Pollution that occurs in widespread areas in developing countries.
Advances in Embryo Transfer",title:"胚胎移植新进展",subtitle:"Advances in Embryo Transfer",reviewType:"peer-reviewed",abstract:"本书阐述了生殖医学相关的技术知识,以21世纪最新进展和发展趋势为重点,注重创新性、实用性。 其内容从最佳的卵巢刺激方案、授精技术新进展,到胚胎移植操作技巧、胚胎冷冻保存以及子宫内膜容受性的最新研究成果等都做了详尽的描 述。本书旨在帮助更多从事辅助生殖技术的人员了解本领域最新进展,更新此领域中科学研究和临床诊治观念,以提高诊疗水平达到最佳活产 率。
Embryo transfer has become one of the prominent high businesses worldwide. This book updates and reviews some new developed theories and technologies in the human embryo transfer and mainly focus on discussing some encountered problems during embryo transfer, which gives some examples how to improve pregnancy rate by innovated techniques so that readers, especially embryologists and physicians for human IVF programs, may acquire some new and usable information as well as some key practice techniques. Major contents include the optimal stimulation scheme for ovaries, advance in insemination technology, improved embryo transfer technology and endometrial receptivity and embryo implantation mechanism. Thus, this book will greatly add new information for readers to improve human embryo transfer pregnancy rate.
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Venkateswarlu",coverURL:"https://cdn.intechopen.com/books/images_new/371.jpg",editedByType:"Edited by",editors:[{id:"58592",title:"Dr.",name:"Arun",surname:"Shanker",slug:"arun-shanker",fullName:"Arun Shanker"}],productType:{id:"1",chapterContentType:"chapter",authoredCaption:"Edited by"}}]},chapter:{item:{type:"chapter",id:"59373",title:"Introductory Chapter: Serious Pollution of Soil and Groundwater and the Necessity of Bioremediation",doi:"10.5772/intechopen.74403",slug:"introductory-chapter-serious-pollution-of-soil-and-groundwater-and-the-necessity-of-bioremediation",body:'Earth has massive amounts of water resources, but drinking water accounts for only 0.01% of the total water. Human beings have taken good care of the use of our precious water resources and had benefitted sufficiently. The limited water resources, however, have reached a critical state. A report published by the United Nations in 2007 suggested that around 1.1 billion people live with serious water shortages and 1.8 million children die every year because they develop various diseases from drinking dirty water [1, 2]. To make matters worse, water shortages have already reached extreme levels for 660 million people living in approximately 30–40 countries. Moreover, the area where drinking water cannot be sufficiently obtained is constantly increasing.
It is estimated that over 60% of people will suffer serious water shortages by 2025. A serious shortage of food resources also occurs because crops cannot be grown in countries where there are water shortages or where water is polluted. The prospect of the eruption of international disputes, or even war, over water sources is also worrying. If the emission of harmful pollutants is not stopped and effective remediation is not performed as soon as possible, the global environment will fall into a terrible situation. As this is the introductory chapter of this book, the author introduces the most recent conditions of pollutants and the causes of pollution. Moreover, the author suggests the ideal bioremediation and phytoremediation processes to apply to large polluted areas.
One of the causes of the shortage of drinking water is the excessive use of river water. An increase in population caused an increase in industrial activities and food production, and many large-scale projects that use irrigation water from rivers for agricultural land have been implemented. Moreover, a massive amount of domestic and industrial water has been used by an increasing population and as a result of the rapid development of world economies. The excessive use of water has caused a shortage of river water. In countries located at or near downstream basins, the shortage is especially serious because river water is excessively consumed by the countries located upstream. For example, Egypt is a country where the desert occupies 95% of the land and where the water of the Nile River is the sole water source. Since the countries located in the upstream area of the Nile River excessively consume water and pollutes the river, Egypt is now troubled by serious water shortages [3]. Similar problems have occurred in the countries located at the Indus river basin. In addition to these causes, increases in population and industrial activities have increased the amount of greenhouse gasses that cause global warming, and abnormal weather such as El Nino events occurs more frequently now. Droughts and flooding as a result of abnormal weather make it difficult to stock drinking water.
The deterioration of water quality as well as the amount is another cause of the shortage of drinking water. Living drainage and industrial wastewater that does not receive proper pretreatment are increasing along with the increase in population. This wastewater is directly poured into rivers and the water quality decreases to inadequate levels and can no longer be used as drinking water [4, 5]. Moreover, excessively used herbicides and exhaust gasses containing various chemical compounds and heavy metals contaminates the soil and groundwater. In countries where the economy is rapidly developing, the deterioration of water quality from these causes is especially serious. Many farm lands are polluted by excessively used fertilizer and herbicides or heavy metals and can no longer be used. Fluorine and arsenic have contaminated the water in tube wells due to soil pollution, and inhabitants that drink from these wells often develop serious cases of poisoning [6, 7]. The typical pollutants are listed inTable 1, and the author has introduced each cause more precisely in the next section.
Main poisoning sources | Main chemical compounds | Serious contaminated sites | Remarks on risks to the environment |
---|---|---|---|
Acid rain | SOx and NOx | Urban places and thermal power stations | Death of fish and aquatic organisms in lakes and acid shock in forests |
Insecticides | POPs (BHC, DDT) OPPs (fenitrothion, diazinon) | Agricultural land Agricultural land | Contamination of crops and drinking water, or direct absorption from polluted air |
Herbicides | Atrazine, simazine | ||
Fertilizer | Nitrate nitrogen | Agricultural land | Eutrophication of soil and rivers due to excess nitrate nitrogen |
Metalloids | As, F | Urban, mining, and metallurgy sites | Contamination of tube wells |
Heavy metals | Pb, Cd, Hg, Cr (IV). etc. | Contamination of crops and drinking water or direct absorption from polluted air |
Pollution that occurs in widespread areas in developing countries.
One of the pollutants causing serious environmental pollution is acid rain. Sulfur and nitrogen oxides (SOx and NOx) are excessively exhausted from factories and cars and acidify rain. In the USA and European countries, in the 1970s, serious acidification of soil and lakes by acid rain occurred in association with economic development. In those days, acid rain at pH 2–3 was recorded in several areas in the United States, and the harmful effects on the ecosystem were observed in the acidification of lakes in European countries. Mg+ and Ca2+ ions, which are important minerals to build bones, were leached from lakes by acidification. Fish are most sensitive to the loss of those ions, and many species of fish with bending bones or abnormal structures appeared in acidified lakes including Little Rock Lake in Sweden [8]. The investigation conducted on 3821 lakes in Norway, Sweden, and Finland suggested that many species of fish living in those lakes had disappeared due to acidification [9].
Acid rain induced the acidification of soil as well as lakes. Soil particles charge negative under normal conditions and can maintain a sufficient amount of minerals for the growth of plants. However, the acidification of soil promotes the leaching of minerals such as Mg2+ and K+ from the soil and the accumulation of harmful metal ions in the soil. Furthermore, the acidification of the soil decreases soil microorganisms that degrade sediments and supply the soil with nutrients, and it also decreases microorganisms that assist with the absorption of nutrients and the adjustment to normal pH values. With the decrease of minerals, microorganisms in the soil can finally cause serious damage to plants. Acid shock, the phenomena where all trees in a forest suddenly wither, had unfortunately occurred in several forests in North America and Europe [10, 11].
Once aquatic organisms and fish have died or forests have been lost to acid shock, it takes several decades for it to return to its original state. Therefore, remediation by neutralization is necessary before serious damage occurs. The neutralization of acid with calcium carbonate and calcium hydrate powder is a general and inexpensive procedure [12, 13]. Several projects to neutralize lake water were conducted by spraying the powder from a small ship or helicopter. For instance, 3 million dollars were invested in the neutralization of lakes with calcium carbonate powder in Sweden. Recently, the acidification of lakes and soil has considerably improved in the European Union (EU) and North America due to the efforts to decrease the emission of SOx and NOx and the implementation of projects to neutralize lakes.
