WO2007097462A1 - 半導体磁器組成物 - Google Patents
半導体磁器組成物 Download PDFInfo
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- WO2007097462A1 WO2007097462A1 PCT/JP2007/053679 JP2007053679W WO2007097462A1 WO 2007097462 A1 WO2007097462 A1 WO 2007097462A1 JP 2007053679 W JP2007053679 W JP 2007053679W WO 2007097462 A1 WO2007097462 A1 WO 2007097462A1
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Definitions
- the present invention relates to a semiconductor ceramic composition having a positive resistance temperature, which is used for a PTC thermistor, a PTC heater, a PTC switch, a temperature detector, and the like.
- compositions have a Curie temperature around 120 ° C. These compositions need to shift the Curie temperature depending on the application.
- the Curie temperature can be shifted by adding SrTiO to BaTiO.
- the Curie temperature shifts only in the negative direction and not in the positive direction.
- PbTiO is known as an additive element that shifts the Curie temperature in the positive direction.
- PbTiO contains elements that cause environmental pollution.
- Patent Document 1 Japanese Published Patent Showa 56-169301
- Patent Document 1 includes, as an example, a composition in which 0.1 mol% of Nd 0 is added as a semiconducting element.
- Patent Document 1 PTC materials that do not contain Pb have excellent jump characteristics, have high room temperature specific resistance, and those with poor jump characteristics have low room temperature specific resistance.
- PTC materials that do not contain Pb have excellent jump characteristics, have high room temperature specific resistance, and those with poor jump characteristics have low room temperature specific resistance.
- the present invention relates to a semiconductor ceramic composition that does not contain Pb, can shift the Curie temperature in the positive direction, can control room temperature resistivity, and has excellent jump characteristics.
- the purpose is to provide
- the inventors can change the composition in the crystal grains and the state of the crystal grain boundaries by adjusting the manufacturing method, thereby changing the amount of formation of the Schottky barrier. Thus, it was found that the control of room temperature resistivity and jump characteristics can be improved, and the present invention has been completed.
- the present invention is a semiconductor ceramic composition in which a part of Ba in BaTiO is replaced with B to Na,
- a semiconductor porcelain composition characterized by having crystals having different compositions in a central portion and an outer shell portion in crystal grains.
- the present invention has a configuration in which the Bi-Na concentration in the central portion and the outer shell portion in the crystal grain is different, and in the configuration, the central partial force in the crystal grain is also directed to the outer shell portion and Bi -Na concentration is high, and the center and outer shells of Bi and Na A configuration with a different ratio is proposed.
- the present invention is a semiconductor ceramic composition in which a part of Ba in BaTiO is replaced with B to Na,
- Crystals with different Bi-Na concentration or Bi Na ratio in the central part and outer shell part in the crystal grain, and multiple crystal grains with different BiNa concentration or Bi: Na ratio in the outer shell part Propose a structure that forms grain boundaries!
- the present invention is a semiconductor porcelain composition in which a part of Ba in BaTiO is substituted with B to Na,
- composition formula is represented as [(BiNa) (Ba R)] TiO (where R is a rare earth element)
- X, y satisfying 0 ⁇ x ⁇ 0.2 and 0 ⁇ y ⁇ 0.02 or the compositional strength of semiconductor ceramic composition is expressed as [(BiNa) Ba] [Ti M] 0 (However, M is Nb, Ta, Sb x 1- ⁇ 1 ⁇ ⁇ 3
- a semiconductor capable of shifting the Curie temperature in the positive direction without using Pb causing environmental pollution, controlling the room temperature resistivity, and having excellent jump characteristics.
- a porcelain composition can be provided.
- the semiconductor ceramic composition according to the present invention is applied to a conventional PTC element containing PbTiO.
- FIG. 1 is a diagram showing composition measurement positions in crystal grains.
- FIG. 2 is a view showing a result of observing a semiconductor ceramic composition according to the present invention with a scanning spreading resistance microscope.
- FIG. 3 is a diagram showing the results of observation of a semiconductor ceramic composition according to a comparative example with a scanning spreading resistance microscope.
- FIG. 4 is a diagram showing composition measurement positions of a semiconductor ceramic composition according to the present invention.
- FIG. 5 shows a PTC element containing a semiconductor porcelain composition according to the present invention and a conventional PbTiO.
