JPH08235933A - Alumina sintered body - Google Patents

Alumina sintered body

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Publication number
JPH08235933A
JPH08235933A JP7039793A JP3979395A JPH08235933A JP H08235933 A JPH08235933 A JP H08235933A JP 7039793 A JP7039793 A JP 7039793A JP 3979395 A JP3979395 A JP 3979395A JP H08235933 A JPH08235933 A JP H08235933A
Authority
JP
Japan
Prior art keywords
alumina
less
sintered body
dielectric loss
terms
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP7039793A
Other languages
Japanese (ja)
Other versions
JP3454957B2 (en
Inventor
Shuzo Iwashita
修三 岩下
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kyocera Corp
Original Assignee
Kyocera Corp
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Abstract

PURPOSE: To provide an alumina sintered body whose dielectric loss is set to 1×10<-4> or less and a sintering property and productivity are improved without using an alumina raw material of high purity. CONSTITUTION: An alumina sintered body contains Na 100ppm or less in terms of Na2 O, Ca 0.5wt.% or less in terms of CaO, and Mg 0.03wt.% or more in terms of MgO to alumina as a main component. When a grain boundary phase is measured by X-ray diffraction, peaks of CaO.6Al2 O3 and MgAl2 O4 exist. It is preferable that dielectric loss tan δin a measurement frequency 14GHz is 1×10<-4> or less.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、アルミナ質焼結体に関
するものであり、特に、例えば、通信用MIC基板やM
ICパッケージ、マイクロ波コンデンサ、マイクロ波通
信装置用部品、高エネルギー粒子加速装置のマイクロ波
透過窓等に用いることができる高周波低損失性のアルミ
ナ質焼結体に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an alumina-based sintered body, and particularly to, for example, a MIC substrate for communication or M.
The present invention relates to a high-frequency low-loss alumina sintered body that can be used in IC packages, microwave capacitors, microwave communication device parts, microwave transmission windows of high-energy particle accelerators, and the like.

【0002】[0002]

【従来技術】従来、例えば、通信用MIC基板やMIC
パッケージ、マイクロ波コンデンサ、マイクロ波通信用
装置用部品、高エネルギー粒子加速装置のマイクロ波透
過窓に用いられるアルミナ質焼結体では、誘電損失は1
0GHz程度のマイクロ波帯において1×10-4以下で
あることが求められる。
2. Description of the Related Art Conventionally, for example, a communication MIC substrate or MIC
Dielectric loss is 1 in the alumina sintered body used for the microwave transparent window of the package, microwave capacitor, microwave communication device, high energy particle accelerator.
It is required to be 1 × 10 −4 or less in the microwave band of about 0 GHz.

【0003】このようなアルミナ質焼結体としては、従
来、誘電損失を1×10-4以下にするために、不純物の
含有量を元素基準のppm単位で、Siを80ppm以
下、Mgを60ppm以下、Si/Mgを1〜5、かつ
他の金属やアルカリ成分等を総量70ppm以下とした
アルミナ質焼結体が知られている(特開平1−2139
10号公報)。
Conventionally, as such an alumina-based sintered body, in order to reduce the dielectric loss to 1 × 10 −4 or less, the content of impurities is in the ppm unit of the element standard, Si is 80 ppm or less, and Mg is 60 ppm. Hereinafter, an alumina-based sintered body in which Si / Mg is 1 to 5 and the total amount of other metals and alkali components is 70 ppm or less is known (Japanese Patent Laid-Open No. 1-2139).
No. 10).

【0004】また、特開平4−356922号公報で
は、マイクロ波透過窓として、マイクロ波を透過させる
性質を持たせるため、含有しているアルカリ金属(Na
2 O、K2 O)の総量を150ppm以下に抑制し、マ
イクロ波帯の誘電損失を1×10-3以下としたアルミナ
質焼結体が開示されている。
Further, in Japanese Patent Laid-Open No. 4-356922, an alkali metal (Na) contained in a microwave transmitting window is added in order to have a microwave transmitting property.
There is disclosed an alumina-based sintered body in which the total amount of 2 O and K 2 O) is suppressed to 150 ppm or less and the dielectric loss in the microwave band is 1 × 10 −3 or less.

