JP3956074B2 - Glass powder - Google Patents

Glass powder Download PDF

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Publication number
JP3956074B2
JP3956074B2 JP36740698A JP36740698A JP3956074B2 JP 3956074 B2 JP3956074 B2 JP 3956074B2 JP 36740698 A JP36740698 A JP 36740698A JP 36740698 A JP36740698 A JP 36740698A JP 3956074 B2 JP3956074 B2 JP 3956074B2
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Japan
Prior art keywords
glass powder
green sheet
glass
boric acid
slurry
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JP36740698A
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JP2000185941A (en
Inventor
俊一 伊藤
一雄 木下
卓司 岡
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Nippon Electric Glass Co Ltd
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Nippon Electric Glass Co Ltd
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Description

【0001】
【発明の属する技術分野】
本発明は、電子部品基板用グリーンシートの作製に用いるガラス粉末に関する。
【0002】
【従来の技術】
一般に、多層基板および誘電体チップ等の電子部品基板の作製には、グリーンシートが使用される。グリーンシートの作製には、図2に示すように、ドクターブレード法によるグリーンシート成形装置が用いられる。この装置は、キャリヤフィルム1が供給ロール1aから引き出され、複数の支持ローラー2上を搬送され、このキャリヤフィルム1の上方に、ドクターブレード3aを具備し、ガラス粉末、セラミックフィラー、有機バインダ、有機溶剤等から調製されたスラリー4が溜められるコーター部3が配設された構成になっている。グリーンシートを成形する場合、コーター部3内のスラリー4をドクターブレード3aとキャリヤフイルム1との間隙3bからャリヤフイルム1の移動に伴って塗布することによりシート状のスラリー4aに形成し、これを乾燥部5で乾燥させてグリーンシート10とし、その後、キャリヤフイルム1と共にグリーンシート10を一対の引出ローラー6a、6bにより引き出して巻取ロール11に巻き取る。
【0003】
上記スラリー4に使用するガラス粉末を作製する場合、溶融ガラスを固化させ粗粉砕し、さらにボールミル等を使用して微粒子に粉砕し、この微粒子を分級して所要の粒径分布を有するガラス粉末を得る。特に、多層基板および誘電体チップ等に使用されるガラス粉末は、粒径が5μm以下の微粒子を多く含む粒径分布が要求される。このような微粒子を得るために、粉砕媒質として液体を用いることによりガラス粒子の表面エネルギーを下げてさらに粉砕を促進させることが可能な湿式粉砕が行われる。
【0004】
【発明が解決しようとする課題】
ところが、微粒子を多く含み比表面積が大きいガラス粉末は、表面からガラスの構成成分が粉砕媒質に溶け出しやすくなる。特に、ホウ珪酸ガラスを粉砕媒質として水または水溶液を用いて湿式粉砕した場合、粉砕された微粒子の表面からホウ酸が粉砕媒質中に溶けだし、乾燥後にホウ酸が析出し、ガラス粉末の表面に付着する。このようにして作製されたガラス粉末は、ホウ酸の付着量が多く、かつ水分含有量も大きいものになる。
【0005】
上記のガラス粉末を用いて調製したスラリー4は、ホウ酸の付着量が多いためにチキソトロピック性を有し、ゲル状となる。このようなスラリー4を上記図2のグリーンシート成形装置に供給した場合、図3に示すように、成形されたグリーンシート10の表面には無数の筋状の凹凸10a及び凹部10bが生じる。これら凹凸10a及び凹部10bは、電子部品基板を作製する際に基板の表面欠陥になるので、このようなグリーンシート10は不良品になるという問題がある。
