WO2011155319A1 - 回路基板用窒化アルミニウム基板及びその製造方法 - Google Patents
回路基板用窒化アルミニウム基板及びその製造方法 Download PDFInfo
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Definitions
- the present invention relates to an aluminum nitride substrate having excellent insulation characteristics at high temperatures and a method for producing the same.
- aluminum nitride substrates with excellent insulation used for semiconductor-mounted circuit boards are used in various fields, such as drive control and industrial applications such as electric railways and electric vehicles. It is used as a substrate material for control of industrial robots. Among them, it is highly reliable as a material to replace the currently used Si chip for the development of next-generation semiconductors with features such as switching loss and energy loss that greatly affect product reliability, and extended control operating temperature. Promising SiC chips are promising. Since the operable temperature of the SiC chip is around 400 ° C., which is higher than the conventional 150 ° C., the aluminum nitride substrate used as an insulating material for the circuit board for semiconductor mounting is excellent even at such a high temperature. It is required to exhibit insulating properties.
- an aluminum nitride sintered body used as the aluminum nitride substrate is generally manufactured by the following method. That is, additives such as a sintering aid, a binder, a plasticizer, a dispersion medium, and a release agent are mixed with the aluminum nitride powder. It is formed into a sheet by extrusion or the like, and processed into a desired shape and size by a press machine (molding / pressing). Next, the molded body is heated to 350 to 700 ° C. in air or in a non-oxidizing atmosphere such as nitrogen to remove the binder (degreasing), and then 0.degree. C. at 1800 to 1900 ° C. in a non-oxidizing atmosphere such as nitrogen. Manufactured by holding (sintering) for 5-10 hours.
- additives such as a sintering aid, a binder, a plasticizer, a dispersion medium, and a release agent are mixed with the aluminum nitride powder. It is formed into a
- the breakdown voltage of the aluminum nitride substrate manufactured by such a method shows high insulation characteristics of about 30 to 40 kV / mm at room temperature, but decreases to around 10 kV / mm at a high temperature of 400 ° C. There was a problem that.
- Patent Document 1 A method of dissolving solid titanium in aluminum nitride crystal particles to increase the unpaired electron concentration (Patent Document 1), A method of controlling the average diameter of aluminum nitride crystal grains and grain boundary pores, and the ratio of grain boundary pores to intragranular pores (Patent Document 2) has been proposed.
- Patent Document 2 A method of controlling the average diameter of aluminum nitride crystal grains and grain boundary pores, and the ratio of grain boundary pores to intragranular pores.
- An object of the present invention is to provide an aluminum nitride substrate having excellent insulating properties at high temperatures and a method for producing the same.
- a dendritic grain boundary phase in an aluminum nitride substrate for circuit boards having aluminum nitride crystal particles having an average particle diameter of 2 to 5 ⁇ m and a thermal conductivity of 170 W / m ⁇ K or more, a dendritic grain boundary phase There is provided an aluminum nitride substrate for a circuit board having a dielectric breakdown voltage at 400 ° C. of 30 kV / mm or more.
- the grain boundary phase is a non-dendritic grain boundary phase dispersed discontinuously.
- the cumulative 10% particle diameter d10 in the number-based particle size distribution of the grain boundary phase measured from the mirror polished surface of the aluminum nitride substrate is 0.6 ⁇ m or more, and the cumulative 50% particle diameter d50 is 1. 6 ⁇ m or less.
- the raw material containing aluminum nitride powder is heated to 1500 ° C. at a pressure of 150 Pa or lower, and then heated to 1700-1900 ° C. as a pressurized atmosphere with a non-oxidizing gas at a pressure of 0.4 MPa or higher.
- a method of manufacturing an aluminum nitride substrate for circuit boards having a dielectric breakdown voltage of 30 kV / mm or more at 400 ° C. comprising a step of cooling to 1600 ° C. at a cooling rate of 10 ° C./min or less after holding.
- the aluminum nitride powder is not particularly limited, but in one embodiment, as impurities, the oxygen content is 1.2 mass% or less, the carbon content is 0.04 mass% or less, the Fe content is 30 ppm or less, A powder having a Si content of 60 ppm or less is exemplified.
- the raw material usually includes a sintering aid, and as such a sintering aid, in one embodiment, a rare earth metal compound, an alkaline earth metal compound, or a transition metal compound is used.
