JP3518445B2 - CMP wastewater treatment equipment - Google Patents
CMP wastewater treatment equipmentInfo
- Publication number
- JP3518445B2 JP3518445B2 JP30437299A JP30437299A JP3518445B2 JP 3518445 B2 JP3518445 B2 JP 3518445B2 JP 30437299 A JP30437299 A JP 30437299A JP 30437299 A JP30437299 A JP 30437299A JP 3518445 B2 JP3518445 B2 JP 3518445B2
- Authority
- JP
- Japan
- Prior art keywords
- water
- cmp
- activated carbon
- membrane
- film
- 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.)
- Expired - Fee Related
Links
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
- Removal Of Specific Substances (AREA)
- Water Treatment By Sorption (AREA)
Description
【発明の詳細な説明】
【０００１】
【発明の属する技術分野】本発明は半導体基板或いは該
基板上に形成された被膜を研磨（化学機械研磨（ＣＭ
Ｐ））した際に排出されるＣＭＰ排水の処理装置に関す
る。
【０００２】
【従来の技術】半導体の製造工程には、半導体基板又は
基板上に形成されたシリコン酸化膜等の被膜の表面を平
坦化するために、研磨剤を用いて該表面を化学機械研磨
（ＣＭＰ）する工程がある。
【０００３】このＣＭＰに用いられる研磨剤としてのＣ
ＭＰスラリーにはシリカ系とメタル系とがあり、シリカ
系ではコロイダル（又はフュームド）シリカ（Ｓｉ
Ｏ２）が、また、メタル系ではアルミナ（Ａｌ２Ｏ３）
や酸化セリウム（ＣｅＯ２）等がそれぞれ研磨粒子とし
て用いられている。これらの研磨粒子はＣＭＰスラリー
中に約１０〜２０重量％含有されている。
【０００４】このＣＭＰプロセス後は、基板上に残留す
るＣＭＰスラリーを除去するために、スラリー使用量の
約１００倍量の超純水（又は洗浄薬剤を含んだ超純水）
で洗浄する。
【０００５】従って、この研磨工程からは、研磨粒子や
研磨屑（研磨粒子や研磨バッドが研磨中に破砕されたも
の、或いは、基板又は基板上の被膜から研磨により削り
取られたもの）等を含むＣＭＰ排水が大量に排出され
る。
【０００６】なお、ＣＭＰ排水には、ＣＭＰスラリーに
由来する過酸化水素（Ｈ２Ｏ２）が含まれている場合が
ある。また、ＣＭＰ処理に続いて行われる、ＣＭＰスラ
リーを取り除くための洗浄工程において、Ｈ２Ｏ２を含
む洗浄水が使用されるため、この洗浄排水を含むＣＭＰ
排水にもＨ２Ｏ２が含まれることとなる。
【０００７】このＣＭＰ排水は、研磨粒子や研磨屑由来
の微粒子、更にはＨ２Ｏ２を含むこと以外は、その水質
は良好なものであるため、この微粒子とＨ２Ｏ２を除去
した後、回収水として、前処理系、一次純水製造系及び
二次純水製造系（サブシステム）からなる超純水製造シ
ステムの一次純水製造系に送られ、前処理系の処理水と
共に処理され、再利用されている。
【０００８】従来、このようなＣＭＰ排水の処理方法と
しては、予めＣＭＰ排水中のＨ２Ｏ ２を分解除去した
後、懸濁物質（ＳＳ）を分離除去する方法が採用されて
おり、特開平９−１１７７６３号公報には、Ｈ２Ｏ２を
Ｈ２Ｏ２分解酵素で予め分解除去した後、高分子膜でＳ
Ｓを膜分離する方法が提案されている。この方法では、
