JP2002241177A - Aluminum nitride sintered body having excellent degassing property - Google Patents

Aluminum nitride sintered body having excellent degassing property

Info

Publication number
JP2002241177A
JP2002241177A JP2001035162A JP2001035162A JP2002241177A JP 2002241177 A JP2002241177 A JP 2002241177A JP 2001035162 A JP2001035162 A JP 2001035162A JP 2001035162 A JP2001035162 A JP 2001035162A JP 2002241177 A JP2002241177 A JP 2002241177A
Authority
JP
Japan
Prior art keywords
sintered body
aluminum nitride
degassing
nitride sintered
mirror surface
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.)
Pending
Application number
JP2001035162A
Other languages
Japanese (ja)
Inventor
Makoto Sakamaki
誠 酒巻
Hiroyuki Matsuo
裕之 松尾
Kazusuke Minamizawa
一右 南澤
Hiromichi Otaki
浩通 大滝
Yukio Kishi
幸男 岸
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.)
Taiheiyo Cement Corp
NTK Ceratec Co Ltd
Original Assignee
Nihon Ceratec Co Ltd
Taiheiyo Cement Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nihon Ceratec Co Ltd, Taiheiyo Cement Corp filed Critical Nihon Ceratec Co Ltd
Priority to JP2001035162A priority Critical patent/JP2002241177A/en
Publication of JP2002241177A publication Critical patent/JP2002241177A/en
Pending legal-status Critical Current

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  • Container, Conveyance, Adherence, Positioning, Of Wafer (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide an aluminum nitride sintered body which has excellent degassing properties and can appropriately be used as a member for a semiconductor production device, to provide a production process of the sintered body and to provide the member for the semiconductor production device using the sintered body as the constituent material. SOLUTION: This sintered body is produced so that the resulting sintered body has a >=98% relative density and, in the sintered body, a grain boundary phase is crystallized, or so that the resulting sintered body has a >=98% relative density and, when the surface of the sintered body is subjected to mirror finish treatment in such a way as to provide a 5 nm average surface roughness (Ra) of a part of the mirror surface of the sintered body, in which a part no crystal grain falling-off is caused, the ratio of the total area of the mirror surface in which crystal grain falling-off is caused to the total area of the mirror surface is <=20%.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、半導体製造装置用
部材として使用される脱ガス特性に優れた窒化アルミニ
ウム焼結体およびその製造方法、ならびにそれを用いた
半導体製造装置用部材に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an aluminum nitride sintered body which is used as a member for a semiconductor manufacturing apparatus and has excellent degassing properties, a method for manufacturing the same, and a member for a semiconductor manufacturing apparatus using the same.

【0002】[0002]

【従来の技術】窒化アルミニウムは、熱伝導性が高く、
かつ耐食性に優れる緻密質セラミックスであるため、半
導体実装用放熱基板や、シャワープレート、チャンバ
ー、ドーム、クランプリング等の半導体製造装置用部材
として用いられている。
2. Description of the Related Art Aluminum nitride has high thermal conductivity,
Further, since it is a dense ceramic having excellent corrosion resistance, it is used as a heat dissipation board for mounting semiconductors, and a member for semiconductor manufacturing equipment such as a shower plate, a chamber, a dome, and a clamp ring.

【0003】しかしながら、従来の窒化アルミニウムは
脱ガス特性が悪く、半導体製造装置用部材として用いる
には、例えば、500℃において真空加熱処理(ベーキ
ング処理)を行って十分に脱ガス処理をした後に使用す
る必要がある。また、真空装置の使用に際しては、真空
系のガス開放が随時実施されるため、そのたびにベーキ
ング処理、あるいは長時間の真空引きを実施しなければ
ならない。このため、実際の半導体製造処理の前処理が
長時間化かつ煩雑化するとともに、装置自身にベーキン
グ処理するための付属設備が必要である等、極めて非効
率である。
However, conventional aluminum nitride has poor degassing properties, and is used after being sufficiently degassed by performing a vacuum heating process (baking process) at 500 ° C. for use as a member for semiconductor manufacturing equipment. There is a need to. Further, when using the vacuum apparatus, since the gas in the vacuum system is released as needed, a baking process or a long-time evacuation must be performed each time. For this reason, the pre-processing of the actual semiconductor manufacturing processing is prolonged and complicated, and the apparatus itself is extremely inefficient, such as requiring an attached facility for baking processing.

