incompatibility can be a technique employed by a lot of flowering plant species to forestall self-fertilisation and thus encourage outcrossing. Above the several years, considerable perception in the mechanisms regulating self-incompatibility has become attained for that Solanaceae gametophytic self-incompatibility programs at the same time as for that sporophytic self-incompatibility technique of the Brassicaceae in vegetable crops. A mix of genetic and molecular reports have resulted while in the identification and characterisation of the self-incompatibility genes associated with this particular reaction.
Moreover, careful investigation on the factors in the signalling cascades of equally the Solanaceae along with the Brassicaceae is necessary for an entire idea of the self-incompatibility reaction in these people. Several mechanisms and approaches have not been exploited for that growth of professional hybrids in vegetable crops between that SI is of crucial relevance. While in the light-weight of the quick progression of biotechnology, it could be expected that SI programs are going to be ever more used near foreseeable future, in vegetable crops [55].
Growth regulators are organic chemical substances which, when applies in small quantities aid in the regulation of plant growth and modify the physiological response in plants. Growth regulators have immense importance in enhancing vegetable production and have been used to improve seed germination, increase in yield and tolerance against diseases and unfavourable conditions [56]. Apart from these functions growth regulators have usefulness in vegetable seed production by altering sex expression, increasing fruit set as well as seed yield and inducing male sterility, without exerting any harmful effects on the environment and human health [57]. Classification and functions of different plant growth regulators (PGRs) are listed below:
Auxins (IAA, NAA, IBA, 2,4-D, 4-CPA): apical dominance, root induction, control fruits drops, regulation of flowering.
Gibberellins (GA3): seed germination, stimulates flowering, increase flower and fruit size.
Cytokinins (kinetin, zeatin): bud initiation and root growth, storage life prolongation of vegetables.
Ethylene (etheral): uniform ripening in vegetables, promotes abscission, senescence of leaf.
Abscisic acid (dormins, phaseic acid): stress hormone, dormancy, seed development and germination.
Flowering hormones (florigen, vernalin).
Natural substances (vitamins, phytochrome tranmatic).
Synthetic substances (synthetic auxins, synthetic cytokinins).
Role of different PGRs in vegetable production of different vegetable crops are reviewed in Table 3:
PGR | Target/response | Crop |
---|---|---|
GA3 | Fruit setting, seed yield and quality | Bittergourd, muskmelon, tomato, chilli, capsicum, brinjal, cauliflower, cabbage, okra, cucurbits, potato, pea |
GA3 | Abnormalities in pollen development and induced the carpelization of stamens | Pepper |
GA3 | Leaf morphogenesis, promote normal stamen and pollen development | Tomato |
GA3 | Production of male sterile flowers | Onion, Brussels sprouts, cabbage, cauliflower and kale |
GA3 | Increased number of female flowers | Bitter gourd |
GA3 | Lower male and female flower ratio | Cucumber |
GA3 | Induce parthenocarpy | Bitter gourd |
Ethrel | Decreased number of staminate flowers | Cucumber, bittergourd, pumpkin, sponge gourd |
Ethrel | Increased number of pistillate flowers | Cucumber, pumpkin, pointed gourd, melons, snake gourd, sponge gourd, bottle gourd, bitter gourd, summer squash |
Ethrel | Lower male female flower ratio | Cucumber |
Ethrel | Increased yield | Cucumber, bitter gourd, cucurbits, potato, pumpkin |
Ethrel | Induction of male sterility | Lettuce, eggplant, squash |
TIBA (triiodobenzoic acid) | Induction of male sterility | Tomato |
TIBA (triiodobenzoic acid) | Producing a favourable female to male ratio and increased number of fruits | Cucumber, squash, watermelon |
MH (maleic hydrazide) | Induction of male sterility | Tomato, coriander, pepper, okra, onion, squash, chilli, eggplant |
MH (maleic hydrazide) | Decreased number of male flowers | Cucumber, sponge gourd |
NAA (naphthalene acetic acid) | Induce male sterility | Tomato and squash |
NAA (naphthalene acetic acid) | Reduce staminate-pistillate flower ratio | Cucumber, squash |
NAA (naphthalene acetic acid) | Increased number of female flowers | Cucurbits, sponge gourd |
NAA (naphthalene acetic acid) | Decreased number of male flowers | Cucumber |
NAA (naphthalene acetic acid) | Induce parthenocarpy | Bitter gourd |
NAA (naphthalene acetic acid) | Increased fruit set/yield | Cucumber, bottle gourd, tomato, chilli, capsicum, brinjal, cauliflower, cabbage, onion, garlic, cucurbits, okra, tomato |
Dalapon (dichloropropionic acid) | Induction of male sterility | Pea, tomato |
Dalapon and a-chloropropionate | Supression of anther dehiscence | Pepper tomato |
FW-450 (sodium 2,3-dichloroisobutyrate) | Induction of male sterility | Tomato |
CCC ((2-chloroethyl) trimethylammonium chloride) | Selectively inhibited the development of stamen or suppressed pollen | Tomato |
ABA (abscisic acid) | Selectively inhibited the development of stamen or suppressed pollen | Tomato |
Indole acetic acid (IAA) | Increased pistillate flowers | Cucurbits, cucumber |
Indole acetic acid (IAA) | Decreased male flowers | Cucumber |
Indole acetic acid (IAA) | Improved yield and quality characteristics | Okra, cauliflower |
Growth regulators used for higher seed production in the vegetables based on Prajapati et al. [58].