On the other hand, the problem of acid rain has gradually occurred in countries in Asia, Africa, and South America. For example, Asian countries including China, India, and Vietnam have realized remarkable economic development during the last half century. The development of industry and an increase in the demand for cars and electronics has caused the release of more emissions containing SOx and NOx. Huge amounts of dust containing PM 2.5 and photochemical smog often appear in urban areas in China and India [14]. As acid rain continuously falls in those areas and effluent control of SOx and NOx by treaties or directives does not function sufficiently, it is difficult to stop or decrease those emissions. Therefore, a serious condition that is similar to that of Europe and the USA in the 1970s will occur in the near future in those countries. The neutralization of soil and lakes by using microorganisms [15, 16] may be necessary until emissions can be controlled successfully.
Pesticides are often used excessively because they generally enhance the productivity of crops. Excess use, however, has harmful effects on the soil. Persistent organic pollutants (POPs) such as dichlorodiphenyltrichloroetane (DDT) and benzene hexachliride (BHC) had been used most frequently as an insecticide in the 1980s. POPs were stable and stayed in the soil for long periods of time [17] and excess use caused the contamination of groundwater and plants. Several studies reported that birds and fish accumulated POPs in their bodies, and milk from cows that ate contaminated straw contained POPs. Thus, the production and use of POPs were banned at the Stockholm Convention on Persistent Organic Pollutants held in 2001, except for its use to kill mosquitoes carrying malaria. Organophosphorus pesticides (OPPs) such as parathion and diazinon were developed as substitutes for POPs. OPPs were thought to be safe because the length of time that they remain in soil was much shorter than that of POPs. However, contamination of drinking water by OPPs was reported in the European Union (EU) in the 2000s. As OPPs inhibit acetylcholine receptors in nervous systems, drinking water containing OPPs may have toxic effects on the nervous system [18]. Thus, the EU banned the use of OPPs, although they are still used in other countries.
The excessive use of herbicides also causes serious soil pollution. The herbicides that are used most frequently are triazine herbicides such as atrazine and simazine which were developed in the 1970s, and have been used in Europe and the United States. However, frogs with deformed fingers were found in a paddy field where atrazine had been used at a high concentration, and it was clarified that they functioned as an endocrine disrupter. Other researchers warned that the decrease of frogs all over the world may be caused by the excessive use of atrazine. Based on these reports, the EU decided on an upper limit for the use of atrazine in fields and the Environment Protection Agency (EPA) in the United States legally regulated the maximum amount (3 ppm) of atrazine in drinking water. However, atrazine and simazine are still widely used outside of the EU and polluted paddy fields are increasing [19, 20].
In order to decrease the harmful effects, insecticides and herbicides were exchanged for low persistence products. Pyrethroid analogs (chrysanthemic acid and pyrethorolone) and nicotine analogs (imidacloprid) were developed to decrease the persistence and toxicity, and they are widely used. Moreover, studies that aimed to decrease the amount of herbicides were also conducted. For example, the Monsanto company developed genetically modified organisms (GMOs) that were resistant to Roundup, which was an herbicide containing glyphosate isopropane as its main component. The amount of Roundup used could be decreased by the use of the GMO, although the decreased amount was much less than expected. Other groups developed insecticides that could attach to leaves more tightly to decrease the necessary amount. Nevertheless, in spite of these efforts to decrease the amount of insecticides and herbicides, farm fields where crops cannot be grown anymore are rapidly increasing, and this is becoming a serious problem in many countries especially in Asia, Africa, and South America [21, 22, 23]. To make matters worse, a huge amount of POP stock produced before the Stockholm Convention on Persistent Organic Pollutants still exist, and POPs are still used in several areas in Asia. According to the assessment of FAO/UNEP/WHO, 1–5 million people have received health damage, and several thousand die every year because of soil pollution [24].
Harmful metals are also causing serious pollution on a global scale. For instance, arsenic (As) is found in arsenopyrite, and sulfide minerals composed of ferric and arsenic are widely present in soil. Concentrations of As are 2–23 μg/g in soil and 0.005–0.1 μg/m3 in the air. Until the 1980s, products using As were not frequently found and those concentrations were sufficiently low and adhered to safety levels. However, As production rapidly increased because Ga-As and Se-As semiconductors were widely used in cellphones, personal computers, and other appliances, and the mining industry that had to produce As were rapidly increasing accompanied by the increased demand. As a result, huge amounts of crude ore, sediments, wastewater, and emission gasses containing As contaminated rivers, groundwater, and soil [25, 26]. Serious health damage has occurred in inhabitants living in areas that surround mining industries.
Furthermore, high concentrations of As are observed in groundwater in several Asian countries including Vietnam, Thailand, India, and China [27, 28, 29]. Many people in those countries use water in tube wells as drinking water, but high concentrations of As have contaminated these wells. In the guideline of the World Health Organization (WHO), the concentration limit of As to avoid harmful effects is 10 μg/L, but the groundwater in those tube wells often exceed 50 μg/L. India and Bangladesh are especially troubled by the contamination. Serious groundwater pollution by As in West Bengal prefecture has been reported and approximately 8 million inhabitants in the prefecture are exposed to the risk of arsenic poisoning. The person who noticed arsenic poisoning as a result of drinking groundwater from tube wells in the prefecture had not reported it until 1983, and the data suggested that the concentration of As in groundwater in the tube wells has been gradually increasing after 1983. Arsenopyrite may be melted by the acidification of soil and release As, although the cause of the increase has not been sufficiently elucidated.
Coal fuel is the third most important cause of As pollution. The content of As in coal fuel used at Guizhou in China is 100–9600 ppm; however, the As content in coal fuel is usually 1–10 ppm, and therefore, the inhabitants have developed serious As poisoning. The Chinese government has now banned the mining of such low-quality coal. Demand for coal fuel is increasing and is accompanied by the development of economies in Asia. Poisoning by As is also increasing in countries where coal is the main fuel source. Furthermore, coal fuel causes fluorine poisoning as well as As poisoning. In some areas in Sichuan and Guizhou in China, coal containing very high levels of fluorine (500 mg/kg) is used, and the inhabitants have developed fluorine poisoning. According to the report of the Chinese Ministry of Health in 1997, around 20 million people developed fluorosis caused by the use of coal as a fuel source. Moreover, many people who drank groundwater from tube wells in India also developed fluorosis in addition to arsenic poisoning.
Other forms of health damage are caused by pollution from harmful heavy metals such as lead, cadmium, mercury, and hexavalent chromium [30, 31, 32, 33, 34]. For instance, contamination by lead and cadmium has recently become serious. Lead poisoning has historically occurred through the organic lead exhausted from cars using lead gasoline (gasoline containing tetraethyl or tetramethyllead) in the 1970s, but from 1980 to 1990, lead gasoline was banned in many countries and changed to lead-free gasoline. As a result of this policy, the lead concentration in the air decreased to the normal level, and the problem was solved. However, lead poisoning became a problem once again. More than 80% of the lead currently utilized is for lead-acid batteries which are used as car batteries. The production amount of lead-acid batteries is rapidly increasing due to the increased demand for cars. In many metallurgy and mining industries, exhaust gasses and wastewater containing high concentrations of lead are directly exhausted without any pretreatment or with insufficient pretreatment, and low-quality ore and used sludge are left on the soil [35, 36]. Therefore, serious lead poisoning has developed in areas surrounding metallurgy and mining industries. The cause of contamination by cadmium is similar to that of lead. Cadmium is mainly used in Li-Cd batteries for home appliances, and the demand is rapidly increasing. As the recycling ratio of Li-Cd batteries is low (around 20%), cadmium poisoning has been reported in various areas as well as in those surrounding mining industries. Burnt ash and incombustible garbage including waste from electrical and electronic equipment (WEEE), metal plates, and pipes also contain heavy metals [37]. The amount of WEEE is steadily increasing at a rate of 5%, and it was approximately 9 tons in 2005 in the EU [38].