【0004】[0004]

【発明が解決しようとする課題】本発明はかかる事情に
鑑みてなされたものであって、脱ガス特性に優れ、半導
体製造装置用部材として好適な窒化アルミニウム焼結体
およびその製造方法、ならびにそのような窒化アルミニ
ウム焼結体を用いた半導体製造装置用部材を提供するこ
とを目的とする。
SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances, and has an aluminum nitride sintered body having excellent degassing properties and suitable as a member for a semiconductor manufacturing apparatus, a method for manufacturing the same, and a method for manufacturing the same. It is an object to provide a member for a semiconductor manufacturing apparatus using such an aluminum nitride sintered body.

【0005】[0005]

【課題を解決するための手段】本発明者等は、窒化アル
ミニウム焼結体が脱ガス特性に劣る原因について検討し
た結果、以下の知見を得た。
Means for Solving the Problems The present inventors have studied the causes of the inferior degassing properties of the aluminum nitride sintered body and obtained the following findings.

【0006】すなわち、半導体製造装置用部材は、通
常、鏡面加工して用いられるが、従来の窒化アルミニウ
ム焼結体は粒界が弱いため、鏡面加工中や洗浄中に粒界
に水分等の揮発分がしみ込みやすく、かつ鏡面加工の際
に結晶が脱落しやすく、このため脱ガス特性が悪くなる
ことを見出した。
That is, a member for a semiconductor manufacturing apparatus is usually used after being mirror-finished, but the conventional aluminum nitride sintered body has a weak grain boundary, so that water or the like volatilizes at the grain boundary during the mirror-polishing or cleaning. It has been found that crystals easily fall off and crystals easily fall off during mirror finishing, which degrades degassing properties.

【0007】そして、このような知見に基づいて、脱ガ
ス特性に優れた窒化アルミニウム焼結体を得るために
は、窒化アルミニウム焼結体の粒界相を強化することが
有効であることに想到した。
[0007] Based on such knowledge, it has been conceived that it is effective to strengthen the grain boundary phase of the aluminum nitride sintered body in order to obtain an aluminum nitride sintered body having excellent degassing properties. did.

【0008】本発明はこのような知見に基づいて完成さ
れたものであり、相対密度が98%以上であり、粒界が
結晶化していることを特徴とする脱ガス特性に優れた窒
化アルミニウム焼結体を提供する。
The present invention has been completed on the basis of these findings, and has a relative density of 98% or more and is characterized in that the grain boundaries are crystallized. Providing unity.

【0009】また、本発明は、相対密度が98%以上で
あり、結晶粒子の脱落のない部分の平均表面粗さRaが
5nmになるように鏡面処理したときの鏡面中に占める
結晶粒子の脱落面積が、鏡面全体の面積の20%以下で
あることを特徴とする脱ガス特性に優れた窒化アルミニ
ウム焼結体を提供する。
Further, according to the present invention, the crystal particles occupying the mirror surface when the mirror surface treatment is performed so that the relative density is 98% or more and the average surface roughness Ra of the portion where the crystal particles do not fall off is 5 nm. An aluminum nitride sintered body having an excellent degassing property, wherein the area is 20% or less of the area of the entire mirror surface.