【0006】
また、上記のガラス粉末は、水分含有量が大きいため、表面の過剰な水分が時間の経過と共にガラス粉末の表面にホウ酸をさらに析出させ、成形されたグリーンシート10の表面に過剰量のホウ酸が付着するので、グリーンシート10の表面に金属等の導体からなる配線パターンを定着させることが困難になるという問題がある。たとえ配線ができた場合でも、グリーンシート10を積層して多層基板にする際に、過剰量のホウ酸が基板間に介在して基板同士の密着性が悪くなり、積層された基板間の配線に導通欠陥及び絶縁欠陥が生じて多層基板が不良品となるという問題もある。
【0007】
そこで、上記の問題を避けるため、アルコール類等の有機溶剤を粉砕媒質として湿式粉砕を行うと、ガラス粉末のホウ酸付着量及び水分含有量が共に小さくなり、このようなガラス粉末を用いて調製したスラリーはチキソトロピック性を示さず、作製されたグリーンシートの表面には筋状の凹凸や凹部等の欠陥も観察されくなる。しかし、ガラス粉末の水分含有量が少ないため、ガラス粉末の表面が活性となってスラリー中の有機溶剤及び有機バインダとの濡れ性が悪くなり、ガラス粉末がスラリー中で十分に分散せず、作製されたグリーンシート中には、有機バインダの偏在部分及びガラス粉末の偏在部分が存在し、グリーンシートの部位により密度に差が生じる。このようなグリーンシートを使用して作製された多層基板等の電子部品基板は、製造ロット中や内部に誘電率、絶縁抵抗値等の電気的特性に差異が生じるという問題がある。
【0008】
また、有機溶剤を使用して粉砕されたガラス粉末は、表面のホウ酸付着量が極めて少ないため、グリーンシート中のガラスの粒子間の結合が弱くなって脆くなり、グリーンシートの引張強度が取扱に必要な値に達しないという問題がある。
【0009】
本発明は、上記従来の問題点を解決し、平滑な表面、均一な密度及び所要の引張強度を有する電子部品基板用グリーンシートを効率良く製造することができるガラス粉末を提供することを目的とする。
【0010】
【課題を解決するための手段】
本願発明に係るガラス粉末は、ホウ珪酸ガラスからなり、50%粒子径D50の値が5μm以下になる粒径分布を有し、表面のホウ酸付着量が0.10〜0.30重量%であり、かつ水分含有量が0.8〜1.3重量%であることを特徴とする。
【0011】
【作用】
本発明に係るガラス粉末は、ホウ珪酸ガラスからなり、湿式粉砕により作製されて50%粒子径D50の値が5μm以下になる粒径分布を有しており、表面のホウ酸付着量が0.30重量%以下であるので、本発明のガラス粉末を用いて調製したグリーンシート用のスラリーは、チキソトロピック性を示さず、このスラリーを用いてドクターブレード法により形成されたグリーンシートの表面には凹凸が生じない。また、表面のホウ酸付着量が0.10重量%以上であるので、ガラスの粒子間に介在するホウ酸が接着剤として作用して所要の引張強度を有するグリーンシートを作製することができる。さらに、本発明のガラス粉末は、水分含有量が0.8重量%以上であるので、ガラス粉末の表面に付着した水分が表面活性を抑制してグリーンシート用のスラリー中にガラス粉末を均等に分散させることができ、かつ水分含有量が1.3重量%以下であるので、成形されたグリーンシートの表面には、ホウ酸の付着量が0.30重量%以下に安定しており、グリーンシートの表面に配線パターンを容易に定着させることができ、配線パターンを有するグリーンシートを積層して多層基板にする際の密着性が良好となる。
【0012】
【発明の実施の形態】
図1は本発明の実施例に係るガラス粉末が有する粒径分布の一例を示すグラフであり、図中、ヒストグラムは、横軸に示した各粒径区分にカウントされた粉末ガラスの頻度%を、折れ線グラフは、頻度%の累積をそれぞれ示している。
【0013】
本発明のガラス粉末は、B23 20重量%、SiO2 75重量%、R2OおよびRO 5重量%(Rはアルカリ金属元素)の組成を有するホウ珪酸ガラスからなり、湿式粉砕により作製され、図1に示すように、50%粒子径D50が3.5μmとなる粒径分布を有している。また、ガラス粉末の表面に付着しているホウ酸の量は0.15〜0.28重量%であり、かつ水分含有量は0.9〜1.2重量%である。
【0014】
ガラス粉末の粒径分布と50%粒子径D50の値は、日機装株式会社製のレーザー回折式粒度分布計「マイクロトラックSPA」を用いて測定した。