- composition having a partially different composition By using a composition having a partially different composition, the amount of Schottky barrier formation is increased and jump characteristics are improved.
- a composition having the following constitution is preferred as the composition having a partially different composition in the crystal grains.
- composition in the crystal grains of each crystal in the semiconductor porcelain composition is different between the central portion and the outer shell portion.
- the concentration of Bi-Na in the crystal grains of each crystal in the semiconductor ceramic composition is different between the central part and the outer shell part.
- the ratio of Bi to Na (Bi: Na) may be the same in the central part and the outer shell part.
- the central partial force in the crystal grains is also directed toward the outer shell portion to increase the Bi-Na concentration.
- the ratio of Bi to Na may be the same in the central portion and the outer shell portion.
- the ratio of Bi to Na (Bi: Na) in the crystal grains of each crystal in the semiconductor porcelain composition is different between the central part and the outer shell part. At this time, the total amount of Bi and Na may be the same in the central portion and the outer shell portion.
- the Bi concentration in the center portion in the crystal grain is 1 mol% or less and the Bi concentration in the outer shell portion in the crystal grain is It can be mentioned that it is lmol% or more, or the ratio of the Bi concentration in the central part and outer shell part (central part: outer shell part) is 1: 2.5 or higher.
- the preferred embodiment varies depending on the component range of the composition.
- the concentration of Bi-Na in the crystal grains of each crystal is different between the central part and the outer shell part, and multiple crystal grains with different Bi-Na concentrations in the outer shell part are combined.
- the crystal grain boundary is formed to form a structure.
- the grain boundaries in this configuration serve as Schottky barriers, and the amount of Schottky barrier formation increases and jump characteristics improve because the Bi-Na concentration of the combined crystal grains is different.
- the ratio of Bi and Na in the crystal grains of each crystal in the semiconductor porcelain composition (Bi: Na) is different between the central part and the outer shell part, and the ratio of Bi and Na in the outer shell part is different.
- a plurality of crystal grains are combined to form a crystal grain boundary.
- the grain boundaries in this configuration serve as Schottky barriers, and the ratio of Bi and Na in the combined crystal grains is different, which increases the amount of Schottky barrier formation and improves jump characteristics.
- a semiconductor porcelain composition according to the present invention has a composition in which a part of Ba in BaTiO is replaced with B to Na.
- x and y are 0 ⁇ x ⁇ 0.2, 0 ⁇ y ⁇ 0.02
- composition formula is expressed as [(BiNa) Ba] [Ti M] ⁇ (where M is Nb, Ta x 1- ⁇ 1 ⁇ ⁇ 3
- At least one of Sb), ⁇ , z satisfying 0 ⁇ x ⁇ 0.2, 0 ⁇ z ⁇ 0.005 the Curie temperature without using Pb can be raised,
- the room temperature specific resistance can be reduced, and the effect of improving the room temperature specific resistance and jump characteristics according to the present invention can be further enhanced.
- R is at least one of rare earth elements
- X represents a component range of (BiNa), and 0 ⁇ x ⁇ 0.2 is a preferable range. If X is 0, the Curie temperature cannot be shifted to the high temperature side, and if it exceeds 0.2, the resistivity at room temperature approaches 10 4 ⁇ cm, making it difficult to apply to a PTC heater or the like.
- y represents a component range of R, and 0 ⁇ y ⁇ 0.02 is a preferable range. If y is 0, the composition does not become a semiconductor, and if it exceeds 0.02, the resistivity at room temperature increases, which is not preferable.
- a part of Ba which is part of Ba
- B the value of y to control the valence
- the trivalent cation is made into a semiconductor.
- the effectiveness of the semiconductor is reduced due to the presence of valent Na ions and There is a problem in that the resistivity at is high. Therefore, a more preferable range is 0.002 ⁇ y ⁇ 0.02.
- 0.1 mol% of Nd 0 is added as a semiconductor element.
- M is at least one of Nb, Ta, and Sb.
- X represents a component range of Bi + Na, and 0 ⁇ x ⁇ 0.2 is a preferable range. If X is 0, the Curie temperature cannot be shifted to the high temperature side, and if it exceeds 0.2, the resistivity at room temperature approaches 10 4 ⁇ cm, making it difficult to apply to a PTC heater or the like.
- z represents a component range of M, and 0 ⁇ z ⁇ 0.005 is a preferable range.