【0010】本発明によれば、焼結体の相対密度を98
%以上として緻密化した上で、粒界相を結晶化するの
で、粒界相を健全で高強度なものとすることが可能とな
り、鏡面加工時または洗浄時の揮発分のしみ込みや鏡面
加工による結晶の脱落を抑制することができる。したが
って、良好な脱ガス特性を得ることができる。また、焼
結体の相対密度を98%以上として緻密化した上で、結
晶粒子の脱落のない部分の平均表面粗さRaが5nmに
なるように鏡面処理したときの鏡面中に占める結晶粒子
の脱落面積が、鏡面全体の面積の20%以下となるよう
にすることにより、揮発分吸着サイトを少なくすること
ができ、良好な脱ガス特性を得ることができる。
According to the present invention, the relative density of the sintered body is set to 98
% And then crystallize the grain boundary phase, which makes it possible to make the grain boundary phase sound and high-strength. Can be prevented from dropping out of the crystal. Therefore, good degassing characteristics can be obtained. Further, after the sintered body is densified with the relative density being 98% or more, the crystal particles occupying the mirror surface when the mirror surface treatment is performed so that the average surface roughness Ra of the portion where the crystal particles do not fall off is 5 nm. By setting the falling area to be equal to or less than 20% of the area of the entire mirror surface, it is possible to reduce the number of volatile adsorption sites and obtain good degassing characteristics.

【0011】半導体製造装置用部品として使用する場合
を考慮すると、300℃に加熱した際の脱ガスピーク値
が30ppb/cm以下であることが好ましい。
In consideration of use as a part for a semiconductor manufacturing apparatus, it is preferable that the peak value of degassing when heated to 300 ° C. is 30 ppb / cm 2 or less.

【0012】さらに、本発明は、窒化アルミニウム原料
および焼結助剤を配合し、成形し、所定の温度で焼成
後、1000℃まで300℃/hr以下の速度で降温す
ることを特徴とする脱ガス特性に優れた窒化アルミニウ
ム焼結体の製造方法を提供する。
Further, the present invention is characterized in that an aluminum nitride raw material and a sintering aid are blended, molded, fired at a predetermined temperature, and then cooled to 1000 ° C. at a rate of 300 ° C./hr or less. Provided is a method for producing an aluminum nitride sintered body having excellent gas properties.

【0013】このような方法を採用することにより、窒
化アルミニウムの粒界が結晶化して強化され、鏡面加工
時または洗浄時の揮発分のしみ込みや鏡面加工による結
晶の脱落を抑制することができる。したがって、良好な
脱ガス特性を得ることができる。なお、粒界は結晶を主
体としていればよく必ずしも完全に結晶化している必要
はない。
By adopting such a method, the grain boundaries of aluminum nitride are crystallized and strengthened, and it is possible to suppress the infiltration of volatile components at the time of mirror polishing or washing and the dropout of crystals due to mirror polishing. . Therefore, good degassing characteristics can be obtained. Note that the grain boundary is only required to be mainly composed of a crystal, and does not necessarily need to be completely crystallized.

【0014】上記本発明の窒化アルミニウム焼結体は、
脱ガス特性が良好であるから、シャワープレート、チャ
ンバー、ドーム、クランプリング等の半導体製造装置用
部材として好適である。
[0014] The aluminum nitride sintered body of the present invention,
Since it has good degassing properties, it is suitable as a member for semiconductor manufacturing equipment such as a shower plate, a chamber, a dome, and a clamp ring.

【0015】[0015]

【発明の実施の形態】以下、本発明について具体的に説
明する。本発明の窒化アルミニウム焼結体は、相対密度
が98%以上であり、粒界が結晶化している。
BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described specifically. The aluminum nitride sintered body of the present invention has a relative density of 98% or more and crystallized grain boundaries.

【0016】相対密度を98%以上としたのは、98%
未満では十分に緻密化しておらず、鏡面加工を施しても
ガス吸着サイトとなる残留気孔が多く存在するため脱ガ
ス特性が低下するからである。
The reason why the relative density is 98% or more is that 98%
If it is less than 10%, it is not sufficiently densified, and even if it is mirror-finished, there are many residual pores serving as gas adsorption sites, so that the degassing property is deteriorated.