Ｈ２Ｏ２で高分子膜が劣化するのを防止するために、予
めＨ２Ｏ２を除去した後、膜分離を行っている。
【０００９】なお、Ｈ２Ｏ２は、活性炭を用いて分解除
去することもできる。この場合、粒状活性炭を充填した
活性炭塔に通水すると、塔内にＳＳが蓄積され、通水不
能となることから、粉末活性炭が用いられる。更に、Ｈ
２Ｏ２は過硫酸塩等で分解除去することもできる。
【００１０】また、ＳＳの分離除去には凝集・砂濾過法
も採用可能である。
【００１１】
【発明が解決しようとする課題】特開平９−１１７７６
３号公報に記載される方法のように、Ｈ２Ｏ２を予め分
解除去した後ＳＳを膜分離して除去する従来の方法で
は、膜面にスライムが急激に付着成長して膜フラックス
が低下するため、長期間連続通水することが不可能であ
った。加えて、分離膜として有機膜を用いた場合には、
コロイダルシリカ等のＳＳにより膜面が摩耗し、長期間
連続使用すると、膜が破断する恐れがあった。更に、Ｃ
ＭＰ排水にはコロイダルシリカ等の研磨粒子の安定化の
ために研磨スラリーに配合されたアルコールや界面活性
剤等の有機成分が含有されている場合もあるが、これら
の有機成分を除去することができないという不具合もあ
った。
【００１２】一方、凝集・砂濾過によるＳＳの分離で
は、膜フラックスの低下や膜劣化の問題はないが、ＳＳ
微粒子が濾過水中にリークし、ＳＳを高度に分離除去す
ることができない。
【００１３】また、Ｈ２Ｏ２の分解除去に際しても、酵
素や過硫酸塩による方法では、処理水を回収水として再
利用する場合、酵素や過硫酸塩が超純水製造システムの
負荷となることから好ましくない。
【００１４】本発明は上記従来の問題点を解決し、研磨
粒子や研磨屑などのＳＳ及びＨ２Ｏ ２と、更には有機成
分をも含むＣＭＰ排水を効率的に処理することができ、
しかも、長期連続運転が可能なＣＭＰ排水の処理装置を
提供することを目的とする。
【００１５】
【課題を解決するための手段】本発明のＣＭＰ排水の処
理装置は、過酸化水素を含むＣＭＰ排水の処理装置にお
いて、該ＣＭＰ排水中の懸濁物質を分離する無機膜分離
装置と、該膜分離装置の透過水を粒状活性炭と接触させ
る活性炭塔とを有することを特徴とする。
【００１６】本発明においては、Ｈ２Ｏ２を含むＣＭＰ
排水を膜分離処理するため、Ｈ２Ｏ ２の殺菌作用で膜面
にスライムが付着、成長することはなく、長期に亘り膜
フラックスを高く維持して安定な膜分離処理を行ってＳ
Ｓを高度に除去することができる。しかも、分離膜とし
て化学的耐久性、機械的強度に優れた無機膜を用いるた
め、Ｈ２Ｏ２による劣化の問題もなく、また、コロイダ
ルシリカ等のＳＳにより膜が削り取られて摩耗すること
もなく、長期間使用可能である。
【００１７】このように無機膜分離装置でＳＳを除去し
た水を次いで活性炭塔に通水して粒状活性炭で処理する
ことにより、Ｈ２Ｏ２を効率的に分解除去すると共に、
有機成分も吸着除去することができるため、著しく高水
質の処理水を得ることができる。
【００１８】
【発明の実施の形態】以下に本発明の実施の形態を詳細
に説明する。
【００１９】図１は本発明のＣＭＰ排水の処理装置の実
施の形態を示す系統図である。
【００２０】図１の方法では、ＣＭＰ排水を受水槽１を
経てポンプＰによりまずセラミックフィルタ２等の無機
膜分離装置に通水して、ＣＭＰ排水中のＳＳを分離除去
する。
【００２１】このＳＳ除去に用いる膜の材質は、無機膜
であれば良く、セラミックの他、焼結金属膜等を用いる
ことができる。また、無機膜分離装置の膜形式（平膜、
中空糸、管状など）、給水方法（加圧式、吸引式）、膜
孔径（精密濾過膜、限外濾過膜）等には特に制限はな
く、要求水質や処理効率等に応じて任意に決定される。
【００２２】このセラミックフィルタ２等の無機膜分離
装置における膜分離処理において、ＣＭＰ排水中のＨ２
Ｏ２による殺菌作用で膜面へのスライムの付着成長は防
止され、膜フラックスは高く維持される。また、膜が無
