JP2000210648A - PREPARATION OF MIXED INORGANIC POWDER OF Al2O3 COMPONENT AND ZrSiO4 COMPONENT FROM WASTE LIQUID ABRASIVE AND MIXED INORGANIC POWDER - Google Patents
PREPARATION OF MIXED INORGANIC POWDER OF Al2O3 COMPONENT AND ZrSiO4 COMPONENT FROM WASTE LIQUID ABRASIVE AND MIXED INORGANIC POWDERInfo
- Publication number
- JP2000210648A JP2000210648A JP11012832A JP1283299A JP2000210648A JP 2000210648 A JP2000210648 A JP 2000210648A JP 11012832 A JP11012832 A JP 11012832A JP 1283299 A JP1283299 A JP 1283299A JP 2000210648 A JP2000210648 A JP 2000210648A
- Authority
- JP
- Japan
- Prior art keywords
- component
- inorganic powder
- zrsio4
- al2o3
- mixed inorganic
- 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
Links
- 239000000843 powder Substances 0.000 title claims abstract description 52
- 229910052845 zircon Inorganic materials 0.000 title claims abstract description 40
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052593 corundum Inorganic materials 0.000 title claims abstract description 30
- 229910001845 yogo sapphire Inorganic materials 0.000 title claims abstract description 29
- 239000002699 waste material Substances 0.000 title claims abstract description 26
- 239000007788 liquid Substances 0.000 title claims description 29
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 25
- 239000010703 silicon Substances 0.000 claims abstract description 25
- 239000007787 solid Substances 0.000 claims abstract description 22
- 229910052742 iron Inorganic materials 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims description 28
- 238000005498 polishing Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910006501 ZrSiO Inorganic materials 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 24
- 239000000919 ceramic Substances 0.000 abstract description 19
- 239000006185 dispersion Substances 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 description 14
- 230000000694 effects Effects 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 239000003082 abrasive agent Substances 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 238000002083 X-ray spectrum Methods 0.000 description 2
- 239000002734 clay mineral Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 102100033040 Carbonic anhydrase 12 Human genes 0.000 description 1
- 102100033041 Carbonic anhydrase 13 Human genes 0.000 description 1
- 102100032566 Carbonic anhydrase-related protein 10 Human genes 0.000 description 1
- 101000867855 Homo sapiens Carbonic anhydrase 12 Proteins 0.000 description 1
- 101000867860 Homo sapiens Carbonic anhydrase 13 Proteins 0.000 description 1
- 101000867836 Homo sapiens Carbonic anhydrase-related protein 10 Proteins 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910000953 kanthal Inorganic materials 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
Landscapes
- Grinding-Machine Dressing And Accessory Apparatuses (AREA)
- Processing Of Solid Wastes (AREA)
- Separation Of Solids By Using Liquids Or Pneumatic Power (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、Ａｌ２Ｏ３成分と
ＺｒＳｉＯ４成分を主体とするシリコンウエハ研磨廃液
からファインセラミックス用の原材料として利用できる
Ａｌ２Ｏ３成分とＺｒＳｉＯ４成分の混合無機粉末の作
成方法および混合無機粉末に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for preparing a mixed inorganic powder of an Al2O3 component and a ZrSiO4 component which can be used as a raw material for fine ceramics from a silicon wafer polishing waste liquid mainly composed of an Al2O3 component and a ZrSiO4 component, and a mixed inorganic powder. Things.