- an aluminum nitride substrate for circuit boards that can be manufactured by the above-described manufacturing method, that is, a raw material containing aluminum nitride powder is heated to 1500 ° C. at a pressure of 150 Pa or less, and then a non-oxidizing pressure of 0.
- An aluminum nitride substrate for a circuit board to be manufactured is also provided by raising and maintaining a pressure atmosphere of 4 MPa or higher up to 1700 to 1900 ° C. and then cooling to 1600 ° C. at a cooling rate of 10 ° C./min or less.
- an aluminum nitride substrate which is excellent in insulation characteristics at high temperatures and suitable for circuit boards, and a method for producing the same.
- An aluminum nitride substrate for a circuit board according to the present invention comprises aluminum nitride crystal grains and a grain boundary phase filling a space between the grains, and has a thermal conductivity of 170 W / m ⁇ K or more at 400 ° C.
- the dielectric breakdown voltage has the meaning normally understood by those skilled in the art.
- JIS C2110 a voltage is applied to the sample, and the voltage when the dielectric breakdown occurs is divided by the thickness of the sample. Can be obtained.
- the average particle diameter of the aluminum nitride crystal particles is preferably 2 to 5 ⁇ m.
- the average particle diameter of the aluminum nitride crystal particles can be determined from the average value of the number of measurements by measuring the particle diameter observed on the fracture surface of the aluminum nitride substrate using a scanning electron microscope.
- the average particle diameter of the aluminum nitride crystal particles is less than 2 ⁇ m, the aluminum nitride substrate is not sufficiently densified, and the thermal conductivity may be lowered.
- the average particle diameter of the aluminum nitride crystal particles exceeds 5 ⁇ m, voids between the aluminum nitride crystal particles become large, and the voids cannot be sufficiently filled with the grain boundary phase. May decrease.
- the aluminum nitride crystal particles are likely to break in the grain at the time of stress load, leading to a decrease in mechanical strength.
- the aluminum nitride substrate of the present invention is an aluminum nitride substrate characterized by not containing a dendritic grain boundary phase.
- the grain boundary phase is a non-dendritic grain boundary phase. It is characterized by. That is, as a result of intensive investigations to achieve improvement in insulation characteristics at high temperatures, the present inventor has made a dendritic shape on the aluminum nitride substrate whose dielectric breakdown voltage at 400 ° C. is below 30 kV / mm. While many grain boundary phases are observed, the dendritic grain boundary phase is not observed at all on the aluminum nitride substrate having a breakdown voltage exceeding 30 kV / mm, and the grain boundary phase is composed of many grain boundary phases.
- the shape of the grain boundary phase is, for example, that 1 g of aluminum nitride substrate is placed in 50 ml of 20% aqueous sodium hydroxide solution, held at 130 ° C. for 12 hours, and allowed to stand until the aluminum nitride crystal particles are dissolved. It can be confirmed by removing the grain boundary phase remaining by filtration, washing and observing with a scanning electron microscope.
- the “dendritic grain boundary phase” referred to here is a grain boundary phase having a shape in which a plurality of grain boundary phases are three-dimensionally connected.
- such a dendritic grain boundary phase portion is not included in the grain boundary phase, and the grain boundary phase is a non-dendritic shape in which many grain boundary phases are discontinuously dispersed. It is a grain boundary phase.
- the micrograph in FIG. 1 shows an example in which the above-described dendritic grain boundary phase is observed, and the micrograph in FIG. 2 does not include the dendritic grain boundary phase and the grain boundary phase is discontinuous. An example is shown in which a dispersed non-dendritic grain boundary phase is observed.
- the following two can be inferred as the influence of the dendritic grain boundary phase on the insulating properties of the aluminum nitride substrate at high temperatures.
- the first is the presence of minute voids caused by the difference in thermal expansion coefficient between the aluminum nitride crystal grains constituting the aluminum nitride substrate and the grain boundary phase. Since the thermal expansion coefficient of the grain boundary phase at 25 to 400 ° C. is about twice that of aluminum nitride, there is a difference in expansion between the aluminum nitride crystal grains and the grain boundary phase at high temperatures. It is thought that minute strains and voids are generated due to. At this time, if there is a dendritic grain boundary phase extending in a three-dimensional manner, minute voids are continuously distributed in the aluminum nitride substrate and the insulation distance is shortened. Is estimated to decline.
