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Tantalum Flake Powders for High Reliability Capacitors

Tantalum Flake Powders for High Reliability Capacitors

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Published by Steve Kirkman
White paper on the properties of Tantalum flakes/powders in the manufacture of capacitors
White paper on the properties of Tantalum flakes/powders in the manufacture of capacitors

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Published by: Steve Kirkman on Feb 26, 2014
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05/15/2014

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Tantalum Flakes – Powders For High Reliability Electrolytic CapacitorApplications
J. Koenitzer, S. Krause, L. Mann, and S. Yuan
Cabot SupermetalsP.O. Box 1608Boyertown, PA 19512Phone: 1-978-671-4075 Email: john_koenitzer@cabot-corp.com
T. Izumi and Y. Noguchi
Cabot Supermetals KK 111 Nagayachi, Higashinagahara,Kawahigashi, Fukushima 969-3431, Japan
Introduction
Tantalum (Ta) powders are used for making highreliability solid electrolytic capacitors. These partsfind applications in various industries, such asautomotive, telecommunications, and computers. Asthe technology in these areas advances, thecharacteristics of the underlying Ta powders mustimprove. It is well known that both the chemicalcomposition and physical structure of Ta powdershave a significant impact on the performance of finished Ta capacitors, including, for example, DCleakage, reliability, and ESR.Today, one challenge is to produce improved Ta powders for high voltage / high temperaturecapactitor applications. Traditionally, the voltagerating (V
) of a capacitor is defined as the maximumvoltage that can be continuously applied attemperatures up to 85 °C. For use at higher temperatures, an additional voltage de-rating needs to be applied to assure the same degree of reliability.This additional de-rating is applied linearly above 85°C and reduces the operating voltage to 2/3 V
 at 125°C.[1] With the use of Ta capacitors in automotivecontrol systems, the operating temperature range isexpanded to 175 °C with voltage ratings up to 50V.[2] Ta flake powders have the necessarycharacteristics to produce high reliability capacitorsfor this application.
Tantalum Flake Technology
Today, most commercial Ta powders are produced by the chemical reduction of K 
2
TaF
7
with Na metal ina molten salt reactor. With this technology, thesurface area of the powder is determined by the ratioof
2
TaF
7
 to diluent salts. Nodular Ta powders have been produced that can be utilized over a wide rangeof anode production conditions. For example, lowsurface area, high voltage powders with capacitancevalues in the range 10k to 30k CV/g and formationvoltages up to 200 V have been in production for over 20 years.Tantalum flake powders are produced by mechanical processes that flatten the initial granular powder. Theraw materials for the flaking process can be either Nareduced Ta powders or crushed Ta EB ingots. Thespecific surface area of the flake powder, and hencespecific capacitance (CV/g), is determined by theflake thickness. Thinner flakes result in products withgreater surface area and corresponding higher CV/g.The first step in the flaking process consists of flattening granular Ta powder in a ball mill. In order to minimize contamination and oxidation, the Ta particles are milled in an organic solvent.Subsequently, an acid leach is performed to purifythe flaked product. Next, the flakes are reduced insize by hydriding and mechanical fragmentation in animpact mill. Heat treatment and de-oxidation processsteps are then used to achieve the proper oxygenconcentration and physical properties, such as flow,Scott density, and particle size distribution, neededfor commercial production of anodes. Themacroscopic and microscopic characteristics of flaked and nodular Ta powders are shown in Figure1.
 
Figure 1.
SEM Photos comparing C350, a highvoltage nodular powder (left), to C275 flake powder (right).The screen cuts of both flake and nodular powdersare similar; however, the underlying particlemorphologies are quite different. This morphologydifference is the fundamental reason flake powdershave superior high formation voltage performance ascompared to nodular powders.
Advantages of Flake Capacitor Powders
Flake capacitor powders have the inherent potentialto achieve higher CV/g at a given formation voltageas compared to nodular powders. Anodes made fromnodular powder can be modeled as a series of interconnecting spheres or cylinders. Likewise,anodes made from flake powder can be modeled as aseries of interconnecting plates.The theoretical specific capacitance, or CV/g, of these different powder structures can be modeledusing the general formula:C = K 
o
K A / twhere C is the capacitance; A is the effective surfacearea; t is dielectric thickness; K 
o
 and K are vacuum permeability and dielectric constant, respectively.The maximum attainable CV/g values of flake andnodular powder (calculated) are shown as a functionof formation voltage in Figure 2. The figure clearlyshows that flake capacitor powders have higher CV/g potential than nodular powders at any givenformation voltage. The focus of current efforts is toachieve the full capability of both flake and nodular materials; however, flake powders inherently havegreater capability and demonstrate improved performance in key areas.
Figure 2.
Maximum CV/g values for flake andnodular Ta powders as a function of V
Current nodular and flake product offerings fromCabot Supermetals (CSM) have been evaluated on acomparable basis to understand relative performance.CSM flake products have historically beenmanufactured in Boyertown, PA. Recently, CSM’sflake technology has been successfully implementedon a commercial scale in Aizu, Japan. The Aizu C-275 and the Boyertown C-275 have beendemonstrated to be equivalent by statistical analysisfor virtually all properties. Additionally, CSM Aizuhas developed specific flake products tailored toAsian customers that offer some advantages for thosecustomers’ specific applications. CSM’s current flake products offer the advantages of higher CV/g andlower DC leakage in wet test analysis. Similar resultsare experienced in solid capacitor products based oncustomer feedback.The performance improvement that results fromusing flake powders at high formation voltages isdemonstrated in Figures 3 and 4. These data comparedifferent high voltage nodular powders from theBoyertown and Aizu sites to C-275 (standard flake)and a newly developed C-275A flake product. Figure3 shows the relative CV/g benefit at differentformation voltages. Figure 4 compares the sintering behavior of these powders, showing similar shrinkagefor the flake products as compared to the nodular  products. For higher formation voltages or evenlower DC leakage at 150 V
 , CSM has the C-255flake product offering.
Figure 3.
Capacitance vs. Formation Voltage of highvoltage nodular to flake powders.
10,000100,0001,000,000050100150200250300
Forming Voltage (V)
   C  a  p  a  c   i   t  a  n  c  e   (  u   F   V   /  g   )
10 Vflake idealnodular ideal
CV/g vs. Ds/Dg Vf=150 V
10,00015,00020,00025,00030,0001.051.101.151.201.25
Ds/Dg
   C   V   /  g   (  u   F   V   /  g   )
C275C275Anodular-1nodular-2nodular-3
CV/g vs. Formation Ts=1600C
10,00015,00020,00025,00030,00050100150200
Formation Voltage.(V)
   C   V   /  g   (  u   F   V   /  g   )
C275C275Anodular-1nodular-2nodular-3
 