【０００２】[0002]
【従来の技術】一般にシリコンウエハ研磨後の廃液は、
どろどろの固形分としての研磨剤であり、アルミナ（Ａ
ｌ２Ｏ３）及びジルコン（ＺｒＳｉＯ４）成分から成
り、粒子の形状は研磨剤特有の鋭角状を有している。ま
た、他の不純物は研磨機からの鉄（Ｆｅ）と、ウエハか
らの珪素（Ｓｉ）が含まれている。この廃液の処理とし
ては、従来、大型の沈降槽をいくつも用いて固液分離
し、上澄み液は濾過後再使用し、固形分は廃棄処分して
いた。しかし、このような処理では、有効資源の無駄で
あるばかりでなく、環境保全上にも問題があった。2. Description of the Related Art Generally, waste liquid after polishing a silicon wafer is:
Abrasive as a mushy solid, alumina (A
l2O3) and zircon (ZrSiO4) components, and the particles have an acute angle characteristic of an abrasive. Other impurities include iron (Fe) from the polishing machine and silicon (Si) from the wafer. Conventionally, this waste liquid is treated by solid-liquid separation using a number of large sedimentation tanks, the supernatant liquid is reused after filtration, and the solid content is discarded. However, such processing not only wastes effective resources but also has a problem in terms of environmental conservation.
【０００３】[0003]
【発明が解決しようとする課題】本発明は、上記の問題
点を解決するもので、Ａｌ２Ｏ３成分とＺｒＳｉＯ４成
分の混合物を主体とする研磨剤でシリコンウエハ研磨後
の廃液を処理して粉末粒子の形状が塊形状を有するＡｌ
２Ｏ３成分とＺｒＳｉＯ４成分の混合無機粉末の作成方
法に関するもので、得られた原料は高純度で安定したフ
ァインセラミックス用の原材料として利用できる無機粉
末である。SUMMARY OF THE INVENTION The present invention solves the above-mentioned problems, and treats a waste liquid after polishing a silicon wafer with an abrasive mainly composed of a mixture of an Al2O3 component and a ZrSiO4 component to form powder particles. Al having a lump shape
The present invention relates to a method for producing a mixed inorganic powder of a 2O3 component and a ZrSiO4 component, and the obtained raw material is an inorganic powder that can be used as a raw material for fine and stable fine ceramics.
【０００４】[0004]
【課題を解決するための手段】前記目的を達成するため
本発明に係るシリコンウエハ研磨剤廃液の処理方法は、
Ａｌ２Ｏ３成分とＺｒＳｉＯ４成分を主体とするシリコ
ンウエハ研磨廃液をフィルターで無機成分と溶液に固液
分離し、前記Ａｌ２Ｏ３成分とＺｒＳｉＯ４成分の固形
分を水に分散させ篩いにより粗い異物を除去し、その
後、湿式分級機により無機成分と珪素に分離し、再度、
固形分を水に分散させたのち、磁力で鉄分を除去し、そ
の後、９００〜１５５０℃の温度範囲で熱処理を施こ
し、その後、粉砕することを備えた構成からなるもので
ある。これにより、従来研磨廃棄物として処理されてい
た使用済みの研磨剤をファインセラミックス用の原料と
して再生することが可能に成り、安価で新しいＡｌ２Ｏ
３成分とＺｒＳｉＯ４成分の混合無機粉末を提供するこ
とを目的としたものである。According to the present invention, there is provided a method for treating a silicon wafer abrasive waste liquid according to the present invention.
A silicon wafer polishing waste liquid mainly composed of an Al2O3 component and a ZrSiO4 component is solid-liquid separated into an inorganic component and a solution using a filter, the solid content of the Al2O3 component and the ZrSiO4 component is dispersed in water, and coarse foreign substances are removed by a sieve. Inorganic components and silicon are separated by a wet classifier, and again
After the solids are dispersed in water, iron is removed by magnetic force, and then heat treatment is performed in a temperature range of 900 to 1550 ° C., and thereafter, pulverization is performed. This makes it possible to regenerate used abrasives that have been conventionally treated as polishing wastes as raw materials for fine ceramics, and to use inexpensive new Al2O3.
An object of the present invention is to provide a mixed inorganic powder of three components and a ZrSiO4 component.