- the composition does not become a semiconductor, and if it exceeds 0.005, the resistivity at room temperature exceeds 0 3 ⁇ cm, which is not preferable.
- the above 0 ⁇ z ⁇ 0.005 is 0 to 0.5 mol% (not including 0) in mol% notation.
- the addition of element M (addition amount 0 ⁇ z ⁇ 0.005) is intended to control the valence of the Ti site, which is a tetravalent element.
- the ratio of Bi and Na is basically 1: 1.
- the content and ratio of Bi-Na in each crystal are different, and the content and ratio of Bi-Na in the center and outer shell are different in each crystal grain. It is.
- the ratio of Bi to Na in the above two compositions is basically 1: 1 because, for example, in the calcination process, Bi volatilizes and shifts to the ratio of Bi to Na. It is also a force that can cause. Ie However, it is 1: 1 at the time of blending, but it is also included in the present invention if it is not 1: 1 in the sintered body.
- the semiconductor ceramic composition according to the present invention In order to obtain the semiconductor ceramic composition according to the present invention, it is necessary to make the composition in the crystal grains partially different.
- a general method for producing a semiconductor porcelain composition raw material powders are blended, mixed, calcined, pulverized, molded, and sintered, but there are conditions for obtaining a composition having a uniform composition. Since it has been selected, the semiconductor porcelain composition according to the present invention cannot be obtained. That is, it is necessary to carry out under a condition that does not result in a uniform composition or a method different from the above general production method.
- an example of a production method for obtaining the semiconductor ceramic composition according to the present invention will be described.
- a small amount of Bi 0 is added to the calcined body.
- BaCO excluding TiO only, mixed, calcined to prepare BaTiO calcined body
- the composition shifts in both calcined powders, and at this time, crystals having partially different compositions in the crystal grains are obtained. Further, according to this method, the volatilization of Bi is suppressed, the compositional deviation of Bi-Na is prevented, the generation of a heterogeneous phase containing Na is suppressed, the resistivity at room temperature is lowered, and the Curie is reduced. Reduces temperature variation be able to.
- the production method according to (c) is characterized by (BaQ) TiO calcined powder (Q is a semiconductor element) and (BiNa) TiO
- a raw material powder of 32 and a semiconducting element, for example, La 0 or Nb 0 is mixed to prepare a mixed raw material powder and calcined.
- the calcining temperature is preferably in the range of 900 ° C to 1300 ° C, and the calcining time is preferably 0.5 hours or more. When the calcining temperature is less than 900 ° C or the calcining time is less than 0.5 hours, (BaQ) TiO is completely formed.
- BaCO power that is not formed and some of the decomposed BaO reacts with water or part of the remaining BaCO
- the step of preparing the (BiNa) TiO calcined powder is first to use Na CO, Bi 0, TiO as raw material powder.
- Bi 0 is excessive (for example, exceeding 5 mol%)
- the mixed raw material powder is calcined.
- the calcining temperature is preferably in the range of 700 ° C to 950 ° C.
- the calcining time is preferably 0.5 hours to 10 hours. If the calcining temperature is less than 700 ° C or the calcining time is less than 0.5 hours, unreacted Na 2 CO 3 or NaO produced by decomposition will not be subjected to atmospheric moisture or wet mixing.
- the calcining temperature (900 ° C
- the calcining temperature of (B iNa) TiO is the calcining time to sufficiently perform the reaction while suppressing the volatilization of Bi.
- pulverization may be performed according to the particle size of the raw material powder when the raw material powder is mixed.
- pure water or ethanol is used.
- Mixing may be either wet mixing using pure water or ethanol, or dry mixing. However, it is preferable to perform dry mixing because the compositional deviation can be further prevented.
- pulverization after mixing, or mixing and pulverization may be performed simultaneously.
- the average particle size of the mixed calcined powder after mixing and pulverization is preferably 0.5 ⁇ m to 2.5 ⁇ m.
- the mixed calcined powder obtained by the process of mixing (BaQ) TiO calcined powder and (BiNa) TiO calcined powder is
- the pulverized powder can be granulated with a granulator before molding! Compact density after the forming is preferred that 2.5 ⁇ 3.5gZcm 3,.
