JP2021024766A - Dielectric powder - Google Patents
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- JP2021024766A JP2021024766A JP2019146616A JP2019146616A JP2021024766A JP 2021024766 A JP2021024766 A JP 2021024766A JP 2019146616 A JP2019146616 A JP 2019146616A JP 2019146616 A JP2019146616 A JP 2019146616A JP 2021024766 A JP2021024766 A JP 2021024766A
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- 239000000843 powder Substances 0.000 title claims abstract description 47
- 150000001875 compounds Chemical class 0.000 claims abstract description 71
- 239000011164 primary particle Substances 0.000 claims abstract description 17
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 7
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 6
- 239000011575 calcium Substances 0.000 claims description 26
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- -1 phosphoric acid compound Chemical class 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- QSGNKXDSTRDWKA-UHFFFAOYSA-N zirconium dihydride Chemical compound [ZrH2] QSGNKXDSTRDWKA-UHFFFAOYSA-N 0.000 claims description 3
- 229910000568 zirconium hydride Inorganic materials 0.000 claims description 3
- 239000002002 slurry Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000010304 firing Methods 0.000 description 5
- 239000011324 bead Substances 0.000 description 4
- 239000003985 ceramic capacitor Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- DJOYTAUERRJRAT-UHFFFAOYSA-N 2-(n-methyl-4-nitroanilino)acetonitrile Chemical compound N#CCN(C)C1=CC=C([N+]([O-])=O)C=C1 DJOYTAUERRJRAT-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910001467 sodium calcium phosphate Inorganic materials 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/54—Electrolytes
- H01G11/56—Solid electrolytes, e.g. gels; Additives therein
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/94—Products characterised by their shape
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/95—Products characterised by their size, e.g. microceramics
Abstract
Description
本発明は、誘電体粉末に関する。 The present invention relates to a dielectric powder.
積層セラミックコンデンサのように、誘電体粉末を用いて製造される電子部品が知られている。電子部品は、近年小型化が進んでおり、それに伴い、電子部品を製造する際に用いられる誘電体粉末も微小化が求められてきている。 Electronic components manufactured using dielectric powder, such as multilayer ceramic capacitors, are known. In recent years, electronic components have been miniaturized, and along with this, the dielectric powder used in manufacturing electronic components is also required to be miniaturized.
しかしながら、誘電体粉末は、その製造過程で加えられる熱により粒成長してしまい、さらなる微小化が難しいという問題がある。 However, the dielectric powder has a problem that it is difficult to further miniaturize it because the particles grow due to the heat applied in the manufacturing process.
本発明は、上記課題を解決するものであり、加熱されたときの粒成長を抑制して微粒化することができる誘電体粉末を提供することを目的とする。 An object of the present invention is to solve the above-mentioned problems, and to provide a dielectric powder capable of suppressing grain growth when heated and atomizing.
本発明の誘電体粉末は、少なくともＣａおよびＺｒを含むペロブスカイト型化合物と、Ｐを含む化合物とを含むことを特徴とする。 The dielectric powder of the present invention is characterized by containing at least a perovskite-type compound containing Ca and Zr, and a compound containing P.
比表面積は５ｍ2／ｇ以上４０ｍ2／ｇ以下であり、かつ、一次粒子径が３０ｎｍ以上３００ｎｍ以下であってもよい。 The specific surface area may be 5 m 2 / g or more and 40 m 2 / g or less, and the primary particle diameter may be 30 nm or more and 300 nm or less.
前記ペロブスカイト型化合物を作製するために用いられるＣａ化合物の一次粒子径は、２０ｎｍ以上１５０ｎｍ以下であってもよい。 The primary particle size of the Ca compound used to prepare the perovskite-type compound may be 20 nm or more and 150 nm or less.
前記ペロブスカイト型化合物を作製するために用いられるＺｒ化合物の一次粒子径は、２ｎｍ以上５０ｎｍ以下であってもよい。 The primary particle size of the Zr compound used to prepare the perovskite-type compound may be 2 nm or more and 50 nm or less.
前記Ｐは、前記Ｚｒ１００モル部に対して０．００１モル部以上１０モル部以下含まれていてもよい。 The P may be contained in an amount of 0.001 mol or more and 10 mol or less with respect to 100 mol of Zr.