【０００５】この混合無機粉末は、アルミナ（Ａｌ２Ｏ
３）約６０〜５５％（以下重量％で示す）、ジルコン
（ＺｒＳｉＯ４） 約４０〜４５％、からなり、そのま
まファインセラミックス用の原料として利用できる程度
の純度を保持している。特にこれにアルミナ（Ａｌ２Ｏ
３）成分、ジルコン（ＺｒＳｉＯ４）成分、さらには他
の鉱化剤、酸化剤、焼成温度調整用助剤等の目的に応じ
た無機原料さらには粘土鉱物等を適宜加えて、任意の組
成比率にすることによって機械的機能、熱的機能、生
物、化学的機能、電気的機能等の広い範囲のファインセ
ラミックス用への用途が期待できる。[0005] This mixed inorganic powder is made of alumina (Al2O).
3) Consisting of about 60 to 55% (hereinafter referred to as% by weight) and about 40 to 45% of zircon (ZrSiO4), and has a purity that can be used as it is as a raw material for fine ceramics. Especially alumina (Al2O)
3) A component, a zircon (ZrSiO4) component, an inorganic raw material according to the purpose such as another mineralizer, an oxidizing agent, an auxiliary for adjusting the firing temperature, and a clay mineral are appropriately added, and the composition is adjusted to an arbitrary composition ratio. By doing so, a wide range of applications for fine ceramics such as mechanical, thermal, biological, chemical, and electrical functions can be expected.
【０００６】[0006]
【発明の実施の形態】本発明の請求項１に記載の発明
は、Ａｌ２Ｏ３成分とＺｒＳｉＯ４成分の混合物を主体
とする研磨廃液をフィルターで無機成分と溶液に固液分
離し、前記Ａｌ２Ｏ３成分とＺｒＳｉＯ４成分の混合物
を主体とする固形分を水に分散させ篩いにより粗い異物
を除去し、その後、湿式分級機により無機成分と珪素に
分離し、再度、固形分を水に分散させたのち、磁力で鉄
分を除去し、その後、９００〜１５５０℃の温度範囲で
熱処理を施こし、その後、粉砕することを備えた構成か
ら成るものである。尚、フィルターを用いることにより
研磨廃液中の研磨剤成分と溶液に固液分離することが可
能であり、Ａｌ２Ｏ３成分とＺｒＳｉＯ４成分の混合物
を主体とするファインセラミックス用の無機粉末として
の優れた作用効果をもつた原料粉末となる。次いでＡｌ
２Ｏ３成分とＺｒＳｉＯ４成分の混合物を主体とする固
形分を水に分散させ篩を用いることにより粗い異物を除
去する作用効果を有する。次いで、湿式分級機を用いる
ことにより研磨剤粉末と珪素成分に分離する作用を有す
る。次いで再度、固形分を水に分散させたのち、磁力で
鉄分を除去し、その後、９００〜１５５０℃の温度範囲
で熱処理を施こすことにより、純度が高く、混合無機粉
末の粒子形が塊形状を有するファインセラミックス用の
無機粉末を得る作用効果がある。次いで、粉砕すること
によって、さらに混合無機粉末の粒子形が均一な塊形状
に成り、そして安定した粒度粉末を有する作用効果があ
る。BEST MODE FOR CARRYING OUT THE INVENTION According to the first aspect of the present invention, a polishing waste liquid mainly composed of a mixture of an Al2O3 component and a ZrSiO4 component is solid-liquid separated into an inorganic component and a solution using a filter, and the Al2O3 component and the ZrSiO4 component are separated. The solid content mainly composed of the mixture of components is dispersed in water and coarse foreign substances are removed by sieving.After that, the inorganic component and silicon are separated by a wet classifier, and again, the solid content is dispersed in water, and then the magnetic force is applied. It is configured to remove iron, then heat-treat in a temperature range of 900 to 1550 ° C., and then pulverize. By using a filter, it is possible to separate solid and liquid into an abrasive component and a solution in the polishing waste liquid, and an excellent effect as an inorganic powder for fine ceramics mainly composed of a mixture of an Al2O3 component and a ZrSiO4 component. It becomes a raw material powder having Then Al
The use of a sieve that disperses a solid content mainly composed of a mixture of the 2O3 component and the ZrSiO4 component in water has the effect of removing coarse foreign substances. Next, it has an effect of separating the abrasive powder and the silicon component by using a wet classifier. Next, after the solid content is again dispersed in water, iron is removed by magnetic force, and then heat treatment is performed in a temperature range of 900 to 1550 ° C., so that the purity is high and the particle shape of the mixed inorganic powder is a lump shape. There is an effect of obtaining an inorganic powder for fine ceramics having the following. Then, by pulverizing, the particle shape of the mixed inorganic powder further becomes a uniform lump shape, and there is an effect of having a stable particle size powder.