- the grain boundary phase does not include a dendritic grain boundary phase and is composed of a non-dendritic discontinuous dispersed phase, the generated minute voids are not connected. It is considered that the insulation characteristics of the material do not deteriorate.
- the second is the formation of a conductive path in the grain boundary phase.
- the sintering aids used for sintering generally use alkaline earth metal compounds or rare earth metal compounds, but these sintering aids are present on the surface of the aluminum nitride powder in the early stage of sintering. It reacts with the oxide to form a complex oxide liquid phase. This liquid phase dissolves impurities in the aluminum nitride crystal grains during the sintering process. As a result, the purified aluminum nitride crystal grains grow and the sintered body structure becomes dense, which leads to high thermal conductivity and high strength of the aluminum nitride substrate.
- the liquid phase containing a large amount of impurities is cooled after the completion of sintering and precipitates as a grain boundary phase. Therefore, it is considered that the electrical insulating property of the grain boundary phase itself is lower than that of the aluminum nitride crystal particles.
- the grain boundary phase having low insulation acts as a conductive path, and the insulating properties of the aluminum nitride substrate are deteriorated.
- the aluminum nitride substrate has a cumulative 10% particle diameter d10 of 0.6 ⁇ m or more in the number-based particle diameter distribution of the grain boundary phase measured from the mirror polished surface, and a cumulative 50% particle The diameter d50 is 1.6 ⁇ m or less.
- a method for measuring the number-based particle size distribution of the grain boundary phase will be described below. That is, an aluminum nitride substrate is embedded in an epoxy resin and solidified, then cut so as to be perpendicular to the thickness direction of the substrate, and the cross section is mirror polished by buffing. The number-based particle size distribution can be determined by observing the polished surface with a scanning electron microscope and measuring the particle size of the grain boundary phase from the image with image analysis software.
- the cumulative 10% particle diameter d10 is less than 0.6 ⁇ m
- a part of the grain boundary phase in the aluminum nitride substrate may exist as a dendritic shape, and when the cumulative 50% particle diameter d50 exceeds 1.6 ⁇ m,
- the grain boundary phases are connected as agglomerated aggregates. In either case, there is a risk that the insulating properties of the aluminum nitride substrate at high temperatures may be deteriorated due to the influence of the grain boundary phase described above.
- the aluminum nitride substrate according to the present invention does not contain a dendritic grain boundary phase, it has excellent insulating properties at high temperatures, but the grain boundary phase is non-dendritic. Any method may be used as long as it can be formed. However, as a result of earnest research, the present inventor can surely form the grain boundary phase in a non-dendritic state only by setting the conditions such as the furnace pressure during cooling and the cooling rate as specific conditions. It has been found that an aluminum nitride substrate having a breakdown voltage at 400 ° C. of 30 kV / mm or more can be produced.
- the manufacturing method of the aluminum nitride substrate according to the present invention is as follows.
- (Ii) The raw material is heated to 1500 ° C. at a pressure of 150 Pa or less, then heated to 1700 to 1900 ° C. as a pressurized atmosphere with a non-oxidizing gas pressure of 0.4 MPa or more, and then held at 10 ° C. to 1600 ° C.
- the aluminum nitride powder is not particularly limited, and an aluminum nitride powder produced by a known method such as a direct nitriding method in which metal aluminum is nitrided in a nitrogen atmosphere or a reducing nitriding method in which alumina is reduced with carbon can be used. However, among these, those having high purity and fine powder are preferable.
- the impurities those having an oxygen content of 1.2 mass% or less, a carbon content of 0.04 mass% or less, an Fe content of 30 ppm or less, and an Si content of 60 ppm or less are preferably used.
- the maximum particle size is more preferably 20 ⁇ m or less.
- oxygen is basically an impurity, but has an action of preventing excessive sintering. Therefore, in order to prevent strength reduction of the sintered body due to excessive sintering, the oxygen content is It is preferable to use a material of 0.7% by mass or more.
- the sintering aid is not particularly limited, and rare earth metal compounds, alkaline earth metal compounds, transition metal compounds, and the like can be used. Among these, yttrium oxide or a combination of yttrium oxide and aluminum oxide is preferable. These sintering aids react with the aluminum nitride powder to form a composite oxide liquid phase (for example, 2Y2O3 ⁇ Al2O3, Y2O3 ⁇ Al2O3, 3Y2O3 ⁇ 5Al2O3, etc.), and this liquid phase increases the density of the sintered body. At the same time, oxygen, which is an impurity in the aluminum nitride crystal grains, is extracted and segregated as an oxide phase at the grain boundaries, thereby achieving high thermal conductivity.