The essence of any seed programme is the excellent quality of seed, and this trait varies from the standpoint of genetic purity. The seed programme with no proper quality management of the seed will tend to fail. For that reason, the quality of vegetable seed is a necessary consideration. Underneath a standard seed technology chain, breeder seed is multiplied from nucleolus seed. The exercise of bulk enhance of breeder seed and endless multiplication cycles of basis seed with no likely again to breeder seed may severely influence the standard of seed and may be discontinued. Importance of good quality seed can be determined from the fact that seed is the indispensable input for crop production. The top-quality seed is the carrier of the resistance gene or good genes selected by the breeder. Seed ensures food supply under adverse production sites; therefore, the importance of seeds for vegetable production cannot be denied.
The authors declare no conflict of interest.
Clays are inorganic, natural, earthy, and fine-grained materials that acquire plasticity when mixed with water [1]. For sedimentologists, a clay is a raw material whose grain size is less than 2 μm. Like clays, in turn, there are rocks made up of clay minerals and may contain other minerals such as quartz, feldspar, mica, calcite, hematite, and organic matter as accessories [2]. A clay, once ground and mixed with water, in addition to presenting excellent workability in the fresh state, after drying, becomes extremely rigid. After burning normally above 800°C, it acquires great resistance [3]. Clays are used worldwide in the ceramic industry, especially in bricks, coatings, and others. However, clays are formed from the weathering of explosion and can be contaminated with several minerals among them or carbonate, which can alter the shape that causes the following burns. Limestone may be present in colloidal form, or coarse particles. However, in all cases it is impossible to separate or calculate this. Some researchers have tried to reduce the size of the variations to improve the chemical changes. According to Barba et al. [4], calcium carbonate and magnesium carbonate are the main constituents of carbonate sedimentary rocks. Anionic carbonate groups are strongly activated units and share oxygen with each other. They are responsible for the properties of these minerals. The most important anhydrous carbonates belong to three isostructural groups: the calcite group, the aragonite group, and the dolomite group. Among these, the minerals most used in the ceramic industry are calcite and dolomite, as they are low-cost raw materials, in addition to having favorable physical and chemical properties and available deposits. Second, Padoa [5] adds that when CaCO3 is small, a decomposition can be complete and the calcium oxide reaches later with other mass components forming calcium silicates and silicon aluminates (wollastonite, anortite, gehlenite etc.) during sintering. Barba et al. [4] mentioned that the raw materials of clay when burned at high temperatures produce crystal phases that influence the properties of ceramic products. Calcite exerts a bleaching action on burnt products when added to a formulated mass of clays (in proportions above 5% and less than 30%) and at the same time decreases its expansion by legislation, as it forms crystalline and liquid phases, including cycles temperature and firing adopted. Calcite and dolomite are the most important representatives of carbonates in the ceramic industry. They are used as main components in the manufacture of ceramic tiles with high water absorption. These coatings include “porous coatings” or “tiles.” These products are designed or used on walls and are not suitable for application on floors, as they have undesirable technical characteristics, such as mechanical resistance, incompatibility with use. According to Amorós [6], properties of parts of a ceramic product are registered by crystalline phases formed based on calcium and magnesium as ghelenite (SiO2⋅Al2O3⋅2CaO) and anortite (2SiO2⋅Al2O3⋅CaO). To achieve these phases, use the dolomite calcium oxide and/or magnesium reaction with a remaining clay structure proven by its thermal decomposition.