【０００７】本発明の請求項２に記載の発明は、再生さ
れたＡｌ２Ｏ３成分とＺｒＳｉＯ４成分の混合無機粉末
の粒子形が塊形状を有することを備えた構成から成るも
のである。尚、混合無機粉末の粒子形が塊形状を有する
ことにより、ファインセラミックス用の原料として混合
および成形が容易になる作用効果がある。According to a second aspect of the present invention, there is provided a configuration in which the particle shape of the regenerated mixed inorganic powder of the Al2O3 component and the ZrSiO4 component has a lump shape. In addition, when the particle shape of the mixed inorganic powder has a lump shape, there is an effect of facilitating mixing and molding as a raw material for fine ceramics.
【０００８】以下、本発明の実施の形態について図１、
図２、図３、図４、（表１）、（表２）を用いて説明す
る。図１は本発明に係るシリコンウエハ研磨廃液の処理
方法を詳述する。 図１において、シリコンウエハ研磨
後の廃液（研磨廃液）は、通常、水溶性の潤滑油と、研
磨剤としてのＡｌ２Ｏ３成分及びＺｒＳｉＯ４成分と、
研磨機からの研磨屑の鉄分と、シリコンウエハからの珪
素と、その他の微量成分を含むどろどろの液体である。
本発明では、この研磨廃液をフィルター１で固液分離す
る。フィルター１は気孔径５μｍの濾材の、真空式ドラ
ムフィルタ−を用い、研磨剤成分と溶液に分離した。Hereinafter, an embodiment of the present invention will be described with reference to FIG.
This will be described with reference to FIGS. 2, 3, 4, (Table 1), and (Table 2). FIG. 1 illustrates a method for treating a silicon wafer polishing waste liquid according to the present invention. In FIG. 1, the waste liquid after polishing the silicon wafer (polishing waste liquid) is usually composed of a water-soluble lubricating oil, an Al2O3 component and a ZrSiO4 component as abrasives,
It is a muddy liquid containing iron in the polishing waste from the polishing machine, silicon from the silicon wafer, and other trace components.
In the present invention, this polishing waste liquid is solid-liquid separated by the filter 1. The filter 1 was separated into an abrasive component and a solution using a vacuum drum filter of a filter medium having a pore diameter of 5 μm.
【０００９】次いで、固形分を分散槽２内で水と混合
し、撹拌し、希釈分散する。その後、篩３を用い粗い異
物を除去する。次いで 希釈された分散液は、ポンプ４
を介して湿式分級機５に掛け研磨剤成分と珪素成分に分
離する。これは、粒度分布が、平均粒径１２μｍ程度で
ある研磨剤成分と、平均粒径が１μｍ以下である珪素と
を比重により分離することができる。分離された珪素は
水とともに抜き取られ排水処理機６へと送られる。次い
で、３５００〜１００００ガウス程度の磁力を有する永
久磁石を用いた除鉄機７に通し鉄分を除去する。Next, the solid content is mixed with water in the dispersion tank 2, stirred, and diluted and dispersed. Thereafter, coarse foreign substances are removed using the sieve 3. The diluted dispersion is then pump 4
Through a wet classifier 5 to separate into an abrasive component and a silicon component. This means that the abrasive component having a particle size distribution of about 12 μm and the silicon having an average particle diameter of 1 μm or less can be separated by specific gravity. The separated silicon is extracted together with the water and sent to the wastewater treatment device 6. Next, iron is removed through an iron removing machine 7 using a permanent magnet having a magnetic force of about 3500 to 10000 gauss.
