WO2013180289A1 - 高耐電圧アルミナ質焼結体および高耐電圧用部材 - Google Patents
高耐電圧アルミナ質焼結体および高耐電圧用部材 Download PDFInfo
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- WO2013180289A1 WO2013180289A1 PCT/JP2013/065247 JP2013065247W WO2013180289A1 WO 2013180289 A1 WO2013180289 A1 WO 2013180289A1 JP 2013065247 W JP2013065247 W JP 2013065247W WO 2013180289 A1 WO2013180289 A1 WO 2013180289A1
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- voltage
- sintered body
- high withstand
- alumina sintered
- withstand voltage
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- C04B2235/5463—Particle size distributions
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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- C04B2235/9646—Optical properties
Definitions
- the present invention relates to a high withstand voltage alumina sintered body used in a portion where high insulation with respect to an applied voltage is required, and a high withstand voltage member comprising an electrode in the high withstand voltage alumina sintered body About.
- Various ceramics are applied to parts that require high insulation.
- Patent Document 1 proposes using alumina ceramics as an insulating member in a high voltage bushing (soot tube) of an X-ray tube.
- the voltage applied between the cathode and the anode instantaneously drops in a medical device such as a CT scan or an analysis device such as a transmission electron microscope (hereinafter referred to as an instantaneous voltage drop).
- a medical device such as a CT scan or an analysis device such as a transmission electron microscope (hereinafter referred to as an instantaneous voltage drop).
- an instantaneous voltage drop There is a problem that important medical data and analysis data are lost.
- miniaturization is desired in medical equipment and analyzers.
- it is essential to shorten the creepage distance, which is the distance between the cathode and anode, Therefore, it is necessary to reduce the possibility of creeping breakdown by reducing oxygen defects on the ceramic surface.
- the present invention has been devised to satisfy the above requirements, and is provided with a high withstand voltage alumina sintered body that is less likely to cause creeping breakdown due to an applied voltage, and an electrode in the high withstand voltage alumina sintered body.
- An object of the present invention is to provide a high withstand voltage member.
- the high withstand voltage alumina sintered body of the present invention comprises an alumina sintered body having alumina as a main crystal, and has a peak intensity of around 5000 nm or less in a measurement using a cathodoluminescence method. To do.
- the high withstand voltage member of the present invention is characterized in that an electrode is provided on the high withstand voltage alumina sintered body having the above-described configuration.
- the allowable voltage leading to creepage breakdown can be increased, so that the occurrence of an instantaneous voltage drop is reduced and data loss due to the instantaneous voltage drop is reduced. Can do.
- the high withstand voltage alumina sintered body of the present invention is provided with an electrode, and the allowable voltage leading to the creeping breakdown is large. Since it can be shortened, it is possible to reduce the size of equipment and devices to be mounted.
- the high withstand voltage alumina sintered body of the present embodiment is composed of an alumina sintered body having alumina as a main crystal, and the peak intensity in the vicinity of a wavelength of 330 nm in the measurement using the cathodoluminescence method is 5000 or less. It is said.
- the high withstand voltage alumina sintered body according to the present embodiment is used in a portion where high insulation is required inside a medical device such as a CT scan or an analyzer such as a transmission electron microscope.
- the alumina sintered body in this embodiment means that alumina accounts for 50% by mass or more out of 100% by mass of all components constituting the sintered body.
- the main crystal appears on the chart as the highest main peak in measurement by an X-ray diffractometer using Cu K ⁇ rays. What is necessary is just to collate with the JCPDS card data about identification of the obtained peak. From another point of view, the main crystal is a crystal that occupies 50% by area or more in the confirmation of the cross section of the sintered body with a scanning microscope (SEM or the like).
- the high withstand voltage alumina sintered body of the present embodiment can increase the allowable voltage leading to creeping breakdown by having a peak intensity around a wavelength of 330 nm in the measurement using the cathodoluminescence method of 5000 or less. Therefore, the occurrence of an instantaneous voltage drop is reduced, and data loss due to the instantaneous voltage drop can be reduced.
- the high voltage endurance alumina sintered body of this embodiment is a creeping dielectric breakdown in the high voltage endurance member comprising the high voltage endurance alumina sintered body and electrodes (cathode electrode and anode electrode). Since the allowable voltage is large, the creepage distance can be shortened as compared with the case where a sintered body having a small allowable voltage is used.