機膜であることから、Ｈ２Ｏ ２による劣化やＳＳによる
摩耗の問題もない。
【００２３】このセラミックフィルタ２等の無機膜分離
装置の透過水は次いで活性炭塔３に通水され、濃縮水は
排水として系外へ排出される。
【００２４】活性炭塔３に充填する粒状活性炭の粒径に
は特に制限はないが、過度に小さ過ぎると通水抵抗が大
きくなり、過度に大き過ぎると接触面積が少なくなり、
Ｈ２Ｏ２分解効率が低下するため、１〜１００メッシュ
の範囲で適当な大きさのものを用いるのが好ましい。
【００２５】この活性炭塔３の通水方式は、下向流であ
っても上向流であっても良いが、固定床が形成され、接
触頻度（接触効率）が向上する点から、下向流通水とす
るのが好ましい。
【００２６】活性炭塔３では、Ｈ２Ｏ２の分解除去と共
に、有機成分の吸着除去が行われることから、著しく高
水質の処理水を得ることができる。
【００２７】この活性炭塔への通水ＳＶは、１ｈｒ−１
以上、特に１０〜５０ｈｒ−１とすることが、過酸化水
素の分解、差圧などの点から好ましい。
【００２８】なお、本発明で処理対象とするＣＭＰ排水
中に含まれる研磨剤の種類には特に制限はなく、シリカ
（コロイダルシリカ）系であっても、アルミナや酸化セ
リウム、酸化マグネシウム等のメタル系のいずれであっ
ても良い。
【００２９】
【実施例】以下に実施例を挙げて本発明をより具体的に
説明する。
【００３０】実施例１
下記水質のＣＭＰ排水を図１に示すＣＭＰ排水の処理装
置により１ｍ３／ｈｒの処理水量で処理した。
【００３１】〔ＣＭＰ排水水質〕
ＳＳ：１００ｐｐｍ
Ｈ２Ｏ２：３００ｐｐｍ
ＴＯＣ：２０００ｐｐｂ
受水槽１の容量は１ｍ３であり、セラミックフィルタ２
及び活性炭塔３としては次のようなものを用いた。セラ
ミックフィルタ２からは透過水０．９５ｍ３／ｈｒと濃
縮水０．０５ｍ３／ｈｒを得、濃縮水は系外へ排出し
た。また、活性炭塔３の通水ＳＶは１０ｈｒ−１とし
た。
【００３２】〔セラミックフィルタ〕
栗田工業（株）製セラミックフィルタ
分画：０．０２μｍ
設計フラックス：１ｍ３／ｍ２・日ａｔ２５℃
【００３３】〔活性炭塔〕
栗田工業（株）製粒状活性炭（石炭系）１０／３２メッ
シュを充填した下向流式活性炭塔
その結果、得られた処理水の水質は下記の通りであり、
回収水として十分な水質を有するものであった。
【００３４】〔処理水水質〕
ＳＳ：＜０．５ｐｐｍ
Ｈ２Ｏ２：＜１ｐｐｍ
ＴＯＣ：２０〜５０ｐｐｂ
また、セラミックフィルタの膜フラックスの経時変化は
図２に示す通りであり、膜フラックス１ｍ３／ｍ２・日
を安定して得ることができることが確認された。
【００３５】
【発明の効果】以上詳述した通り、本発明のＣＭＰ排水
の処理装置によれば、ＣＭＰ排水を長期に亘り効率的に
処理して、ＳＳ、Ｈ２Ｏ２、ＴＯＣ等が高度に除去さ
れ、超純水製造システムの補給水として有効利用するこ
とができる高水質の処理水を安定に得ることができる。DETAILED DESCRIPTION OF THE INVENTION
[0001]
BACKGROUND OF THE INVENTION 1. Field of the Invention
Polishing the film formed on the substrate (chemical mechanical polishing (CM
P)) related to the treatment equipment for CMP wastewater discharged
The
[0002]
2. Description of the Related Art In a semiconductor manufacturing process, a semiconductor substrate or
Flatten the surface of the silicon oxide film or other film formed on the substrate.