The calculation in general can affect the ceramic product in two ways: low percentages (up to 3%) and high temperature (above 1180°C) result in flow agents, that is, materials that contribute to reduce water absorption and increase the resistance of ceramic products. Above 3%, they can act as a foundation at temperatures above 1170°C [7].
In this chapter, we will highlight properties of limestone clays and their application in the ceramic industry.
Clays are hydrated aluminum silicates with crystalline structure arranged in layers, consisting of continuous sheets of SiO4 tetrahedrons, ordered in a hexagonal shape, condensed with octahedral sheets of di and trivalent metal hydroxides, usually below 2 μm. They are materials that in contact with water become plastic, a fundamental characteristic for conformation of ceramic products because it provides mechanical resistance in the pressing, extrusion, or gluing process. Clays are mixtures of various clay minerals such as kaolinite, illite, and montmorillonite, which may or may not contain impurities [3, 8].
The kaolinite with structural formula Al2O3⋅2SiO2⋅2H2O has a dioctahedral structure, which consists of a tetrahedral layer linked by an octahedral layer. Pure kaolinites usually have low plasticity, see Figure 1.
Kaolinite structure. (a) Si▬O tetrahedra on the bottom half of the layer and Al▬O,OH octahedra on the top half. (b) Dioctahedral structure.
Montmorillonites are a set of family of clay minerals, composed of dioctahedral and trioctahedral silicate sheets, see Figure 2(a) and (b). The most outstanding feature of these minerals is their ability to absorb water molecules [8, 9]. It has 80% of exchangeable cations in the galleries and 20% on the lateral surfaces. The modification of montmorillonite clays has aroused scientific and technological interest for providing significant improvements when incorporated into pure polymeric materials and conventional composites. The clay modification process occurs preferably through the ionic exchange of the exchangeable cations of its crystalline structure.
Crystalline structure of a montmorillonite. (a) Montmorillonite structure, composed of Si, Al, and O. (b) Sheets of dioctahedral and trioctahedral silicates.
The basic structural unit of the illites is the same as that of the montmorillonites except that in illites, the silicon atoms in the silica layers are partially replaced by aluminum. Therefore, there are free valences in the boundary layers of the structural units, which are neutralized by K cations, arranged between the overlapping units. The structural scheme of the illites is shown in Figure 3. The K cation is the one that best adapts to the hexagonal meshes of the oxygen planes of the layers of silica tetrahedron and is not displaced by other cations. The water adsorption and cation exchange capacity is due only to the broken connections at the ends of the layers. The average diameter of the illites varies between 0.1 and 0.3 μm. When the replacement of silicon in the tetrahedron layers by aluminum in the illites is small, the connections between the structural units provided by the K cations may be deficient and will allow water to enter. When this occurs, the properties of the illites are close to the properties of montmorillonites [3].
Crystalline structure of an illite. (a) Silicon atoms in the silica layers partially replaced by aluminum in the illites. (b) Structural scheme of illites.
Chlorites are minerals made up of four hydrated aluminum and magnesium silicate layers, containing Fe (II) and Fe (III) as shown in Figure 4.
Crystalline structure of chlorite [9].
The most common clay minerals are interstratified, characteristic of mixtures of clay minerals, classified by subgroup and mineralogical species, see most common classification in Table 1. Clay minerals are divided into several classes. A large majority of clays do not have in just one crystalline phase. Two or more chemical species may be present.