- the cathodoluminescence method is a method for detecting light emitted when an electron beam is irradiated on the surface of a sample (in this embodiment, ceramics).
- a sample in this embodiment, ceramics.
- the results obtained by this measurement can be confirmed with a chart in which the horizontal axis indicates the wavelength of light and the vertical axis indicates the intensity of light.
- the peak intensity around the wavelength of 330 nm in the measurement using the cathodoluminescence method was selected because this peak intensity is on the surface of the high withstand voltage alumina sintered body. This is because it represents the amount of oxygen defects (F + centers) that can capture one electron. Therefore, if the peak intensity in the vicinity of the wavelength of 330 nm is small, it indicates that there are few oxygen defects (F + center) on the surface, and oxygen defects (F + center) that cause the electrons emitted when voltage is applied to repeat the discharge. ) Is small, it is possible to suppress an increase in the flow of electrons, and thus the occurrence of an instantaneous voltage drop can be reduced.
- a cathodoluminescence spectroscope SEM: Hitachi S-4300SE, spectroscope: Ehime Bussan HR-320
- the conditions are room temperature (20 ) And measured at an acceleration voltage of 10 kv.
- the allowable voltage level leading to creepage breakdown can be confirmed by the value of creepage breakdown voltage.
- the creeping breakdown voltage is obtained by dividing the voltage (kV) when an instantaneous voltage drop occurs due to creeping breakdown by the creeping distance (mm).
- the creeping breakdown voltage in the high withstand voltage alumina sintered body of the present embodiment is 5 kV / mm or more.
- the peak intensity near the wavelength of 330 nm in the measurement using the cathodoluminescence method is less than 5000, the creeping breakdown voltage is less than 5 kV / mm.
- a voltmeter may be used.
- this creepage breakdown voltage is large means that the allowable voltage leading to creepage breakdown is large, leading to the shortening of the creepage distance, thereby reducing the size of equipment and devices to be mounted. Therefore, it is possible to improve accuracy and reduce weight.
- the high withstand voltage alumina sintered body of the present embodiment preferably includes spinel that is an oxide crystal composed of an alkaline earth metal and aluminum, and the alumina and spinel preferably include a transition metal. That is, in the sintered body, spinel is present in addition to alumina which is the main crystal, and the transition metal is contained in alumina and spinel.
- the alkaline earth metal is any one of beryllium (Be), magnesium (Mg), calcium (Ca), strontium (Sr), barium (Ba) and radium (Ra), and the transition metal is scandium ( Sc), titanium (Ti), vanadium (V), chromium (Cr), manganese (Mn), iron (Fe), cobalt (Co), nickel (Ni), copper (Cu), yttrium (Y), etc. It consists of
- the phrase “contains a transition metal” means that when mapping is performed using an energy dispersive X-ray analyzer (EPMA), when the transition metal is titanium, with respect to alumina, titanium and Al are present at locations where O and O exist.
- EPMA energy dispersive X-ray analyzer
- MgAl 2 O 4 refers to the case where titanium is confirmed at the locations where Al, Mg and O are present.
- TEM transmission electron microscope
- EDS attached energy dispersive X-ray spectrometer
- the transition metal when the transition metal is contained in the alumina and the spinel, the reason is not clear, but the transition metal fills the oxygen defect existing in the alumina and the spinel. It is considered that oxygen defects are reduced. Therefore, the allowable voltage that reaches the dielectric breakdown voltage can be increased.
- the transition metal is titanium and the alkaline earth metal is magnesium.
- the transition metal is titanium and the alkaline earth metal is magnesium, the allowable voltage leading to the breakdown voltage can be increased. Although the reason for this is not clear, it is based on the result that the creepage breakdown voltage is highest in the confirmation of the combination of the above-mentioned alkaline earth metal and transition metal.
- the high withstand voltage alumina sintered body of the present embodiment satisfying the above composition formula and having a peak intensity near a wavelength of 330 nm in the measurement using the cathodoluminescence method of 3000 or less has a creeping breakdown voltage of 10 kV. / Mm or more.
- the Al 2 O 3, TiO 2, mol% ratio of each component of MgO contained in the high withstand voltage alumina sintered body was ground part of the high withstand voltage alumina sintered body, resulting After the powder is dissolved in a solution such as hydrochloric acid, it is measured using an ICP (Inductively Coupled Plasma) emission spectroscopic analyzer (manufactured by Shimadzu Corporation: ICPS-8100), and the obtained metal amounts of Al, Ti, and Mg are respectively measured. Convert to Al 2 O 3 , TiO 2 , MgO.