【0015】
ガラス粉末の表面に付着しているホウ酸の量は、ガラス粉末を純水に分散した後、マンニット等の多価アルコールを相当量加えて、錯ホウ酸化合物を生成させ、この錯ホウ酸化合物を既知の規定度のNaOHにより中和して定量する中和滴定法により測定する。
【0016】
また、ガラス粉末の水分含有量は、ガラス粉末を400℃で加熱脱水し、出てきた水分を窒素気流でカールフィッシャー溶液(ヨウ素、二酸化硫黄、ピリジンのメタノール溶液)中に送り込み、消費されたヨウ素を検出電極で電気分解により再びヨウ素に再生させる際に使用される電気量により水分を定量するカールフィッシャー電量法により測定する。
【0017】
本発明のガラス粉末を作製する場合、ホウ珪酸ガラスとして、B23 20重量%、SiO2 75重量%、R2OおよびRO 5重量%(Rはアルカリ金属元素)の組成のものを使用し、エタノールを用いて湿式粉砕を行い、さらに粉砕されたスラリ状のガラス粉末を撹拌しながら、所定量の純水を加えることにより析出するホウ酸量及び水分含有量の調製を行い、その後乾燥してガラス粉末にする。
【0018】
作製したガラス粉末に、セラミックフィラーとしてアルミナ粉末、有機バインダーとしてポリビニルブチラール、有機溶剤等を加えて攪拌してスラリー4を調製し、先記の図2に示したグリーンシート成形装置のコーター部3に供給して、グリーンシート10を作製した。
【0019】
まず、グリーンシート10の表面を観察して外観の評価を行った。また、グリーンシート10の引張強度は、グリーンシート10の試験片を作製し、この試験片を引張試験器を使用して測定することにより行った。さらに、グリーンシート10の密度は、電子天秤により試験片の質量を測定し、試験片の寸法を測定して体積を算出し、質量÷体積の計算を行うことにより求めた。上記の観察結果及び測定値を表1にまとめた。
【0020】
従来技術との対比のため、粉砕媒質にアルコールを使用し、その他の条件を上記の実施例と同一にして作製したガラス粉末の評価結果を比較例1として、粉砕媒質として水を使用し、その他の条件を上記の実施例と同一にして作製したガラス粉末の評価結果を比較例2としてそれぞれ表1に示す。
【0021】
【表1】

Figure 0003956074
【0022】
評価の結果、作製したグリーンシート10の表面には、従来見られたような凹凸は観察されず、グリーンシート10の各部位から作製した試験片の密度は1.5±0.005g/cm3 以内であり、部位による差異がほとんど無く均一性に優れており、引張試験による引張強度も、グリーンシートの取扱に必要とされる引張強度の300gf/mm2 を大きく上回る650〜900gf/mm2 という高い引張強度を有するものが得られた。これに対して、比較例1では、成形されたグリーンシートに欠陥は観察されないものの、グリーンシートの各部位から作製された試験片の密度が1.5±0.03g/cm3 で部位により0.06g/cm3の大きな差異が生じており、引張強度も100〜200gf/mm2 と所要値とされる300gf/mm2 に達していない。また、比較例2では、作製したグリーンシートが表面の欠陥のために外観の評価で不良品となり、その他の評価については、表面の欠陥のために密度の測定基準となる体積そのものがバラついてしまっており、また、引張強度も試験片の表面の欠陥に応力集中が生じてが欠陥から破壊を起こすので評価の意味をなさないというものであった。
【0023】
【発明の効果】
本発明のガラス粉末によれば、表面が平滑であり、均一な密度及び所要の引張強度を有する電子部品基板用グリーンシートを効率良く製造することができる実用上優れた効果を奏するものである。
【図面の簡単な説明】
【図1】本発明のガラス粉末が有する粒径分布の一例を示すグラフ。
【図2】グリーンシート成形装置の説明図
【図3】従来のガラス粉末を用いて作製したグリーンシートの説明図であって(A)は従来のグリーンシートの断面図、(B)は従来のグリーンシートの表面の欠陥の説明図。
【符号の説明】
1 キャリヤフィルム
2 支持ローラー
3 コーター部
3a ドクターブレード
4 スラリー
5 乾燥部
6a、6b 引出ローラー
10 グリーンシート[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a glass powder used for producing a green sheet for an electronic component substrate.