【0017】本発明の窒化アルミニウム焼結体は、特に
制限はないが、典型的には、90〜99.99mass
%の窒化アルミニウムと、0.01〜10mass%の
酸化イットリウムを主体とする焼結助剤から実質的にな
るものである。この場合には、相対密度を98%以上と
する観点から、嵩密度が3.25g/cm以上が好ま
しく、3.28g/cm以上がより好ましい。
The aluminum nitride sintered body of the present invention is not particularly limited, but typically has a size of 90 to 99.99 mass.
% Of aluminum nitride and 0.01 to 10% by mass of yttrium oxide. In this case, the relative density from the viewpoint of 98% or more, a bulk density of preferably 3.25 g / cm 3 or more, 3.28 g / cm 3 or more is more preferable.

【0018】窒化アルミニウム焼結体において粒界相を
結晶化させるのは、これにより粒界相を健全で高強度な
ものとすることが可能となり、表面研磨加工時または洗
浄時の揮発分のしみ込みや表面研磨加工による結晶の脱
落を抑制し、もって良好な脱ガス特性を得ることがで
き、半導体製造装置部材として適したものとなるからで
ある。
The crystallization of the grain boundary phase in the aluminum nitride sintered body makes it possible to make the grain boundary phase sound and high-strength, and the stain of volatile components during surface polishing or cleaning. This is because it is possible to suppress the falling of the crystal due to the embedding and the surface polishing, thereby obtaining good degassing properties, and to be suitable as a member of a semiconductor manufacturing apparatus.

【0019】粒界相が非晶質の場合には、粒界相に気孔
が多くなりやすく粒界相の強度も低下するから、揮発分
のしみ込みや鏡面加工による結晶の脱落が生じやすく、
脱ガス特性が低いものとなる。なお、焼結助剤として酸
化イットリウムを主体とするものを用いた場合には、粒
界相の結晶としてはYAG(イットリウム・アルミニウ
ム・ガーネット)、YAM(イットリウム・アルミニウ
ム・モノクリニック)、YAP(イットリウム・アルミ
ニウム・ペロブスカイト)等のY−Al−O系化合物が
晶出する。
When the grain boundary phase is amorphous, pores tend to increase in the grain boundary phase, and the strength of the grain boundary phase is reduced.
Degassing characteristics are low. When yttrium oxide is mainly used as the sintering aid, YAG (yttrium aluminum garnet), YAM (yttrium aluminum monoclinic), and YAP (yttrium A Y-Al-O-based compound such as aluminum perovskite is crystallized.

【0020】本発明の窒化アルミニウム焼結体は、ま
た、上記相対密度を満たし、かつ結晶粒子の脱落のない
部分の平均表面粗さRaが5nmになるように鏡面処理
したときの鏡面中に占める結晶粒子の脱落面積が、鏡面
全体の面積の20%以下であることが好ましい。
The aluminum nitride sintered body of the present invention occupies the mirror surface when the mirror surface treatment is performed so that the above-mentioned relative density is satisfied and the average surface roughness Ra of the portion where crystal grains do not fall off is 5 nm. It is preferable that the falling area of the crystal particles is 20% or less of the area of the entire mirror surface.

【0021】鏡面加工により結晶粒子が脱落するとその
部分に揮発分が吸着され、脱ガスの原因となるが、上記
のように鏡面処理したときに結晶粒子の脱落面積が鏡面
全体の20%以下であれば、揮発分吸着サイトを十分に
少なくすることができ、半導体製造装置用部材として良
好な脱ガス特性を得ることができる。
When crystal grains fall off due to mirror finishing, volatile components are adsorbed to the parts and cause degassing. However, when the mirror finishing is performed as described above, the falling area of the crystal grains is less than 20% of the entire mirror surface. If so, the number of volatile adsorption sites can be sufficiently reduced, and good degassing properties can be obtained as a member for a semiconductor manufacturing apparatus.

