CE room wheat trial treatments.
\r\n\tto cover major health conditions that may benefit from Tai Chi, including neurodegenerative diseases, cardiopulmonary rehabilitation, psychosocial benefits, chronic fatigue and fibromyalgias, osteoporosis ad bone metabolism, and other chronic degenerative conditions that plague modern health. We seek to include reviews of underlying basic science as well as clinical trial data that demonstrate that multiplicity of benefits of this ancient exercise form to advance evidence-based understanding of Tai Chi exercise as an adjunct treatment.
",isbn:null,printIsbn:"979-953-307-X-X",pdfIsbn:null,doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!1,hash:"4d83cf3e19d5ba6dea45cba1386b5f27",bookSignature:"Dr. Wei-Zen Sun and Dr. Raymond Chang",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/10125.jpg",keywords:"fibromyalgia, pain, balance, falling, cognition, dementia, Osteoporosis, Osteopenia, chronic obstructive pulmonary disease, pulmonary rehabilitation, Tai Chi, Depression",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:null,numberOfDimensionsCitations:null,numberOfTotalCitations:null,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"August 29th 2019",dateEndSecondStepPublish:"December 31st 2019",dateEndThirdStepPublish:"May 30th 2020",dateEndFourthStepPublish:"July 31st 2020",dateEndFifthStepPublish:"November 30th 2020",remainingDaysToSecondStep:"a year",secondStepPassed:!0,currentStepOfPublishingProcess:5,editedByType:null,kuFlag:!1,biosketch:null,coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"310791",title:"Dr.",name:"Wei-Zen",middleName:null,surname:"Sun",slug:"wei-zen-sun",fullName:"Wei-Zen Sun",profilePictureURL:"https://mts.intechopen.com/storage/users/310791/images/system/310791.jpg",biography:null,institutionString:"National Taiwan University",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"0",totalChapterViews:"0",totalEditedBooks:"0",institution:null}],coeditorOne:{id:"310792",title:"Dr.",name:"Raymond",middleName:null,surname:"Chang",slug:"raymond-chang",fullName:"Raymond Chang",profilePictureURL:"https://mts.intechopen.com/storage/users/310792/images/system/310792.jpg",biography:null,institutionString:"Institute of East West Medicine",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"0",totalChapterViews:"0",totalEditedBooks:"0",institution:null},coeditorTwo:null,coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"16",title:"Medicine",slug:"medicine"}],chapters:null,productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"},personalPublishingAssistant:{id:"177731",firstName:"Dajana",lastName:"Pemac",middleName:null,title:"Ms.",imageUrl:"https://mts.intechopen.com/storage/users/177731/images/4726_n.jpg",email:"dajana@intechopen.com",biography:"As a Commissioning Editor at IntechOpen, I work closely with our collaborators in the selection of book topics for the yearly publishing plan and in preparing new book catalogues for each season. 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Soybeans have a myriad of health benefits for humans including their ability to stimulate metabolism, promote heart health and osteotropic activity, protect against cancer, prevent birth defects, aid digestion, increase circulation and decrease the risk of diabetes [2], but in this chapter we focus on the use of soybean oil (SBO) in agriculture to improve plant health.
Soybean oil is a vegetable oil that is solvent-extracted from pressed seeds of soybean, followed by refinement, blending and optional hydrogenation, and is one of the world’s most widely consumed edible plant oils [3, 4]. While plant-derived oils, such as SBO, are predominantly used in agriculture as an adjuvant to aid the spread of pesticides over plant surfaces and also to help the pesticide to stick to the plant surface [5, 6], SBO is also directly antimicrobial against a range of powdery mildew fungi [7, 8, 9, 10], Botrytis cinerea [11] and bacteria such as Staphylococcus aureus and Escherichia coli [12]. In addition, SBO has insecticidal activity against mites [13], whitefly and aphids [14, 15] and insects associated with stored grain products [16] . However, there are few commercial products in horticulture that use plant oils as the active ingredient (the most notable exception being neem oil), with most spray oils comprising mineral oils that are refined from petroleum. Commercial development of SBO as a pesticide offers the advantages of reduced reliance on petroleum products, and the use of an edible oil is considered to be less toxic to human health and the environment. However, fats and oils are often associated with chlorosis and necrosis of plant tissue [13, 17, 18, 19], and other problems include inconsistent activity, handling and application difficulties, spoilage and development of unpleasant odours, and these issues need to be considered when developing a SBO fungicide.
Powdery mildew (PM) disease is characterised by fluffy white lesions on the surfaces of aerial plant tissues. It is caused by pathogens from the Erysiphales order and is responsible for significant yield losses globally in crops such as cucurbits, apples, roses, tomatoes, grapes and various cereals such as wheat and barley [20, 21]. PM is one of the most economically damaging plant diseases around the world. For instance, losses to barley PM in the State of Western Australia have been estimated at $30 million (AUD) annually [22]; losses account for approximately 15% of total crop revenue for American North Western hop growers, which equated to over $30 million USD in the year 2000 [23]; and the introduction of PM-resistant grape varieties into the State of California alone has been estimated to yield $48 million (USD) in annual cost savings [24]. There are serious limitations with existing PM control methods, such as pathogen resistance to demethylation inhibitor fungicides [25, 26]. Moreover, synthetic pesticide use has been clearly linked to human health concerns such as increased incidence of respiratory disease and cancer [27]. There are also limitations on the use of sulphur and copper-based fungicides, considered to be more natural fungicides, in organic systems because sulphur can act as a nose and eye irritant [28] and because heavy metals like copper accumulate in soils with intensive copper fungicide use over time, resulting in phytotoxicity [29]. These issues are driving the development of biofungicides (fungicides comprising biological control agents and/or natural products) that are suitable for both organic and conventional growers, considered safer in terms of human health and which provide an environmentally benign option for durable disease control. Furthermore, PM strains mutate and develop resistance rapidly to synthetic pesticides, but there are few documented instances of resistance development to oils [30, 31]. Biofungicides can be used as standalone products, or in integrated disease control programmes that combine treatments with multiple modes of action, to reduce the application number of traditional synthetic pesticides and to delay the onset of resistance.
The principal aim of this study was to investigate the potential of SBO as a biofungicide to control powdery mildew. To achieve this aim, SBO effects on disease control efficacy and plant health and yield were compared under regulated conditions found in a controlled environment room and a glasshouse versus the more variable conditions in a field situation. SBO performance was also compared versus conventional fungicides and another lipid biofungicide-emulsified anhydrous milk fat (AMF) from cows’ milk, since SBO and AMF were the two top candidates from a preliminary study investigating lipid biofungicide action against PM [32]. Product mode of action (MoA) was also investigated using scanning electron microscopy (SEM), because knowledge of the MoA permits a product to be used more effectively in relation to timing and mode of application, and helps to manage the risk of target organisms developing resistance to the control product [33, 34]. MoA is also often necessary for product registration. Wheat (Triticum aestivum) was chosen as the ideal crop for this study because it is a global food staple for which PM is a common disease problem [35, 36] and because wheat plants can be easily and quickly grown. Given that the leaf surface of wheat is non-hairy and robust, it is also more likely to produce clear images in SEM following sample preparation by cold stage freezing and sputter coating with gold.
Findings obtained from the data are discussed with respect to the commercialisation potential of SBO biofungicide.