- a composite oxide liquid phase for example, 2Y2O3 ⁇ Al2O3, Y2O3 ⁇ Al2O3, 3Y2O3 ⁇ 5Al2O3, etc.
- the aluminum nitride powder and the sintering aid are mixed by a mixing device, a binder is added to the mixed raw material powder, and then molded by sheet molding or the like to obtain a molded body. This is further degreased to obtain a degreased body as a raw material for sintering.
- the mixing method of aluminum nitride powder or the like is not particularly limited, and a known mixing apparatus such as a ball mill, a rod mill, or a mixer can be used.
- the binder is not particularly limited, but it is preferable to use a methylcellulose-based binder having plasticity or a surface-active effect or an acrylate ester-based binder excellent in thermal decomposability.
- a plasticizer, a dispersion medium, etc. are used together as needed. In one example, glycerin or the like is used as the plasticizer, and ion-exchanged water or ethanol is used as the dispersion medium.
- the method for degreasing the molded sheet is not particularly limited, but it is preferable to remove the binder by heating the molded sheet to 300 to 700 ° C. in a non-oxidizing atmosphere such as air or nitrogen.
- the degreasing time needs to be appropriately determined according to the size of the molded sheet and the number of processed sheets, but is usually 1 to 10 hours.
- the temperature is raised to 1700 to 1900 ° C. and held as a pressurized atmosphere of 0.4 MPa or more in a non-oxidizing atmosphere.
- a pressurized atmosphere of 0.4 MPa or more As a result, an aluminum nitride sintered body having high thermal conductivity and improved insulation characteristics can be obtained.
- the liquid phase sintering aid is less likely to volatilize, and void generation between aluminum nitride crystal particles can be effectively suppressed. It is considered that the insulating properties of the substrate can be improved.
- the non-oxidizing atmosphere means an inert gas atmosphere or a reducing atmosphere that does not contain an oxidizing gas such as oxygen.
- the grain boundary phase precipitates so as to fill the voids existing between the aluminum nitride crystal grains, so that the grain boundary phases are not connected to each other, and the dendritic grain boundaries Phase precipitation can be suppressed.
- the grain boundary phase precipitates while relaxing the strain between the aluminum nitride crystal grains, it is considered that the resulting aluminum nitride substrate is suppressed from generating microcracks at high temperature and has improved insulating properties. After the slow cooling to 1600 ° C. is completed, it can be rapidly cooled to room temperature as in the prior art.
- the pressure in the furnace is preferably 0.4 MPa or more, and if it is less than 0.4 MPa, the liquid phase sintering aid volatilizes before being precipitated as a grain boundary phase, and voids are formed between aluminum nitride crystal particles. As a result, the insulating properties of the aluminum nitride substrate are degraded.
- the cooling method can be carried out by controlling the heater temperature of the sintering furnace.
- Example 1 3 parts by mass of yttrium oxide powder was added to 97 parts by mass of aluminum nitride powder and mixed for 1 hour in a ball mill to obtain a mixed powder. To 100 parts by mass of the mixed powder, 6 parts by mass of a cellulose ether binder, 5 parts by mass of glycerin, and 10 parts by mass of ion-exchanged water were added and mixed for 1 minute in a Henschel mixer to obtain a mixture. Next, this mixture was formed into a sheet having a thickness of 0.8 mm using a single screw extruder, and punched out to a size of 90 mm ⁇ 90 mm using a press machine with a die.
- Aluminum nitride powder Average particle size 1.2 ⁇ m, oxygen content 0.8 mass%.
- Yttrium oxide powder manufactured by Shin-Etsu Chemical Co., Ltd., trade name “Yttrium Oxide”
- Binder Shin-Etsu Chemical Co., Ltd., trade name “Metrozu”
- Glycerin Product name “Exepal” manufactured by Kao Corporation Boron nitride powder: manufactured by Denki Kagaku Kogyo Co., Ltd., trade name “DENKABORON NITRIDE MGP”
- Number-based particle size distribution of grain boundary phase The fracture surface of an aluminum nitride substrate is polished with an “automatic polishing device Ecomet 3” manufactured by Bühler, and the polished surface is magnified 500 times with a scanning electron microscope. The distribution state was observed (observation area 155 ⁇ m ⁇ 231 ⁇ m).