Chemical mechanical polishing of the surface with an abrasive to support
There is a step of (CMP).
C as an abrasive used in this CMP
There are two types of MP slurry: silica and metal.
Colloidal (or fumed) silica (Si
O2), But in the case of metal, alumina (Al2O3)
And cerium oxide (CeO2) Etc. as abrasive particles
It is used. These abrasive particles are CMP slurry
About 10 to 20% by weight is contained therein.
After this CMP process, it remains on the substrate.
To remove the CMP slurry
About 100 times the amount of ultrapure water (or ultrapure water containing cleaning chemicals)
Wash with.
Therefore, from this polishing step, abrasive particles and
Abrasive debris (abrasive particles and polishing pads that were crushed during polishing)
Or by polishing from the substrate or coating on the substrate
A large amount of CMP wastewater including
The
In addition, CMP waste water is used for CMP slurry.
Derived hydrogen peroxide (H2O2) May be included
is there. In addition, a CMP slurry, which is performed following the CMP process, is performed.
In the cleaning process for removing Lee, H2O2Including
CMP that includes this cleaning wastewater
H for drainage2O2Will be included.
This CMP waste water is derived from abrasive particles and polishing debris.
Fine particles, and even H2O2The water quality except that
Is good, so these fine particles and H2O2Remove
After that, as recovered water, pretreatment system, primary pure water production system and
Ultrapure water production system consisting of secondary pure water production system (subsystem)
Sent to the primary pure water production system of the stem and treated water of the pretreatment system
They are both processed and reused.
Conventionally, such a CMP wastewater treatment method and
In advance, H in the CMP waste water2O 2Was removed
After that, a method of separating and removing suspended solids (SS) was adopted.
JP-A-9-117763 discloses H2O2The
H2O2After decomposing and removing in advance with a degrading enzyme, S
A method for membrane separation of S has been proposed. in this way,
H2O2In order to prevent the polymer film from
Me H2O2After removing the film, membrane separation is performed.
In addition, H2O2Release minutes using activated carbon
You can leave. In this case, filled with granular activated carbon
When water is passed through the activated carbon tower, SS accumulates in the tower and water passage is not possible.
Powdered activated carbon is used because of its capability. In addition, H
2O2Can be decomposed and removed with persulfate or the like.
In addition, the separation and removal of SS is performed by a coagulation / sand filtration method.
Can also be adopted.
[0011]
SUMMARY OF THE INVENTION Problems to be Solved by the Invention
As in the method described in No. 3 publication, H2O2In advance
After removing the solution, the conventional method of removing SS by membrane separation
Is the film flux due to the rapid growth of slime on the film surface.
It is impossible to continuously pass water for a long time because
It was. In addition, when an organic membrane is used as the separation membrane,
The film surface is worn by SS such as colloidal silica, and it is long-term
When used continuously, the membrane may break. In addition, C
MP drainage is used to stabilize abrasive particles such as colloidal silica.
Alcohol and surface activity added to the polishing slurry
In some cases, organic components such as agents are contained.
There is also a problem that it is not possible to remove the organic components of
It was.
On the other hand, by separation of SS by coagulation and sand filtration
There is no problem of membrane flux reduction or membrane degradation, but SS
Fine particles leak into filtered water, and SS is separated and removed to a high degree
I can't.
Also, H2O2When decomposing and removing
In the method using elemental or persulfate, treated water is recycled as recovered water.
When used, enzymes and persulfate are used in ultrapure water production systems.
Since it becomes a load, it is not preferable.
The present invention solves the above-mentioned conventional problems and polishes them.
SS and H such as particles and polishing waste2O 2And even organic
CMP wastewater including water can be treated efficiently,
Moreover, a CMP wastewater treatment device that can be operated for a long period of time.
The purpose is to provide.
[0015]
[Means for Solving the Problems] Treatment of CMP waste water of the present invention
The physical equipment is used in the treatment equipment for CMP wastewater containing hydrogen peroxide.