【0022】結晶粒子の脱落面積が鏡面全体の面積の2
0%を超える場合には、揮発分の吸着サイトが多く、半
導体製造装置用部材として良好な脱ガス特性を得ること
が困難となる。
The area where crystal grains fall off is 2 times the area of the entire mirror surface.
If it exceeds 0%, there are many adsorption sites for volatile components, and it becomes difficult to obtain good degassing properties as a member for a semiconductor manufacturing apparatus.

【0023】また、本発明者らの実験により、窒化アル
ミニウム焼結体の脱ガス特性が、300℃に加熱した際
の脱ガスピーク値が30ppb/cm以下になるよう
なものであれば、半導体製造装置用部材として用いた場
合の真空加熱処理(ベーキング処理)を簡略化すること
ができ、半導体製造装置用部材として適したものとなる
ことが判明したが、上述のように相対密度が98%以上
であり、かつ粒界が結晶化しているか、または結晶粒子
の脱落のない部分の平均表面粗さRaが5nmになるよ
うに鏡面処理したときの鏡面中に占める結晶粒子の脱落
面積が鏡面全体の面積の20%以下であるような特性を
満たす場合には、鏡面加工により容易にこのような脱ガ
ス特性を満たすことができる。しかし、このような範囲
を外れる場合には、鏡面加工を十分に行ってもこのよう
な脱ガス特性を満たすことが極めて困難である。
According to experiments by the present inventors, if the degassing characteristic of the aluminum nitride sintered body is such that the degassing peak value when heated to 300 ° C. becomes 30 ppb / cm 2 or less, the semiconductor It has been found that the vacuum heating process (baking process) when used as a member for a manufacturing apparatus can be simplified and is suitable as a member for a semiconductor manufacturing apparatus. However, as described above, the relative density is 98%. When the grain boundary is crystallized, or when the mirror surface treatment is performed so that the average surface roughness Ra of the portion where the crystal particles do not fall off is 5 nm, the area where the crystal particles fall off in the mirror surface is the entire mirror surface. When the characteristics satisfying 20% or less of the area are satisfied, such degassing characteristics can be easily satisfied by mirror finishing. However, if it is out of such a range, it is extremely difficult to satisfy such degassing properties even if the mirror finishing is sufficiently performed.

【0024】なお、脱ガス特性を測定する方法として
は、例えば、500℃まで100℃ずつ段階的に加熱
し、そのときのガス発生量を適宜のガス分析装置で測定
し、300℃で加熱したときのガス発生量のピーク値を
求める方法が採用される。また、この際に用いるガス分
析装置としては、ガスを直接高感度で質量分析すること
ができることから大気圧イオン化質量分析装置(API
−MS)が好ましい。
As a method of measuring the degassing characteristics, for example, heating was performed in steps of 100 ° C. in steps of up to 500 ° C., and the amount of gas generated at that time was measured by an appropriate gas analyzer, and heating was performed at 300 ° C. A method of obtaining the peak value of the gas generation amount at the time is adopted. As a gas analyzer used in this case, since gas can be directly subjected to mass analysis with high sensitivity, an atmospheric pressure ionization mass analyzer (API)
-MS) is preferred.

【0025】上述の粒界相が結晶化した窒化アルミニウ
ム焼結体を得るためには、窒化アルミニウム原料および
焼結助剤を配合し、成形し、所定の温度で焼成後、10
00℃まで300℃/hr以下の速度で降温することが
好ましい。一般的に、焼成温度では粒界相は液相である
から、1000℃まで300℃/hr以下と比較的緩冷
却することにより、液相状態から固化する間に十分に結
晶化される。300℃/hrを超えると粒界相が非晶質
となりやすく、粒界相が十分に強化されない。
In order to obtain an aluminum nitride sintered body in which the above-mentioned grain boundary phase is crystallized, an aluminum nitride raw material and a sintering aid are blended, molded, fired at a predetermined temperature, and heated.
It is preferable to lower the temperature to 00 ° C at a rate of 300 ° C / hr or less. In general, at the firing temperature, the grain boundary phase is a liquid phase. Therefore, by relatively slow cooling to 300 ° C./hr or less up to 1000 ° C., the crystal is sufficiently crystallized during solidification from the liquid phase state. If it exceeds 300 ° C./hr, the grain boundary phase tends to be amorphous, and the grain boundary phase is not sufficiently strengthened.