- Sintering is preferably performed in the air, in a reducing atmosphere, or in an inert gas atmosphere having a low oxygen concentration and a sintering temperature of 1250 ° C to 1380 ° C and a sintering time of 2 hours to 6 hours. If the sintering temperature exceeds 1380 ° C, the sintering time is 4 hours or longer, the Bi concentration in the crystal grains becomes uniform, and the jump characteristics deteriorate, so the sintering temperature is preferably 1250 ° C to 1380 ° C. However, if the sintering time exceeds 8 hours, the Bi concentration in the crystal grains becomes uniform and the jump characteristics deteriorate, which is not preferable. Also, the rate of temperature increase to the sintering temperature or the rate of temperature decrease from the sintering temperature Even if the temperature is lower than 50 ° CZhr, the Bi concentration in the crystal grains becomes uniform and the jump characteristics are deteriorated.
- the composition in the crystal grains and the state of the crystal grain boundaries can be changed.
- the room temperature resistivity can be controlled by changing the amount of formation of the barrier.
- the obtained mixed raw material powder was calcined in the air at 800 ° C. for 2 hours to prepare (Bi Na) TiO calcined powder.
- the prepared (BaLa) TiO calcined powder and (BiNa) TiO calcined powder have a target composition of [(Bi Na
- TiO is mixed and mixed in a pot mill using pure water as a medium.
- the obtained sintered body was processed into a plate shape of 10mm x 10mm x 1mm to prepare test pieces, and each test piece was subjected to temperature change in resistance value from room temperature to 270 ° C with a resistance measuring instrument. Was measured.
- the measurement results are shown in sample numbers 1 to 5 and 7 to 12 in Table 1.
- the Bi concentration and Na concentration in the crystal grains of the obtained sintered body were measured by energy dispersive X-ray spectroscopy using an energy dispersive X-ray spectral transmission electron microscope. As shown in FIG. 1, the measurement position was measured with the portion where the crystal grain B was bonded to the crystal grain A as the outer shell partial composition and the vicinity of the center of the crystal grain B as the central partial composition.
- sample No. 7 has a heating rate of up to sintering and a cooling rate of sintering power of 25 ° CZhr.
- R is the specific resistance at ⁇
- ⁇ is the temperature indicating R
- ⁇ is the Curie temperature
- the obtained mixed raw material powder was calcined in the atmosphere at 1000 ° C. for 4 hours to obtain a calcined powder.
- the obtained calcined powder was mixed and pulverized with a pot mill using pure water as a medium until the mixed calcined powder became 0.9 m, and then dried.
- PVA was added to and mixed with the pulverized powder of the calcined powder, and then granulated by a granulator.
- the obtained granulated powder was molded with a uniaxial press machine, and the molded body was debindered at 700 ° C and then sintered in air at a sintering temperature of 1320 ° C for 1 hour to obtain a sintered body.
- the obtained sintered body was processed in the same manner as in Example 1 and measured under the same conditions. The measurement results are shown in Sample No. 6 in Tables 1 and 2.
- Example Nos. 1 to 5 were prepared separately, mixed, molded, sintered under favorable conditions, and the semiconductor porcelain composition according to the present invention (Sample Nos. 1 to 5) in Example 1 and all the constituents of the composition as before.
- the concentration of Bi-Na and the ratio of Bi and Na are different between the central part and the outer shell part, the room temperature resistivity 30) is reduced, and the jump characteristics (resistance It can be seen that the temperature coefficient is improved.
- sample numbers? To 12 which are comparative examples, are the same as the sample numbers 1 to 5 in Example 1 in the process up to calcination, but the temperature increase rate until sintering and the temperature decrease from sintering. If the speed is slow or the sintering temperature is high, the sintering temperature is long. In these semiconductor porcelain compositions, it can be seen that the Bi concentration in the crystal grains is made uniform and the jump characteristics are lowered.
- the mixture was mixed and pulverized until the mixed calcined powder became 0.9 m, and then dried.
- PVA was added to the pulverized powder of the mixed calcined powder and mixed, and then granulated by a granulator.
- the resulting granulated powder is molded with a uniaxial press, and the molded body is debindered at 700 ° C and then sintered in air at a sintering temperature of 1320 ° C for 1 to 4 hours to obtain a sintered body. It was.
- the obtained sintered body was subjected to caloring as in Example 1 and measured under the same conditions. The measurement results are shown in Sample Nos. 13 and 14 in Tables 3 and 4. In Tables 3 and 4, the sample number with an * is a comparative example. Sample No. 17 is Bi 0 with 5.0 mol% added.