Inorganic membrane separation for separating suspended substances in the CMP waste water
The apparatus and the permeated water of the membrane separator are brought into contact with the granular activated carbon.
And an activated carbon tower.
In the present invention, H2O2CMP including
H is used for membrane separation treatment of wastewater.2O 2Membrane surface by bactericidal action
Slime does not adhere to and grow on the film for a long time
Stable membrane separation treatment with high flux maintained
S can be removed to a high degree. Moreover, as a separation membrane
Use an inorganic film with excellent chemical durability and mechanical strength.
H2O2There is no problem of deterioration due to
The film is scraped and worn by SS such as rusilica.
It can be used for a long time.
Thus, SS is removed by the inorganic membrane separator.
Water is then passed through an activated carbon tower and treated with granular activated carbon.
H2O2Is efficiently decomposed and removed,
Organic components can also be adsorbed and removed, resulting in extremely high water
Quality treated water can be obtained.
[0018]
DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the present invention are described in detail below.
Explained.
FIG. 1 is a diagram of an apparatus for treating CMP waste water according to the present invention.
It is a systematic diagram showing an embodiment.
In the method of FIG. 1, the CMP waste water is passed through the water receiving tank 1.
After that, inorganic such as ceramic filter 2 etc. by pump P first
Pass through the membrane separator to separate and remove SS in the CMP waste water
To do.
The material of the film used for removing SS is an inorganic film.
It is sufficient if a sintered metal film or the like is used in addition to ceramic.
be able to. In addition, the membrane type of the inorganic membrane separator (flat membrane,
Hollow fiber, tubular, etc.), water supply method (pressurization, suction), membrane
There are no particular restrictions on the pore size (microfiltration membrane, ultrafiltration membrane), etc.
In addition, it is arbitrarily determined according to the required water quality and treatment efficiency.
Inorganic membrane separation of the ceramic filter 2 and the like
In membrane separation processing in the equipment, H in CMP waste water2
O2Prevents slime adhesion and growth on the film surface due to bactericidal action
The membrane flux is kept high. Also, no membrane
Because it is a film, H2O 2Due to deterioration or SS
There is no problem of wear.
Inorganic membrane separation of this ceramic filter 2 and the like
The permeated water of the apparatus is then passed through the activated carbon tower 3, and the concentrated water is
Wastewater is discharged outside the system.
The particle size of the granular activated carbon charged in the activated carbon tower 3
There is no particular restriction, but if it is too small, the resistance to water flow is large.
If it is too large, the contact area will decrease,
H2O21-100 mesh because degradation efficiency decreases
It is preferable to use a material having an appropriate size within the range.
The water flow system of the activated carbon tower 3 is a downward flow.
However, a fixed bed is formed and contacted.
From the point that touch frequency (contact efficiency) improves, it is considered as downward circulation water.
It is preferable.
In the activated carbon tower 3, H2O2Co-decomposing and removing
In addition, since organic components are removed by adsorption,
Treated water with quality can be obtained.
The water flow SV to the activated carbon tower is 1 hr.-1
Above, especially 10-50hr-1Can be peroxidized water
It is preferable from the viewpoints of elemental decomposition and differential pressure.
Incidentally, the CMP waste water to be treated in the present invention.
There is no particular limitation on the type of abrasive contained in the silica.
(Colloidal silica)
Either metal such as lithium or magnesium oxide
May be.
[0029]
The present invention will be described in more detail with reference to the following examples.
explain.
Example 1
The following water quality CMP wastewater treatment equipment shown in Figure 1
1m depending on the position3Treated with an amount of treated water of / hr.
[CMP wastewater quality]
SS: 100 ppm
H2O2: 300ppm
TOC: 2000ppb
Capacity of receiving tank 1 is 1m3The ceramic filter 2
As the activated carbon tower 3, the following was used. Sera
Permeated water 0.95m from Mick filter 23/ Hr and dark
Shrinkage 0.05m3/ Hr is obtained, and the concentrated water is discharged out of the system.
It was. Moreover, the water flow SV of the activated carbon tower 3 is 10 hours.-1age
It was.
[Ceramic filter]
Ceramic filter made by Kurita Kogyo Co., Ltd.