PM-susceptible ‘Endeavour’ wheat plants, were sown at a density of four plants per 12 cm diam. pot. Plants were maintained in two blocks (1 pot/treatment/block) in a CE room at 20°C with a 16-hour photoperiod. After 1 week, the experimental plants were artificially inoculated by taking potted wheat plants infected with Blumeria graminis f. sp. tritici (formerly classified as Erysiphe graminis f. sp. tritici) (wheat PM), and trailing the infected leaves from these plants across the leaf surfaces of the healthy plants, such that spores from lesions on the infected leaves would brush off onto the healthy wheat plants. Treatment application (Table 1) commenced when the plants were 2 weeks old and at plant growth stage (PGS) 1, as defined by [37]. Leaves were sprayed to run-off (i.e., the point where the leaf is completely saturated and liquid starts to drip off the leaf) using a hand-held spray bottle (500 mL Garden Trigger Sprayer, Hills, Australia), with a total of 9 spray applications applied over a course of 7 weeks (2 sprays/week for the first fortnight, and 1 spray/week thereafter).
Treatment | Treatment code |
---|---|
Unsprayed control—no fungicides | Unsprayed |
Water control | Water |
Amistar® WG fungicide1 (0.4 g/L) | Amistar |
AMF2 (7 g/L) + DATEM3 (5 g/L) + Grindox4 122™ (1 g/L) | AMF |
Soybean oil5 (20 g/L) + DATEM (5 g/L) + Grindox 122™ (1 g/L) | SBO |
CE room wheat trial treatments.
Amistar® WG fungicide, containing 250 g/L azoxystrobin active ingredient, was supplied by Syngenta, Basel, Switzerland, and is effective against both powdery mildew and rust pathogens.
AMF = anhydrous milk fat—a highly saturated solid milk fat, obtained from New Zealand Milk Products Ltd. (now trading as Fonterra).
DATEM = an emulsifier containing diacetyl tartaric acid esters of mono- and di-glycerides. Sold by Danisco Ltd., Brabrand, Denmark as: Panodan® AL 10.
Grindox 122™ = an antioxidant produced by Danisco Ltd., Brabrand, Denmark.
Soybean oil (Amco brand) was obtained from the supermarket.
The first disease assessment (designated time 0) was made immediately before the first treatment application, followed by an assessment after 7 weeks (PGS = 8–10). Disease severity on the three most basal leaves of each plant was assessed using percent leaf area infection diagrams (Figure 1), and the rating scale shown in Table 2. Disease ratings for the three leaves were averaged to give one value per plant. Disease assessments had to be made on different leaves on each assessment date, because as the plants mature, the most basal leaves wither and die, so data from each assessment date were analysed separately by SAS, version 8.02 (SAS Institute, Cary, NC), using a nested design, with treatments nested within pots and plants within treatments and pots.
Standard disease area diagrams to show four severities of wheat powdery mildew infection, from [37].
Rating | Percent leaf area infected |
---|---|
0 | No infection |
1 | 1% infection |
1.5 | 1–5% infection |
2 | 5% infection |
2.5 | 5–25% infection |
3 | 25% infection |
3.5 | 25–50% infection |
4 | 50% infection |
4.5 | >50% infection |
Wheat powdery mildew (PM) leaf disease rating scale, from James [37].
At time 0, there were no consistent treatment differences evident (Figure 2), but after 7 weeks, “Amistar”, “AMF” and “SBO” all provided significantly greater control of PM than “Unsprayed” and “Water” treated controls (Figure 3), and the amount of disease on plants treated with “AMF”, “SBO” and “Amistar” was lower than that recorded at time 0, i.e. before any treatment application (Figure 2 vs. Figure 3).
PM disease severity on the basal leaves of ‘Endeavour’ wheat plants from the controlled environment (CE) wheat trial at time = 0, i.e. prior to any treatment application. Treatment codes are given in Table 1. The least significant difference (LSD) bar applies to within-column comparisons only, owing to the hierarchical nature of the nested design, where the number of replicate plants (n) for each data point on the graph = 4.
PM disease severity on the basal leaves of ‘Endeavour’ wheat plants from the CE trial at time = 7 weeks, i.e. after 7 weeks of treatment application. Treatments are described fully in Table 1 and comprised leaving the plants unsprayed, or spraying with water, Amistar® fungicide or emulsified anhydrous milk fat (AMF) or soybean oil (SBO). The LSD bar applies to within-column comparisons only, owing to the hierarchical nature of the nested design, where n for each data point on the graph = 4.
There were no visual signs of leaf damage associated with the treatments. (Figure 4).
‘Endeavour’ wheat plants in the CE room that have (A) not received any protection against PM (treatments “water” and “unsprayed”); or (B) were sprayed with “AMF”, “SBO” or “Amistar” fungicides. The fungicides provided effective control of PM, without any visual adverse effects on plant health.
Thus, under the controlled conditions of the CE room, SBO could perform as effectively as both the commercial fungicide Amistar and the AMF biofungicide, in terms of disease control and lack of adverse effects on plant health. Given that disease severity measured at the end of the experiment (after 7 weeks of treatment application) was lower than the disease severity measured at time 0 (before treatments commenced), this might suggest that all three fungicides have eradicant as well preventative activity against PM on wheat. However, this conclusion cannot be made for sure until assessments are made on whole plants throughout the course of the experiment, since different leaves were assessed at the start and the end of the CE experiment, owing to natural attrition of the oldest leaves.
For the glasshouse trial (performed during February–March in Hamilton, New Zealand), the setup was similar to the CE trial, except that wheat seeds were sown into 6.75 L black polythene planter bags (PB12, Easy Grow Ltd., New Zealand). There were four replicate bags of four plants/treatment, and one replicate bag from each treatment was randomly positioned on a separate table (block). Treatments were the same as in the CE trial, except for omission of the unsprayed control. A total of seven spray applications were made throughout the course of the experiment (1 spray for the first fortnight, and 1 spray/week thereafter). Treatment application commenced when the plants were 11 days old and at plant growth stage (PGS) 1, as defined by [37].
Disease severity on the three most basal leaves/plant was assessed as described in the CE trial, with the initial disease assessment (designated Time 0) made immediately before the first treatment application, followed by an assessment after 7 weeks (PGS = 9–10.3). At the end of the trial, plants were considerably larger than those in the CE trial, so an additional disease assessment was also made at week 7 on the whole plant rather than the three most basal leaves, using the scale defined in [38], as shown in Figure 5 and Table 3. Experimental design and statistical analysis was the same as for the CE trial.
PM disease severity on whole wheat plants, from [38] .
Numeric scale | Characteristics |
---|---|
0 | Free from infection. |
1 | Very resistant. Few isolated lesions on lowest leaves only. |
2 | Resistant. Scattered lesion on 2nd set of leaves, with first leaves infected at light intensity. |
3 | Moderately resistant. Light infection of lower third of plant. |
4 | Low intermediate. Moderate to severe infection of lower leaves, with scattered to light infection extending to the leaf immediately below the mid-point of the plant. |
5 | Intermediate. Severe infection of lower leaves, with moderate to light infection extending to the mid-point of the plant, but not beyond. |
6 | High intermediate. Severe infection of the lower third of the plant, moderate degree on middle leaves, and scattered lesions beyond the mid-point of the plant. |
7 | Moderately susceptible. Lesions severe on the lower and middle leaves, with infections extending to the leaf below the flag leaf, or with trace infections on the flag leaf. |
8 | Susceptible. Lesions severe on lower and middle leaves. Moderate to severe infection of upper third of plant. Flag leaf infected in amounts more than a trace. |
9 | Very susceptible. Severe infection on all leaves, and the spike infected to some degree. |
Scale for appraising foliar intensity of wheat diseases on whole plants, from Saari & Prescott [38].