Unfortunately, the Japanese have experienced several tragedies resulting from heavy metal poisoning. A Japanese mining company eliminated cadmium waste into nearby rivers and the inhabitants developed “ouch-ouch disease,” which exhibited symptoms such as dizziness, leg pain, and fragile bones. In another case, a company eliminated waste containing methylmercury into a nearby river and it resulted in a form of neuroparalysis named “Minamata disease.” Recently reported metal contamination of groundwater and rivers in China and India is much worse than the case in Japan. Therefore, we have to pay attention to this problem and perform countermeasures as soon as possible.
Contamination of soil and groundwater has worsened in countries in Asia, South America, and Africa as described in Section 3, and therefore, those countries have to take effective countermeasures without delay. The best countermeasure to stop the progress of such contamination is to decrease the emission of pollutants with strict legal regulation and treaties.
We can remark on the case of acid rain as a successful model case. In order to improve the problem of acid rain, the Canada-U.S. Air Quality Agreement had decided on the restriction of SOx emissions and acted accordingly. As a result, the pH of lakes increased gradually. In the lakes of Killarney Park, the pH value of the lake water increased to nearly 6.0 with the decrease of air pollutants in Sudbury [39], and the acidification of soil in forests such as Boemina Forest and lakes in Europe such as Finishing lake was gradually improved as a result of the decrease in air pollution. Moreover, the convention on Long-range Transboundary Air Pollution (LRTAP) which was attended by 48 countries was conducted in 1983, and the emission of polluted air was more strictly controlled. These efforts had good results in the decrease of damage done by acid rain [40].
We can also remark on the directives of WEEE in the EU as another successful example. The EU has created several countermeasures to solve the problems of increased garbage containing harmful metals. First, the EU promulgated the Directive of End-of-Life Vehicles (ELV) in 2000, which necessitated the recycling of ELV to prevent the illegal dumping of used batteries. Second, the EU promulgated two directives, the WEEE Directives and the RoHS Directive, in 2003. Recycling of WEEE was obligated, and the amount of harmful metals used in WEEE was strictly restricted by those directives. The target products of the RoHS Directives were expanded to approximately 20,000 products by the revised RoHS Directive (RoHS2) in 2011. Countries exporting electric appliances to the EU had to follow these strict directives. As a result of these strict directives, the ratio of recycling of lead-batteries was over 90%, and substitutes without harmful metals such as alkaline batteries, lead-free solders, and lead-free glass have been developed.
In spite of the countermeasures in the EU, 44.7 million tons of WEEE were discarded globally in 2016 and, according to a report by Kokuren University in Japan, this amounts to an increase of 8% from 2013. The total ratio of the recycling of WEEE is only 20%. The result suggests that further efforts to decrease WEEE are necessary in other countries as well as in the EU. Similar directives to that of the EU are promulgated in several countries in Asia. However, it is difficult to keep pace among Asian countries where economies have rapidly developed and emission control is insufficient because the development of the economy is more important than environmental problems. If strict regulation by legal countermeasures is not conducted as soon as possible, there is no doubt that soil and groundwater will fall into a dilapidated state in the near future.
Once groundwater and soil have been fatally polluted, several decades are needed for it to recover even if the emission of pollutants can be stopped by strict directives and treaties. Therefore, the remediation of soil and groundwater must be implemented in parallel with efforts to decrease emissions. Various remediation processes such as bioventing, bioremediation with Fenton reactions, and oxygen release compounds (ORC) have been developed, and those conventional processes are successfully applied to contamination spread in a narrow area [41, 42]. However, they are inadequate when pollution has spread in a large area because they are expensive processes. Novel and inexpensive bioremediation processes that can be applied to pollution spread on a global scale must be developed.
An outline of the ideal bioremediation process for contamination of a massive area, which is recommended by the author, is shown in Figure 1. In order to realize such a remediation process, the zone where remediation is performed is an important factor. Emission gasses containing various harmful pollutants contaminate the air, fall on the soil as rain, and penetrate the soil surface. This process first causes the accumulation of pollutants in the shallow layer of the soil. Following this process, the polluted zone is gradually expanded to a deeper zone of the soil, and pollutants finally reach the deepest zone where groundwater is present.
Scheme of the ideal bioremediation and phytoremediation process in soil and rivers. A and B, BSPs and alginate gels immobilizing microorganisms; C and D, mosses and cover grasses (after mowing) covering the soil surface; E and F, plants in a river before and after mowing.
At the deeper and deepest zones, the oxygen concentration and the amount of microorganisms are very low, and large-scale equipment and high pressure pumps that supply oxygen and microorganisms are very expensive and are necessary in the remediation process. Therefore, the remediation of pollutants is extremely difficult once pollutants reach the deeper or deepest zones. On the other hand, remediation at the shallow layer of the soil has many advantages [43]. The addition and control of both nutrients and microorganisms to the soil is very easy at the shallow layer because sufficient oxygen is present in the zone, and nutrients and microorganisms can be supplied by using a normal sprayer. Furthermore, since plant roots that may absorb pollutants cannot reach under several meters of soil, remediation at the shallow layer is absolutely necessary in the case of phytoremediation. These aspects suggest that the removal of the pollutants at the shallow layer of the soil is an absolute requirement in order to realize the ideal remediation process.
As rain transports pollutants to a deeper zone, the retention time of pollutants in the shallow layer of the soil is not long. Therefore, a device is necessary to implement the rapid removal of pollutants within the shallow layer. To realize this, microorganisms showing abilities of degradation and absorption of pollutants must be immobilized at high densities in the shallow layer. Several kinds of immobilization technology can be used for this purpose, and immobilization with alginate gel or κ-carrageenan gel is the general procedure. The advantage of this method is that it can be applied to various kinds of nonflocculent microorganisms. Otherwise, in the case where the microorganisms show characteristics of flocculent or fungi-like shapes, biomass-supported particles (BSPs) (photo A in Figure 1) and self-immobilization methods (BSIS) are more useful and inexpensive processes [44, 45, 46]. For instance, when
If absorption processes can be implemented by covering the surface of the soil as well as at the shallow layer, more prominent remediation processes can be constructed. Mosses may be applied to this process as shown in photo C in Figure 1. The advantages of mosses are: (1) they can cover the ground completely without disturbing the flow of rain water, (2) they can grow at a faster rate with little water, and (3) they have advantages in the reuse of metals because they can accumulate metals at high concentrations. In fact,
Many perennial plants can accumulate metals in their stems and leaves and can reproduce them after the removal of stems and leaves. As pea sprouts can accumulate several heavy metals, it may be one of the desirable plants. Mamenae, the young herbs of pea sprouts, can recover in a week after mowing, and therefore, a continuous adsorption process can be constructed. Moreover, there are many wild grasses known as “ground cover” that are shown in photo D in Figure 1. They can cover the ground completely and grow even after mowing. Additionally, they are very strong in harsh climates. Therefore, they may be the best plants to use to realize a continuous process. The plants that can accumulate components in the roots at high levels may also be useful. For example,
In the case of river remediation, another concept is necessary. Once domestic and industrial wastewater containing huge amounts of pollutants is directly discharged into rivers, it is extremely difficult to remove the pollutants. Therefore, the establishment of pretreatment equipment is necessary to remove the pollutants. Many countries, however, cannot afford the cost of waste processing. Inexpensive remediation processes for river pollution must be developed before pollutants deal fatal damage to the living things in the rivers and to the inhabitants near rivers. Plants that can live in rivers may provide effective processes, although it is difficult to realize. Photos E and F in Figure 1 show the scheme of such a process (this river is not being used for phytoremediation, and therefore, this photo is merely an image for the sake of comprehension). The plants shown in the photos can live in rivers where the depth of the river water is 20–30 cm, and can live after being mowed every 6 months and grow again. These plants can live in rivers for many years. Inexpensive pretreatment processes for river pollution may be realized by using this process.