【0026】なお、焼結体の焼成温度から1000℃ま
で300℃/hr以下で冷却する代わりに、炉内徐冷後
に再熱処理を実施しても同様の効果が得られる。
The same effect can be obtained by performing re-heat treatment after slow cooling in the furnace, instead of cooling from the firing temperature of the sintered body to 1000 ° C. at 300 ° C./hr or less.

【0027】本発明の窒化アルミニウム焼結体はこのよ
うに脱ガス特性が良好なことから、本発明の窒化アルミ
ニウム焼結体を用いて製造されたシャワープレート、チ
ャンバー、ドーム、クランプリング等の半導体製造装置
用部材は、脱ガスが抑制された極めて良好な特性を示
す。
Since the aluminum nitride sintered body of the present invention has such good degassing properties, semiconductors such as shower plates, chambers, domes, and clamp rings manufactured using the aluminum nitride sintered body of the present invention. The member for a manufacturing apparatus exhibits extremely good characteristics in which degassing is suppressed.

【0028】[0028]

【実施例】以下、本発明の実施例について説明する。Y
を焼結助剤として含有する窒化アルミニウム顆粒
(Y:5mass%)をCIPにより成形して成
形体を作成した後、その成形体をN雰囲気中の所定温
度で2hr焼成後、種々の冷却条件で冷却し、窒化アル
ミニウム焼結体を製造した。これら焼結体について、嵩
密度を測定するとともに、相対密度を計算により求め
た。また、X線回折により粒界相の状態を確認した。次
に、これら焼結体を切断加工し、4×3×30(mm)
の6面鏡面仕上げの試験片を得た。このときの鏡面加工
は結晶粒子の脱落がない部分の平均表面粗さRaが5n
mになるまで行い、電子顕微鏡観察により、□200μ
mの視野における結晶粒子の脱落面積を求めた。さら
に、各試験片の結晶粒子脱落部分をも含めた平均表面粗
さRaを測定するとともに、各試験片をArフロー中高
純度石英管の中で室温から500℃まで段階的に加熱し
ながらAPI−MSにより脱ガス量の測定を行い、30
0℃における脱ガスのピーク値を脱ガス量として求め、
30ppb/cm以下を○、30ppb/cmを超
えた場合を×として脱ガス特性を評価した。これら結果
を表1に示す。
Embodiments of the present invention will be described below. Y
Aluminum nitride granules (Y 2 O 3 : 5 mass%) containing 2 O 3 as a sintering aid are molded by CIP to form a molded body, and the molded body is fired at a predetermined temperature in a N 2 atmosphere for 2 hours. Thereafter, cooling was performed under various cooling conditions to produce an aluminum nitride sintered body. For these sintered bodies, the bulk density was measured, and the relative density was determined by calculation. Further, the state of the grain boundary phase was confirmed by X-ray diffraction. Next, these sintered bodies were cut and processed into 4 × 3 × 30 (mm)
Of 6 mirror finishes were obtained. At this time, the mirror-finished surface had an average surface roughness Ra of 5 n in a portion where crystal grains did not fall off.
m and observed with an electron microscope.
The falling area of the crystal particles in the field of view of m was determined. Furthermore, the average surface roughness Ra including the crystal particle falling-off portions of each test piece was measured, and the API-T was heated while gradually heating each test piece from room temperature to 500 ° C. in a high-purity quartz tube in an Ar flow. The degassing amount was measured by MS, and 30
The degassing peak value at 0 ° C. is determined as the degassing amount,
30 ppb / cm 2 or less ○, it was evaluated degassing properties if it exceeds 30 ppb / cm 2 as ×. Table 1 shows the results.