Only data from the first (time = 0) and last (time = 7 weeks) disease assessments are presented. At time 0, disease levels in block 1 were significantly higher in the “Water” control than all other treatments, but this trend was not repeated in other blocks, and overall there were no consistent treatment differences evident at the start of the experiment (Figure 6). After 7 weeks, “Amistar”, “AMF” and “SBO” all provided significantly greater control of PM than “Water” treated controls, regardless of whether disease severity was measured on the three most basal leaves (Figure 7), or the whole plant (Figure 8). All three fungicides performed as well as each other. In all blocks, the amount of disease on whole plants treated with “AMF”, “SBO” and “Amistar” was lower than that recorded at the start of the experiment, i.e. before any treatment application (Figure 7 c.f. Figure 8). This suggests that eradicant activity may be possible, under low initial inoculum loads (at the start of this experiment, there was <1% leaf infection) and corroborates the results found in the CE trial. However, the glasshouse environment is still relatively controlled and the plants are more widely spaced than in a field experiment, so field testing was the next step in the research.
Average PM disease severity on the basal leaves of ‘Endeavour’ wheat plants in the glasshouse trial at time = 0, i.e. prior to any treatment application. Treatment codes are given in Table 1. The LSD bar applies to within-column comparisons only, owing to the hierarchical nature of the nested design, n for each data point on the graph = 4.
Average PM disease severity on the basal leaves of ‘Endeavour’ wheat plants in the glasshouse trial at time = 7 weeks, i.e. after 7 weeks of treatment application. Treatment codes are given in Table 1. The LSD bar applies to within-column comparisons only, owing to the hierarchical nature of the nested design, n for each data point on the graph = 4.
Whole plant assessments of PM disease severity on ‘Endeavour’ wheat plants in the glasshouse trial at time = 7 weeks, i.e. after 7 weeks of treatment application. Treatment codes are given in Table 1. The LSD bar applies to within-column comparisons only, owing to the hierarchical nested design, n for each data point on the graph = 4.
Three spring wheat cultivars were used in this trial: ‘Janz’, an Australian cultivar highly susceptible to PM and resistant to brown leaf rust but susceptible to stripe rust; ‘Karamu’, a New Zealand cultivar that is susceptible to PM and leaf rust but resistant to stripe rust; and ‘Gundaroi’, a durum wheat cultivar that is susceptible to PM, but resistant to both rusts.
The three wheat cultivars were sown in separate adjacent areas in early September (spring) in Christchurch, New Zealand. Each cultivar was grown in two strips 24 m long and 1 m wide. Each strip was divided into 20 plots (1.2 m long × 1 m wide) and each plot contained approximately 150 plants. Adjacent, or nearly adjacent plots were randomly assigned to each of the five treatments to make a block and this procedure was repeated to give five blocks (25 plots), spread along the two strips, with block 3 split across both strips. The remaining 15 plots were untreated (buffers). Within each treatment plot five plants were labelled with block and treatment number. These labelled plants were used for repeat disease assessments over the trial period, with data analysed separately for each cultivar as a repeated measures design using SAS version 8.02 (SAS Institute, Cary, NC).
The five treatments were identical to those used in the CE trial, except that Amistar® fungicide was applied at the recommended field rate of 750 mL/ha and 1.4 mL of fungicide liquid concentrate /12 L water. During the growing season, there were five applications applied to designated treatment plots, sprayed to run-off using 20 L backpack pressure spray units (Backpack 435, Solo, New Zealand), of the water and biofungicide treatments (on average 17 days apart), and two applications of Amistar fungicide (7 weeks apart, according to manufacturer recommendations). After treatment application, plants were left to dry for several hours before disease assessments were carried out. At each assessment, the growth stage of each wheat cultivar was noted, as defined by James [37] . The five labelled plants in each plot were assessed according to a PM rating system from 0 to 9 (Figure 5 and Table 3). The same rating system was used for a rust assessment on ‘Janz’, 123 days after sowing.
Plants were left in the field for 6½ weeks after the last spray until harvest in late February (summer). The trial was harvested with a rice binder (Model 210B, Mitsubishi, Japan) and each treatment/block rep was processed through a thresher (Nursery Master Stationary Thresher, Wintersteiger, Austria) to separate the wheat grain from the chaff and straw. The grain was placed into paper bags, which were taken back to the field lab and weighed. The following day, each bag was sorted through a 2 mm sieve screen (Endecott, United Kingdom) that separated grain into two lots: seconds (<2 mm) and first grade (>2 mm). The 1000 seed weights were measured on a machine (Numigral II, Tripette & Renaud, France) that automatically counts 250 seeds, which were weighed and then the weight was multiplied by four. Harvest data was analysed as a nested design (with blocks and treatments nested within cultivar) using SAS version 8.02.
For all three wheat cultivars, SBO was the most effective fungicide against PM, and provided significantly greater protection than the commercial synthetic fungicide, Amistar, during the middle part of the season, i.e. 90–120 days from sowing (Figure 9). The total degree of PM control was not as great as that observed in the CE and glasshouse trial, most likely because the close proximity of plants in the field trial resulted in overlapping growth leading to ineffective spray penetration and possible build-up of inoculum in protected parts of the canopy. The increase in disease was most marked in the final two disease assessments and under these heavy inoculum loads, Amistar was completely ineffective in the most PM-susceptible cultivar ‘Janz’ (Figure 9). No evidence of eradicant activity was observed for any of the products under the heavy inoculum loads and more variable conditions of the field trial.
Powdery mildew disease ratings in three field-grown wheat cultivars following application with Amistar® WG fungicide (750 mL product concentrate/ha at and 1.4 mL of fungicide liquid concentrate/12 L water), emulsified anhydrous milk fat (AMF) at 7 g/L and emulsified soybean oil (SBO) at 20 g/L. control treatments involved spraying the plants with water or leaving them unsprayed. Data were assessed as a repeated measures design with the bars indicating the least significance difference at each assessment date.
Rust was only present in the ‘Janz’ cultivar, and SBO (and AMF) do not appear to provide control of this pathogen (Figure 10). Amistar claims to control rust, but there were no significant differences among the treatments (Figure 10).
Stripe rust levels in field-grown ‘Janz’ wheat, 123 days after sowing. Treatments are the same as described in Figure 9. Data were assessed as a randomised block design with means separation by least significant difference (LSD, P < 0.05).
Irrespective of wheat cultivar, SBO was associated with significantly lower harvest yields than all other treatments (Table 4). Yields in the AMF treatment were lower but not significantly different from the controls and plants sprayed with Amistar had significantly higher yields than both the other treatments (Table 4). This suggests that there is a yield cost associated with SBO and AMF use in the field trial. There are two possible explanations for this. The first is that oil use can be associated with damage to plant tissue, which affects the ability to produce and store photosynthates [13, 17, 18, 19]. However, we did not observe any chlorosis or necrosis associated with SBO or AMF use in any of our trials on wheat. More likely is the second explanation that disease severity has escalated to a greater degree in the plants treated with lipid fungicide than in the Amistar treatment in the 6 1/2 week interval between the final spray application and harvest. Work in other crops (cucurbits and grapes) has shown that SBO and AMF need to be applied at fortnightly intervals to maintain effective disease control (Wurms, Plant & Food Research, unpublished data), whereas Amistar is a systemic fungicide (i.e., it is absorbed into the plant) and provides disease control over a more sustained period, and therefore only needed to be applied twice during the same trial period to provide effective control of PM [39] .