Fraction: 0.02 μm
Design flux: 1m3/ M2・ Day at 25 ℃
[Activated carbon tower]
Kurita Industries Co., Ltd. granular activated carbon (coal) 10/32 mesh
Downflow type activated carbon tower packed with
As a result, the quality of the treated water obtained is as follows,
The recovered water had sufficient water quality.
[Processed water quality]
SS: <0.5ppm
H2O2: <1ppm
TOC: 20-50ppb
Also, the change over time in the membrane flux of the ceramic filter is
As shown in FIG. 2, the membrane flux is 1 m3/ M2·Day
It was confirmed that can be obtained stably.
[0035]
As described in detail above, the CMP waste water of the present invention.
According to this processing equipment, CMP drainage can be efficiently conducted over a long period of time.
Process, SS, H2O2, TOC, etc. are highly removed
It can be effectively used as makeup water for the ultrapure water production system.
It is possible to stably obtain high-quality treated water that can be obtained.
【図面の簡単な説明】
【図１】本発明のＣＭＰ排水の処理装置の実施の形態を
示す系統図である。
【図２】実施例１における膜フラックスの経時変化を示
すグラフである。
【符号の説明】
１ 受水槽
２ セラミックフィルタ
３ 活性炭塔BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a system diagram showing an embodiment of a CMP wastewater treatment apparatus of the present invention. FIG. 2 is a graph showing the change with time of the membrane flux in Example 1. [Explanation of symbols] 1 Receiving tank 2 Ceramic filter 3 Activated carbon tower
フロントページの続き (56)参考文献 特開 平11−33362（ＪＰ，Ａ) 特開 平10−235351（ＪＰ，Ａ) 特開 平７−171561（ＪＰ，Ａ) 特開 平10−309576（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) B01D 61/00 - 71/82 C02F 1/44 C02F 1/58 Continuation of front page (56) References JP-A-11-33362 (JP, A) JP-A-10-235351 (JP, A) JP-A-7-171561 (JP, A) JP-A-10-309576 (JP , A) (58) Fields surveyed (Int.Cl. 7 , DB name) B01D 61/00-71/82 C02F 1/44 C02F 1/58
Claims (1)
において、該ＣＭＰ排水中の懸濁物質を分離する無機膜
分離装置と、該膜分離装置の透過水を粒状活性炭と接触
させる活性炭塔とを有することを特徴とするＣＭＰ排水
の処理装置。(57) Claims 1. An apparatus for treating CMP waste water containing hydrogen peroxide, an inorganic membrane separation device for separating suspended substances in the CMP waste water, and permeated water of the membrane separation device. An apparatus for treating CMP waste water, comprising: an activated carbon tower for contacting the activated carbon with granular activated carbon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30437299A JP3518445B2 (en) | 1999-10-26 | 1999-10-26 | CMP wastewater treatment equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30437299A JP3518445B2 (en) | 1999-10-26 | 1999-10-26 | CMP wastewater treatment equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2001121144A JP2001121144A (en) | 2001-05-08 |
| JP3518445B2 true JP3518445B2 (en) | 2004-04-12 |
Family
ID=17932237
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30437299A Expired - Fee Related JP3518445B2 (en) | 1999-10-26 | 1999-10-26 | CMP wastewater treatment equipment |
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| Country | Link |
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| JP (1) | JP3518445B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003300070A (en) * | 2002-04-09 | 2003-10-21 | Ngk Insulators Ltd | Treatment method of metal-based cmp waste water |
| JP4722776B2 (en) * | 2006-06-21 | 2011-07-13 | オルガノ株式会社 | Wastewater treatment method and apparatus |
| JP5910635B2 (en) * | 2011-12-05 | 2016-04-27 | 栗田工業株式会社 | Method for treating hydrogen peroxide-containing water |
| CN110605027B (en) * | 2018-06-14 | 2022-03-15 | 中国石油化工股份有限公司 | Alkaline cleaning solution, acidic cleaning solution and ultrafiltration membrane cleaning method |
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1999
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| JP2001121144A (en) | 2001-05-08 |
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