【0029】[0029]

【表1】 [Table 1]

【0030】表1に示すように、本発明を満たす実施例
1〜5は良好な脱ガス特性を示したが、焼結体の相対密
度は本発明の範囲内ではあるが粒界相が非晶質の比較例
1,2、粒界相は結晶であるが相対密度が低い比較例
3,4は、結晶粒子脱落面積が20%を超えており、粒
子脱落部分も含めた表面粗さが大きく脱ガス特性も30
ppb/cmを超えていた。
As shown in Table 1, Examples 1 to 5 satisfying the present invention exhibited good degassing properties, but the relative density of the sintered body was within the range of the present invention, but the grain boundary phase was not. In Comparative Examples 1 and 2 of crystallinity, and Comparative Examples 3 and 4 in which the grain boundary phase is a crystal but the relative density is low, the crystal particle falling area exceeds 20%, and the surface roughness including the particle falling part is low. Large degassing characteristics 30
ppb / cm 2 .

【0031】[0031]

【発明の効果】以上説明したように本発明によれば、焼
結体の相対密度を98%以上として緻密化した上で、粒
界相を結晶化するので、粒界相を健全で高強度なものと
することが可能となり、鏡面加工時または洗浄時の揮発
分のしみ込みや鏡面加工による結晶の脱落を抑制するこ
とができる。したがって、良好な脱ガス特性を得ること
ができる。また、焼結体の相対密度を98%以上として
緻密化した上で、結晶粒子の脱落のない部分の平均表面
粗さRaが5nmになるように鏡面処理したときの鏡面
中に占める結晶粒子の脱落面積が、鏡面全体の面積の2
0%以下となるようにすることにより、揮発分吸着サイ
トを少なくすることができ、良好な脱ガス特性を得るこ
とができる。
As described above, according to the present invention, the sintered body is densified with the relative density of 98% or more, and the grain boundary phase is crystallized. It is possible to suppress the infiltration of volatile components at the time of mirror polishing or washing, and the drop of crystals due to mirror polishing. Therefore, good degassing characteristics can be obtained. Further, after the sintered body is densified with the relative density being 98% or more, the crystal particles occupying the mirror surface when the mirror surface treatment is performed so that the average surface roughness Ra of the portion where the crystal particles do not fall off is 5 nm. The falling area is 2 of the area of the entire mirror surface.
By controlling the content to be 0% or less, the number of sites for adsorbing volatile components can be reduced, and good degassing properties can be obtained.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 松尾 裕之 宮城県仙台市泉区明通三丁目5番 株式会 社日本セラテック本社工場内 (72)発明者 南澤 一右 宮城県仙台市泉区明通三丁目5番 株式会 社日本セラテック本社工場内 (72)発明者 大滝 浩通 宮城県仙台市泉区明通三丁目5番 株式会 社日本セラテック本社工場内 (72)発明者 岸 幸男 宮城県仙台市泉区明通三丁目5番 株式会 社日本セラテック本社工場内 Fターム(参考) 4G001 BA09 BA36 BB09 BB36 BC51 BC54 BD36 BD38 BE26 BE33 BE35 5F031 HA02 PA26  ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Hiroyuki Matsuo 3-5 Akimitsu, Izumi-ku, Sendai City, Miyagi Prefecture Inside of Japan Ceratech Co., Ltd. No. 3-5, Tsudori Japan Ceratech Head Office Factory (72) Inventor Hirotsumaki Otaki 3-chome, Akimichi, Izumi-ku, Sendai, Miyagi Prefecture, Japan Inside Ceratech Japan Head Office Factory (72) Inventor Yukio Kishi Sendai, Miyagi Prefecture F-term (reference) 4G001 BA09 BA36 BB09 BB36 BC51 BC54 BD36 BD38 BE26 BE33 BE35 5F031 HA02 PA26