Cultivar | Treatment1 | Total grain weight (g) | First grade weight2 (g) | Weight 1000 grains (g) |
---|---|---|---|---|
‘Janz’ | Unsprayed | 616 | 599 | 44.5 |
Water | 658 | 641 | 45.1 | |
Amistar | 672 | 656 | 46.6 | |
AMF | 592 | 575 | 42.6 | |
SBO | 481 | 463 | 38.4 | |
LSD3 | 69.4 | 67.2 | 2.15 | |
‘Karamu’ | Unsprayed | 619 | 578 | 37.5 |
Water | 609 | 569 | 36.7 | |
Amistar | 840 | 797 | 42.9 | |
AMF | 605 | 570 | 37.2 | |
SBO | 526 | 479 | 33.0 | |
LSD | 49.3 | 50 | 1.62 | |
‘Gundaroi’ | Unsprayed | 619 | 578 | 37.5 |
Water | 609 | 569 | 36.7 | |
Amistar | 840 | 797 | 42.9 | |
AMF | 605 | 570 | 37.2 | |
SBO | 526 | 479 | 33.0 | |
LSD | 49.3 | 50 | 1.62 |
Yield data of field-grown wheat: Total grain weight (g), first grade grain weight (g) and weight of 1000 grains (g), harvested approximately 170 days after sowing.
Control plants were left untreated or sprayed with water. Fungicide treated plants were sprayed with Amistar® fungicide (750 mL product concentrate/ha and 1.4 mL of fungicide liquid concentrate/12 L water), emulsified anhydrous milk fat (AMF) at 7 g/L and emulsified soybean oil (SBO) at 20 g/L.
First grade grain has a size >2 mm.
Least significant difference (P < 0.05).
Experimental set-up was the same as for the CE trial, except that there was no water treatment, and there were two spray applications, 3 days apart. Four days after the second spray, lesions from all the treatments were sampled for electron microscopy.
Leaf pieces (5 × 10 mm) were cut from plants and mounted on a copper specimen stub, then processed for observation using a sputter cryo system (Emscope SP2000, Hemel Hempstead, United Kingdom). Mounted samples were first frozen using liquid nitrogen slush and then transferred under vacuum to a preparation chamber. There they were thermally etched for 5 min at −80°C, radiantly etched for 30–60 s, and then sputter coated with gold. The coated material was transferred under vacuum to a cold stage in the specimen chamber of a Philips SEM 505 scanning electron microscope (Philips, Eindhoven, Netherlands) and examined at an accelerating voltage of 15 kV and a specimen temperature of between −150 and −180°C [40].
Amistar®, SBO and AMF fungicides all exhibited eradicant activity via a non-toxic (physical) MoA, as illustrated by direct effects on the fungus, since these treatments caused conidiophores (spore bearing structures) to collapse (Figure 11), conidia (asexual spores) to wither (Figure 12) and extrude cellular contents (Figures 12 and 13) and hyphae to wither/desiccate (Figure 13). This is supported by the CE and glasshouse trial data which showed that, under low initial inoculum loads, disease severity decreased on the same wheat plants monitored over time (Figures 2, 3,6–8). The MoA of SBO is most likely created by disruption of membrane transport of the pathogen since the SEM images indicate that SBO causes plasmolysis of mycelia and cell rupture and leakage of cell contents, especially in conidia (Figures 11–13). This is in agreement with a review on the antimicrobial mode of action of essential plant oils, where antimicrobial action was most commonly due to membrane permeabilization/disruption leading to loss of water, leakage of cell contents and sometimes total lysis [41] . In contrast, AMF may have a different MoA to SBO, as SEM demonstrated that AMF caused deep ridging and distortion of conidia, rather than extrusion of cell contents (Figures 11–13). Combination of products with different complimentary MoA has the potential to increase product durability and efficacy, since it is more difficult for the pathogen to develop resistance. In addition, pathogens do not tend to develop resistance to agricultural sprays containing oils [30, 31, 42], because membrane transport is such a fundamental life process. The combination of reduced amounts of SBO and AMF has been shown to be as effective as greater concentrations of each biofungicide on its own [10]. Non-toxic (physical) rather than toxic (chemical/antibiotic) MoAs are also advantageous when it comes to product registration, since the latter higher-risk product group requires expensive and time consuming toxicology testing.
SEM images of powdery mildew colonies on ‘Endeavour’ wheat leaves that were either A, untreated; or sprayed with: B, Amistar® fungicide; C, anhydrous milk fat (AMF); or D, soybean oil (SBO). In healthy, unsprayed colonies (A), turgid hyphal threads can be seen growing along the leaf surface in among pointy/tapered trichomes (leaf hairs), an example of which is arrowed in A, and upright conidiophores bearing chains of spherical conidia (asexual spores) are visible extending upwards and outwards from the leaf surface. Conversely, hyphae appear shrivelled and conidiophores have completely collapsed in sprayed colonies (B-D).
Higher magnification SEM images of powdery mildew conidia on ‘Endeavour’ wheat leaves that were either A, untreated; or sprayed with: B, Amistar® fungicide; C, AMF; or D, SBO. In unsprayed plants (A), the conidia are present in chains attached to conidiophores that protrude outwards from the leaf surface. Unsprayed conidia have a plump/turgid appearance and the spore surface appears to be quite smooth. In contrast, conidia on sprayed plants are lying collapsed on the leaf surface and have a withered/dehydrated appearance (B-D). Ridging of the conidial surface is apparent in AMF-treated plants (C), and grainy exudates, most probably cell contents, surround conidia sprayed with fungicide (B) and soybean oil (D).
SEM close-ups of powdery mildew hyphae on ‘Endeavour’ wheat leaves that were either A, untreated; or sprayed with: B, Amistar® fungicide; C, AMF; or D, SBO. In unsprayed plants (A), the hyphae growing on the leaf surface are plump and turgid. A trichome is arrowed in A. By contrast, hyphae on sprayed plants are completely withered/dehydrated (B-D). A plant stomate (pore for gaseous exchange) on the leaf surface is arrowed in C.
SBO biofungicide shows great commercial promise, given that it provided PM control on wheat in both controlled internal conditions and more variable field environments (at least for part of the growing period) that equalled or exceeded that provided by conventional fungicides. Moreover, SBO is cost effective and simple to produce (data not presented), has a physical mode of action (thus making registration easier) and contains Generally Recognised As Safe (GRAS) [43], edible ingredients. However, there are critical factors that must be taken into consideration to ensure optimal performance and success of this product.
The most important consideration for use of this type of fungicide is that it has a direct, non-systemic mode of action [44] and therefore requires direct contact with the plant surface that it is to protect. This explains why disease control was much higher in the CE and glasshouse trials, where plants were more widely spaced, and why PM pustules were observed on the undersides of leaf blades close to the stems of plants in the field trial (data not presented), because heavily overlapping foliage prevented spray access. Our research has also shown that the percentage of grape bunch surfaces directly exposed to spray (i.e., not covered by leaves), as determined by leaf plucking, was a significant factor in the efficacy of SBO fungicide against Botrytis cinerea [11]. Consequently spray penetration and the density of plant architecture/growing systems are key considerations to the success of this fungicide.
We believe that other disadvantages that may be associated with SBO can be managed with careful use. Although phytotoxicity is sometimes associated with oils, optimisation of formulation (as well as rate and frequency of application) has been shown to minimise toxic effects [11, 45]. Our SBO formulation [46] has managed to achieve the balance of efficacy without adverse effects on plant health. Phytotoxicity can also be avoided by taking care not to tank mix products such as elicitors [32] or sulphur [44, 47] as these may react together to form plant damaging compounds causing foliar injury and leaf drop. However, these products can still be successfully used together in an integrated spray programme provided that their use is alternated [11]. SBO has also been demonstrated to have a much less adverse effect on plant health than AMF [32]. Another effective option is that SBO can be tank mixed with AMF at much lower concentrations than either product on its own [10]. This offers the dual advantages of reduced cost of goods and greater durability, due to differing modes of action as described in the preceding SEM section. Other recommendations include not spraying below 4°C (40°F), because the emulsion breaks down, and avoiding sprays on newly emerged foliage or floral tissue, although we have treated rose blooms without any toxic effects [10].