【0005】[0005]

【発明が解決しようとする問題点】一般に、アルミナ質
焼結体の誘電損失の増加に粒界相のガラス質が大きく寄
与していると言われている。このため、低損失磁器を得
るためには、粒界相の生成を制御する必要がある。一般
に粒界相の生成を極力さける目的で、生成原因となる不
純物を避けるために、高純度の原料を用いて不純物の総
量を規制している。
It is generally said that the glassy material of the grain boundary phase greatly contributes to the increase of the dielectric loss of the alumina-based sintered body. Therefore, in order to obtain a low loss porcelain, it is necessary to control the generation of the grain boundary phase. In general, in order to prevent the generation of the grain boundary phase as much as possible, the total amount of impurities is regulated by using a high-purity raw material in order to avoid the impurities causing the generation.

【0006】その中でも、ガラス相を形成しやすいアル
カリ成分は極力避ける必要がある。
[0006] Among them, it is necessary to avoid as much as possible an alkaline component which easily forms a glass phase.

【0007】しかしながら、実際には高純度アルミナ原
料(純度99.999%程度)を用いても、必ずしも誘
電損失が1×10-4以下にならないという問題があっ
た。
However, in practice, even if a high-purity alumina raw material (purity of about 99.999%) was used, there was a problem that the dielectric loss did not always become 1 × 10 −4 or less.

【0008】また、特開平1−213910号公報に開
示されるアルミナ質焼結体では、アルカリ金属酸化物以
外の不純物含有量も減少させ、全体的に磁器を高純度化
させる必要があるため、生産性が低下するという問題が
あった。さらに焼成温度が高くなりがちであった。
Further, in the alumina-based sintered body disclosed in Japanese Patent Application Laid-Open No. 1-213910, it is necessary to reduce the content of impurities other than alkali metal oxides and to highly purify the porcelain as a whole. There was a problem that productivity fell. Further, the firing temperature tends to be high.

【0009】さらに、特開平4−356922号公報に
開示されるアルミナ質焼結体では、低誘電損失化させる
ためアルカリ金属(Na2 O、K2 O)総量を抑制して
いるが、この場合でも必ずしも1×10-4以下の誘電損
失を達成できるとは限らないという問題があった。
Further, in the alumina sintered body disclosed in Japanese Patent Laid-Open No. 4-356922, the total amount of alkali metals (Na 2 O, K 2 O) is suppressed in order to reduce the dielectric loss. In this case, However, there is a problem that it is not always possible to achieve a dielectric loss of 1 × 10 −4 or less.

【0010】本発明は、高純度アルミナ原料を用いるこ
となく、誘電損失を確実に1×10-4以下とすることが
できるとともに、生産性および焼結性を向上することが
できるアルミナ質焼結体を提供することを目的とする。
The present invention makes it possible to reliably reduce the dielectric loss to 1 × 10 −4 or less without using a high-purity alumina raw material, and to improve the productivity and the sinterability. Intended to provide the body.

【0011】[0011]