- the mixture was mixed and pulverized by a pot mill using pure water as a medium until the mixed calcined powder became 0.9 / zm, and then dried.
- PVA was added to and mixed with the pulverized powder of the calcined powder, and then granulated with a granulator.
- the obtained granulated powder was molded with a uniaxial press, and the molded body was debindered at 700 ° C and then sintered in air at a sintering temperature of 1320 ° C for 4 hours to obtain a sintered body.
- the obtained sintered body was processed in the same manner as in Example 1 and measured under the same conditions. The measurement results are shown in sample number 15 in Tables 3 and 4.
- the mixture was mixed and pulverized until the mixed calcined powder became 0.9 m, and then dried.
- PVA was added to and mixed with the pulverized powder of the mixed calcined powder, and then granulated by a granulator.
- the obtained granulated powder was molded with a uniaxial press, and the molded body was debindered at 700 ° C and then sintered in air at a sintering temperature of 1320 ° C for 1 to 4 hours to obtain a sintered body. .
- the obtained sintered body was processed in the same manner as in Example 1 and measured under the same conditions. The measurement results are shown in Sample Nos. 18 and 19 in Tables 5 and 6. In Tables 5 and 6, the sample number with an * is a comparative example.
- Examples 3 to Examples were prepared by adding B and Na to the calcined powder, mixing, grinding, molding, and sintering under favorable conditions.
- the semiconducting porcelain composition according to the present invention (Sample Nos. 13, 14, 15, 18, 19) in Fig. 5 differs in the concentration of Bi-Na and the ratio of Bi and Na in the central part and the outer shell part in the crystal grains. It can be seen that the room temperature resistivity (p30) is reduced and the jump characteristics (resistance temperature coefficient) are improved.
- Sample Nos. 16 and 17 are the same as Example 3 Sample Nos. 13 and 14, and Sample No. 20 is the same as Example 5 Sample Nos. 18 and 19. Depending on how you add
- Example 1 The results obtained by observing the semiconductor porcelain composition according to the present invention obtained in Example 1 (Sample No. 6) and the semiconductor porcelain composition as a comparative example (Sample No. 10) using a scanning spreading resistance microscope are shown in FIGS. Shown in 3. 2 shows the present invention, and FIG. 3 shows a comparative example.
- the light-colored part shows low resistance
- the dark-colored part shows high resistance
- the black part shows high resistance.
- a portion where dark portions are connected in a band shape is a crystal grain boundary.
- the crystal grain boundary has a high resistance.
- These high resistance parts are Schottky barriers. That is, according to the present invention, since the composition of the outer shell portion and the central portion in the crystal grains are different, the crystal grains and the crystal grains are formed by being combined. It can be seen that many Schottky barriers are formed at the grain boundaries. As a result, jump characteristics are improved as shown in Table 1.
- the semiconductor porcelain composition of the comparative example shown in FIG. 3 does not have a black portion with few high-resistance crystal grain boundaries. That is, it can be seen that the amount of Schottky barrier formation is very small in the semiconductor ceramic composition of FIG.
- the comparative example shown in FIG. 3 is sintered at 1320 ° C for 10 hours, but because the sintering time is long, the composition of the outer shell portion and the central portion in the crystal grains is made uniform, For this reason, the amount of Schottky barrier formation is reduced at the crystal grain boundary formed by the combination of crystal grains.
- the Curie temperature is adjusted to about 220 ° C.
- the obtained mixed raw material powder was calcined in the atmosphere at 1000 ° C. for 4 hours to prepare (BaLa) TiO calcined powder.
- the mixture was mixed and pulverized until dried.
- PVA was added to and mixed with the pulverized powder of the mixed calcined powder, and then granulated by a granulator.
- the obtained granulated powder is molded with a uniaxial press machine, the above molded body is debindered at 700 ° C, and then sintered in air at sintering temperatures of 1290 ° C and 1320 ° C for 4 hours. Obtained.
- the obtained sintered body was processed in the same manner as in Example 1, and the temperature change of the resistance value was measured under the same conditions as in Example 1. The measurement results are shown in sample numbers 23 and 24 in Table 9.
- FIG. 4 in the obtained sintered body, two crystal grains bonded via a grain boundary are close to the center of one crystal grain (FIG.