Although SBO exhibited both preventative and eradicant activity in this study, eradicant activity was not effective against heavy, established inoculum loads in the field trial, and consequently SBO is best used as a preventative. Given that horticultural oils degrade readily and are not very persistent [31], they also need to be applied at regular (e.g. fortnightly) intervals. A lack of PM control over the last 6 weeks between spraying and harvest could be the reason for loss of yield in the wheat field trial, although further work would need to be carried out to confirm this by carrying out a PM disease assessment at harvest. SBO is particularly well-suited for use in an integrated pest management (IPM) programme. In New Zealand, our SBO formulation has been registered as MIDI-Zen® by BotryZen 2010 Limited, and is intended to be used a part of a residue-free IPM programme for control of Botrytis cinerea on grapes. Although use of MIDI-Zen right up to vintage in grapes has been shown to delay the increase in soluble sugars (°Brix), which would necessitate delaying harvest for 1–2 weeks to allow Brix to rise, this problem is normally avoided by using MIDI-Zen in the middle part of the grape growing season (from pre-bunch closure to version) and another biofungicide in the final 3 weeks leading up to harvest [11].
In summary, the potential for SBO is very exciting as it offers the potential for effective, environmentally benign and durable control. Armed with a good formulation and an understanding of how best to optimise its use and minimise any adverse effects, we should see increased use of SBO in agriculture to improve plant health.
Special thanks to Nicole Shukker, former employee of NZ Milk Products Ltd. (now Fonterra), to Lisa Marcroft, former business manager (BM) at HortResearch, and to Claire Hall (current BM at Plant & Food Research Ltd) for their drive and enthusiasm for this project. We are very grateful to Dr. Siva Ganesh for guidance with statistics and use of SAS software, and to Mike Spiers and Dr. Philip Elmer for reviewing this manuscript. This research was funded by the Pre-Seed Accelerator Fund, New Zealand.
Titanium was discovered in 1791, but it came into effective application only in the 1950s. After 115 years, i.e., in the year 1906, M. A Hunter at General Electric Company prepared pure titanium for the first time [1]. Since 1950s, titanium holds a prime position in aerospace, biomedical, automotive, and chemical processing industries due to unique features listed below:
Low density (60% of steel or super alloy’s density),
Higher tensile strength (Higher than ferritic stainless steel and comparable to martensitic stainless steel and Fe- base superalloys)
Higher operating temperature (Up to 595°C for commercially available alloys and >595°C for titanium aluminides)
Excellent corrosion resistance (Higher than stainless steel and biocompatible)
Forgeability
Castability (Mostly by investment casting)
Despite being the fourth-most abundant structural metal available in the earth crust, its commercial exploitation has been low compared to steel and aluminium due to high cost of production.
\nPure Titanium has an hcp crystal structure. Due to the allotropic nature of titanium, the room temperature hcp crystal structure (alpha phase) will be transformed to bcc (beta phase) structure on heating to a particular temperature called beta transus temperature (882.5°C). Alloying elements of titanium are classified on the basis of their influence on the transus temperature. For example, if the transus temperature is increased on the addition of the certain elements, then they are called as alpha stabilisers (Al, O, N, and C); similarly there are some other elements which bring the transus temperature down and they are termed as beta stabilisers (V, Mo, Ta and Nb). The elements Sn and Zr have little or no effect on transus temperature and are termed as neutral elements.
\nBeta alloys form the metastable beta phase upon quenching rather than undergoing martensitic transformation. A schematic representation of the beta isomorphous phase diagram is shown in the Figure 1. Beta alloys can also be classified as those which have alloy which has enough beta stabilisers to avoid the martensitic start (Ms) pass through upon quenching. Beta alloys are further classified into metastable and stable beta alloys based on the content of beta stabilisers. Commercially available beta alloys are metastable beta alloys and stable beta alloys are not commercially available [2]. The metastable beta phase can precipitate the fine alpha phase upon ageing/thermal treatment. Hence, beta alloys are hardenable and can attain a higher strength level than alpha + beta alloys and higher specific strength compared to many other alloys [3].
\nBeta isomorphous phase diagram.
Corrosion resistance of beta alloys is also found to be better than that of alpha + beta alloys. Higher hydrogen tolerance makes beta alloys to perform better in the Hydrogen-rich environments [2]. Increased fracture toughness for a given strength level and amenability to room temperature forming and shaping are superior attributes compared to alpha + beta alloys [1]. Ti-13V-11Cr-3Al (B120VCA) was the first beta alloy produced/developed and used in the SR-71 (Surveillance aircraft) as a sheet product.
\nBeta alloys’ inherent characteristics such as pronounced ductility owing to the crystal structure (bcc), heat treatability, and superior cold rollability make them an effective alternative to alpha + beta alloys [4]. Furthermore, beta alloys have lower beta transus temperature than the alpha + beta alloys [5]. Hence, beta alloys are considered to be the economical choice in perspective of processing compared to the alpha + beta alloys. For example, despite the higher formulation cost, Ti-15V-3Al-3Cr-3Sn alloy’s thinner gauges (<2 mm thick) cost one-tenth of those of Ti-6Al-4V [3].
\nThe initial step is the fabrication of ingot from sponge for conversion to mill products. The melting practices to produce beta titanium alloy ingots can be broadly categorised into Vaccum Arc Remelting (VAR) and Cold Hearth Melting.
\nThe conventional method used for the melting of beta titanium alloys is the Vacuum Arc Remelting (VAR) in a consumable arc furnace. In VAR, the furnace is initially evacuated for required vacuum and a dc arc is struck between the two electrodes. Here a consumable electrode (material to be melted) is employed as the cathode and starting materials such as titanium-based metal chips or machine turnings act as the anode. The consumable electrode can be fabricated from either of the two strategies.
From the compacted sponge and/or scrap
From plasma/electron beam hearth melting
Among these methods, the first method of predensification by compacting using a hydraulic press is widely used to fabricate electrodes. Compacted electrodes with nominal alloy composition are made by the pressing of blended clean and uniform-sized titanium sponge and alloying elements devoid of any harmful inclusions. These compacts (called as briquettes) are then assembled with bulk scrap to form the first melt electrode (called as a stick) by appropriate welding methods.
\nFinally, these fabricated electrodes are placed inside a vacuum furnace. When the electric arc is established, associated heat generation will result in the dripping of molten metal down to the water-cooled copper crucible to form the ingot. Initially, a layer of solid titanium or skull will be formed on the surface of cooled copper crucible which will hold the subsequently falling molten metal. In order to ensure chemical homogeneity, the ingots will be inverted and remelting will be performed. Ingots produced during first stage melting are again used as consumable electrodes during double or triple remelting. In addition to this, electrical coils are provided in most of the VAR furnaces to generate an electromagnetic field capable of stirring the molten metal thereby further enhancing the homogeneity. Cold hearth melting is another developing technique which uses either plasma arc (PAM) or electron beam (EBM) melting furnace.
\nProper monitoring should be ensured to control the solidification of beta titanium based ingots. Specifically, beta eutectoid compositions containing Fe, Mn, Cr, Ni and Cu are associated with depressed freezing temperatures [2]. This allows for solidification over a significant temperature range, consequently leading to solute segregation during solidification of the ingot. Such type of segregation results in regions with lower beta transus and results in a microstructure distinctive from the surrounding material. These solute segregated regions are clearly visible in beta titanium alloys subjected to heat treatment below/near to beta transus and are termed as beta flecks. Beta flecks, which range from a scale of few hundred micrometres to a few millimetres, can act as crack nucleation sites leading to fatigue failure. Beta flecks are mostly developed in large diameter ingots. However, beta isomorphous alloys containing Nb, Mo and V are not associated with these depressed solidification temperatures and are less prone to solute segregation.