【００１０】その後、電気炉８を用い温度９００〜１５
５０℃の温度範囲で熱処理を施こし粒子形状を塊形状に
すると共に安定したＡｌ２Ｏ３成分とＺｒＳｉＯ４成分
の混合無機粉末を得る。尚、熱処理温度が９００℃以下
では安定した塊状の粒子形を得ることが困難になり、ま
た１５５０℃以上では粒子が硬くなり粉末として取り扱
いが困難に成るため好ましくない。尚、粒子形状が塊形
状を有することによって、他の添加物との反応が良くな
るものであつた。その後、粉砕機９としてボ−ルミルを
用い粉砕し粒度の均一化と塊形状の粒子形を持った再生
無機粉末原料を得ることが出来る。その成分は、アルミ
ナ約５５〜６０％、ジルコン約４０〜４５％が含まれて
おり、得られた無機粉末は、ファインセラミックス用の
原料としてそのまま利用できる程の純度を有する。ま
た、得られたアルミナ成分とジルコン成分の混合物に、
新しいアルミナ成分あるいはジルコン成分を適宜加えて
アルミナ成分及びジルコン成分の組成比率を変化させる
ことも可能であり、さらには、他の鉱化剤、酸化剤、焼
成温度調整用助剤等の目的に応じた無機原料さらには粘
土鉱物を添加することによって機械的機能、熱的機能、
生物、化学的機能、電気的機能等の広い範囲のファイン
セラミックスを作ることが可能である。尚、Ａｌ２Ｏ３
成分とＺｒＳｉＯ４成分の混合無機粉末およびファイン
セラミックスに用いた場合の特長は、１．耐熱性温度が
非常に高い、２．比重が大きい、３．耐衝撃性に強い、
４．ビッカ−ス硬度が高い、５．抗折力が高い、６．公
害成分が含まれていない、７．他の無機成分との反応性
が良い等、数多くの特長をもつており、目的に応じたフ
ァインセラミックス用の原材料として利用することが出
来る。After that, the temperature is set to 900 to 15 using the electric furnace 8.
Heat treatment is performed at a temperature of 50 ° C. to obtain a lump-shaped particle shape and to obtain a stable mixed inorganic powder of an Al 2 O 3 component and a ZrSiO 4 component. If the heat treatment temperature is 900 ° C. or lower, it is difficult to obtain a stable massive particle shape, and if the heat treatment temperature is 1550 ° C. or higher, the particles become hard and difficult to handle as a powder. In addition, when the particle shape had a lump shape, the reaction with other additives was improved. Thereafter, a ball mill is used as the pulverizer 9 to obtain a regenerated inorganic powder raw material having a uniform particle size and a lump-shaped particle form. The component contains about 55 to 60% of alumina and about 40 to 45% of zircon, and the obtained inorganic powder has such a purity that it can be used as it is as a raw material for fine ceramics. In addition, in the mixture of the obtained alumina component and zircon component,
It is also possible to change the composition ratio of the alumina component and the zircon component by appropriately adding a new alumina component or zircon component, and further according to the purpose of other mineralizers, oxidizing agents, sintering temperature adjustment assistants and the like. By adding inorganic raw materials and clay minerals, mechanical functions, thermal functions,
It is possible to make fine ceramics with a wide range of biological, chemical and electrical functions. In addition, Al2O3
The characteristics when used for the mixed inorganic powder of the component and the ZrSiO4 component and fine ceramics are as follows. 1. High heat resistance temperature; 2. High specific gravity; Strong impact resistance,
4. 4. High Vickers hardness; 5. High bending strength; 6. Contains no pollution components. It has many features, such as good reactivity with other inorganic components, and can be used as a raw material for fine ceramics according to the purpose.