前記ペロブスカイト型化合物を作製するために用いられるＣａ化合物は、炭酸カルシウムおよび水酸化カルシウムのうちの少なくとも一方であってもよい。 The Ca compound used to prepare the perovskite-type compound may be at least one of calcium carbonate and calcium hydroxide.
前記ペロブスカイト型化合物を作製するために用いられるＺｒ化合物は、酸化ジルコニウムおよび水酸化ジルコニウムのうちの少なくとも一方であってもよい。 The Zr compound used to prepare the perovskite-type compound may be at least one of zirconium oxide and zirconium hydride.
前記Ｐを含む化合物は、リン酸化合物であってもよい。 The compound containing P may be a phosphoric acid compound.
上記誘電体粉末は、前記Ｃａを含むＣａ化合物、前記Ｚｒを含むＺｒ化合物、および、Ｐを含む化合物の混合物を７００℃以上１５００℃以下の温度で熱処理することによって作製することができる。その場合、前記熱処理の後に粉砕するようにしてもよい。 The dielectric powder can be produced by heat-treating a mixture of the Ca compound containing Ca, the Zr compound containing Zr, and the compound containing P at a temperature of 700 ° C. or higher and 1500 ° C. or lower. In that case, it may be pulverized after the heat treatment.
本発明によれば、加熱時の粒成長を抑制して微粒化することができる誘電体粉末を提供することができる。 According to the present invention, it is possible to provide a dielectric powder capable of suppressing grain growth during heating and atomizing.
以下に本発明の実施形態を示して、本発明の特徴を具体的に説明する。 Embodiments of the present invention will be shown below, and the features of the present invention will be specifically described.
本発明の誘電体粉末は、下記の要件（以下、本発明の要件と呼ぶ）、すなわち、少なくともＣａおよびＺｒを含むペロブスカイト型化合物と、Ｐを含む化合物とを含むという要件を満たす。少なくともＣａおよびＺｒを含むペロブスカイト型化合物は、例えばＣａＺｒＯ3である。誘電体粉末がＰを含む化合物を含有することにより、加熱による粒成長を抑制することができる。 The dielectric powder of the present invention satisfies the following requirements (hereinafter referred to as the requirements of the present invention), that is, a requirement that a perovskite-type compound containing at least Ca and Zr and a compound containing P are contained. The perovskite-type compound containing at least Ca and Zr is, for example, CaZrO 3 . When the dielectric powder contains a compound containing P, grain growth due to heating can be suppressed.
本発明の誘電体粉末において、比表面積は５ｍ2／ｇ以上４０ｍ2／ｇ以下であり、かつ、一次粒子径が３０ｎｍ以上３００ｎｍ以下であることが好ましい。微粒化すると、粒子の結晶性が低下する場合があるが、後述するように、比表面積を４０ｍ2／ｇ以下とすることにより、結晶性の低下を抑制することができる。 In the dielectric powder of the present invention, the specific surface area is preferably 5 m 2 / g or more and 40 m 2 / g or less, and the primary particle size is preferably 30 nm or more and 300 nm or less. When atomized, the crystallinity of the particles may decrease, but as will be described later, the decrease in crystallinity can be suppressed by setting the specific surface area to 40 m 2 / g or less.
本発明の誘電体粉末において、Ｐは、Ｚｒ１００モル部に対して、０．００１モル部以上１０モル部以下含まれていることが好ましい。 In the dielectric powder of the present invention, P is preferably contained in an amount of 0.001 mol part or more and 10 mol part or less with respect to 100 mol parts of Zr.
上述した誘電体粉末は、例えば、一次粒子径が２０ｎｍ以上１５０ｎｍ以下であるＣａ化合物、一次粒子径が２ｎｍ以上５０ｎｍ以下であるＺｒ化合物、および、Ｐを含む化合物を用いて製造することができる。 The above-mentioned dielectric powder can be produced, for example, using a Ca compound having a primary particle size of 20 nm or more and 150 nm or less, a Zr compound having a primary particle size of 2 nm or more and 50 nm or less, and a compound containing P.