【問題点を解決するための手段】本発明者は、上記問題
を解決すべく鋭意検討した結果、アルミナ質焼結体中に
生成する粒界相には様々な結晶相があり、そのすべてが
誘電損失を増加させているわけではなく、誘電損失増加
の原因としてはNa含有量だけでなく、粒界相中の析出
結晶相のうちCaO・6Al2 3 の存在も、アルミナ
質焼結体の誘電損失を増加させていることを見出した。
また、Caはアルミナに殆ど固溶せず、粒界にCaO・
6Al2 3 として析出するため、アルミナ質焼結体の
誘電損失を低下させるためには、Ca量を減少させ、粒
界相中におけるCaO・6Al2 3 の析出量を少なく
すれば良いことを見出した。さらに、MgOは、微量添
加(0.03〜10重量%)で粒界にMgAl2 4
生成し、アルミナの焼結性を促進する効果があることが
知られている。しかし、CaOを添加せず、粒界にCa
O・6Al2 3 が生成しないと、緻密化が阻害され、
焼成温度が高くなり生産上好ましくない。このため、ア
ルミナ焼結体の粒界相中にMgAl2 4 とCaO・6
Al2 3 を析出させるとともに、Na含有量を一定以
下に抑制することにより、アルミナ質焼結体の誘電損失
を確実に1×10-4以下とすることができるとともに、
生産性および焼結性を向上することができることを見出
し、本発明に至った。
As a result of intensive studies to solve the above problems, the present inventor has found that there are various crystal phases in the grain boundary phase formed in the alumina-based sintered body, all of which are This does not mean that the dielectric loss is increased, and the cause of the increase in the dielectric loss is not only the content of Na but also the presence of CaO.6Al 2 O 3 in the precipitated crystal phase in the grain boundary phase. It has been found that the dielectric loss of is increased.
In addition, Ca hardly forms a solid solution in alumina, and CaO
Since 6Al 2 O 3 precipitates, in order to reduce the dielectric loss of the alumina-based sintered body, the amount of Ca should be decreased and the amount of CaO · 6Al 2 O 3 precipitated in the grain boundary phase should be reduced. Found. Furthermore, it is known that MgO produces MgAl 2 O 4 at grain boundaries when added in a small amount (0.03 to 10 wt%), and has the effect of promoting the sinterability of alumina. However, Ca was not added to the grain boundary without adding CaO.
If O · 6Al 2 O 3 is not generated, densification is hindered,
The firing temperature becomes high, which is not preferable in production. Therefore, in the grain boundary phase of the alumina sintered body, MgAl 2 O 4 and CaO.
By precipitating Al 2 O 3 and suppressing the Na content to a certain level or less, the dielectric loss of the alumina-based sintered body can be reliably reduced to 1 × 10 −4 or less, and
They have found that productivity and sinterability can be improved, and have reached the present invention.

【0012】即ち、本発明のアルミナ質焼結体は、主成
分としてのアルミナに、Na含有量がNa2 O換算で1
00ppm以下、CaがCaO換算で0.5重量%以
下、MgがMgO換算で0.03重量%以上含有し,か
つ、粒界相をX線回折測定した場合に、CaO・6Al
2 3 とMgAl2 4 のピークが存在するものであ
り、測定周波数14GHzにおける誘電損失tanδが
1×10-4以下であることが望ましい。
That is, in the alumina sintered body of the present invention, the content of Na in the alumina as the main component is 1 in terms of Na 2 O.
In the case of containing less than 00 ppm, Ca of 0.5 wt% or less in terms of CaO, Mg of 0.03 wt% or more in terms of MgO, and measuring the grain boundary phase by X-ray diffraction, CaO · 6Al
2 O 3 and MgAl 2 O 4 have peaks, and it is desirable that the dielectric loss tan δ at a measurement frequency of 14 GHz is 1 × 10 −4 or less.

【0013】本発明のアルミナ質焼結体では、Na含有
量をNa2 O換算で100ppm以下としたのは、Na
含有量がNa2 O換算で100ppmよりも大きくなる
と、誘電損失が1×10-4よりも大きくなるからであ
る。Na含有量は少ない方が良く、Naを含む結晶相の
ピークは、X線回折測定ではピークが実質的に存在しな
いことが望ましい。
In the alumina sintered body of the present invention, the Na content is 100 ppm or less in terms of Na 2 O because
This is because if the content is greater than 100 ppm in terms of Na 2 O, the dielectric loss will be greater than 1 × 10 −4 . The Na content is preferably as low as possible, and the peak of the crystal phase containing Na is preferably substantially absent in the X-ray diffraction measurement.

【0014】また、CaをCaO換算で0.5重量%以
下としたのは、0.5重量%よりも多い場合にはCaO
・6Al2 3 の析出量が多く、誘電損失が1×10-4
よりも大きくなるからである。CaはCaO換算で0.
0001〜0.5重量%、特には0.05〜0.1重量
%が望ましい。
Further, Ca is set to 0.5% by weight or less in terms of CaO because CaO is more than 0.5% by weight.
・ A large amount of 6Al 2 O 3 is deposited, resulting in a dielectric loss of 1 × 10 -4
Because it will be larger than. Ca is 0 in terms of CaO.
0001 to 0.5% by weight, particularly 0.05 to 0.1% by weight is desirable.