In order to realize remediation processes for pollution spread on a global scale, it is also important to choose microorganisms and plants with the best capacities. Many microorganisms that are exceptional at degrading or removing pollutants have been discovered. For example, fungi that could neutralize acid by secreting basic compound was discovered [45]. Those fungi may effectively neutralize acidified soil and lakes. Additionally, many microorganisms that show increased abilities to degrade triazine pesticides such as atrazine and organophosphorus herbicides such as diazinon have been discovered, along with many microorganisms that can absorb heavy metals [49, 50, 51, 52]. Their degradation pathways or mechanisms of absorption were elucidated, and many genes for degradation have already been cloned. Moreover, many plants that can effectively absorb and accumulate metal ions have been discovered and those plants are known as hyperaccumulators [53, 54]. For example,
However, in the case of the remediation of a large polluted area, the capacities of those microorganisms and hyperaccumulators are insufficient. The author’s rough estimate for lead and nickel suggests that the expenditure of plant growth is much higher than the gains of obtained metal, even if the best hyperaccumulators are used under ideal conditions. Therefore, microorganisms and plants that have even more excellent capacities must be developed. There are several advantages to the use of recombinant microorganisms and plants [56, 57, 58]. For instance, the capacity of degradation or absorption per cell in recombinant microorganisms can be enhanced several (or several 10) times, and its amount of expression can be freely controlled by using an adequate promoter.
Another advantage in utilizing recombinant microorganisms and plants is that their capacity for degradation or absorption can be maintained under harsh climates. The activity of microorganisms and the growth of plants are very sensitive to harsh climates, and this is a disadvantage of the biological process. Pollution spread over a large area has mainly occurred under severe climates such as acidic, cold, and dry weather, and this lowers the bioremediation efficiency. Therefore, the addition of the capacity to maintain high activity under harsh climates by using gene technology is very important. In the case of cold climates where the activity of microorganisms is inhibited, the use of cold-resistant microorganisms may be adequate as a host strain for gene manipulation. Cold shock proteins may also be useful for the activation of microorganisms [59]. In the case of a shortage of rainfall, moisturizing of the soil is necessary in order to prevent fatal damage to microorganisms and plants. Polymers such as poly-glutamic acid, chondroitin, hyaluronic acid, and those microorganisms or polymers that are secreted from animal cells and microorganisms can be used as soil moisturizing agents [60]. Moreover, several plants can grow in dry climates. For instance, an aloe can grow with little water, accumulate huge amounts of moisture components in its leaves, and continuously grow new leaves without withering. Therefore, aloes have become a prominent host plant for gene manipulation.
The combination of microorganisms and plants as well as the enhancement of their capacity is important in the enhancement of effectiveness. Plants and microorganisms help each other live in natural places [61, 62]. For instance, plants grow by photosynthesis and their fallen leaves or withered plants are degraded by soil microorganisms. The degraded products become nutrients for microorganisms and plants. This energy cycling is necessary to realize the remediation process for long periods of time at a high level of performance. Therefore, the best selection and combination is necessary to realize the energy cycle of the coculture of microorganisms and plants at the polluted site. This is important for the construction of an effective process. In the case of the adsorption of harmful metal ions, synergy is especially important. Many microorganisms show high resistance to heavy metals and high abilities of adsorption, but the removal of microorganisms adsorbing metals from the soil is difficult. On the other hand, although the removal of plants absorbing metals from the soil is easy, resistance to heavy metals in plants is lower than that of microorganisms and they cannot absorb pollutants at the deeper zone (lower than 1–2 m in depth). Therefore, a combination of microorganisms and plants makes the remediation process more effective.
The removal efficiency of metal ions can be enhanced further by using the electric method. Recently, microorganisms that can generate a current have been reported [63, 64, 65, 66]. Novel electric processes may be constructed by using those microorganisms, although it is not sufficient to utilize them as a power supply. These aspects suggest that synergetic utilization among plants, microorganisms, and chemical reactions are absolutely necessary to construct the best remediation processes. With the exception of the microorganisms listed earlier, there are many microorganisms that show specific characteristics, and they will become the fighting powers in the remediation process. The author expects that a process that will overcome the spread of serious pollution on a global scale will be developed in the near future.
In this introductory chapter, the present conditions of soil and groundwater pollution occurring all over the world, and the necessity of bioremediation have been introduced. Pollution in several Asian, African, and South American countries is much more serious than most people image, and there will be a shortage of food and drinking water in the world in the near future. Strict restrictions by directives or international treaties are the only way to limit and lessen pollution, but the effort is currently insufficient. Therefore, large-scale projects for remediation must be performed in parallel with the effort to stop the emission of pollutants before it results in a fatal condition. Bioremediation and phytoremediation are the most prominent procedures for remediation, but the enhancement of performance is absolutely necessary to fight pollution on a global scale. The author thinks that (1) rapid remediation at the shallow layer of the soil, (2) the use of high-performance recombinant microorganisms that are resistant to harsh climates, and (3) synergy among microorganisms, plants, and chemical reactions that are necessary to realize such a remediation system.
Capacitors are one of the primary components in power electronic devices, some of which are required to operate in hostile environments across a variety of consumer, industrial, and military sectors. For example, the sensors in “down hole” electronics for characterizing oil, gas, and geothermal wells can experience temperatures exceeding 200°C depending on the well depth. In the aircraft industry, new engine control systems require placement of sensor/actuator and signal conditioning electronics in or near aircraft engines where temperature can be in range of 200–300°C. Similar demands exist in the automobile industry, with power electronics located in the engine compartment and near the wheels of hybrid and electric vehicles where temperatures can reach 150°C [1, 2, 3, 4, 5].
For high voltage (>500 V [6]) applications, metallized polymer film capacitors are generally selected over polymer-film-metal-foil, ceramic, or electrolytic capacitors because of the enhanced volumetric efficiency and improved safety. Failure of a charged high energy capacitor (>10 kJ) is equivalent to a bomb, which requires design engineering with an appropriate failsafe mechanism such that energy is released gradually as the capacitor fails. Presently, the only compatible technology is based on polymer film capacitors with thin metallization as electrodes, for which a thin layer of vacuum-deposited metallization (usually 20–100 nm of aluminum, zinc, or alloy [7]) functions as a fuse. When a localized breakdown of the film occurs during operation, (i) the current flowing through the breakdown site is limited by the metallization resistivity and (ii) the energy dissipated in the breakdown is sufficient to vaporize/oxidize the metallization near the breakdown, isolating the breakdown site. This results in a small decrease in capacitance but continued operation of the capacitor at the rated voltage. This “graceful” recovery mechanism is known as “self-clearing” and a photograph of a breakdown (“clearing”) site in a metallized polymer film is shown in Figure 1. In contrast, polymer film capacitors with metal-foil electrodes (5–10 μm thick [9]) and ceramic capacitors, for which the electrode is a thick metal coating, often fail catastrophically if shorted [10, 11].
Photograph of a breakdown site in a metallized polymer film. Figure reproduced from Figure 3 of [
With power system designers striving for miniaturization and reliability at high temperatures and operating voltages, they must turn to specialized components. These applications are enabled, in part, by wide bandgap semiconductors (e.g., silicon carbide), which support operation at temperatures well above 150°C [3, 12]. However, these types of environments are too aggressive for conventional polymer capacitor dielectrics unless the voltage is derated, or an active cooling mechanism is implemented, introducing additional cost and complexity while reducing energy efficiency. High temperature polymer film capacitors offer a promising solution for these issues due to reduced thermal management requirements and elimination of the voltage derating due to improved stability of the breakdown strength at high temperatures. Aromatic polyimides are one specific class of high temperature polymers which have been commercially available since the early 1960s [13], but the form in which these materials are manufactured generally does not meet the specifications required for capacitor films. One of the main requirements is the processability of the polymer into a continuous thin film (<12 μm thickness), since the capacitance scales inversely with film thickness [14]. This limitation precludes the use of Kapton® polyimide as a capacitor dielectric [15], even though it has been used extensively as wire and cable insulation for aircraft with a continuous operating temperature of 300–350°C since the early 1980s [16, 17, 18].