[0002]
[Prior art]
In general, green sheets are used for the production of electronic component substrates such as multilayer substrates and dielectric chips. As shown in FIG. 2, a green sheet forming apparatus using a doctor blade method is used for producing the green sheet. In this apparatus, a carrier film 1 is pulled out from a supply roll 1a, conveyed on a plurality of support rollers 2, and provided with a doctor blade 3a above the carrier film 1, and comprises glass powder, ceramic filler, organic binder, organic binder. A coater unit 3 is provided in which slurry 4 prepared from a solvent or the like is stored. When forming a green sheet, the slurry 4 in the coater unit 3 is applied to the carrier film 1 through the gap 3b between the doctor blade 3a and the carrier film 1 to form a sheet-like slurry 4a, which is then dried. The green sheet 10 is dried at the section 5 to form the green sheet 10, and then the green sheet 10 is drawn out together with the carrier film 1 by the pair of pull-out rollers 6 a and 6 b and wound around the take-up roll 11.
[0003]
When producing the glass powder used for the slurry 4, the molten glass is solidified and coarsely pulverized, and further pulverized into fine particles using a ball mill or the like, and the fine particles are classified to obtain a glass powder having a required particle size distribution. obtain. In particular, glass powders used for multilayer substrates and dielectric chips are required to have a particle size distribution containing many fine particles having a particle size of 5 μm or less. In order to obtain such fine particles, wet pulverization is performed, in which a liquid is used as a pulverizing medium to lower the surface energy of the glass particles and further promote pulverization.
[0004]
[Problems to be solved by the invention]
However, glass powder containing a large amount of fine particles and having a large specific surface area tends to cause glass components to dissolve into the grinding medium from the surface. In particular, when borosilicate glass is wet pulverized using water or an aqueous solution as a pulverizing medium, boric acid dissolves in the pulverizing medium from the surface of the pulverized fine particles, boric acid precipitates after drying and adheres to the surface of the glass powder To do. The glass powder thus produced has a large amount of boric acid attached and a large water content.
[0005]
The slurry 4 prepared using the above glass powder has thixotropic properties due to the large amount of boric acid attached, and becomes a gel. When such a slurry 4 is supplied to the green sheet forming apparatus shown in FIG. 2, innumerable line-like unevenness 10 a and recess 10 b are formed on the surface of the formed green sheet 10 as shown in FIG. 3. Since the unevenness 10a and the recess 10b become surface defects of the substrate when the electronic component substrate is manufactured, there is a problem that such a green sheet 10 becomes a defective product.
[0006]
Further, since the glass powder has a high moisture content, excessive moisture on the surface further precipitates boric acid on the surface of the glass powder over time, and an excessive amount of boron is formed on the surface of the formed green sheet 10. Since the acid adheres, there is a problem that it is difficult to fix a wiring pattern made of a conductor such as a metal on the surface of the green sheet 10. Even when wiring is made, when the green sheets 10 are laminated to form a multilayer substrate, an excessive amount of boric acid is interposed between the substrates, resulting in poor adhesion between the substrates, and wiring between the stacked substrates In addition, there is a problem that a conduction defect and an insulation defect occur, resulting in a defective multilayer substrate.
[0007]
Therefore, in order to avoid the above problem, when wet pulverization is performed using an organic solvent such as alcohol as a pulverization medium, both the boric acid adhesion amount and the water content of the glass powder are reduced, and the glass powder is prepared using such a glass powder. The resulting slurry does not exhibit thixotropic properties, and defects such as streak-like irregularities and recesses are not observed on the surface of the produced green sheet. However, since the water content of the glass powder is small, the surface of the glass powder becomes active and the wettability with the organic solvent and organic binder in the slurry is deteriorated, and the glass powder is not sufficiently dispersed in the slurry. In the green sheet thus formed, there are unevenly distributed portions of the organic binder and unevenly distributed portions of the glass powder, and the density varies depending on the portion of the green sheet. An electronic component substrate such as a multilayer substrate manufactured using such a green sheet has a problem in that electrical characteristics such as a dielectric constant and an insulation resistance value are different in a manufacturing lot and inside.
[0008]
In addition, glass powder crushed using an organic solvent has a very small amount of boric acid on the surface, so the bonds between the glass particles in the green sheet become weak and brittle, and the tensile strength of the green sheet is handled. There is a problem that the required value is not reached.