\nLower values of tensile ductility and low cycle fatigue life of near-β Ti alloy Ti–10V–2Fe–3Al was found to be due to the presence of beta flecks [6]. Under tensile loading, crack nucleation occurred at beta fleck grain boundaries leading to intergranular and quasi-cleavage fracture. In the case of fatigue loading, the inhomogeneous strains developed due to the presence of beta flecks accelerated the crack nucleation and early crack propagation.
\nFor an expensive material such as titanium, casting is the perfect choice in attaining a (near) net shape in the fabrication of components with complex geometry without incurring much wastage. A significant weight (35%) saving can be achieved by employing the titanium casting instead of stainless steel casting in B-777 aircraft [7]. In general, rammed graphite mould and investment casting were utilised in titanium casting. Investment casting is preferred to obtain thin sections and better surface finish [8]. Ti-5Al-5V-5Mo-3Cr castings followed by HIP (Hot Isostatic Pressing) possess a superior strength compared to hipped Ti-6Al-4V castings with almost same ductility [9]. To extend brake life of fighter aircraft (F-18 EF)Ti-15V-3Al-3Cr-3Sn castings were used instead of Ti-6Al-4V castings due to the higher specific strength of the former [10].
\nTo exploit the ductile nature of the beta phase (bcc crystal structure), even for alpha and alpha + beta alloys, ingot break down forging is done above the beta transus temperature. In general, to avoid thermal stress cracking, titanium alloys are subjected to preheating before high-temperature forging.
\nForging is performed to produce billets and bars of titanium with the optimum combination of strength and ductility [11]. Forging is performed using hydraulic presses. Both straight-forging and upset forging are performed in case of Ti alloys. For greater deformation and larger size, upset-forging is preferred [1]. Higher reactivity of the titanium demands the inert / vacuum processing to prevent surface contamination during high-temperature processing [1]. Drawing operation of titanium is prone to galling and seizing. Hence, proper lubricants have to be employed to avoid those effects [1]. Compared to all other Ti alloys, beta alloys can withstand high pressure before cracking. Ti- 13V-11Cr-3Al can withstand up to 690 MPa without cracking. In contrast, Ti-6Al-4V can withstand 585 MPa before cracking [1].
\nThe microstructure of the ingots of beta alloys varies from small equiaxed grains (at the surface) to elongated columnar grains and large equiaxed grains at the bulk/centre of the ingot [4]. Beta Ti alloys are more suitable for low temperature working without being vulnerable to rupture or cracking compared to other Ti alloys [1] and this effect is attributed to the availability of enough slip systems to accommodate the deformations.
\nSecondary forging refers to the forging process employed to obtain the final shape/components. The temperature required for this kind of forging is lower than that for ingot breakdown forging. Unlike alpha and alpha + beta alloys, beta alloys show a significant increase in strength at high strain rates [1]. Hence, higher pressures are to be applied for forging of beta alloys; the pressure required to induce crack during forging is higher for beta alloys compared to alpha and alpha + beta alloys [1]. Beta titanium alloys have a broader range of forging temperature compared to alpha/alpha + beta alloys.
\nDue to the lower beta transus temperature, beta alloys have lower hot working temperature compared to alpha and alpha + beta alloys, For example, Ti–10V–2Fe–3Al has a secondary working temperature range between 700–870°C [12]. Types of forging and features are given in the Table 1.
\nS.No. | \nForging type | \nFeatures | \n
---|---|---|
1 | \nOpen-Die Forging | \n\n
| \n
2 | \nClosed-Die Forging | \n\n
| \n
3 | \nHot-die forging | \n\n
| \n
4 | \nIsothermal Forging | \n\n
| \n
5 | \nPrecision forging | \n\n
| \n
Types of forging and its features [1].
Unlike other alloys, rolling of titanium requires higher working pressure and extreme control in temperature. Cylindrical rollers are used to produce the strips, sheet and plate. In contrast, grooved rollers are employed in producing the rounds and other structural shapes. In sheet and plate rolling process, cross rolling is done to reduce the anisotropy in mechanical properties. Texture strengthening is less pronounced in the beta alloys compared to alpha alloys [1]. The lower rate of strain hardening of the beta alloy makes it more acquiescent to cold working.
\nIn Ti-3.5Al-5Mo-6V-3Cr-2Sn-0.5Fe alloy, rolling and ageing in the sub-transus (alpha + beta field) temperature yielded a better combination of the strength and ductility compared to working in the beta field [13]. Sheet beta Ti alloys are amenable to cold rolling. Cold rolling has a strong effect upon mechanical properties. For example, Rosenberg [14] reported the effect of cold rolling on tensile strength, yield strength and ductility of Ti-15-3 alloy:
UTS (Rolled alloy) = UTS (un-rolled) + 0.75 × Percentage of reduction (%)
YS (Rolled alloy) = YS (un-rolled) + 0.65 × Percentage of reduction (%)
Ductility (Rolled alloy) = EL (un-rolled) − 0.65 × Percentage of reduction (%)
Two high roll mill and three high roll mill are commonly used for rolling titanium and its alloys.
\nMaterial processing performed with the aid of both mechanical force and thermal/ heat treatment can be termed as thermomechanical processing. The primary objective of this processing is to obtain a component in functional design with pre-determined microstructure and corresponding mechanical properties. Thermomechanical processing of beta Ti alloys can be done both above transus temperature (Super-transus processing) and below the transus temperature (Sub-transus processing). Super-transus processing with hot deformation is optimised to obtain fine recrystallised beta grains. Sub-transus processing is optimised to obtain fine beta grains with controlled alpha phase morphology [12]. Size, volume fraction, morphology, and the spatial distribution of the alpha precipitates formed during the thermomechanical processing have a vital influence over the mechanical properties of the end product.
\nIn Ti-15V-3Al-3Cr-3Sn alloy, Boyer et al. [15], showed the usefulness of thermomechanical treatment for attaining a wide range of tensile strength (from 1070 to 1610 MPa.)
\nHeat treatment is the basic metallurgical process through which optimization of hardness, tensile strength, fatigue strength and fracture toughness can be achieved. All the metastable beta alloys are heat treatable to attain higher strength than alpha + beta alloys.
\nDuplex ageing treatment yielded a superior combination of mechanical properties with no precipitation free zone and finer alpha precipitation compared to single ageing in Ti-15V-3Al-3Cr-3Sn-3Zr [16] and Ti-3Al-8V-6Cr-4Mo-4Zr [17]. The rate of heating to ageing temperature was found to have a substantial effect on the evolution of microstructure and mechanical properties [18]. Choice of solution treatment temperature is important. For example, for Ti-1Al-8V-5Fe (Ti185), solution treatment near beta transus temperature leads to a highest tensile and yield strength [19].
\nSolution treatment followed by ageing in metastable beta alloys will lead to a microstructure consisting of soft alpha in the beta grain boundaries. Hence, this softer alpha phase may lead to the decline in the HCF behaviour [20] and tensile ductility by augmenting the intergranular fracture [17]. For example, Sauer and Luetjering [21] have also reported the adverse effect of alpha phase layers along the beta grain boundaries on the tensile and fatigue behaviour of Ti-5Al-2Sn-4Zr-4Mo-2Cr-1Fe (β CEZ).
\nModifying the surface is an effective and economical way to enhance the tribological and fatigue properties of the material. Thermo-chemical and mechanical surface modification techniques are common in beta alloys.