- ICP Inductively Coupled Plasma
- the molar ratio is calculated from the respective molecular weights, each molar ratio is used as the numerator, and the total molar ratio is used as the denominator. By multiplying by 100, the mol% ratio can be obtained.
- the peak intensity around the wavelength of 420 nm in the measurement using the cathodoluminescence method was selected because this peak intensity is present on the surface of the high withstand voltage alumina sintered body and can capture two electrons. This is because it represents the amount of defects (F center). Therefore, when this peak intensity is small, it indicates that there are few oxygen defects (F center) on the surface.
- the specific measuring apparatus and conditions in the cathodoluminescence method are the same as those described above.
- the two electrons trapped in this oxygen defect are likely to be released when a voltage is applied, and are the beginning of creeping breakdown. Therefore, when the peak intensity near the wavelength of 420 nm in the measurement using the cathodoluminescence method is 160 or less, the number of electrons that start the creeping breakdown is reduced, so that it is difficult to cause the creeping breakdown. .
- the difficulty of causing the creeping breakdown can be confirmed by the value of the initial creeping voltage.
- This initial creeping voltage is, for example, the voltage at which electrons emitted by an applied voltage between the cathode and anode first reach the anode along the surface divided by the creeping distance.
- the method is the same as the method for measuring the creeping breakdown voltage described above.
- the voltage at the initial creeping voltage is smaller than the voltage leading to the voltage drop, which is creeping breakdown, satisfying the above composition formula, and the peak intensity near the wavelength of 420 nm in the measurement using the cathodoluminescence method. Is 160 or less, the high withstand voltage alumina sintered body of the present embodiment has an initial creeping voltage of 4 kV / mm or more.
- the peak intensity near the wavelength of 330 nm in the measurement using the cathodoluminescence method is 3000 or less, and the peak intensity near the wavelength of 420 nm is 160 or less. Is preferred.
- the surface of the high withstand voltage alumina sintered body has few oxygen defects (F + center) capable of capturing one electron and oxygen defects (F center) capable of capturing two electrons.
- F + center oxygen defects
- F center oxygen defects
- the peak intensity near the wavelength of 330 nm is 850 or less, and the peak intensity near the wavelength of 420 nm is 100 or less.
- the composition formula is expressed as ⁇ Al 2 O 3 ⁇ ⁇ TiO 2 ⁇ ⁇ MgO
- the peak intensity near the wavelength of 330 nm in the measurement using the cathodoluminescence method is further reduced, and the creeping breakdown voltage value is further increased.
- the peak intensity near the wavelength of 420 nm in the measurement using the cathodoluminescence method is further reduced, and the initial creeping arrival voltage shows a larger value.
- the existence of oxygen defects (F + center, F center) is small, it is possible to suppress an increase in the flow of electrons and to release electrons that are the origin of creeping breakdown. Since it is suppressed, creepage breakdown can be further prevented.
- the high withstand voltage alumina sintered body of the present embodiment preferably has a ratio ⁇ / ⁇ ratio ⁇ / ⁇ in the composition formula of 0.5 or more and 2.0 or less.
- the value ⁇ / ⁇ of ⁇ and ⁇ is 0.5 or more and 2.0 or less, the value of the creeping breakdown voltage is high, and titanium and magnesium easily enter oxygen defects in the alumina crystal. Since oxygen defects (F + center, F center) can be reduced, the value of the creeping breakdown voltage and the initial creeping voltage reaches a larger value, and it is considered that the creeping breakdown can hardly occur.
- the high withstand voltage alumina sintered body of the present embodiment includes at least one of Si and Ca oxides, and SiO 2 with respect to a total of 100 mass% of Al 2 O 3 , TiO 2 , and MgO.
- CaO is preferably 5% by mass or less (excluding 0% by mass).
- at least one of Si and Ca oxide acts as a sintering aid, and the firing temperature can be lowered and the density can be improved.
- the density may be measured according to JIS R1634-1998.
- an aluminum oxide powder having an average particle size of about 1 ⁇ m and a cumulative 80% particle size distribution with a particle size distribution of 1.75 ⁇ m or less is prepared as a primary material.