[0009]
An object of the present invention is to solve the above-mentioned conventional problems and to provide a glass powder capable of efficiently producing a green sheet for an electronic component substrate having a smooth surface, a uniform density and a required tensile strength. To do.
[0010]
[Means for Solving the Problems]
Glass powder according to the present invention comprises a borosilicate glass has a particle size distribution value of 50% particle diameter D 50 is 5μm or less, boric acid deposition amount of surface 0.10 to 0.30 wt% And the water content is 0.8 to 1.3% by weight.
[0011]
[Action]
The glass powder according to the present invention is made of borosilicate glass, has a particle size distribution in which the value of 50% particle diameter D 50 is 5 μm or less, produced by wet grinding, and has a boric acid adhesion amount of 0 on the surface. 30% by weight or less, the slurry for the green sheet prepared using the glass powder of the present invention does not exhibit thixotropic properties, and this slurry is used for the surface of the green sheet formed by the doctor blade method. No irregularities. Moreover, since the boric acid adhesion amount on the surface is 0.10% by weight or more, the boric acid intervening between the glass particles acts as an adhesive to produce a green sheet having a required tensile strength. Furthermore, since the water content of the glass powder of the present invention is 0.8% by weight or more, the water adhering to the surface of the glass powder suppresses the surface activity, and the glass powder is evenly distributed in the slurry for the green sheet. Since it can be dispersed and the water content is 1.3% by weight or less, the amount of boric acid adhered to the surface of the molded green sheet is stable to 0.30% by weight or less. The wiring pattern can be easily fixed on the surface of the sheet, and adhesion when a green sheet having the wiring pattern is laminated to form a multilayer substrate is improved.
[0012]
DETAILED DESCRIPTION OF THE INVENTION
FIG. 1 is a graph showing an example of the particle size distribution of the glass powder according to the embodiment of the present invention. In the figure, the histogram shows the frequency% of the powder glass counted in each particle size category shown on the horizontal axis. The line graph shows the cumulative frequency%.
[0013]
The glass powder of the present invention is made of borosilicate glass having a composition of 20% by weight of B 2 O 3 , 75% by weight of SiO 2 , R 2 O and 5% by weight of RO (R is an alkali metal element), and is prepared by wet grinding. As shown in FIG. 1, the particle size distribution has a 50% particle diameter D 50 of 3.5 μm. The amount of boric acid adhering to the surface of the glass powder is 0.15 to 0.28% by weight, and the water content is 0.9 to 1.2% by weight.
[0014]
The particle size distribution of the glass powder and the value of the 50% particle size D 50 were measured using a laser diffraction particle size distribution analyzer “Microtrac SPA” manufactured by Nikkiso Co., Ltd.
[0015]
The amount of boric acid adhering to the surface of the glass powder is determined by dispersing the glass powder in pure water and then adding a considerable amount of polyhydric alcohol such as mannitol to form a complex boric acid compound. The compound is measured by a neutralization titration method in which the compound is neutralized and quantified with a known normality NaOH.
[0016]
In addition, the water content of the glass powder is dehydrated by heating the glass powder at 400 ° C., and the resulting water is fed into a Karl Fischer solution (iodine, sulfur dioxide, pyridine in methanol) in a nitrogen stream. Is measured by the Karl Fischer coulometric method in which moisture is quantified by the amount of electricity used when regenerating iodine again by electrolysis with a detection electrode.
[0017]
When producing the glass powder of the present invention, a borosilicate glass having a composition of 20% by weight of B 2 O 3 , 75% by weight of SiO 2 , 5% by weight of R 2 O and RO (R is an alkali metal element) is used. Then, wet pulverization is performed using ethanol, and the amount of precipitated boric acid and water content are adjusted by adding a predetermined amount of pure water while stirring the pulverized slurry-like glass powder, followed by drying. To make glass powder.
[0018]
Alumina powder as a ceramic filler, polyvinyl butyral as an organic binder, an organic solvent, and the like are added to the prepared glass powder and stirred to prepare a slurry 4, which is applied to the coater unit 3 of the green sheet forming apparatus shown in FIG. The green sheet 10 was produced by supplying.