- FIG. 3 shows an example in which the mirror-polished surface of an aluminum nitride substrate is observed with a scanning electron microscope. The obtained image was subjected to image analysis processing by “Image-Pro Plus 6.2J” manufactured by Media Cybernetics, and a cumulative 10% particle diameter d10 and a cumulative 50% particle diameter d50 were calculated.
- Dielectric breakdown voltage at 25 ° C. and 400 ° C . It can be measured by providing an electrode in a heating furnace that can be heated to 400 ° C. and providing an AC withstand voltage measuring device. In order to eliminate the influence of the atmosphere at the time of measurement, the atmosphere in the furnace was measured with a nitrogen atmosphere of 0.3 MPa. In a heating furnace maintained at a predetermined temperature, spherical electrodes were arranged on the upper and lower surfaces of the aluminum nitride substrate, voltage was applied to the sample according to JIS C2110, and the voltage when dielectric breakdown occurred was measured. The dielectric breakdown voltage was calculated by dividing the voltage at which dielectric breakdown occurred by the thickness of the sample.
- Examples 4 and 5 An aluminum nitride substrate was obtained in the same manner as in Example 1 except that the sintering atmosphere from 1500 ° C. to the sintering temperature was changed as shown in Table 1. The results are shown in Table 1.
- Examples 6 and 7 An aluminum nitride substrate was obtained in the same manner as in Example 1 except that the sintering temperature was changed as shown in Table 1. The results are shown in Table 1.
- Example 8 and 9 An aluminum nitride substrate was obtained in the same manner as in Example 1 except that the cooling rate was changed as shown in Table 1. The results are shown in Table 1.
- an aluminum nitride substrate which is excellent in insulation characteristics at high temperatures and suitable for circuit boards, and a method for producing the same.
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Abstract
Description
上記において、一態様では、粒界相は、不連続に分散した非樹枝状の粒界相である。また別の態様では、窒化アルミニウム基板の鏡面研磨面から測定される粒界相の個数基準粒子径分布における累積10%粒子径d10が0.6μm以上であり、累積50%粒子径d50が1.6μm以下である。
ここで、窒化アルミニウム粉末は、特に限定されないが、一実施態様では、不純物として、酸素含有量が1.2質量%以下、カーボン含有量が0.04質量%以下、Fe含有量が30ppm以下、Si含有量が60ppm以下である粉末が挙げられる。また、原料には、通常は焼結助剤が含められるが、かかる焼結助剤としては、一実施態様では、希土類金属化合物、アルカリ土類金属化合物、遷移金属化合物が使用される。