Subgroup | Chemical species | Minerals |
---|---|---|
Kaolin Xn(Y2O5)(OH)4 | Kaolinites | Nacrite (Al2(Si2O5)(OH)4) Dikite (Al2(Si2O5)(OH)4) Livesite (Al2(Si2O5)(OH)4) Halloysite (Al2(Si2O5)(OH)4) |
Talc XB(Y2O5)(OH)2ZmH2O | Montmorillonites | Montmorillonites (Al1,51Fe0,07Mg0,60)(Al0,28Si3,72)O10(OH)2Na0,33 |
Beidellite (Al1,46Fe0,50Mg0,08)(Al0,36Si3,64)O10(OH)2Na0,4 | ||
Nontronite (Fe1,67Mg0,33)(Si4O10)(OH)2Na0,33 and Fe2,22(AlSi3O10)(OH)2Na0,33 | ||
Hectorite (Mg2,67Li0,33)(Si4O10)(F,OH)2Na0,33 | ||
Saponite Mg3(Al0,33Si3,67)O10(OH)2Na0,33 | ||
Illites | Wide variety of minerals | |
Chlorite | Chlorites | Chlorite |
X2n(Y2O5)2(OH)2 | [Mg2(Al,Fe(III))(OH)6][Mg3(AlSi3O10)(OH)2] |
The clays used in the ceramic manufacturing process can be classified into:
Carbonitic clays: they are formed by associations of illitic-chloritic and eventually illitic-kaolinite clay minerals. The amount of calcium carbonate present can be variable. These clays give the dough plasticity. Generally, after burning they have colors ranging from beige to orange [4].
Non-carbonitic clays: they are characterized by the almost total absence of carbonates. The clay minerals present are of the illitic-chloritic type. It has the function of giving plasticity to the dough, and generally after firing they give rise to well-sintered materials.
White plastic clays: the clay matrix is kaolinitic, with little illite. They give plasticity to the dough, and after burning they have a white color.
Kaolinitic clays: clays of low plasticity and normally free of fluxing oxides such as K2O and Na2O, therefore, with refractory characteristics.
According to Mackenzie [10], when a ceramic raw material is subjected to the action of heat, it experiences volumetric variations, usually permanent and irreversible, which can be classified as:
Oxidation of organic matter
Decomposition of compounds containing oxygen, such as sulfates, carbonates, etc.
Dehydroxylation of the clayey mineral
Crystallization by increasing the temperature
Vitreous phase formation
Solid solutions: adjacent crystals of two different materials but of similar structure can react with each other, forming a solid solution.
Kaolinitic clay: the scheme according to Figure 5 shows an endothermic peak between 560 and 590°C referring to the elimination of hydroxyls from the constitution water present in the clays, and an exothermic peak between 980 and 1000°C, due to the formation of mullite, which can be represented by the reactions 1 and 2 [8].
Differential thermal analysis of a kaolinitic clay [10].
Montmorillonite: montmorillonites have water that lodges in the mineral structure, that is, hydration water of adsorbed ions. The elimination of hydroxyl groups occurs at 700°C. At 850°C, a small endothermic peak may occur due to the loss of montmorillonite crystallinity. Illites can present loss of adsorbed water between 100 and 200°C and water loss in the constitution between 550 and 600°C, see Figure 6.
Differential thermal analysis of a montmorillonite clay [10].
Quartz: it appears in clays in colored or colorless round grains, whose percentage ranges from 0 to 60%. For high levels of quartz, the clay is called sandy and has low plasticity [11].
Hematite: iron can be present in the forms of hematite (α-Fe2O3), goethite (α-FeO⋅OH), and lemonade (a mixture of iron oxides and hydroxides of a weakly crystalline nature), or simply as Fe3+ ions in the clay structure. In the illite group, Fe3+ ions can replace Al3+ ions in the octahedral structure [11]. Fe2O3 is formed during sintering under oxidation conditions and from minerals in the clays, giving a reddish color to ceramic materials.
Feldspar: feldspars refer to a group of aluminum silicate minerals. The feldspar contained in the clays is a source of sodium and potassium oxides and plays an important role in ceramic materials with quality of flow agents, temperatures such as sintering temperatures, porosity after firing and facilitating phase formation [6]. The most representative are the orthoclase (KAlSi3O8) and albite (NaAlSi3O8).
Carbonates: calcium or magnesium carbonates can appear as coarse or small grains. If they are presented as large grains (>125 μm), they may not react completely and the resulting oxides may rehydrate causing expansion according to reactions [12, 13].
Ceramic enamels and frits: can be used in matte enamels as a source of CaO to form crystals such as wollastonite, anorthite, gehlenite or in transparent enamels giving shine.
Masses for ceramic coating: as a source of CaO up to the limit of 3%, CaCO3 assists in the formation of the vitreous phase. CaO levels that vary from 8 to 14% favor the formation of crystalline phases such as gehlenite, wollastonite, pseudo wollastonite, and anortite.