【００１１】[0011]
【実施例１】次に、本発明の具体例を説明する。本実施
例におけるシリコンウエハ研磨廃液の処理方法について
説明する。まず、シリコンウエハ研磨後の廃液２００リ
ットルを、真空式ドラムフィルター１として、商品名Ｐ
Ｃセパレータ（カネボウ製）を用い真空度は６００〜６
４０ｍｍＨｇ、濾材には平均気孔径５．０μｍのものを
使用し研磨剤成分と溶液に固液分離した、尚、ドラム上
に付着した固形分はスクレバーで掻きとった。固形分は
約１４．０ｋｇ、含水率は１４％で、色は灰色、平均粒
径１２．０μｍであった。固液分離した固形分は分散槽
２内で、粘度を下げるため約１００リットルの水を注入
し希釈分散した。その後、４００メッシュのナイロン製
の篩３を用い粗い試料の破片等の異物を除去した。次い
で、ポンプ４を介して湿式分級機５として商品名スーパ
ークリーン（村田工業製）に掛け研磨剤成分と珪素成分
に分離した。Embodiment 1 Next, a specific example of the present invention will be described. A method for treating silicon wafer polishing waste liquid in this embodiment will be described. First, 200 liters of waste liquid after polishing a silicon wafer was used as a vacuum drum filter 1 under the trade name P
Vacuum degree is 600-6 using C separator (made by Kanebo)
A filter medium having a pore size of 40 mmHg and an average pore diameter of 5.0 μm was used, and solid-liquid separation was carried out into an abrasive component and a solution. The solid matter adhering to the drum was scraped off with a screver. The solid content was about 14.0 kg, the water content was 14%, the color was gray, and the average particle size was 12.0 μm. The solids separated into solid and liquid were diluted and dispersed in the dispersion tank 2 by injecting about 100 liters of water to reduce the viscosity. Thereafter, foreign substances such as coarse sample fragments were removed using a 400-mesh nylon sieve 3. Next, the mixture was subjected to a super classifier (trade name, manufactured by Murata Industry Co., Ltd.) as a wet classifier 5 via a pump 4 to separate an abrasive component and a silicon component.
【００１２】次いで、研磨剤に含まれている鉄成分の除
去として、商品名マグクリーン（カネテック製）の除鉄
機７で、磁力約３５００ガウスの永久磁石を用いた除鉄
機に２回通し鉄分を除去したところ、鉄分１．４ｋｇが
除去された。（鉄分の除去率は約９９．５％であった） その後、エレマ発熱体を用いた電気炉８で９００〜１５
５０℃の温度範囲で熱処理を施こすことにより塊状の粒
子形を有するＡｌ２Ｏ３成分とＺｒＳｉＯ４成分の混合
無機粉末を得た。その後、粉砕機９としてアルミナ磁器
内張りのボ−ルミル（大島鉄工製）を用いジルコニア玉
石と共に混合粉砕し、均一性に富んだ粒度と塊状の粒子
形を持った無機粉末を得た。Next, in order to remove the iron component contained in the abrasive, the iron is passed twice through an iron remover 7 using a permanent magnet having a magnetic force of about 3500 gauss with an iron remover 7 of Magclean (manufactured by Kanetec). When iron was removed, 1.4 kg of iron was removed. (The iron removal rate was about 99.5%.) Thereafter, the electric furnace 8 using an elema heating element was used to remove the heat from 900 to 15%.
By performing a heat treatment in a temperature range of 50 ° C., a mixed inorganic powder of an Al 2 O 3 component and a ZrSiO 4 component having a massive particle shape was obtained. Thereafter, a ball mill (manufactured by Oshima Tekko Co., Ltd.) lined with alumina porcelain was used as the pulverizer 9 and mixed and pulverized together with zirconia cobblestone to obtain an inorganic powder having a highly uniform particle size and a massive particle shape.