(i)窒化アルミニウム粉末を含む原料を準備する原料準備工程と、
(ii)前記原料を圧力150Pa以下で1500℃まで加熱し、その後、非酸化性ガスで圧力0.4MPa以上の加圧雰囲気として1700~1900℃まで昇温、保持した後、1600℃まで10℃/分以下の冷却速度で冷却する焼結工程と
を具備する。
窒化アルミニウム粉末の他に、焼結助剤、バインダー、可塑剤、分散媒、離型剤等の添加剤が適宜使用される。窒化アルミニウム粉末は、特に限定されるものではなく、金属アルミニウムを窒素雰囲気下で窒化する直接窒化法、アルミナをカーボンで還元する還元窒化法等の公知の方法で製造された窒化アルミニウム粉末が使用できるが、中でも、高純度かつ微粉であるものが好ましい。具体的には、不純物として、酸素含有量が1.2質量%以下、カーボン含有量が0.04質量%以下、Fe含有量が30ppm以下、Si含有量が60ppm以下であるものが好適に使用され、また、最大粒子径が20μm以下であることがより好ましい。ここで、酸素は基本的には不純物であるが、焼結過多を防止する作用を有しており、よって、焼結過多による焼結体の強度低下を防止するためには、酸素含有量が0.7質量%以上のものを使用するのが好ましい。
原料準備工程(i)で得られた原料(脱脂体)を焼結して窒化アルミニウム焼結体を得る。当該工程では、先ず、焼結炉内の圧力を150Pa以下とし、1500℃まで加熱する。これにより、脱脂体中の残留カーボンが除去され、好ましい焼結体組織と熱伝導性を有する窒化アルミニウム焼結体が得られる。ここで、炉内圧力が150Paを越えると、カーボンの除去が不十分となり、また1500℃を越えて加熱すると、窒化アルミニウム結晶粒子の緻密化が一部で進行し、カーボンの拡散経路が閉ざされてしまうため、カーボンの除去が不十分となってしまう。
ここで、非酸化性雰囲気とは、酸素等の酸化性ガスを含まない不活性ガス雰囲気や還元性雰囲気等を意味する。
また、炉内の圧力は、0.4MPa以上とするのが好ましく、0.4MPa未満では液相化した焼結助剤が粒界相として析出する前に揮発し、窒化アルミニウム結晶粒子間に空隙が発生するため、窒化アルミニウム基板の絶縁特性が低下してしまう。また、冷却方法は、焼結炉のヒーター温度を制御することにより、実施できる。
窒化アルミニウム粉末97質量部に、酸化イットリウム粉末3質量部を添加し、ボールミルにおいて1時間混合して混合粉末を得た。この混合粉末100質量部にセルロースエーテル系バインダー6質量部、グリセリン5質量部、イオン交換水10質量部を添加し、ヘンシェルミキサーにおいて1分間混合し、混合物を得た。次に、この混合物を単軸押出機において厚み0.8mmのシート状に成形し、金型付きプレス機により90mm×90mmの寸法に打ち抜いた。成形シートに離型剤として窒化ホウ素粉を塗布した後、15枚を積層し、空気中において570℃で5時間加熱し脱脂した。次に、脱脂体を真空・加圧炉に移し、炉内圧力100Paで1500℃まで加熱した。その後、窒素を導入して炉内圧力0.6MPaの加圧雰囲気として1750℃まで昇温し、2時間保持した後、1600℃までを1℃/分の冷却速度で冷却し、窒化アルミニウム基板を得た。得られた窒化アルミニウム基板について、窒化アルミニウム結晶粒子の平均粒子径、樹枝状粒界相の有無、粒界相の個数基準粒子径分布、熱伝導率、25℃及び400℃における絶縁破壊電圧を評価した。結果を表1に示す。
窒化アルミニウム粉末:平均粒径1.2μm、酸素含有量0.8質量%。
酸化イットリウム粉末:信越化学工業社製、商品名「Yttrium Oxide」
バインダー:信越化学工業社製、商品名「メトローズ」
グリセリン:花王社製、商品名「エキセパール」
窒化ホウ素粉:電気化学工業社製、商品名「デンカボロンナイトライドMGP」
窒化アルミニウム結晶粒子の平均粒子径:窒化アルミニウム基板の破断面を走査型電子顕微鏡で2000倍に拡大し、50個の窒化アルミニウム結晶粒子の粒子径を測定し、平均値を算出した。
樹枝状粒界相の有無:1gの窒化アルミニウム基板を50mlの20%水酸化ナトリウム水溶液に入れ、130℃で12時間保持し、窒化アルミニウム結晶粒子が溶解するまで静置し、その後、濾過、洗浄により残留した粒界相を取り出し、走査型電子顕微鏡によって観察することで確認した。
粒界相の個数基準粒子径分布:窒化アルミニウム基板の破断面をビューラー社製「自動研磨装置エコメット3」により研磨し、その研磨面を走査型電子顕微鏡で500倍に拡大し、粒界相の分布状態を観察した(観察領域155μm×231μm)。図3に窒化アルミニウム基板の鏡面研磨面を走査型電子顕微鏡で観察した一例を示す。得られた画像をMedia Cybernetics社製「Image-Pro Plus 6.2J」により画像解析処理し、累積10%粒子径d10及び累積50%粒子径d50を算出した。
熱伝導率:アルバック理工社製「レーザーフラッシュ法熱定数測定装置TC-7000」により測定した。
25℃及び400℃における絶縁破壊電圧:400℃に加熱できる加熱炉内に電極を設け、交流耐電圧測定装置を併設することにより測定できる。測定時の雰囲気の影響を排除するために、炉内の雰囲気を窒素雰囲気0.3MPaとして測定を行った。所定の温度に保たれた加熱炉において、窒化アルミニウム基板の上下面に球状電極を配置し、JIS C2110に準じて試料に電圧を加え、絶縁破壊が生じたときの電圧を測定した。絶縁破壊が生じたときの電圧を試料の厚みで除することで絶縁破壊電圧を算出した。