Putties for limestone porcelain: calcium carbonates provide the CaO that are used as a flux in limestone porcelain masses.
Ceramic pigments: the calcium carbonate provides calcium oxide, which together with SnO2 produces pink pigments.
Glasses: glasses based on NaOH and CaO use CaCO3 in their composition.
Obtaining settlement mortars: as a plasticizing agent for water retention and aggregate incorporation.
Steel: CaCO3 acts as a flux and pH regulator in water treatment and as lubricant for drawing steel rebars.
Sánchez et al. [14] defined some specification parameters for choosing raw materials for formulations of coating masses, as shown in Table 2 below.
Product | (%) of carbonates | Max. particle size of CaCO3 (μm) | Organic matter (%) | Sulfate content max. (%) | IP (%) |
---|---|---|---|---|---|
Stoned | ≤3 | ≤125 | ≤0.3 | 0.2 | 20–40 |
Porous | ≤40 | ≤125 | ≤0.3 | 0.2 | 20–40 |
Specifications for choosing raw materials.
IP: index of plasticity.
Calcium or magnesium carbonates can appear as coarse or small grains. If they are presented as large grains (>125 μm), they may not react completely, and the resulting oxides may rehydrate causing expansion.
In compositions of ceramic floor covering with low water absorption, CaCO3 acts as a flux until the limit of 3%; above this value, CaCO3 increases porosity and can be accepted up to 40% in porous coatings.
Enrique [15] recommends that the CaCO3 particle size should be less than 125 μm, because particles of larger sizes, the CaO resulting from the dissociation of carbonates when calcined at 900°C, do not react with the SiO2 present in the clays and feldspars that should form the pseudo-wollastonite and wollastonite phases, which can give rise to Ca(OH)2 formed by the hydration of CaO, when the part comes into contact with the humidity of the air, generating problems of expansion by humidity, with consequent cracking.
The ceramic tile and brick industry have grown enormously in recent years in Brazil. The clays must have sufficient plasticity to provide mechanical resistance when forming by pressing, in order to guarantee the integrity of the piece in the path between the press and the oven. The feldspar contained in the clays are sources of sodium and potassium oxides, acting as fluxes at temperatures above 800°C for bricks and above 1100°C for ceramic tiles, which facilitates the formation of a vitreous phase and reduces porosity [16, 17].
Quartz is mixed with clay during geological formation. If it is present in a smaller proportion, it helps in the formation of the vitreous phase, in the degassing of organic matter and water. However, large proportions of quartz lead to a drastic reduction in mechanical strength after firing [18]. Iron oxide is present in ceramic raw materials in the form of hematite or goethite, giving the finished product a red color.
Calcite, which appears in most clays used in the production process of ceramic tiles of type BIIb, is a mineral that needs special care in its use due to its high loss to fire. When present in a proportion equal to or less than 3%, this mineral acts as a flux. However, in higher proportions, calcite can cause an increase in the final porosity of the product. In addition, the size of the calcite particle for processing ceramics must be less than 125 μm. For larger sizes, it is observed that the CaO resulting from the dissociation of carbonates can hydrate after burning, promoting variations in the dimension of the piece. Therefore, the use of limestone clays is a challenge, requiring care in processing and control in the formulation and burning of coatings. To ensure the correct sintering of the product, proper grinding and pressing of the raw material are necessary, in addition to efficient, fast burning with the lowest possible energy consumption.
Table 3 shows the chemical compositions of a typical Brazilian limestone clay used in ceramics [19]. The chemical compositions of the raw materials were determined by X-ray fluorescence spectroscopy by wavelength dispersion (WDFRX), in a Bruker S8 Tiger equipment, in which the percentages of constituent oxides were estimated by the method semi-quantitatively. For these measurements, samples with a mass of 10.0 g were pressed as discs with 40.0 mm diameter and 4.0 mm thickness. During measurements, the samples were kept in a vacuum of 10−6 bar. A mixture of P-10 (90% argon and 10% methane) was used in the proportional counter.