上記Ｃａ化合物は、Ｃａを含む化合物であって、例えば、炭酸カルシウムおよび水酸化カルシウムのうちの少なくとも一方である。また、上記Ｚｒ化合物は、Ｚｒを含む化合物であって、例えば、酸化ジルコニウムおよび水酸化ジルコニウムのうちの少なくとも一方である。また、Ｐを含む化合物は、例えば、リン酸化合物である。 The Ca compound is a compound containing Ca, and is, for example, at least one of calcium carbonate and calcium hydroxide. The Zr compound is a compound containing Zr, and is, for example, at least one of zirconium oxide and zirconium hydride. The compound containing P is, for example, a phosphoric acid compound.
本発明の誘電体粉末は、上述したＣａを含むＣａ化合物、Ｚｒを含むＺｒ化合物、および、Ｐを含む化合物を混合した混合物を７００℃以上１５００℃以下の温度で熱処理し、熱処理後に粉砕することによって作製することができる。 The dielectric powder of the present invention is obtained by heat-treating a mixture of the above-mentioned Ca compound containing Ca, Zr compound containing Zr, and a compound containing P at a temperature of 700 ° C. or higher and 1500 ° C. or lower, and then pulverizing the mixture. Can be produced by.
本発明の誘電体粉末は、積層セラミックコンデンサなどの電子部品の製造に用いることができる。 The dielectric powder of the present invention can be used in the manufacture of electronic components such as multilayer ceramic capacitors.
＜実施例＞
初めに、一次粒子径が２０ｎｍ以上１５０ｎｍ以下で、比表面積が７ｍ2／ｇ以上６０ｍ2／ｇ以下であるＣａ化合物と、一次粒子径が２ｎｍ以上５０ｎｍ以下で、比表面積が１０ｍ2／ｇ以上２００ｍ2／ｇ以下であるＺｒ化合物と、Ｐを含む化合物とを用意した。ここでは、Ｃａ化合物として炭酸カルシウムを用意し、Ｚｒ化合物として酸化ジルコニウムを用意した。
<Example>
First, a Ca compound having a primary particle size of 20 nm or more and 150 nm or less and a specific surface area of 7 m 2 / g or more and 60 m 2 / g or less, and a primary particle diameter of 2 nm or more and 50 nm or less and a specific surface area of 10 m 2 / g or more. A Zr compound having a thickness of 200 m 2 / g or less and a compound containing P were prepared. Here, calcium carbonate was prepared as the Ca compound, and zirconium oxide was prepared as the Zr compound.
続いて、用意したＣａ化合物とＺｒ化合物とを溶媒に投入して溶解させ、スラリーを作製した。溶媒として、純水を用いた。溶媒に投入するＣａ化合物とＺｒ化合物とのモル比（Ｃａ化合物／Ｚｒ化合物）は、０．９８０以上１．０２５以下であることが好ましく、０．９９３以上１．０１４以下であることがより好ましい。 Subsequently, the prepared Ca compound and Zr compound were put into a solvent and dissolved to prepare a slurry. Pure water was used as the solvent. The molar ratio of the Ca compound to the Zr compound (Ca compound / Zr compound) charged into the solvent is preferably 0.980 or more and 1.025 or less, and more preferably 0.993 or more and 1.014 or less. ..
続いて、作製したスラリーに、Ｐを含む化合物を添加してボールミルで混合した後、ビーズミルにより粉砕し、攪拌しながら、７０℃以上３００℃以下の温度で乾燥させた。Ｐを含む化合物は、リン酸化合物であり、ここではリン酸水素アンモニウムを用いた。ただし、リン酸化合物がリン酸水素アンモニウムに限定されることはなく、リン酸ナトリウム、リン酸カルシウムなどを用いることもできる。 Subsequently, a compound containing P was added to the prepared slurry, mixed with a ball mill, pulverized with a bead mill, and dried at a temperature of 70 ° C. or higher and 300 ° C. or lower while stirring. The compound containing P was a phosphoric acid compound, and here, ammonium hydrogen phosphate was used. However, the phosphoric acid compound is not limited to ammonium hydrogen phosphate, and sodium phosphate, calcium phosphate and the like can also be used.