\nIn order to enhance the surface hardness, wear resistance and near-surface strength, thermo-chemical surface processing techniques such as nitriding and carburising are employed. Among various thermo-chemical surface processing techniques, nitriding is extensively used. In this process, the nitrogen is fused into the titanium base alloy. Among the various technologies used for Nitriding, i.e., gas nitriding, laser nitriding, plasma nitriding, Ion nitriding and gas Nitriding are used widely [22]. Titanium nitrides will be formed on the surface as a result of the nitriding and these nitrides increase the surface hardness drastically and improve the tribological properties at the expense of the ductility of the material. Increased hardness due to TiN formation was made use in flap tracks of Military airplanes [23]. However, nitriding has a negative influence on the tensile strength and fatigue strength of the material.
\nMechanical surface modifications such as shot peening, ball burnishing and laser peening are developed to enhance the fatigue behaviour of the target material by inducing the residual compressive stress and work hardening effect in near surface region. Both crack nucleation and crack propagation during fatigue loading were found to be affected by the surface modification treatment. However, surface roughness will be significantly increased at the end of the mechanical surface modification such as shot peening and this may lead to early crack initiation.
\nSince 1970s, shot peening is being employed in enhancing the mechanical behaviour of Ti alloys in aerospace industries [24]. Schematic representation of shot peening is shown in the Figure 2. Shot peening of beta alloys, i.e. Ti-10V-2Fe-3Al and Ti-3Al-8V-6Cr-4Mo-4Zr yielded a marginal increase in the fatigue life compared to electro polished sample [25]. In LCB beta alloy, in order to compensate the residual compressive stress induced in the surface after peening, substantial tensile residual stress formed in the subsurface region and this deteriorated the fatigue behaviour compared to polished sample [26]. It is important to control the shot peening conditions to get the desired enhancement in fatigue life.
\nSchematic representation of shot peening.
Unlike shot peening and laser peening, roller burnishing reduces the surface roughness by stressing the surface with a roller ball with optimised pressure. Schematic representation of the roller burnishing is shown in the Figure 3. Roller burnishing of Ti-10V-2Fe-3Al beta alloy induced deeper and higher magnitude residual stress compared to shot peening. In roller burnishing of LCB beta alloy, higher the rolling pressure, deeper was the site for fatigue crack nucleation [27]. In Beta C (Ti-3Al-8V-6Cr-4Mo-4Zr) alloy, deep rolling ended up with deeper residual stress distribution compared to shot peening, but the magnitude of the residual stress remained high for the shot peened sample. A marginal increase in fatigue life was achieved through deep rolling of Beta C alloy [28].
\nSchematic representation of the ball burnishing.
Compared to shot peening, laser peening has unique features like the capability of inducing deeper and stable residual stress with extreme control in operation. Conventionally, laser peening is performed using Nd: Glass lasers after applying the coating, i.e. black paint on the target surface. To make this process simple, economical and more portable, LPwC (Laser peening without Coating) was developed in 1995 [29]. LPwC has proven to be an effective technique by inducing a relatively high compressive residual stress. For example, a residual stress of approx. −825 MPa was induced at a depth of ~75 μm from the surface in LCB (Ti-6.8Mo-4.5Fe-1.6Al) beta alloy [30].
\nIn the case of implant materials, the interaction between the biological environment and the implanted materials occurs on the biomaterial surface. Clinical success of implant materials is greatly dependent on various surface characteristics viz. chemical inertness, texture, corrosion resistance and surface energy [31] . In the case of orthopaedic implants, the surface should possess more bone forming ability and for blood contacting devices, it should not initiate any blood clot formation. Hence surface modification of biomedical grade beta titanium alloys is very significant. Oxide layer formation will occur spontaneously on the surface of titanium on exposure to air. This TiO2 film possesses a thickness of about 1.5 to 10 nm at room temperature. Chemical stability and structural characteristics of this oxide film greatly influence the biocompatibility of titanium implant materials. Some of the potential methods to enhance the properties of native TiO2 film are anodisation, sol–gel methods, acidic and alkaline treatments [32]. In addition to these, specific surface topographies and roughness induced by mechanical surface modifications (sandblasting, grit blasting, peening) have improved the clinical success of implant materials. An overview of the various surface modification techniques employed for biomedical beta titanium alloys is schematically shown in Figure 4.
\nOverview of surface modification of beta titanium alloys for biomedical application [33].
In dental applications, Laser Nitriding has proved to be an effective process in enhancing the surface hardness, the coefficient of friction and corrosion resistance of the Ti-20Nb-13Zr and wear and corrosion resistance of Ti-13Nb-13Zr biomedical-beta alloys [34, 35]. Plasma nitrided beta 21S (Ti-15Mo-3Nb-3Al-0.2Si) alloy showed higher hardness but inferior corrosion resistance compared to the untreated alloy [36]. In line with the Nitriding, carburising of Ti-13Nb-13Zr (a biomedical beta alloy used for artificial joints) improved the surface hardness and wear resistance through the formation of the titanium carbide [37].
\nAs mentioned in the introduction (Section 1), a major limiting factor for the titanium application is its high production cost. In addition to the high raw material cost, the forging, machining contribute majorly to the production cost. This limitation instigated the industries to work towards processing methods through which the near net shape (NNS) could be obtained. Despite the higher cost involved, Powder metallurgy of titanium is capable of yielding almost same or better mechanical properties compared to wrought and cast components along with accurate net shape capability. This merit is mainly attributed to the absence of texture, segregation and nonuniformity in the grain size encountered in conventional processing.
\nEven for the components made through powder metallurgy route, solution treatment followed by ageing (STA) leads to an enhancement in mechanical properties such as tensile strength and yield strength compared to the as-sintered condition [38]. Ti-10V-2Fe-3Al and Ti-11.5Mo-6Zr-4.5Sn alloys have been produced through powder metallurgy route. However, 90% of the powder metallurgy is focussed on the alpha + beta alloy Ti-6Al-4V.
\nGuo et al. [39] reported a remarkable increase in the mechanical properties of Ti-10V-2Fe-3Al powder alloy compared to the wrought and cast products through isothermal forging of the sintered alloy. Jiao et al. [40] studied the model of alpha phase spatial distribution in laser additive manufactured Ti-10V-2Fe-3Al. The influence of nano-scale alpha precipitates on tensile properties of age hardened laser additive manufactured Ti-5Al-5Mo-5V-1Cr-1Fe (Ti-55,511) alloy was studied by He et al. [41] and the authors reported that precipitated nanoscale alpha precipitates have led to a decline in ductility.
\nA recent forecast released by Airbus Industries [42], confirms the promising development of air transport requiring 37,400 aircraft at a value of 5.8 trillion US dollars business in the next 20 years. However, reducing the fuel consumption to control the emission of CO2 and NOx is the driving factor for the aerospace industries and this could be possible by reducing the overall weight [43]. Similarly, in space application weight of the payload is more crucial than civil/cargo aviation. Ti-6Al-4V is a workhorse for the aerospace industry for several decades and 65% of total titanium production in the United States belongs to Ti-6Al-4V alloy [3].Even though the alpha +beta alloys dominated the scene, beta alloys with their unique characteristics such as excellent hardenability, heat treatability to high strength levels and a high degree of sheet formability, are becoming increasingly important for the aerospace sector. Beta alloys and their aerospace application are listed in the Table 2.