Oxide (%) | C1 | C2 | C3 | C4 |
---|---|---|---|---|
SiO2 | 63.0 | 52.1 | 50.2 | 45.3 |
Al2O3 | 16.7 | 18.6 | 15.5 | 14.1 |
Fe2O3 | 4.7 | 6.8 | 6.2 | 7.1 |
CaO | 0.9 | 2.1 | 7.2 | 12.7 |
K2O | 3.8 | 4.7 | 3.2 | 3.2 |
Na2O | 0.6 | 0.4 | 0.5 | 0.7 |
MgO | 1.5 | 2.3 | 2.2 | 2.3 |
TiO2 | 0.6 | 0.8 | 0.7 | 0.8 |
L.O.I | 8.2 | 12.1 | 14.3 | 13.8 |
The results show that all clays are composed mainly of SiO2 and Al2O3. These elements are associated with clay minerals, quartz, and feldspar structures [17]. The highest amount of SiO2 was determined for sample C1. This component is important for the manufacture of ceramic tiles, as it improves workability and favors compaction. However, SiO2 can also cause low mechanical strength of sintered ceramic bodies, in addition to reducing shrinkage during firing.
The amount of Fe2O3 detected in the samples was between 4.7 and 7.1%. These values are acceptable for use in ceramic tiles, such as bricks and tiles, this element being responsible for the reddish color of the sintered pieces as well as being a powerful flux [20]. The high content of calcium oxide in C4 (12%) and C3 (7%) stands out, characterizing these clays as limestone [21]. C4 clay was previously studied in Alcântara [16], which reports the formation of stains on the ceramic bodies produced with this material, after sintering at 1120°C. This behavior was associated with a high content of CaO, estimated at 10%, which during the burning phase, the dissociation of CaCO3, promotes a high mass loss. C4 (13%) generates many pores, reducing water absorption and resistance of the final product. Thus, the higher the CaO content, the higher the CaCO3 content and in addition, the higher the mass loss.
Analyzing the levels of alkaline oxides, it is observed that the sample C2 has the highest concentration of K2O, while the concentration of Na2O is approximately the same in the four samples studied. Alkaline and alkaline earth compounds have a melting effect, which facilitates the formation of liquid phase and linear shrinkage during burning [13].
Table 4 was arranged according to the increasing amount of CaO present in the clays. Note that C1 and C2 have CaO content below 3%. According to Enrique [15], CaO acts as a flux until the limit of 3% in masses of ceramic coating. The percentage of alkali oxides (Na2O and K2O), also presented in Table 3, is another major factor for the densification process, due to the great tendency of liquid phase formation during burning. Considering the sum of the percentages of CaO and alkali oxides in samples C3 and C2, it can be concluded that C2 has a higher proportion of fluxing oxides, suggesting that this sample is the most promising. On the other hand, clays with a high limestone content, such as C3 and C4, tend to have greater porosity and less mechanical resistance after firing. Additionally, these two raw materials have lower alkaline oxide ratios than those observed for C3 and C2.
Clay | CaO (%) | Na2O + K2O (%) |
---|---|---|
C1 | 0.9 | 4.4 |
C2 | 2.1 | 5.1 |
C3 | 7.2 | 3.7 |
C4 | 12.7 | 3.9 |
The X-ray diffraction patterns of the clays are shown in Figure 7 and correlate positively with the results observed by X-ray fluorescence. The X-ray diffractometry (XRD) technique was used to determine the crystalline phases. The samples were dried in an oven at 110 °C for 24 h, ground, and passed through a 150-μm mesh sieve. The diffraction patterns were obtained in a Rigaku D-MAX 100 equipment, using Cu Kα1 radiation (λ = 1.5418 Å). All measurements were carried out in the continuous scanning mode with speed of 1°/min, in the range of 5 to 65° and in the range of 2 to 15° in samples saturated with ethylene glycol for 1 h to identify montmorillonite by displacing the diffraction peaks at smaller angles compared to dry sample testing. The crystalline phases were identified through Match! (Phase Identification by Powder Diffraction) in the demo version, according to the ICSD (Inorganic Crystal Structure Database).
X-ray diffraction patterns of the clays [19].
The main phases identified were quartz, kaolinite, muscovite, montmorillonite, calcite, feldspar, and hematite. Minerals from kaolinite and montmorillonite clay were identified in all analyzed clays. According to Celik [20], these clay minerals provide the necessary plasticity to guarantee conformation through the pressing process. The percentage of each crystalline phase present in the samples was estimated from the relative intensity of the main peaks in each phase. The values are shown in Table 5. The percentage of carbonates increases from 0.9% in C1 to 12.4% in C4.