Figure 4.
Capacitance vs. Shrinkage of high voltagenodular to flake powders. (Ds/Dg = ratio of sintered/green anode density)A second key performance benefit of flake powder islower DC leakage. In Figure 5, SEM photos of formed anodes made from high voltage nodular andflake powders are compared. Flake primary particlesare generally much larger than their nodular counterparts in two dimensions. It is believed thatduring sintering, flake particles form stronger inter- particle connections because of their relatively largecontact area. In addition, the curvature of thedielectric is minimized because of the flat structure. Itis commonly believed that significant stresses build between the particles at high formation voltage as thedielectric layer becomes thicker, thus inducing theformation of dielectric defects. This is especially trueat inter-particle connections or in areas of highsurface curvature. Since flakes are flat, have larger  primary particle size, and are capable of formingstrong inter-particle connections with low curvature,they can handle stress better than their nodular counterpart. This results in lower DC Leakage, asshown in Figure 6. The data in Figure 6 are from thesame samples as the data in Figures 3 and 4. Thisdata shows the relative benefit of lower DC leakageand higher capacitance for anodes made from flake powders.
Figure 5.
SEM of formed high voltage nodular (left)and flake (right) powders.
DCL vs. Formation Voltage.Ts=1600C
020406050100150200
Formation Voltage.(V)
   D   C   L   (  u   A   /  g   )
C275C275Anodular-1nodular-2nodular-3
Figure 6.
DC Leakage Current as a function of Formation VoltageFlake powders are agglomerated, as shown in Figure1, to achieve optimal physical properties, such asflow and anode crush strength, deemed critical to processing by capacitor manufacturers. Further customization has been accomplished to matchspecific physical properties (crush, flow, density, andfines) to individual customer’s applications. Howeach capacitor manufacturer utilizes the improvedcapabilities of flake powders in their product designswill depend on their specific anode design,formation/impregnation schedules, and other  processing techniques.
Future Opportunities for Tantalum FlakePowders
Current flake products are able to achieve higher CV/g than their nodular counterparts at highformation voltages, while exhibiting lower DCleakage. There are, however, opportunities for improving the capabilities of flake products in highformation voltage applications (150 V to 200 V) andfor extending the application of flake products intomoderate formation voltage applications (down to100 V or lower).One focus of improvement is the production of flake powders with more uniform thickness distribution,and another is developing flake products withthicknesses that are optimized for both higher andlower formation voltages. Current flake productsconsist of individual flakes with a distribution of flake thickness. As shown in Figure 7, the CV/g of individual flakes at a given formation voltage is astrong function of flake thickness. At a formationvoltage of 150 V, flakes with thickness less thanabout 250 nm will be formed through, and haveessentially zero CV/g, while flakes with a thicknessof about 300 nm will exhibit a maximum CV/g of about 44,000. Flakes that are thicker than 300 nmwill exhibit lower CV/g values, declining to about22,000 CV/g at 700 nm thickness. Of course, theoptimum flake thickness depends on the intendedformation voltage, with higher formation voltageshaving thicker optimum flake thickness.In order to achieve the very highest CV/g for a givenformation voltage, one would like to utilize a flake product with a very narrow distribution of flakethickness, centered just slightly above the optimalthickness for that formation voltage. The effect of the distribution of flake thickness on CV/g can beseen in Figures 8 and 9. Figure 8 depicts four normaldistributions of flake thickness, each centered at 500nm (0.5 microns). Figure 9 illustrates the expectedCV/g for different flake thickness distributions whenformed at 150 V. At a formation voltage of 150 V,

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