- the cumulative particle size distribution of 80% in the particle size distribution of the aluminum oxide powder may be measured by a laser diffraction scattering method using, for example, a microtrack device (manufactured by Nikkiso MT3300EXII).
- a predetermined amount of aluminum oxide powder is weighed, and 100% by mass of the aluminum oxide powder as the primary raw material, for example, 5% by mass or less of sintering aid and 1 to 1.5% by mass of PVA (polyvinyl alcohol), etc.
- a binder, 100% by mass of solvent, and 0.1 to 0.5% by mass of a dispersant are placed in a stirrer and mixed and stirred to form a slurry, which is then granulated with a spray granulator (spray dryer). To obtain granules.
- the obtained granule is molded into a predetermined shape by various molding methods such as a die press molding method and an isostatic press molding (rubber press) method, and after cutting as necessary, Bake in a firing furnace at a maximum temperature of 1400-1700 ° C in an air atmosphere. Then, when the temperature is lowered after being held at the maximum temperature for a predetermined time, it is exposed to a temperature range from the maximum temperature to 1000 ° C for a long time. By using an alumina primary raw material with few coarse particles and exposing it to a temperature range from the maximum temperature to 1000 ° C. for a long time, oxygen can be sufficiently supplied into the Al 2 O 3 crystal particles during firing. Oxygen defects can be reduced. And after baking, the high voltage endurance alumina sintered compact of this embodiment can be obtained by carrying out final finishing by grinding.
- the alkaline earth metal is magnesium and the transition metal is titanium
- the particle size ratio of the aluminum oxide powder to the magnesium hydroxide powder is 0.6 or less (for example, the aluminum oxide powder is 0.6 ⁇ m or less with respect to 1 ⁇ m of the magnesium hydroxide powder), and the aluminum oxide powder having a small particle size is used. This facilitates the activity of alumina and facilitates the formation of spinel.
- a powder having a cumulative particle size of 80% in the particle size distribution is 1.75 times the average particle size or less.
- the particle size ratio of the titanium oxide powder to the aluminum hydroxide powder is set to 0.6 or less (for example, the titanium oxide powder is 0.6 ⁇ m or less with respect to 1 ⁇ m of the aluminum hydroxide powder) so that it is easily contained in alumina and spinel.
- the subsequent steps may be the same as in the first example described above.
- Al is 80% by mass to 99.8% by mass in terms of Al 2 O 3
- Ti is 0.1% by mass to 10% by mass in terms of TiO 2
- Mg is 0.1% by mass to 10% by mass in terms of MgO, and What is necessary is just to weigh so that the sum total may become 100 mass%.
- the particle size ratio of the magnesium hydroxide powder to the aluminum oxide powder used as the primary raw material and the titanium oxide powder to the aluminum oxide powder is in the range of 0.8 to 1.5 (for example, magnesium hydroxide powder with respect to 1 ⁇ m of aluminum oxide powder) And the titanium oxide powder is preferably 0.8 ⁇ m or more and 1.5 ⁇ m or less).
- the rate of temperature increase up to the maximum temperature during firing is preferably 200 ° C./h or less.
- Such a temperature rise rate is based on the result of earnest study, and by using such a temperature rise rate, the peak intensity near the wavelength of 330 nm in the measurement using the cathodoluminescence method is reduced. Can do.
- the rate of temperature decrease from the highest temperature during firing to 800 ° C. is preferably 200 ° C./h or less.
- Such a temperature decrease rate is based on the result of earnest study, and by setting such a temperature decrease rate, the peak intensity near the wavelength of 420 nm in the measurement using the cathodoluminescence method can be reduced. .
- At least one of silicon oxide (SiO 2 ) and calcium carbonate (CaCO 3 ) may be added at the time of slurry preparation.
- content it is preferable to set it as 5 mass% or less in total with respect to 100 mass% of total of aluminum oxide, titanium oxide, and aluminum hydroxide.
- an aluminum oxide powder having an average particle size of about 1 ⁇ m and a cumulative particle size distribution of 80% in the value shown in Table 1 was prepared as a primary material. Then, the aluminum oxide powder is weighed, and 100% by mass of the weighed aluminum oxide powder, 3% by mass of sintering aid, 1% by mass of binder (PVA), 100% by mass of solvent, 0.2% by mass of The dispersant was placed in a stirrer and mixed and stirred to obtain a slurry. Thereafter, the slurry was granulated with a spray granulator (spray dryer) to obtain granules.