One major impediment to the development and integration of new capacitor dielectrics is that specialty film chemistries optimized specifically for high performance polymer capacitors represent relatively small markets (i.e. military, aerospace, and down hole exploration [3, 12]) compared to those necessary for profitable commercial production of a polymer resin. Other than biaxially oriented polypropylene (BOPP) and polyethylene terephthalate (BOPET), which are commodity films in a variety of commercial applications such as packaging [19, 20], nearly all commercial polymer capacitor films are specialty polymers synthesized for other applications. For example, poly (phenylene sulfide) (PPS) and poly(ethylene 2,6-naphthalate) (PEN) are available as premium capacitor dielectrics, but the majority of their use is in automotive, household, and food packaging applications [21, 22, 23, 24].
This chapter discusses the important criteria for high temperature polymer capacitor dielectrics and presents a comprehensive review on commercial resin development up to recent research progress on polyimide (PI) targeted for operating temperature above 150°C. While many review articles on various aspects of polymeric capacitor dielectrics are available [25, 26, 27, 28, 29, 30, 31, 32], this chapter has a specific focus on polyimides for high temperature applications.
The deliverable energy density of a capacitor scales linearly with the dielectric constant and quadratically with breakdown strength. As such, engineers and scientists often focus on these two properties while neglecting other relevant characteristics, such as thermal conductivity and the implications of chemical composition of a polymer on self-clearing capability. These properties will be discussed in the following subsections.
For reliable operation at elevated temperatures, efficient heat removal from the interior of capacitors is essential but often challenging, especially in metallized polymer film designs due to the low thermal conductivity of both the polymer dielectric and the thin metallization [33]. As electrical insulators, polymer dielectrics are poor thermal conductors with thermal conductivities ranging from 0.1 W/(m·K) for amorphous polymers [34] to about 0.6 W/(m·K) for the present state-of-the-art BOPP capacitor films [35]. As for the electrodes, while the thermal conductivity of metals are typically three orders of magnitude higher than those of polymers, the metallization is also ~1000 times thinner than the dielectric and may not have the thermal conductivity of the bulk metal from which it is deposited. One approach to increase thermal conductivity of the polymer is by blending in ceramic nano-fillers. Researchers have shown that mixing 10 vol% boron-nitride nano-sheets (BNNS) with an amorphous polymer resulted in a six-fold increase in thermal conductivity from 0.3 to 1.8 W/(K·m) [36]. The resulting BNNS/polymer nanocomposite also exhibited an increase in dielectric constant, breakdown strength, and charge-discharge efficiency, the latter of which was attributed to reduction of the conduction current. A similar trend has also been observed in other polymer systems including polyimides [37, 38].
For a self-clearing event to occur successfully, the metallization needs to be thin enough to be vaporized/oxidized by the energy dissipated during the dielectric breakdown. In addition, the polymer also needs to be oxidized completely, leaving no conductive paths from free carbon in the region of cleared metallization around the breakdown site, as shown in Figure 1 [8]. Based on an in-depth study of the physics and chemistry of clearing phenomena, polymers with low ratios of carbon to (hydrogen + oxygen) in the repeating units, such as cellulose, often exhibit excellent self-clearing. Conversely, polymers with high carbon to (hydrogen + oxygen) ratios, like polystyrene, tend to form greater amounts of free carbon for a given clearing energy and clear poorly [7]. This trend is illustrated in Table 1, in which the chemical composition of various polymer dielectrics is correlated with the amount of carbon residue, both measured and calculated, based on comparison between amount of carbon in the gaseous by-products and composition of the dielectrics [5, 7]. Kapton® polyimide, also shown in Table 1, has a high degree of aromaticity in the structure and has a tendency toward carbonization (arc-tracking), as observed in wire insulation in commercial aircraft before fluoropolymers were applied as thin coatings to resist arc-tracking [39, 40]. Poor self-clearing can be mitigated to some degree by applying a thin coating of acrylate over the dielectric to increase the oxygen content. The clearing energy can also be reduced by increasing the metallization resistance in order to avoid damaging adjacent layers of dielectric during clearing (Figure 2), given that a metallized film capacitor is typically wound from two layers of single-side-metallized dielectric film as illustrated in Figure 3 [8]. However, the trade-offs for increasing metallization resistance include higher equivalent series resistance (ESR), lower thermal conductivity, and lower ripple current handling capability. Thus, achieving an optimum balance between capacitor ESR and clearing energy depends on the application requirements.
Photograph of an unwound metallized film capacitor having poor self-clearing behavior with damage involving adjacent layers.
Schematic of the construction of a metallized polymer film capacitor winding without the end connections.
In order to withstand the tension applied by winding machines during capacitor manufacturing, a polymer dielectric must have sufficient tensile strength. A typical value of tension used by capacitor manufacturers is about 10 MPa while the typical tensile strength for various commercially available capacitor films is in the range of 160–200 MPa [41]. In comparison, Kapton® polyimide has a tensile strength of 72 MPa and poly(ether imide) 97 MPa [31]. Based on these values, the tensile strengths of the polymers discussed herein are sufficient for capacitor winding.
Polar polymers often exhibit a substantial increase in dielectric constant when the temperature passes through the glass transition temperature (Tg) of the polymer; however, non-polar polymers, which have only electronic polarization, are less temperature-dependent (Figure 4). The temperature dependence of dielectric constant for polar polymers is the result of increased polymer chain mobility as temperature increases through the Tg. This leads to greater freedom in accessible molecular dipole orientations at frequencies below 1012 Hz, while the electronic and atomic contributions tend to occur at around 1012 Hz and above [44]. Furthermore, polymers tend to have a broad distribution of response times as a result of interconnectivity and steric-hindrance imposed by neighboring molecules [45]. Substantial increases in dielectric constant near Tg limit capacitor operation for polar dielectrics to somewhat below Tg for many applications requiring a stable capacitance, including power conditioning/conversion in electronic circuitry, where the operating frequency ranges from tens of kHz for silicon-based switches to a few GHz for gallium nitride transistors [46].
Typical change in capacitance and dissipation factor (DF) of various polymer film capacitors as a function of temperature at 1 kHz. PET: poly(ethylene terephthalate), PEN: poly(ethylene 2,6-naphthalate), PPS: poly(phenylene sulfide), PC: poly(carbonate), PP: poly(propylene). Data adapted from [
Dissipation factor (DF) of a dielectric is a measure of electrical energy dissipated, usually in the form of heat, when an oscillating electric field is applied. Similar to the dielectric constant, the DF is temperature and frequency-dependent and is more pronounced for polar polymers (Figure 4). In a capacitor, the total DF is a combination of contributions from the electrode and the polymer. For the electrode, metallization has a characteristic DF of ~0.1%, while the DF of metal foils is negligible. For polymers, DF can range from 0.01% for nonpolar polymers like PP, to as high as 1% for polar polymers such as PET, as shown in Figure 4. Depending on the capacitor applications, such as in a snubber or DC link, the requirement for dissipation factor ranges from ~0.01% for the former, to 0.1% for the latter [47, 48, 49, 50]. Thus, for a snubber to meet the low DF requirement, metal foil electrodes with a BOPP polymer film is a common capacitor configuration.
The breakdown strength of a dielectric is defined as the maximum electric field that a dielectric can sustain for a given electrode configuration, test area, [51, 52] and voltage waveform (e.g. linear voltage ramp rate for DC breakdown [53]). The breakdown field is a statistical parameter, typically characterized by a Weibull distribution, although sometimes the log-Normal distribution provides a better fit [54]. It is usually determined by extrinsic factors such as weak points or defects such as embedded foreign particles in the dielectric [55]. Therefore, when reporting the breakdown field at the film level (as opposed to a wound capacitor), measurement conditions such as the electrode configuration (ball-plane or parallel plates) and test area should be included. For comparison purposes, all breakdown field data contained in this chapter included a description of the measurement conditions or control measurements with other capacitor-grade polymer films. Presently, BOPP capacitor films have the highest breakdown field of ~700 MV/m (at the 63% Weibull cumulative probability for a test area of ~2 cm2 and 300 V/s linear ramp voltage) among all commercial polymer capacitor films [56]. The breakdown field of polymers decreases as temperature approaches Tg of amorphous (e.g. poly-ether-imide or PEI) or Tm of semi-crystalline polymers, [such as BOPP and BO poly-phenylene-sulfide (PPS)], as shown in Figure 5 [57]. Hence, the operating voltage of a capacitor is usually derated at elevated temperatures to protect against failure and prolong operational lifetime (Figure 6). Although many breakdown mechanisms have been proposed [58, 59, 60, 61], extrinsic breakdown in solids is generally driven by power dissipation and eventually “thermal runaway”, which leads to breakdown [62, 63].