その後、生成物をふるいにかけてから熱処理、具体的には、７００℃以上１５００℃以下の温度で焼成した。焼成温度が７００℃未満の場合には、合成不足となり、１５００℃より高い場合には、粒成長が抑制されにくくなる。 Then, the product was sieved and then heat-treated, specifically, fired at a temperature of 700 ° C. or higher and 1500 ° C. or lower. If the firing temperature is less than 700 ° C., the synthesis becomes insufficient, and if the firing temperature is higher than 1500 ° C., grain growth is less likely to be suppressed.
その後、焼生物を水溶液に混ぜてスラリーにした後、ビーズミルで粉砕することによって、誘電体粉末を得た。この誘電体粉末において、Ｐは、Ｚｒ１００モル部に対して０．００１部モル以上１０モル部以下含まれている。Ｐの含有量がＺｒ１００モル部に対して０．００１モル部未満の場合には、焼成時に粒成長が抑制されるという効果が得られにくく、１０モル部より多い場合には、結晶性が悪化し、Ｐを入れすぎているので、ジルコニアとカルシウムが接触しなくなり、ジルコン酸カルシウムを得にくい。したがって、セラミックコンデンサの材料として意味をなさなくなる。 Then, the roasted organism was mixed with an aqueous solution to form a slurry, which was then pulverized with a bead mill to obtain a dielectric powder. In this dielectric powder, P is contained in an amount of 0.001 part mol or more and 10 mol part or less with respect to 100 mol part of Zr. When the P content is less than 0.001 mol part with respect to 100 mol part of Zr, it is difficult to obtain the effect of suppressing grain growth during firing, and when it is more than 10 mol part, the crystallinity deteriorates. However, since P is added too much, zirconia and calcium do not come into contact with each other, making it difficult to obtain calcium zirconate. Therefore, it becomes meaningless as a material for ceramic capacitors.
ここで、試料番号２の誘電体粉末の作製方法において、より詳しい数値を補足しておく。初めに、Ｃａ化合物とＺｒ化合物とを溶媒に投入して溶解させ、スラリーを作製した。溶媒として、純水を用いた。溶媒に投入するＣａ化合物とＺｒ化合物とのモル比（Ｃａ化合物／Ｚｒ化合物）は１．０００とした。作製したスラリーに、Ｐを含む化合物を添加してボールミルで混合した後、ビーズミルにより粉砕し、攪拌しながら、１００℃の温度で乾燥させた。Ｐを含む化合物は、リン酸化合物であり、ここではリン酸水素アンモニウムを用いた。生成物をふるいにかけてから１０００℃の温度で焼成し、焼生物を水溶液に混ぜてスラリーにした後、ビーズミルで粉砕することによって、誘電体粉末を得た。 Here, more detailed numerical values will be supplemented in the method for producing the dielectric powder of sample number 2. First, the Ca compound and the Zr compound were put into a solvent and dissolved to prepare a slurry. Pure water was used as the solvent. The molar ratio (Ca compound / Zr compound) of the Ca compound and the Zr compound added to the solvent was 1.000. A compound containing P was added to the prepared slurry, mixed with a ball mill, pulverized with a bead mill, and dried at a temperature of 100 ° C. with stirring. The compound containing P was a phosphoric acid compound, and here, ammonium hydrogen phosphate was used. The product was sieved and then fired at a temperature of 1000 ° C., the calcined organism was mixed with an aqueous solution to form a slurry, and then pulverized with a bead mill to obtain a dielectric powder.
ここでは、Ｐの添加量の異なる複数種類の誘電体粉末を作製して、比表面積およびＸ線回折によるＣａＺｒＯ3の第二ピークの半値幅を測定した。比表面積は、例えば、流動法やＢＥＴ１点法などにより測定することができる。また、Ｘ線回折によるＣａＺｒＯ3の第二ピークの半値幅は、数値が低い方が結晶性が高いことを意味する。作製した試料番号１〜１５の誘電体粉末の比表面積、一次粒子径の平均値、Ｘ線回折によるＣａＺｒＯ3の第二ピークの半値幅、および、Ｐの添加量を表１に示す。Ｐの添加量は、Ｚｒ１００モル部に対するモル量である。 Here, a plurality of types of dielectric powders having different amounts of P added were prepared, and the specific surface area and the half width of the second peak of CaZrO 3 by X-ray diffraction were measured. The specific surface area can be measured by, for example, a flow method or a BET one-point method. Further, the half width of the second peak of CaZrO 3 by X-ray diffraction means that the lower the value, the higher the crystallinity. Table 1 shows the specific surface area of the prepared dielectric powders of Sample Nos. 1 to 15, the average value of the primary particle size, the half width of the second peak of CaZrO 3 by X-ray diffraction, and the amount of P added. The amount of P added is a molar amount with respect to 100 mol parts of Zr.