\nS. No. | \nAlloy | \nApplication/components | \n
---|---|---|
1 | \nTi-15V-3Al-3Cr-3Sn | \nLanding gear, springs, sheet, plate and airframe castings, environmental control system ducting | \n
2 | \nTi-6V-6Mo-5.7Fe-2.7Al | \nFasteners | \n
3 | \nTi-13V-11Cr-3Al | \nAirframe, landing gear and springs | \n
4 | \nTi-3Al-8V-6Cr-4Mo-4Zr (β-C) | \nSprings and fasteners | \n
5 | \nTi-11.5Mo-6Zr-4.5Sn | \nRivbolts—Boeing 747 | \n
6 | \nTi-5Al-5Mo-5V-3Cr | \nAircraft landing gear, Fuselage components and high lift devices | \n
7 | \nTi-10V-2Fe-3Al | \n\n
| \n
8 | \nBeta 21s | \n\n
| \n
9 | \nTi-35V-15Cr (Alloy C) | \nCompressor and exhaust nozzle components | \n
Titanium is the ultimate choice for biomedical applications as they outperform conventionally used biomedical alloys such as 316L stainless steel and cobalt-chromium alloys [47]. The formation of a nanometre thick oxide layer on titanium when exposed to any environment imparts high corrosion resistance and superior biocompatibility [48]. All classes of titanium α, α + β, near β and β alloys are widely used for biomedical applications.
\nDespite being initially developed for aerospace applications, CP titanium and Ti-6Al-4V are still the most widely used Ti grades being used for biomedical applications. However, CP Ti is associated with lower wear resistance and Ti-6Al-4V when implanted inside the body releases Al and V ions which can lead to severe neurological disorders and allergic reactions. Moreover, the elastic modulus values of these alloys (~110 GPa) are almost four times than that of human cortical bone (20–30 GPa) which can lead to stress shielding effect. This led to the development of β-Ti alloys composed of non-toxic elements and their inherent lower elastic modulus assists in reducing the stress shielding effect when used for orthopaedic applications [3]. Alloy systems based on Ti-Nb, Ti-Mo, Ti-Ta and Ti-Zr are potential materials for biomedical applications. Some of these β-Ti alloys initially developed are Ti-15Mo-5Zr-3Al, Ti-12Mo-6Zr-2Fe (TMZF), Ti-15Mo-3Nb-0.3O (21SRx) and Ti-13Nb-13Zr possessing modulus values in the range of 70–90 GPa.
\nIn the early 1990s, medical device industry focused on developing these low modulus β-Ti alloys for orthopaedic applications. Initially, two β-Ti alloys Ti-13Nb-13Zr specified by ASTM F1713 and Ti-12Mo-6Zr-2Fe (TMZF) specified by ASTM F1813 received Food and Drug Administration approval as implant materials. Among these, TMZF alloy possesses an elastic modulus of about 74–85 GPa, with a yield strength of 1000 MPa. During the early 2000s, this metastable β-Ti alloy was used for making hip stems, which rub against a modular neck made from a cobalt-chromium based alloy. However, in 2011, the US Food and Drug Administration recalled the use of this TMZF alloy due to the unacceptable level of wear debris formation. Another β-Ti alloy 21SRx is derived from the aerospace alloy 21S from which aluminium was eliminated over biocompatibility concerns. In addition, alloys such as Ti-29Nb-13Ta-4.6Zr and Ti-35Nb-7Zr-5Ta are receiving increasing attention due to their lower elastic moduli of about 65 and 55 GPa, respectively, lower than other β-Ti alloys [50].
\nApart from orthopaedics, titanium is extensively used in the dental applications [49]. In the case of orthodontic wire material, it should possess three general characteristics viz. large spring back (ability to be deflected over longer distances without permanent deformation), lower stiffness and high formability [51]. The initially utilised materials for orthodontic wire application were gold based alloys containing copper, palladium, platinum or nickel. However, spring back values of these gold alloys were limited owing to their lower yield strength. In the 1960s gold was replaced by stainless steel and cobalt-chromium based alloy (elgiloy). These materials continue to be the standard orthodontic wire material for the past 70 years and possess higher springiness and strength with comparable corrosion resistance. During the early 1970s, nickel-titanium alloy Nitinol (Nickel Titanium Naval Ordinance Laboratory) was also used for orthodontic wires. Even though Nitinol orthodontic archwires are widely used owing to their superior superelastic properties, their use is hampered by reduced formability during the final stages of treatment. Moreover, there are serious concerns over the nickel ion release from these materials in the oral environment. It was later demonstrated that orthodontic wires made from β-Ti alloy Ti-11.3Mo-6.6Zr-4.3Sn (TMA alloy) possess enhanced spring back and formability, along with reduced stiffness. TMA alloys possess ideal elastic modulus values lower than that of stainless steels and higher than nitinol [51]. The higher surface roughness associated with these TMA wires can, however, lead to arch wire-bracket sliding friction due to the high coefficient of friction of TMA alloys. One of the most successful approaches to tackle this problem is the ion implantation process which renders the TMA wires with lower surface roughness and reduced friction coefficients. Another beta titanium alloy Ti-6Mo-4Sn was also investigated for orthodontic wire applications. By proper heat treatment procedures, this alloy exhibited an elastic modulus of 75 GPa and a tensile strength of 1650 MPa [52]. Ti-13V-11Cr-3Al, metastable Ti-3Al-8V-6Cr-4Mo-4Zr, metastable Ti-15V-3Cr-3Al-3Sn, near-beta Ti-10V-2Fe-3Al were also researched for dental archwire applications.
\nThough beta titanium alloys possess superior haemocompatibility, which is beneficial for cardiovascular devices, they are not fully exploited for cardiovascular applications. Despite higher haemocompatibility, no β-Ti alloy based stents have been commercialised which can be attributed to their lower ductility and modulus as compared to 316L stainless steel and cobalt-chromium based stent materials. Recently, research based on the development of new β-Ti alloy compositions for coronary stent applications has been getting increased attention. Initial studies on Ti-12Mo (wt %) and ternary Ti-9Mo-6W (wt %) demonstrated a ductility of about 46% and 43% respectively [53]. Apart from this, initial investigations on Ti-50Ta, Ti-45Ta-5Ir and Ti-17Ir for stent applications were performed by Brien et al. [54]. Among the three alloys, Ti-17Ir exhibited a favourable elastic modulus of 128 GPa owing to the eutectoid Ti3Ir phase precipitation; iridium content will also assist in improving the fluoroscopic visibility of the stents during interventional procedures [54].
\nBeta titanium alloys have shown much promise and extensive research and development work has been devoted to this group of alloys over the last four decades. For aerospace applications, their heat treatability, high hardenability, high strength to weight ratio and excellent hot and cold workability are major attractions. For orthopaedic applications, their corrosion resistance to biofluids, biocompatibility and low elastic modulus coming close to that of human bone are the important attractive features. Accordingly, development of cost-effective processing techniques has also assumed importance. Problems unique to beta titanium alloys such as high degree of proneness to segregation, high loads to be applied during hot working etc. have since been resolved. Powder processing and additive manufacturing of the alloys have recently received attention and hold promise. Surface modification has been an important part of the developmental efforts and has taken a prominent place, especially for biomedical applications. Coming years are bound to witness increased exploitation of this group of alloys, particularly in biomedical and aerospace applications.
\nThe authors would like to express their gratitude to the Management of Vellore Institute of Technology (VIT)—Vellore campus, Tamil Nadu, India, for allowing us to submit this manuscript.
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\\n"}]'},components:[{type:"htmlEditorComponent",content:'When submitting a manuscript, the Author is required to accept the Terms and Conditions set out in our Publication Agreement – Monographs/Compacts as follows:
\n\nCORRESPONDING AUTHOR'S GRANT OF RIGHTS
\n\nSubject to the following Article, the Author grants to IntechOpen, during the full term of copyright, and any extensions or renewals of that term, the following:
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\n\nPolicy last updated: 2018-09-11
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