- a spray granulator spray dryer
- the obtained granule was filled in a mold and pressed, and then subjected to cutting to obtain a molded body having a predetermined shape.
- the obtained molded body was put in a firing furnace and held at a maximum temperature of 1600 ° C. in an air atmosphere, and a sintered body was obtained with the temperature lowering condition from the maximum temperature as shown in Table 1. Then, the obtained sintered body was ground to obtain a plurality of disk-shaped samples each having an outer diameter of ⁇ 20 mm and a thickness of 5 mm.
- each sample was measured by the cathodoluminescence method.
- a cathodoluminescence spectrometer SEM: Hitachi, S-4300SE, spectrometer: HR-320, manufactured by Ehime Bussan Co., Ltd.
- measurement was performed at room temperature (20 ° C.) and acceleration voltage: 10 kv.
- a chart showing the result of light emitted when the sample surface was irradiated with an electron beam (the horizontal axis represents the wavelength of light and the vertical axis represents the light intensity) was obtained.
- Table 1 shows the peak intensity around the wavelength of 330 nm.
- sample No. with a cumulative particle size distribution of 80% in the particle size distribution is 2 ⁇ m. 1 to 3, without setting the temperature lowering condition from the maximum temperature, sample No. Nos. 4, 7, 10, 13, and 16 had peak intensities in the vicinity of a wavelength of 330 nm in the chart obtained by measurement using the cathodoluminescence method, exceeding 5000, and the creeping breakdown voltage reached was as low as less than 5 kV / mm.
- a peak near a wavelength of 330 nm in a chart obtained by measurement using the cathodoluminescence method by setting the particle size of 80% cumulative in the particle size distribution to 1.75 ⁇ m or less and exposing to a temperature range from the highest temperature to 1000 ° C. for a long time. It was found that the strength could be 5000 or less.
- an aluminum hydroxide powder having an average particle diameter of 1 ⁇ m and an aluminum oxide powder and a titanium oxide powder having a particle diameter ratio with respect to the aluminum hydroxide powder shown in Table 2 were prepared as primary materials.
- the aluminum oxide powder a powder whose cumulative particle size of 80% in the particle size distribution is 1.75 times the average particle size is used.
- Al 2 O 3 is 80 mol%
- TiO 2 is 10 mol%
- such MgO is 10 mol%
- aluminum oxide powder and a primary raw material is weighed titanium oxide powder and magnesium hydroxide powder.
- the obtained granule was filled in a mold and pressed, and then subjected to cutting to obtain a molded body having a predetermined shape.
- the obtained molded body was put in a firing furnace and fired in an air atmosphere. Note that the firing conditions were the sample No. 1 of Example 1. It was the same as 6. Then, grinding was performed after firing, and a plurality of disk-shaped samples each having an outer diameter of ⁇ 20 mm and a thickness of 5 mm were obtained.
- Sample No. Nos. 22, 23, and 26 have high creepage breakdown voltage values, and it has been found that the allowable voltage to creepage breakdown can be increased by including alumina and spinel and including titanium in the alumina and spinel. It was.
- composition formula When the composition formula is expressed as ⁇ Al 2 O 3 ⁇ ⁇ TiO 2 ⁇ ⁇ MgO, the molar percentages ⁇ , ⁇ , and ⁇ are weighed so as to have the values shown in Table 4, and the heating conditions shown in Table 4 are used as firing conditions.
- a sample was prepared as a velocity, and the peak intensity near the wavelength of 330 nm and the creeping breakdown voltage were compared in the measurement using the cathodoluminescence method. A method for manufacturing the sample is described below.
- the obtained molded body was put in a firing furnace, heated in the air atmosphere at a heating rate shown in Table 4, and fired at a maximum temperature of 1600 ° C. Then, grinding was performed after firing, and a plurality of disk-shaped samples each having an outer diameter of ⁇ 20 mm and a thickness of 5 mm were obtained.
- Example 2 measurement by the cathodoluminescence method was performed under the same conditions. Further, similarly to Example 1, metal electrodes were joined to the ends of both main surfaces of each sample by metallization, and creeping breakdown voltage was calculated, and shown in Table 4.