Weibull characteristic breakdown field as a function of temperature for various polymers. Electrode area: ~2 cm2. BOPP: biaxially oriented poly(propylene), PPS: poly(phenylene sulfide), PEI: poly(ether imide). Figure taken from [
Typical derating of operating voltage for various polymer film capacitors as a function of temperature. PET: poly(ethylene terephthalate), PEN: poly(ethylene 2,6-naphthalate), PPS: poly(phenylene sulfide), PC: poly(carbonate), PP: poly(propylene). Data adapted from [
In the early 1990s, the lack of suitable high temperature polymer film capacitors prompted a concerted effort funded by NASA and the U.S. Air Force to develop new capacitor dielectrics based on commercially available heat-resistant polymers with operating temperatures above 200°C. While Kapton® polyimide has been used extensively since the early 1980s as wire and cable insulation for aircraft (continuous operating temperature of 300–350°C [16, 17, 18]), it has never been used as a capacitor dielectric due in part to its previous inability to be manufactured in thin films. Nevertheless, it is a common benchmark for development of new dielectrics. One study reported that the dissipation factor of Kapton® at the film level increased from 0.1% at 25°C and 1 kHz to 6% at 300°C, while that the dielectric constant decreased from 3.1 at 25°C and 1 kHz to 2.8 at 300°C [64, 65]. At 10 kHz, Kapton® showed a similar decreasing trend with increasing temperature for the dielectric constant while the dissipation factor remained constant at 0.1% at temperature up to 300°C, as shown in Figure 7 [36]. Another recent study showed that Kapton® at 1 kHz in a film-foil capacitor configuration exhibited a gradual decrease in capacitance from 25 up to 225°C, followed by an abrupt increase at higher temperature, as illustrated in Figure 8. In this configuration, the dissipation factor of Kapton® remained constant at 0.1% up to 200°C and then increased sharply as temperature was further increased [66].
Dielectric constant and dissipation factor at 10 kHz for Kapton® film as a function of temperature. Data adapted from [
Normalized capacitance and dissipation factor at 1 kHz as a function of temperature for an 8-μm Kapton® HN-30 film capacitor wound with 12-μm copper foil. Data adapted from [
Another aromatic polyimide is SIXEF-44™ (Figure 9), which is manufactured by Hoechst Celanese based on 2,2-bis(3,4dicarboxyphenyl) hexafluoropropane dianhydride (6FDA) and 2,2-bis(4-aminophenyl) hexafluoropropane diamine (4,4′-6F diamine). This fluorinated polyimide has a glass-transition temperature (Tg) of 323°C [67] and a dielectric constant of 2.8 at 1 kHz with <10% change across temperature range from −55 to 300°C. The dissipation factor is around 0.1% over the temperature range of 25–250°C from 100 Hz to 10 kHz, as illustrated in Figure 10 [68]. The reduced dielectric constant in SIXEF-44™ relative to nonfluorinated counterparts was attributed to the symmetry of the fluorine atoms on the polymer backbone [67, 69, 70].
Chemical structure of SIXEF-44™.
Dissipation factor of SIXEF-44™ as a function of temperature at various frequencies. Data adapted from [
Other aromatic polyimides investigated include perfluoropolyimide (PFPI) (Figure 11) and Upilex-S® (Figure 12). PFPI was developed by TRW, Inc., and is a perfluoroisopropylidene diamine of 2,2-bis(4,4-aminophenoxy)-phenyl-hexafluoropropane (4-BDAF) and pyromellitic dianhydride (PMDA) [71]. Upilex-S® was originally synthesized by ICI Americas, Inc. from monomers of 3,3′,4,4′-biphenyl tetracarboxylic dianhydride (BPDA) and p-phenylene diamine (p-PDA). The Tg for PFPI is above 390°C [72] while that of Upilex-S® is 355°C [73]. The dielectric constant of PFPI is 3.1 at 25°C but decreases to 2.9 at 300°C [64, 65], while that of Upilex-S® is 3.3 for 1 kHz and temperatures from 25 to 300°C. The dissipation factor for both PFPI and Upilex-S® at 1 kHz is about 0.1% at both 25 and 300°C.
Chemical structure of PFPI.
Chemical structure of Upilex-S®.
Most aromatic polyimides suffer from the same processing issues as a result of the high degree of aromaticity, which led researchers to develop modified systems with flexible moieties such as ether linkages and alkyl groups in the polymer backbone. One example is Ultem™, which is poly(ether imide) (PEI) (Figure 13) that is synthesized from the disodium salt of bisphenol A and 1,3-bis(4-nitrophthalimido)benzene [74]. Subsequent development efforts focused on melt-extrusion and stretching of PEI films have enabled film thicknesses as thin as 5 μm [31]. The Tg of PEI is ~215°C, which is considerably lower than many of the wholly aromatic polyimides due to the increase in flexibility imparted by the ether linkages and alkyl groups [17]. The dielectric constant and dissipation factor of PEI are about 3.1 and 0.2%, respectively, at frequencies from 100 Hz to 10 kHz and temperatures from 25 to 200°C; however, they increase sharply as temperature approaches the Tg, as shown in Figure 14 [36, 57]. Such temperature dependence for the dielectric constant and dissipation factor is a characteristic for polymers with molecular dipoles as discussed in Section 2.4.
Chemical structure of PEI.
Dielectric constant and dissipation factor at 10 kHz for PEI film as a function of temperature. Data adapted from [
Over the past 10 years, research efforts have continued to develop new polyimides for capacitor dielectrics. The thermal stability of these new polymers is primarily derived from a high degree of aromaticity and fused-ring heterocyclic rigid structures. As energy density of a capacitor scales with the dielectric constant, some researchers have specifically focused on designing new aromatic polyimides (PIs) that have a higher dielectric constant than the typical value of 3 while preserving the essential thermal/mechanical properties.
One common approach to increasing the dielectric constant is by incorporating polar moieties into the backbone of a polymer chain to enhance the dipole moment. The nitrile group (▬CN) is one of the polar moieties that was explored by Wang et al. [75, 76] and Treufeld et al. [77], in which the number of ▬CN dipoles on the diamine was varied between 0, 1, and 3. The nitrile-containing diamines synthesized in the study were aminophenoxy-benzonitrile (APBN)-based with the two amino groups varying between three isomeric positions (m,m, m,p, and p,p) (Figure 15) to explore the effect of isomeric position on the 6FDA-based PIs. A nitrile-free analog, LaRC-CP2™ [78, 79], was used as a control.
Reaction schemes of various polyimides: (a) LaRC-CP2 from 2,2-bis(phthalic anhydride)-1,1,1,3,3,3-hexafluoroisopropane (6FDA) and the 1,3-bis(3-aminophenoxy) benzene (APB) diamine, (b) with one benzonitrile (BN) group, (c) with three benzonitrile groups. Reaction schemes adapted from [
Among the 6FDA-based PIs, the addition of one nitrile group in the diamine increased the room temperature dielectric constant from 2.9 (independent of frequency between 0.1 Hz and 1 MHz for the nitrile-free PI) to between 3.1 and 3.5 depending on the frequency and isomeric positions of the diamine linkage. In general, the m,m- and m,p-positions exhibited higher values (3.25–3.5) as compared to the p,p-position (Figure 16). Further increasing the nitrile content to three nitrile groups per diamine monomer resulted in an additional increase of the room temperature dielectric constant to between 3.5 and 3.7 (frequency dependent) for the 6FDA-based PIs with p,p-linkage. Interestingly, substitution of the other two isomeric positions had no significant effect (Figure 17). The investigators explained that the greater flexibility of the three ▬CN dipoles in the p,p-linkage as compared to the m,m- or m,p-linkage in the diamine resulted in greater dipolar polarization. An increase in dielectric constant was also observed in the OPDA-based PIs with m,m diamine linkage with increasing content of ▬CN dipoles.