- the Na concentration and Bi concentration were measured in the middle 1), the outer shell (2 in the figure), the outer shell of the other crystal grain (3 in the figure), and the part near the center (4 in the figure).
- the measurement was performed by energy dispersive X-ray spectroscopy using an energy dispersive X-ray spectral transmission electron microscope in the same manner as in Example 1.
- Table 10 shows the measurement results. Note that FIG. 4 is a diagram showing the case of sample number 24. In the case of force sample number 23, the same measurement method was used.
- the two crystal grains bonded through the grain boundary have different Na concentrations and Bi concentrations in the portion near the center and the outer shell portion of each crystal grain, and the crystal It can be seen that the Na concentration and the Bi concentration in the outer shell of each crystal grain connected through the grain boundary are different. This increases the amount of Schottky barrier formation at the grain boundaries and improves jump characteristics.
- the mixture was mixed and pulverized until dry, and then dried.
- Add and mix PVA to the pulverized powder of the mixed calcined powder And then granulated with a granulator.
- the obtained granulated powder is molded with a uniaxial press machine, and the molded body is debindered at 700 ° C and then sintered in the atmosphere at sintering temperatures of 1320 ° C and 1350 ° C for 4 hours.
- the obtained sintered body was processed in the same manner as in Example 1 and measured under the same conditions. The measurement results are shown in Sample Nos. 25 and 26 in Table 11 and Table 12.
- This example changes the blending ratio when mixing (BaLa) TiO calcined powder and (BiNa) TiO calcined powder.
- Patent Document 1 This is close to the composition of Reference 1.
- all elements constituting the composition are initially mixed, mixed, dried, calcined in air or nitrogen at 850 ° C to 1150 ° C, and the resulting calcined powder is obtained. After granulation and molding, it is sintered at 1250 ° C to 1380 ° C in nitrogen and then heat treated at 1100 ° C to 1380 ° C in an acidic atmosphere.
- Patent Document 1 as has been conventionally performed, in order to obtain a composition having a uniform composition, sintering at a high temperature and heat treatment for a long time as described above were performed. Further, the heat treatment in an oxidizing atmosphere in Patent Document 1 is thought to improve the jump characteristics by introducing oxygen into the grain boundaries.
- the composition of the outer shell portion and the central portion in the crystal grain is made uniform, and the amount of Schottky barrier formation at the grain boundary due to the difference in BiNa concentration is small, and a barrier is formed by the introduction of oxygen. It is considered a thing.
- the semiconductor ceramic composition according to this example is completely different from the ceramic composition disclosed in Patent Document 1, and the jump characteristic is the same level when converted to the same composition, but the room temperature resistivity is greatly increased. It has been improved.
- Example 7 even if the composition was changed by changing the blending ratio, the concentration of Bi-Na and Bi in the central part and the outer shell part in the crystal grains were changed. Crystals with different Na ratios can be obtained, and jump characteristics can be improved.
- BaTiO It is clear that the present invention can be implemented with a semiconductor ceramic composition in which a part of Ba is substituted with Bi-Na.
- a portion of BaTiO in BaTiO is substituted with B to Na, and does not contain Pb.
- Figure 5 shows the relationship between the temperature and specific resistance of a semiconductor ceramic composition having crystals with different compositions in the central part and outer shell part and a conventional PTC element containing PbTiO.
- black circle
- the specific resistance peak value of a conventional PTC element containing PbTiO is around 240 ° C. This
- the semiconductor ceramic composition according to the present invention has a peak value of PTC element containing conventional PbTiO.
- the semiconductor ceramic composition obtained by the present invention is optimal as a material for PTC thermistors, PTC heaters, PTC switches, temperature detectors, and the like.
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Also Published As
Publication number | Publication date |
---|---|
JP5218042B2 (ja) | 2013-06-26 |
EP2014626A4 (en) | 2012-01-04 |
TW200744979A (en) | 2007-12-16 |
KR20090007283A (ko) | 2009-01-16 |
KR101152453B1 (ko) | 2012-06-01 |
EP2014626A1 (en) | 2009-01-14 |
CN101389581B (zh) | 2012-10-24 |
CN101389581A (zh) | 2009-03-18 |
US20090036293A1 (en) | 2009-02-05 |
JPWO2007097462A1 (ja) | 2009-07-16 |
US8067325B2 (en) | 2011-11-29 |
TWI401236B (zh) | 2013-07-11 |
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