【0015】さらに、MgをMgO換算で0.03重量
%以上としたのは、0.03重量%よりも少ない場合に
は焼成温度が高くなり、誘電損失が1×10-4以上とな
るからである。MgはMgO換算で0.03〜10重量
%であることが誘電損失の点から望ましい。
Further, the reason why Mg is 0.03% by weight or more in terms of MgO is that if it is less than 0.03% by weight, the firing temperature becomes high and the dielectric loss becomes 1 × 10 −4 or more. Is. From the viewpoint of dielectric loss, it is desirable that Mg be 0.03 to 10 wt% in terms of MgO.

【0016】そして、粒界相をX線回折測定した場合
に、CaO・6Al2 3 とMgAl2 4 のピークを
存在させた理由は、上記したように誘電損失を1×10
-4以下にし、さらにアルミナ質焼結体の焼結性を向上す
るためである。CaO・6Al2 3 が多いと誘電損失
が高くなるため、なるべく少なくする必要がある。X線
回折測は、例えば、波長λ=1.5418ÅのCuKα
線により行う。
The reason why the peaks of CaO.6Al 2 O 3 and MgAl 2 O 4 exist when the grain boundary phase is measured by X-ray diffraction is that the dielectric loss is 1 × 10 as described above.
-4 or less, in order to further improve the sinterability of the alumina-based sintered body. If CaO.6Al 2 O 3 is large, the dielectric loss becomes high, so it is necessary to reduce it as much as possible. X-ray diffraction measurement is, for example, CuKα with a wavelength λ = 1.5418Å
Do by lines.

【0017】本発明のアルミナ質焼結体は、例えば、高
純度アルミナ粉末にMg(OH)2粉末およびCaCO
3 粉末を所定量添加し、イソプロピルアルコール(IP
A)と混合し、アルミナボールで粉砕混合する。混合後
のスラリーを乾燥し、仮焼して得られた粉末を、例え
ば、金型プレスで成形し、焼結助剤によっても異なる
が、例えば、大気中において1500〜1600℃で
0.5〜4時間焼成することにより、本発明のアルミナ
質焼結体が得られる。
The alumina-based sintered body of the present invention comprises, for example, high-purity alumina powder, Mg (OH) 2 powder and CaCO.
Add a certain amount of 3 powder, and add isopropyl alcohol (IP
Mix with A) and crush with an alumina ball. The mixed slurry is dried, and the powder obtained by calcination is molded by, for example, a die press, and varies depending on the sintering aid, but is, for example, 0.5 to 1600 ° C. in the air at 1500 to 1600 ° C. By firing for 4 hours, the alumina-based sintered body of the present invention is obtained.

【0018】[0018]

【作用】本発明のアルミナ質焼結体では、Na含有量を
Na2 O換算で100ppm以下、CaをCaO換算で
0.5重量%以下、MgをMgO換算で0.03重量%
以上とし、粒界相にCaO・6Al2 3 とMgAl2
4 を存在させることにより、焼結体の誘電損失を1×
10-4以下とすることが可能となる。
In the alumina sintered body of the present invention, the Na content is 100 ppm or less in terms of Na 2 O, Ca is 0.5 wt% or less in terms of CaO, and Mg is 0.03 wt% in terms of MgO.
As described above, CaO.6Al 2 O 3 and MgAl 2 are contained in the grain boundary phase.
The presence of O 4 reduces the dielectric loss of the sintered body to 1 ×.
It is possible to make it 10 −4 or less.

【0019】また、本発明のアルミナ質焼結体では、高
純度のアルミナ原料を用いなくてもよく、アルミナ純度
99.9%程度の汎用原料を用いても1×10-4以下の
誘電損失が得られるため、適切な焼結助剤を用いて焼成
温度を低下させることが可能となり、焼結性および生産
性を向上することができる。
Further, in the alumina sintered body of the present invention, it is not necessary to use a high-purity alumina raw material, and even if a general-purpose raw material having an alumina purity of about 99.9% is used, a dielectric loss of 1 × 10 -4 or less is obtained. Therefore, the firing temperature can be lowered by using an appropriate sintering aid, and the sinterability and the productivity can be improved.