Dielectric constant and dielectric loss as a function of frequency at ambient conditions for 6FDA-APB nitrile free PI and the three analogs containing one ▬CN dipole per diamine at different isomeric positions. Data adapted from [
Dielectric constant and dissipation factor as a function of temperature at various frequencies for the 6FDA-based PIs containing three nitrile groups in different isomeric positions (a–c) and the nitrile-free analog, LaRC-CP2 (d). Data taken from [
The key drawback of the addition of nitrile groups was the increase in temperature dependence in both the dielectric constant and dissipation factor, as illustrated in Figure 17. For example, the dielectric constant of the nitrile-free 6FDA-based PI at 10 kHz increased by only 1.4% over a temperature range of −150 to 190°C, whereas that of the three nitrile-containing analogs with the m,m-, p,p-, and m,p-linkages rose 6.3, 8.3, and 15%, respectively. With respect to the dissipation factor, the nitrile-free PI remained below 0.5% over the tested temperature/frequency range, while the same nitrile-containing PIs increased from below 0.1% at −150°C to above 1% at 190°C between 10 Hz and 100 kHz. The temperature scan was limited to 190°C to avoid deforming the sample significantly. The investigators attributed the increase in dielectric constant with temperature at high frequencies to increased short-range segmental motion as the Tg was approached, which resulted in stronger dipolar polarization. However, since the ▬CN dipoles were attached to the polymer backbone in a 90° configuration, the segmental motion was hindered, causing friction with the neighboring chains and leading to high dissipation factor at high temperatures and frequencies. At low frequencies (<10 Hz), the increase in dielectric constant and dissipation factor with temperature was attributed to ions present from residual solvent and unreacted poly(amic acid) precursors in the 35–50 μm thick samples.
The investigators also compared the structural effect of four dianhydrides on the dielectric properties of PIs with three ▬CN dipoles in the diamine unit. The four dianhydride monomers under study were 2,2-bis(phthalic anhydride)-1,1,1,3,3,3-hexafluoroisopropane (6FDA), 4,4′-oxydiphthalic dianhydride (OPDA), 4,4′-benzophenonetetracarboxylic dianhydride (BTDA), and pyromellitic dianhydride (PMDA). The chemical structures of these dianhydrides are shown in Figure 15. A comparison of the increase in dielectric constant (Δε) from −150 to +190°C shows that for the p,p-linkage, PMDA exhibited the largest increase (e.g. ~25% at 10 kHz from ~3.4 at −150°C), followed by OPDA (23% from ~3.3), 6FDA (16% from ~3.4), and finally BTDA with the lowest increase (10% from ~3.6 at 10 kHz at −150°C) (Figure 18a,c, and e). The values of Δε decreased with increasing frequency for all four PIs and followed a decreasing order PMDA > OPDA > 6FDA > BTDA, which agreed with the trends observed in the polarization from dipole orientation determined experimentally and predicted based on a freely rotating single-dipole model. This model assumes an anti-parallel configuration for the dianhydride and diamine dipoles, such that the net dipole moment of a repeat unit is the difference between the dianhydride and diamine dipole moments without an external electric field. PMDA, being a symmetrical dianhydride, has no net dipole moment, whereas BTDA has the largest dipole moment (2.96 Debye) as a result of the benzophenone functional group. The 1.14 D dipole moment of OPDA results from the diphenyl ether, and the 2.0 D dipole moment of 6FDA from the 1,1,1,3,3,3-hexafluoropropane. The diamine portion has a dipole moment of 17.1 D which is the sum of three benzonitrile groups (4.18 D) and four diphenyl ethers (1.14 D). The largest Δε value for PMDA-based PI was accompanied by the highest dissipation factor relative to the other three PIs, but all four PIs had dissipation factor in the range of 3–8% at 190°C between 1 and 100 kHz (Figure 18b,d, and f). The results suggest that the PMDA-based PI with p,p diamine linkage had greater chain flexibility, which led to larger dipole motion at 190°C. In comparison to the p,p-linkage, the m,m-linkage resulted in a smaller increase in dielectric constant and slightly lower dissipation factor at 190°C, although the trends with respect to the dianhydrides and frequency dependence were similar. In addition, the 6FDA-based PI with m,m-linkage shows a dielectric constant of 3.1, which is noticeably lower than the p,p-linkage (ε = 3.4) and other PIs (ε ~ 3.3 to 3.6) at −150°C.
(a, c, and e) increase in dielectric constant (Δε) from −150 to +190°C and (b, d, and f) dissipation factor at 190°C at various frequencies for PIs containing three nitrile groups per diamine with various dianhydride (labeled as 3–6) and different isomeric diamine linkage (denoted as a: p,p; b: m,m; c: m,p). 3–6 represent PMDA-based, OPDA-based, 6FDA-based, and BTDA-based, respectively. Data adapted from [
In terms of discharge energy density and efficiency, as characterized by measuring electric displacement as a function of electric field, the nitrile-containing PIs delivered 25–40% greater discharge energy density than the nitrile-free analog at an applied electric field of 100 MV/m at 190°C and frequencies of 10 Hz and 1 kHz (Figure 19a). For comparison, the investigators also evaluated Kapton® PI and Ultem® PEI, both of which gave similar discharge energy density to the nitrile-free PI. While the nitrile-containing PIs delivered more energy than the nitrile-free counterparts, their discharge efficiency was generally lower, as shown in Figure 19b. The discharge energy losses for the nitrile-containing PIs were 15–40% compared to ~5% for the nitrile-free counterpart at 190°C at 10 Hz. Kapton® PI and Ultem® PEI exhibited 15–20% loss at that temperature and frequency.
(a) Discharge energy density and (b) percent energy loss of various polyimides (PIs) at 100 MV/m at various temperatures and frequencies. PI-1 is nitrile-free 6FDA/m,m-APB (LaRC-CP2). Group 2 represents one nitrile group with OPDA. Groups 3–6 contain three nitrile groups with various dianhydrides labeled 3 as PMDA, 4 OPDA, 5 6FDA, and 6 BTDA. Labels a–c denote p,p-, m,p-, and m,m diamine linkage, respectively, while K and U represent Kapton® PI and Ultem® PEI, respectively. Electrode area: 0.05 cm2. Data adapted from [
With respect to the thermal properties, based on the limited glass transition temperature (Tg) data provided by the investigators, the addition of nitrile groups in the polymer backbone appears to increase Tg, but the enhancement decreased with increasing nitrile content, as indicated by the comparison of Tg for the seven 6FDA-based PIs (Figure 20). The structure of the dianhydride also affects the Tg. The four PMDA-based nitrile-containing PIs appear to have the highest Tg values (300–350°C with high crystallinity), whereas the other three dianhydride families of 6FDA, BTDA, and OPDA were mostly amorphous with Tg values ranging from 220 to 300°C. By comparison, these values were at least 20°C above that of the nitrile-free LaRC-CP2 (Tg = 200°C). Additionally, the PIs with m,m diamine linkage appeared to have lower Tg than those with a p,p linkage. This effect was attributed to the greater free volume created between polymer chains by the two bent amino groups in the m,m-linkage.