1500℃までの焼結雰囲気を表1に示すように変えたこと以外は、実施例1と同様にして窒化アルミニウム基板を得た。結果を表1に示す。
1500℃から焼結温度までの焼結雰囲気を表1に示すように変えたこと以外は、実施例1と同様にして窒化アルミニウム基板を得た。結果を表1に示す。
焼結温度を表1に示すように変えたこと以外は、実施例1と同様にして窒化アルミニウム基板を得た。結果を表1に示す。
冷却速度を表1に示すように変えたこと以外は、実施例1と同様にして窒化アルミニウム基板を得た。結果を表1に示す。
焼結雰囲気と冷却速度を表1に示すように変えたこと以外は、実施例1と同様にして窒化アルミニウム基板を得た。結果を表1に示す。
1500℃までの焼結雰囲気を表1に示すように変えたこと以外は、実施例1と同様にして窒化アルミニウム基板を得た。結果を表1に示す。
1500℃から焼結温度までの焼結雰囲気を表1に示すように変えたこと以外は、実施例1と同様にして窒化アルミニウム基板を得た。結果を表1に示す。
焼結温度を表1に示すように変えたこと以外は、実施例1と同様にして窒化アルミニウム基板を得た。結果を表1に示す。
冷却速度を表1に示すように変えたこと以外は、実施例1と同様にして窒化アルミニウム基板を得た。結果を表1に示す。
Claims (5)
- 平均粒子径が2~5μmである窒化アルミニウム結晶粒子を有し、熱伝導率が170W/m・K以上である回路基板用窒化アルミニウム基板において、樹枝状の粒界相を含有せず、400℃における絶縁破壊電圧が30kV/mm以上である、回路基板用窒化アルミニウム基板。
- 粒界相が不連続に分散した非樹枝状の粒界相である、請求項1に記載の回路基板用窒化アルミニウム基板。
- 窒化アルミニウム基板の鏡面研磨面から測定される粒界相の個数基準粒子径分布における累積10%粒子径d10が0.6μm以上であり、累積50%粒子径d50が1.6μm以下である、請求項1又は2に記載の回路基板用窒化アルミニウム基板。
- 窒化アルミニウム粉末を含む原料を圧力150Pa以下で1500℃まで加熱し、その後、非酸化性ガスで圧力0.4MPa以上の加圧雰囲気として1700~1900℃まで昇温、保持した後、1600℃まで10℃/分以下の冷却速度で冷却することにより製造される、請求項1から3の何れか一項に記載の回路基板用窒化アルミニウム基板。
- 窒化アルミニウム粉末を含む原料を圧力150Pa以下で1500℃まで加熱し、その後、非酸化性ガスで圧力0.4MPa以上の加圧雰囲気として1700~1900℃まで昇温、保持した後、1600℃まで10℃/分以下の冷却速度で冷却する工程を具備する、請求項1から3の何れか一項に記載の回路基板用窒化アルミニウム基板の製造方法。
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- 2011-05-24 CN CN201180028274.6A patent/CN102933520B/zh active Active
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2020158375A (ja) * | 2019-03-28 | 2020-10-01 | 京セラ株式会社 | 窒化アルミニウム基板、電子装置及び電子モジュール |
JP2021130571A (ja) * | 2020-02-18 | 2021-09-09 | 京セラ株式会社 | 窒化アルミニウム基板、電子装置及び電子モジュール |
JP7441070B2 (ja) | 2020-02-18 | 2024-02-29 | 京セラ株式会社 | 窒化アルミニウム基板、電子装置及び電子モジュール |
Also Published As
Publication number | Publication date |
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CA2801857C (en) | 2018-01-23 |
CA2801857A1 (en) | 2011-12-15 |
TWI519503B (zh) | 2016-02-01 |
US9190189B2 (en) | 2015-11-17 |
EP2581357A4 (en) | 2014-03-05 |
CN102933520A (zh) | 2013-02-13 |
EP2581357A1 (en) | 2013-04-17 |
JP5919190B2 (ja) | 2016-05-18 |
KR101693071B1 (ko) | 2017-01-04 |
KR20130087481A (ko) | 2013-08-06 |
EP2581357B1 (en) | 2018-02-21 |
US20130149530A1 (en) | 2013-06-13 |
CN102933520B (zh) | 2015-08-19 |
TW201202170A (en) | 2012-01-16 |
JPWO2011155319A1 (ja) | 2013-08-01 |
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