Claims (5)

【特許請求の範囲】[Claims] 【請求項1】 相対密度が98%以上であり、粒界相が
結晶化していることを特徴とする脱ガス特性に優れた窒
化アルミニウム焼結体。
1. An aluminum nitride sintered body having an excellent degassing property, characterized in that the relative density is 98% or more and the grain boundary phase is crystallized.
【請求項2】 相対密度が98%以上であり、結晶粒子
の脱落のない部分の平均表面粗さRaが5nmになるよ
うに鏡面処理したときの鏡面中に占める結晶粒子の脱落
面積が、鏡面全体の面積の20%以下であることを特徴
とする脱ガス特性に優れた窒化アルミニウム焼結体。
2. The method according to claim 1, wherein the relative density is 98% or more, and the area of the crystal particles falling out of the mirror surface when the mirror surface treatment is performed so that the average surface roughness Ra of the portion where the crystal particles do not fall off is 5 nm. An aluminum nitride sintered body having an excellent degassing property, wherein the sintered body is 20% or less of the entire area.
【請求項3】 300℃に加熱した際の脱ガスピーク値
が30ppb/cm 以下であることを特徴とする請求
項1または請求項2に記載の脱ガス特性に優れた窒化ア
ルミニウム焼結体。
3. Degassing peak value when heated to 300 ° C.
Is 30 ppb / cm 2Claims characterized by the following
Item 3. The nitride according to item 1 or 2, which is excellent in degassing properties.
Luminium sintered body.
【請求項4】 窒化アルミニウム原料および焼結助剤を
配合し、成形し、所定の温度で焼成後、1000℃まで
300℃/hr以下の速度で降温することを特徴とする
脱ガス特性に優れた窒化アルミニウム焼結体の製造方
法。
4. An excellent degassing property characterized by blending an aluminum nitride raw material and a sintering aid, molding, firing at a predetermined temperature, and cooling down to 1000 ° C. at a rate of 300 ° C./hr or less. Of producing a sintered aluminum nitride body.
【請求項5】 請求項1から請求項3のいずれかの窒化
アルミニウム焼結体で形成された半導体製造装置用部
材。
5. A member for a semiconductor manufacturing apparatus formed of the aluminum nitride sintered body according to any one of claims 1 to 3.
JP2001035162A 2001-02-13 2001-02-13 Aluminum nitride sintered body having excellent degassing property Pending JP2002241177A (en)

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Country Link
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002097075A (en) * 2000-07-19 2002-04-02 Nihon Ceratec Co Ltd Ceramic material
JP2008297136A (en) * 2007-05-29 2008-12-11 Taiheiyo Cement Corp Method of manufacturing ceramic component for semiconductor manufacture and method of fitting the same

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06191953A (en) * 1992-12-28 1994-07-12 Kyocera Corp Aluminum nitride sintered compact
JP2000264737A (en) * 1999-03-11 2000-09-26 Agency Of Ind Science & Technol Aluminum nitride sintered compact and its production
JP2000327430A (en) * 1999-05-18 2000-11-28 Tokuyama Corp Aluminum nitride sintered compact and its production

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06191953A (en) * 1992-12-28 1994-07-12 Kyocera Corp Aluminum nitride sintered compact
JP2000264737A (en) * 1999-03-11 2000-09-26 Agency Of Ind Science & Technol Aluminum nitride sintered compact and its production
JP2000327430A (en) * 1999-05-18 2000-11-28 Tokuyama Corp Aluminum nitride sintered compact and its production

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002097075A (en) * 2000-07-19 2002-04-02 Nihon Ceratec Co Ltd Ceramic material
JP2008297136A (en) * 2007-05-29 2008-12-11 Taiheiyo Cement Corp Method of manufacturing ceramic component for semiconductor manufacture and method of fitting the same

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