- composition formula is expressed as ⁇ Al 2 O 3 ⁇ ⁇ TiO 2 ⁇ ⁇ MgO
- the molar percentages ⁇ , ⁇ , and ⁇ are weighed so as to have the values shown in Table 5, and the temperature drop shown in Table 5 as firing conditions.
- a sample was prepared as a velocity, and the peak intensity near the wavelength of 420 nm and the initial creeping voltage were compared in the measurement using the cathodoluminescence method. A method for manufacturing the sample is described below.
- the difference from Example 4 is that the average particle size of titanium oxide is the value shown in Table 5 in terms of the ratio (particle size ratio) to the particle size of aluminum oxide, and the average particle size of magnesium hydroxide The diameter is 1 ⁇ m, and the cooling rate from the maximum temperature to 800 ° C. is the value shown in Table 5.
- Example 5 measurement by the cathodoluminescence method was performed under the same conditions, and the peak intensity around 420 nm is shown in Table 5.
- metal electrodes were metallized on the ends of both main surfaces of each sample, and the voltage applied was applied when gradually applying a high voltage in the same manner as when measuring the creeping dielectric breakdown voltage.
- the initial creeping voltage is calculated by dividing the voltage when the electrons emitted by the first reaches the end point of the creeping distance along the surface by the creeping distance (sample thickness 5 mm), which is the distance between the metal electrodes.
- the results are shown in Table 5.
- the molar ratio of Al 2 O 3 , TiO 2 , and MgO was determined in the same manner as in Example 2, and the results are shown in Table 5.
- the initial creeping arrival voltage is a value of 4 kV / mm or more, and the beginning of creeping breakdown when a voltage is applied.
- composition of Al 2 O 3 , TiO 2 , and MgO was changed to the sample No. 38, 53, 62, Al 2 O 3 / MgO particle size ratio and Al 2 O 3 / TiO 2 particle size ratio are both 1.05, and the rate of temperature rise to the maximum temperature during firing is 100 ° C.
- Sample A composition equivalent to sample No. 38
- B composition equivalent to sample No. 38
- C composition equivalent to sample No. 62
- the samples A, B, and C were measured by the cathodoluminescence method as in the previous example. Further, the creeping breakdown voltage and the initial creeping voltage were measured.
- the peak intensity around the wavelength of 330 nm was 80, the peak intensity around the wavelength of 420 nm was 45, the creeping breakdown voltage reached 17.8 kV / mm, and the initial creeping voltage reached 10.5 kV / mm.
- the peak intensity around the wavelength of 330 nm was 250, the peak intensity around the wavelength of 420 nm was 72, the creeping breakdown voltage was 17.3 kV / mm, and the initial creeping voltage was 9.2 kV / mm.
- the peak intensity near the wavelength of 330 nm was 2650
- the peak intensity near the wavelength of 420 nm was 153
- the creeping breakdown voltage was 10.6 kV / mm
- the initial creeping voltage was 4.6 kV / mm.
- samples having ⁇ / ⁇ values in the composition formula shown in Table 6 were prepared, and the peak intensity near the wavelength of 330 nm and the creeping breakdown voltage reached were compared in the measurement using the cathodoluminescence method.
- a sample was prepared in the same manner as in Example 1 except that the particle size ratio of Al 2 O 3 / MgO was 1.05, the temperature elevation rate was 100 ° C./h, and the ⁇ / ⁇ values were varied.
- Sample No. Nos. 120 to 124 have a small peak intensity near the wavelength of 330 nm in the measurement using the cathodoluminescence method and a large creepage breakdown voltage, and the value of ⁇ / ⁇ in the composition formula is 0.5 or more and 2.0 or less. It turned out to be preferable.
- samples having ⁇ / ⁇ values in the composition formula shown in Table 7 were prepared, and the peak intensity near the wavelength of 420 nm and the creeping breakdown voltage in comparison using the cathodoluminescence method were compared.
- Samples were prepared in the same manner as in Example 5 except that the particle size ratio of Al 2 O 3 / TiO 2 was 1.05, the temperature drop rate was 100 ° C./h, and the ⁇ / ⁇ values were varied.
- Example 7 the measurement was performed in the same manner as in Example 5, and the results of obtaining the peak intensity and the initial creepage voltage near the wavelength of 420 nm are shown in Table 7. Further, the mol% ratio was calculated by the same method as in Example 2 and shown in Table 7. Sample No. Sample No. 127 81, sample no. Sample No. 129 No. 80, sample no. Sample No. 131 Same as 79.