Minerals (%) | C1 | C2 | C3 | C4 |
---|---|---|---|---|
Quartz | 55.7 | 51.8 | 65.1 | 57.1 |
Kaolinite | 6.3 | 10.7 | 7.4 | 5.5 |
Muscovite | 11.8 | 14.0 | 11.2 | 12.1 |
Montmorillonite | 5.6 | 4.9 | 4.6 | 6.7 |
Calcite | 8.6 | 2.8 | 1.1 | 13.7 |
Feldspar | 6.3 | 9.9 | 6.2 | 3.2 |
Hematite | 5.7 | 5.9 | 4.4 | 1.7 |
Mineralogical compositions of clays determined by XRD.
To verify the dimensional changes of expansion and thermal retraction of the samples, dilatometry tests were performed on a Netzsch dilatometer, model DIL 402PC, under synthetic air flow at 130 ml/min. For these analyses, the samples were compacted in a cylindrical shape, 12.0 mm in length and 6.0 mm in diameter. Under a constant heating rate of 10°C/min, the length of the compacted body is measured as a function of time and temperature, which varied from room temperature to 1150°C.
In Figure 8 we can observe a slight expansion in all curves up to approximately 850°C, and at 573°C, the expansion was more pronounced due to the transformation of α quartz to β [22, 23], except for C2, which presents a lower percentage of free quartz. From 573°C, there was a gradual reduction in the expansion rate, occurring or starting with sintering, followed by an exponential retraction [22].
Dilatometric curves of clays at a heating rate of 10°C/min [19].
The results shown in Table 5 with the percentages of CaO, Na2O, and K2O recommended by XRF measurements point out that sample C2 has a greater amount of funds (calcium carbonate up to a limit of 3% and alkaline oxides), or what is known as a greater linear shrinkage. Despite its advantages over the other samples, the C2 clay underwent deformation during firing up to 1150°C. This effect, known as pyroplastic deformation, may be due to the large proportion of funds in the sample, a high content of Fe2O3, and, even, the amount of organic matter [24]. One of the ways to control deformation during firing is to adjust the thermal cycle through the dilatometric curves, so that the plate remains within the required standards [25].
Clays containing limestone when subjected to burning, CaCO3 after heating, in the temperature range between 850 and 920°C, form CaO and release CO2. An intense endothermic peak of approximately 35–44% of the mass loss can be observed in differential thermal analysis. In ternary diagrams, it is observed that there is a eutectic point (above 1170°C), which reduces the dimensional stability in ceramic products, which can melt quickly (Figure 9).
Ternary diagram of CaO, SiO2, and Al2O3.
Clays when mixed with limestone can behave differently, as shown by Sánchez [25]. Figure 10 shows a standard clay with 5 and 10% of incorporated limestone. It was observed that as the limestone and temperature increase, respectively, the dimensional instability increases. In other words, the retraction increases constantly, when it undergoes an exponential increase, reaching the melting point.
Ceramic coating mass with incorporated calcite waste.
This phenomenon can be explained as follows: when exhibiting CaO up to the limit of 3%, this, associated with SiO2 and Al2O3 present in clays and feldspars, helps in the formation of eutectic systems at 1170°C, with consequent formation of liquid phase and contributing to obtain the desired mechanical strength and porosity. When introduced in percentages above 4%, CaCO3 levels are increased, and the composition moves from the eutectic line, forming crystalline phases such as CaSiO3 (pseudo-wollastonite) and 2CaO⋅Al2O3⋅SiO2 (gehlenite). So, a larger number of pores is left by the eliminated CO2. In this way, the porosity of the final product is increased, as shown in Figure 11. In Figure 12 is shown a photo of a clay mass with 10% calibration in which the porosity exerted can be observed.
Firing curve of a calcite clay.
Scanning electron microscopy of a ceramic with 10% of CaO.
Limestone is a contaminant for clay that above 125 μm can cause expansion and consequently cracks.
Rapid tests that mix clay with HCl can promote effervescence due to the release of CO2 and contribute to decrease the amount of limestone.
In the ceramic industry, wet grinding of components is carried out in ball mills and grinding will be more efficient if the sieves are 150 to 325 μm. In ceramic mass formulations, the amount of CaO up to 3% contributes to the formation of the vitreous phase, however, between 8 and 14%, it favors the formation of crystalline phases, reducing the absorption of water and increasing the mechanical resistance.
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