[0019]
First, the appearance of the green sheet 10 was evaluated by observing the surface. The tensile strength of the green sheet 10 was measured by preparing a test piece of the green sheet 10 and measuring the test piece using a tensile tester. Further, the density of the green sheet 10 was determined by measuring the mass of the test piece with an electronic balance, measuring the size of the test piece, calculating the volume, and calculating the mass / volume. The observation results and measured values are summarized in Table 1.
[0020]
For comparison with the prior art, alcohol was used as the grinding medium, and the evaluation results of the glass powder produced with the other conditions being the same as those in the above example were set as Comparative Example 1, water was used as the grinding medium, and others. Table 1 shows the results of evaluation of glass powders produced under the same conditions as in the above-mentioned example as Comparative Example 2.
[0021]
[Table 1]
Figure 0003956074
[0022]
As a result of the evaluation, the surface of the produced green sheet 10 was not observed to have irregularities as conventionally observed, and the density of the test piece produced from each part of the green sheet 10 was 1.5 ± 0.005 g / cm 3. is within, is excellent in little uniformity difference by site, the tensile strength according to the tensile test, that 650~900gf / mm 2 far exceeding the tensile strength of 300 gf / mm 2, which is required for handling of the green sheet Those having a high tensile strength were obtained. On the other hand, in Comparative Example 1, although no defect was observed in the molded green sheet, the density of the test piece prepared from each part of the green sheet was 1.5 ± 0.03 g / cm 3 and 0 depending on the part. large difference of .06g / cm 3 has occurred is, tensile strength 100~200gf / mm 2 does not reach the 300 gf / mm 2, which is a required value. Further, in Comparative Example 2, the produced green sheet was defective in appearance evaluation due to surface defects, and in other evaluations, the volume itself as a density measurement standard was varied due to surface defects. Also, the tensile strength was not meaningful for evaluation because stress concentration occurred on the surface defect of the test piece, but the defect was destroyed.
[0023]
【The invention's effect】
According to the glass powder of the present invention, the green sheet for electronic component substrates having a smooth surface, a uniform density and a required tensile strength can be effectively produced, and thus has an excellent practical effect.
[Brief description of the drawings]
FIG. 1 is a graph showing an example of a particle size distribution possessed by the glass powder of the present invention.
FIG. 2 is an explanatory view of a green sheet forming apparatus. FIG. 3 is an explanatory view of a green sheet manufactured using a conventional glass powder, where (A) is a sectional view of the conventional green sheet, and (B) is a conventional green sheet. Explanatory drawing of the defect of the surface of a green sheet.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 Carrier film 2 Support roller 3 Coater part 3a Doctor blade 4 Slurry 5 Drying part 6a, 6b Extraction roller 10 Green sheet

Claims (3)

ホウ珪酸ガラスからなり、50%粒子径D50の値が5μm以下になる粒径分布を有し、表面のホウ酸付着量が0.10〜0.30重量%であり、かつ水分含有量が0.8〜1.3重量%であることを特徴とするガラス粉末。It is made of borosilicate glass, has a particle size distribution in which the value of 50% particle diameter D 50 is 5 μm or less, the boric acid adhesion amount on the surface is 0.10 to 0.30% by weight, and the water content is Glass powder characterized by being 0.8 to 1.3% by weight. 請求項1のガラス粉末を含むことを特徴とするグリーンシート作製用スラリー。A slurry for producing a green sheet comprising the glass powder of claim 1. 請求項1のガラス粉末を含むことを特徴とするグリーンシート。A green sheet comprising the glass powder of claim 1.
JP36740698A 1998-12-24 1998-12-24 Glass powder Expired - Lifetime JP3956074B2 (en)

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Publication number Priority date Publication date Assignee Title
CN108264346A (en) * 2018-02-06 2018-07-10 厦门嘉联科技开发有限公司 A kind of preparation process of compound glass phase zircite ceramic electronic components

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Publication number Priority date Publication date Assignee Title
JP4953626B2 (en) * 2004-12-24 2012-06-13 京セラ株式会社 Manufacturing method of ceramic electronic component

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108264346A (en) * 2018-02-06 2018-07-10 厦门嘉联科技开发有限公司 A kind of preparation process of compound glass phase zircite ceramic electronic components

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