- Sample No. 127 to 131 have a small peak intensity near the wavelength of 420 nm in the measurement using the cathodoluminescence method and a large initial creepage voltage, and the ⁇ / ⁇ value in the composition formula is 0.5 or more and 2.0 or less. Was found to be preferable.
- the content of silicon oxide and calcium oxide in each sample was measured using an ICP emission spectroscopic analyzer after pulverizing a part of the sample and dissolving the obtained powder in a solution such as hydrochloric acid.
- the obtained metal amounts of Al, Ti, Mg, Si and Ca were converted into Al 2 O 3 , TiO 2 , MgO, SiO 2 and CaO, respectively.
- the amounts of SiO 2 and CaO when the total of Al 2 O 3 , TiO 2 and MgO was 100% by mass were calculated and shown in Table 6.
- the composition was similar to 38.
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Abstract
Description
Claims (9)
- アルミナを主結晶とするアルミナ質焼結体からなり、カソードルミネッセンス法を用いた測定における波長330nm付近のピーク強度が5000以下であることを特徴とする高耐電圧アルミナ質焼結体。
- アルカリ土類金属およびアルミニウムからなる酸化物の結晶であるスピネルを含み、前記アルミナおよび前記スピネルに遷移金属を含んでいることを特徴とする請求項1に記載の高耐電圧アルミナ質焼結体。
- 前記遷移金属がチタンであり、前記アルカリ土類金属がマグネシウムであることを特徴とする請求項2に記載の高耐電圧アルミナ質焼結体。
- 組成式を、αAl2O3・βTiO2・γMgOと表したとき、モル%比率α,β,γが下記を満足してなり、カソードルミネッセンス法を用いた測定における波長330nm付近のピーク強度が3000以下であることを特徴とする請求項1乃至請求項3のいずれかに記載の高耐電圧アルミナ質焼結体。
80≦α≦99.8
0.1≦β≦10
0.1≦γ≦10
α+β+γ=100 - 組成式を、αAl2O3・βTiO2・γMgOと表したとき、モル%比率α,β,γが下記を満足してなり、カソードルミネッセンス法を用いた測定における波長420nm付近のピーク強度が160以下であることを特徴とする請求項1乃至請求項4のいずれかに記載の高耐電圧アルミナ質焼結体。
80≦α≦99.8
0.1≦β≦10
0.1≦γ≦10
α+β+γ=100 - 前記組成式におけるモル%比率α,β,γが下記を満足してなることを特徴とする請求項4または請求項5に記載の高耐電圧アルミナ質焼結体。
90≦α≦98.5
0.5≦β≦5
0.5≦γ≦5
α+β+γ=100 - 前記組成式におけるβとγとの比率β/γの値が0.5以上2.0以下であることを特徴とする請求項4乃至請求項6のいずれかに記載の高耐電圧アルミナ質焼結体。
- Si,Caの少なくともいずれかの酸化物を含み、前記組成式の成分100質量%に対して、それぞれSiO2,CaOに換算した値の合計が5質量%以下(0質量%を除く)であることを特徴とする請求項4乃至請求項6のいずれかに記載の高耐電圧アルミナ質焼結体。
- 請求項1乃至請求項8のいずれかに記載の高耐電圧アルミナ質焼結体に電極を備えてなることを特徴とする高耐電圧用部材。
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US14/403,752 US9548142B2 (en) | 2012-05-31 | 2013-05-31 | High-withstanding-voltage alumina sintered compact and high-withstanding-voltage member |
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JP2014144897A (ja) * | 2013-01-30 | 2014-08-14 | Kyocera Corp | アルミナ質焼結体およびこれを用いた耐電圧部材 |
JPWO2020036097A1 (ja) * | 2018-08-13 | 2021-08-10 | 京セラ株式会社 | セラミック焼結体 |
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JPWO2020036097A1 (ja) * | 2018-08-13 | 2021-08-10 | 京セラ株式会社 | セラミック焼結体 |
JP7170729B2 (ja) | 2018-08-13 | 2022-11-14 | 京セラ株式会社 | セラミック焼結体 |
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US20150136452A1 (en) | 2015-05-21 |
US9548142B2 (en) | 2017-01-17 |
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