【0020】[0020]

【実施例】Na2 O含有量の異なるアルミナ原料(純度
99.9%)と、CaCO3 及びMg(OH)2 を、表
1の組成となるように秤量し、この混合粉末を、純度9
9.9%のアルミナボール、イソプロピルアルコール
(IPA)と共に1リットルポリポットに投入し、42
時間回転ミル台にて混合した。混合後のスラリーにバイ
ンダーとしてパラフィンワックスを6重量%加え混合攪
拌した。このスラリーを80℃大気中にて乾燥し、評価
粉末得た。尚、表1では、CaCO3 はCaOに換算
し、また、Mg(OH)2 はMgOに換算して記載し
た。
[Examples] Alumina raw materials having different Na 2 O contents (purity 99.9%), CaCO 3 and Mg (OH) 2 were weighed so as to have the composition shown in Table 1, and the mixed powder was purified to have a purity of 9%.
Put it in a 1 liter polypot with 9.9% alumina balls and isopropyl alcohol (IPA),
The mixture was mixed on a time rotary mill stand. 6% by weight of paraffin wax as a binder was added to the mixed slurry and mixed and stirred. This slurry was dried in the air at 80 ° C. to obtain an evaluation powder. In Table 1, CaCO 3 is converted into CaO and Mg (OH) 2 is converted into MgO.

【0021】この粉末を金型プレスにて1000kg/
cm2 で直径12mm、厚み8mmに成形した。成形体
は、大気中において400℃で2時間脱脂を行い、その
後、表1に示す焼成温度で2時間保持して焼成した。焼
結体は、直径10mm、厚み5mmに加工研磨した。こ
の試料の高周波誘電損失を測定周波数14GHzで測定
した。また、波長λ=1.5418ÅのCuKα線によ
るX線回折測により試料の結晶相を同定した。これらの
結果を表1に示す。
This powder was pressed with a die press at 1000 kg /
It was molded to have a diameter of 12 mm and a thickness of 8 mm in cm 2 . The molded body was degreased in the air at 400 ° C. for 2 hours, and then held at the firing temperature shown in Table 1 for 2 hours for firing. The sintered body was processed and polished to have a diameter of 10 mm and a thickness of 5 mm. The high frequency dielectric loss of this sample was measured at a measurement frequency of 14 GHz. Further, the crystal phase of the sample was identified by X-ray diffraction measurement with CuKα ray having a wavelength λ = 1.5418Å. Table 1 shows the results.

【0022】[0022]

【表1】 [Table 1]

【0023】この表1から、粒界相中にCaO・6Al
2 3 の他に、MgAl2 4 が析出した本発明の試料
については、1×10-4以下の低誘電損失を示すことが
判る(試料No.2〜5,8〜11)。また、本発明の試
料では、焼成温度が1600℃以下となっており、従来
よりも低温で焼成できることが判る。さらに、CaOの
添加量が増加するにしたがって誘電損失が増加し、Mg
O添加量が増加するに伴い焼成温度が低下することが判
る。
From Table 1, CaO.6Al was found in the grain boundary phase.
It is found that the samples of the present invention in which MgAl 2 O 4 is precipitated in addition to 2 O 3 exhibit low dielectric loss of 1 × 10 −4 or less (Samples No. 2 to 5, 8 to 11). Further, in the sample of the present invention, the firing temperature is 1600 ° C. or lower, and it can be seen that the sample can be fired at a lower temperature than before. Furthermore, the dielectric loss increases as the amount of CaO added increases, and
It can be seen that the firing temperature decreases as the amount of O added increases.