表１において、試料番号に＊が付されていない試料番号２〜１５の誘電体粉末は、本発明の要件を満たす誘電体粉末であり、試料番号に＊が付されている試料番号１の誘電体粉末は、本発明の要件を満たしていない誘電体粉末である。 In Table 1, the dielectric powders of sample numbers 2 to 15 without * in the sample number are dielectric powders satisfying the requirements of the present invention, and the dielectrics of sample number 1 in which * is added to the sample number. The body powder is a dielectric powder that does not meet the requirements of the present invention.
Ｐを含有しておらず、本発明の要件を満たしていない試料番号１の誘電体粉末は、焼成時に粒成長が進み、結晶粒が粗大化する。 The dielectric powder of Sample No. 1, which does not contain P and does not satisfy the requirements of the present invention, undergoes grain growth during firing and the crystal grains become coarse.
これに対して、Ｐを含む化合物を含有しており、本発明の要件を満たす試料番号２〜１５の誘電体粉末は、焼成時の粒成長が抑制される。したがって、本発明の要件を満たす誘電体粉末を用いて、積層セラミックコンデンサのような電子部品を製造すると、誘電体層を薄層化することができ、特性の優れた電子部品を製造することができる。 On the other hand, the dielectric powders of sample numbers 2 to 15 containing a compound containing P and satisfying the requirements of the present invention suppress grain growth during firing. Therefore, when an electronic component such as a multilayer ceramic capacitor is manufactured using a dielectric powder satisfying the requirements of the present invention, the dielectric layer can be thinned, and an electronic component having excellent characteristics can be manufactured. it can.
また、本発明の要件を満たす誘電体粉末のうち、比表面積が５ｍ2／ｇ以上４０ｍ2／ｇ以下であり、かつ、一次粒子径が３０ｎｍ以上３００ｎｍ以下である、試料番号２〜１４の誘電体粉末は、Ｘ線回折によるＣａＺｒＯ3の第二ピークの半値幅が１．０未満であり、結晶性が高い。したがって、本発明の要件を満たす誘電体粉末は、比表面積が５ｍ2／ｇ以上４０ｍ2／ｇ以下であり、かつ、一次粒子径が３０ｎｍ以上３００ｎｍ以下であることが好ましい。 Further, among the dielectric powders satisfying the requirements of the present invention, the dielectrics of sample numbers 2 to 14 having a specific surface area of 5 m 2 / g or more and 40 m 2 / g or less and a primary particle size of 30 nm or more and 300 nm or less. The body powder has a half-value width of the second peak of CaZrO 3 by X-ray diffraction of less than 1.0, and has high crystallinity. Therefore, the dielectric powder satisfying the requirements of the present invention preferably has a specific surface area of 5 m 2 / g or more and 40 m 2 / g or less and a primary particle size of 30 nm or more and 300 nm or less.
一方、表１に示すように、比表面積が４０ｍ2／ｇより大きい試料番号１５の誘電体粉末は、Ｘ線回折によるＣａＺｒＯ3の第二ピークの半値幅が１．０より大きく、結晶性が低い。 On the other hand, as shown in Table 1, the dielectric powder of sample number 15 having a specific surface area larger than 40 m 2 / g has a half width of the second peak of CaZrO 3 by X-ray diffraction larger than 1.0 and crystallinity. Low.
本発明は、上記実施形態に限定されるものではなく、本発明の範囲内において、種々の応用、変形を加えることが可能である。 The present invention is not limited to the above embodiment, and various applications and modifications can be added within the scope of the present invention.
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