Glass transition temperatures of PIs prepared from various dianhydrides: PMDA, 6FDA, BTDA, OPDA, and APB diamine isomers containing 0, 1 or 3 benzonitrile (BN) groups. Data adapted from [
An ether (▬O▬) linkage is another polar moiety explored for the potential enhancement in dielectric constant of PIs [80, 81]. Jeffamines® EDR-104, D230 and HK511 (Figure 21), which are commercial polyether aliphatic diamines, were used to introduce ether linkages into PIs. The rationale behind the use of linear alkyl diamines was to impart close-packing for reducing the overall free volume while maintaining a high density of the imide functional groups in the polymer backbone. For comparison, 1,3-diaminopropane (1,3-DAP) and 1,6-diaminohexane (1,6-DAH), were synthesized as ether-free PIs with commercial linear alkyl diamines. The dianhydrides used in the study were PDMA, BTDA, OPDA, and 6FDA. Depending on the dianhydride, the PIs with diamine D230 exhibited dielectric constants of 2.5 for 6FDA and ~4.5 for the other three dianhyrides at room temperature and 1 kHz, while those containing diamine HK511, because of the greater ether content, produced higher dielectric constants (~5.3 for PMDA and 6FDA, 6.2 for OPDA, and 7.8 for BTDA) (Figure 22a). Hence, the general trend for dielectric constant of the ether-containing PIs with respect to the dianhydrides followed the order BTDA ≥ OPDA > PMDA > 6FDA. The lowest dielectric constant of 2.5 observed in the PI with 6FDA/D230, was attributed to the weak electronic interaction between chains caused by the bulky CF3 groups, which disrupted close packing. In comparison, the ether-free PIs, namely PMDA/1,3-DAP, BTDA/1,3-DAP, and BTDA/1,6-DAH exhibited dielectric constants of 5.6, 4, and 3.6, respectively. While the dielectric constants at room temperature were frequency independent in the range from 0.1 Hz to 10 kHz; the dissipation factor of the ether-containing PIs showed a strong frequency dependence with dielectric relaxation peaks of 1–2% occurring at 1 kHz and above, except for BTDA/D230 and OPDA/D230, which remained below 1% at 10 kHz (Figure 22b). In terms of temperature dependence, the ether-containing PIs showed almost an order of magnitude increase in dissipation factor up to 1% at frequencies of 1 kHz and 10 kHz as the temperature approached their corresponding Tg (50–100°C) (Figure 23). The low Tg was attributed to free volume created by the methyl side groups in the two diamines, D230 and HK511. In comparison, the two ether-free PIs, BTDA/1,3-DAP and BTDA/1,6-DAH, which were prepared from linear alkyl diamines, showed Tg of 175°C and 150°C, with crystal melting temperature of 271 and 234°C, respectively.
Chemical structures of polyether aliphatic diamines: Jeffamines EDR-104, D230, and HK511, and linear alkyl diamines of 1,3-DAP and 1,6-DAH.
(a) Dielectric constant and (b) dissipation factor at room temperature as a function of frequency for various ether-containing PIs with A–D represent PMDA, BTDA, OPDA, and 6FDA, respectively, while 3 denotes D230 polyether diamine and 4 is HK511. Figure reproduced from Figure 2 of [
Dissipation factor at (a) 1 kHz and (b) 10 kHz as a function of temperature for various ether-containing PIs (solid symbols) and an ether-free analog (inverted green triangle). Data adapted from [
Another group of researchers utilized bipyridines and bipyrimidines, which are electron-rich diamines, to enhance the dielectric constant of PIs [82, 83]. The compounds of interest included 5,5′-bis(4-aminophenoxy)-2,2′-bipyridine (BPBPA) and 5,5′-bis(4-aminophenoxy)-2,2′-bipyrimidine (BAPBP) (Figure 24). The dianhydrides used in the study were BTDA, OPDA, PMDA, and BPDA (3,3′,4,4′-biphenyltetracarboxylic dianhydride). The resulting PIs with BPBPA diamine possessed relatively high Tg, which differed depending on the dianhydride unit, giving a decreasing order PMDA (320°C) > BTDA (296°C) > BPDA (285°C) > OPDA (275°C). Analogously, the PI containing BAPBP diamine and BPDA dianhydride showed a Tg of 291°C. The dielectric constants for the BPBPA-based PIs ranged from ~5.5 for the PMDA-based PI to ~6.9 for the BTDA-based at room temperature and frequencies from 1 to 100 kHz, following a decreasing order of BTDA > BPDA > OPDA > PMDA (Figure 25). At 220°C, the dielectric constants decreased about 4% with the same decreasing trend with respect to the dianhydrides over the same frequency range. The dissipation factor for all the BPBPA-based PIs was below 4% at both room temperature and 220°C from 100 Hz to 100 kHz. For the BAPBP/BPDA PI, the dielectric response at room temperature was similar to that of the BPBPA analog.
Chemical structures of (a) 5,5′-bis(4-aminophenoxy)-2,2′-bipyridine (BPBPA) and (b) 5,5′-bis(4-aminophenoxy)-2,2′-bipyrimidine (BAPBP), and (c) various dianhydrides.
Dielectric constant and dissipation factor as a function of frequency for the BPBPA-based PIs with various dianhydrides at (a) room temperature and (b) 220°C. data adapted from [
The demand for even higher operating temperatures (~350°C) for avionics prompted researchers to develop new polymers with increased degrees of aromaticity and heterocyclic rings in the polymer backbone. In the work by Venkat et al. [84], one of the polymers synthesized was a fluorinated polyimide based on 6FDA and a diamine of 2,2-bis(4-aminophenyl) hexafluoropropane grafted with adamantane (ADE) ester pendant groups (Figure 26). The Tg of the PI-ADE is 305°C with a dielectric constant of 2.85–2.91 for the temperature range of 25–250°C at 10 kHz while the dissipation factor increased from 0.6% at 25°C to 0.8% at 250°C (Figure 27).
Chemical structure of PI-ADE. Structures adapted from [
Capacitance (a) and dissipation factor (b) of PI-ADE as a function of temperature at 10 kHz. Data adapted from [
Researchers have achieved some progress in developing polyimides for capacitor dielectrics targeted for operating temperature above 150°C, but there is still major room for improvement. There is a promising new strategy of combining polymer synthesis and computational techniques (e.g., computational quantum mechanics and molecular dynamics) to synergistically search the material space for polymers with desirable material properties (dielectric constant, glass transition temperature, etc.) for capacitor applications. The ultimate goal is to develop synthesis pathways for polymers that are as close as possible to those “discovered” through computational methods [85, 86, 87, 88, 89]. The synergy comes in (i) directing the focus of synthesis and (ii) providing data which simplifies characterization of synthesized polymers through computation of likely crystalline structures (with relative energy differences), IR spectra, and NMR spectra. Work in this area is still relatively limited in that some critical properties cannot be estimated through computational methods, including thermal conductivity, dielectric breakdown field (other than intrinsic), and dielectric loss at frequencies of practical interest (in the kHz region). These deficiencies in the present state of the art result in the approach being somewhat “hit or miss,” but with greater guidance than conventional trial and error approaches. For example, a computational approach uncovered a new chemistry based on organotin esters that was subsequently synthesized and shown to provide greater dielectric constant than is normally available from organic polymers while maintaining a reasonable band gap [90]. This interplay between predictive modeling and synthetic chemistry will become increasingly productive with integration of additional material properties into the explored materials space, and polyimides will certainly be one material class of continued interest to researchers.
The use of power electronics in a growing list of high temperature and high voltage (>500 V) applications currently requires voltage derating and/or active cooling of capacitors with state of the art polymer dielectrics (such as BOPP). High temperature polymers such as polyimides offer promising advantages over the status quo by eliminating this need for voltage derating, easing thermal management requirements, and providing a failsafe for HV applications. However, the lack of commercial interest in processing some polyimides or other specialty polymers as thin films for these comparatively niche polymer applications currently limits implementation of high temperature polymers.
This chapter is dedicated in memory to Dr. Steven Boggs who was a rigorous and passionate researcher, a selfless mentor, an intellectual sounding board, a great inspiration, and a truly amazing friend.
The authors declare no conflict of interest.
IntechOpen publishes different types of publications
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