【0024】[0024]

【発明の効果】以上のように、本発明のアルミナ質焼結
体ではNa含有量をNa2 O換算で100ppm以下と
し、CaおよびMgを所定量含有させ、さらに、粒界相
にCaO・6Al2 3 とMgAl2 4 を存在させる
ことにより、焼結体の誘電損失を確実に1×10-4以下
とすることができるとともに、高純度のアルミナ原料を
用いなくても、純度99.9%程度の汎用原料を用いて
も1×10-4以下の誘電損失を得ることができるため、
焼結性および生産性を向上することができる。
As described above, in the alumina-based sintered body of the present invention, the Na content is set to 100 ppm or less in terms of Na 2 O, Ca and Mg are contained in a predetermined amount, and further CaO · 6Al is contained in the grain boundary phase. The presence of 2 O 3 and MgAl 2 O 4 ensures that the dielectric loss of the sintered body is 1 × 10 −4 or less, and the purity is 99.000 even without using a high-purity alumina raw material. Since a dielectric loss of 1 × 10 −4 or less can be obtained even if a general-purpose raw material of about 9% is used,
Sinterability and productivity can be improved.

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】主成分としてのアルミナに、Na含有量が
Na2 O換算で100ppm以下、CaがCaO換算で
0.5重量%以下、MgがMgO換算で0.03重量%
以上含有し、かつ、粒界相をX線回折測定した場合に、
CaO・6Al2 3 とMgAl2 4 のピークが存在
することを特徴とするアルミナ質焼結体。
1. Alumina, which is a main component, has a Na content of 100 ppm or less in terms of Na 2 O, Ca of 0.5 wt% or less in terms of CaO, and Mg 0.03 wt% in terms of MgO.
When the above is contained and the grain boundary phase is measured by X-ray diffraction,
An alumina-based sintered body having peaks of CaO · 6Al 2 O 3 and MgAl 2 O 4 .
【請求項2】測定周波数14GHzにおける誘電損失t
anδが1×10-4以下であることを特徴とする請求項
1記載のアルミナ質焼結体。
2. A dielectric loss t at a measurement frequency of 14 GHz.
The alumina sintered body according to claim 1, wherein an δ is 1 × 10 −4 or less.
JP03979395A 1995-02-28 1995-02-28 Alumina sintered body Expired - Fee Related JP3454957B2 (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001155546A (en) * 1999-11-29 2001-06-08 Ngk Spark Plug Co Ltd Insulator for spark plug and spark plug having the same
JP2007254273A (en) * 2006-02-24 2007-10-04 Kyocera Corp Alumina sintered compact, and member for treatment apparatus using the same, treatment apparatus, and treatment method
WO2009069770A1 (en) * 2007-11-28 2009-06-04 Kyocera Corporation Aluminous sinter, process for producing the same, member for semiconductor production apparatus, member for liquid-crystal-panel production apparatus, and member for dielectric resonator
US8247337B2 (en) 2007-11-28 2012-08-21 Kyocera Corporation Alumina sintered article
JP2015163569A (en) * 2014-01-30 2015-09-10 京セラ株式会社 Alumina sintered body and member for semiconductor manufacturing apparatus, and member for liquid crystal panel manufacturing apparatus
JP2016184513A (en) * 2015-03-26 2016-10-20 京セラ株式会社 Window member for high frequency, member for semiconductor manufacturing apparatus, and member for flat panel display (fpd) manufacturing apparatus

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001155546A (en) * 1999-11-29 2001-06-08 Ngk Spark Plug Co Ltd Insulator for spark plug and spark plug having the same
US6559579B2 (en) 1999-11-29 2003-05-06 Ngk Spark Plug Co., Ltd. Alumina-based sintered body insulator for spark plugs
JP2007254273A (en) * 2006-02-24 2007-10-04 Kyocera Corp Alumina sintered compact, and member for treatment apparatus using the same, treatment apparatus, and treatment method
WO2009069770A1 (en) * 2007-11-28 2009-06-04 Kyocera Corporation Aluminous sinter, process for producing the same, member for semiconductor production apparatus, member for liquid-crystal-panel production apparatus, and member for dielectric resonator
US8247337B2 (en) 2007-11-28 2012-08-21 Kyocera Corporation Alumina sintered article
JP2015163569A (en) * 2014-01-30 2015-09-10 京セラ株式会社 Alumina sintered body and member for semiconductor manufacturing apparatus, and member for liquid crystal panel manufacturing apparatus
JP2016184513A (en) * 2015-03-26 2016-10-20 京セラ株式会社 Window member for high frequency, member for semiconductor manufacturing apparatus, and member for flat panel display (fpd) manufacturing apparatus

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