【００１３】上記実施例で得られた混合無機粉末を、Ｆ
Ｐ法により定量分析した。分析機器は蛍光Ｘ線分析装置
（島津製作所製ＳＸＦ−１２００）を用いた。試料はア
ルミリングを用いて全圧３００トンで加圧成型し、蛍光
Ｘ線スペクトルを測定した。得られた蛍光Ｘ線スペクト
ルに基づく主な検出元素のＦＰ法による推定定量分析結
果を表１に示す。含有量は、単純酸化物換算で示した。The mixed inorganic powder obtained in the above example was
Quantitative analysis was performed by the P method. An X-ray fluorescence analyzer (SXF-1200 manufactured by Shimadzu Corporation) was used as an analyzer. The sample was pressure molded using an aluminum ring at a total pressure of 300 tons, and the fluorescent X-ray spectrum was measured. Table 1 shows the estimated quantitative analysis results of the main detection elements by the FP method based on the obtained fluorescent X-ray spectrum. The content is shown in terms of simple oxide.
【００１４】[0014]
【表１】 [Table 1]
【００１５】また、Ｘ線回折、さらには粒子形状を顕微
鏡観測した、その結果としてＸ線回折を図２に、また粒
子形状の顕微鏡観察結果を図３（ａ）に示した。（尚、
比較例として温度処理のしていない粉末を対比出来るよ
う図３（ｂ）に、また、処理温度が９００℃以下のもの
を図４（ｃ）に、１５５０℃以上のものを図４（ｄ）に
示した） また、解析条件としては Ｘ線回折：（株）島津製作所
製Ｘ線回折装置ＸＤ−１を用い、測定条件は下記のとお
りである。 Ｘ線管球 ターゲット ：Ｃｕ 管電圧 ：３５ （ｋＶ） 管電流 ：１５ （ｍＡ） スリット 発散スリット ：１（ｄｅｇ） 空気散乱防止スリット ：１（ｄｅｇ） 検出スリット ：０．３０（ｍｍ）Further, X-ray diffraction and further the particle shape were observed with a microscope. As a result, the X-ray diffraction is shown in FIG. 2 and the result of the microscopic observation of the particle shape is shown in FIG. 3 (a). (still,
As a comparative example, FIG. 3 (b) shows that powders not subjected to temperature treatment can be compared, FIG. 4 (c) shows a powder having a treatment temperature of 900 ° C. or less, and FIG. 4 (d) shows a powder having a treatment temperature of 1550 ° C. or more. The analysis conditions were as follows: X-ray diffraction: X-ray diffractometer XD-1 manufactured by Shimadzu Corporation, and the measurement conditions were as follows. X-ray tube Target: Cu Tube voltage: 35 (kV) Tube current: 15 (mA) Slit Divergence slit: 1 (deg) Air scattering prevention slit: 1 (deg) Detection slit: 0.30 (mm)
【００１６】顕微鏡観測：オリンパス株式会社製顕微鏡
を用い、倍率は×２０００であった。Microscopic observation: A microscope manufactured by Olympus Corporation was used, and the magnification was × 2000.
【００１７】表１から明らかなように定量分析の結果、
得られたＡｌ２Ｏ３成分とＺｒＳｉＯ４成分の混合無機
粉末は不純物が殆どなく、純度の高い粉末であることが
確認できた。また、図２のＸ線回折から明らかなように
混合無機粉末は、Ｘ線ピークパターンではコランダム結
晶のアルミナとジルコンのビ−クが明確に析出してお
り、Ａｌ２Ｏ３成分相とＺｒＳｉＯ４成分相の２相から
成っていることも確認できた。図３ａの顕微鏡観測結果
から明らかなように粒子の形状が塊形状を有し、さらに
は均一化された粒度であることが確認できた。尚、比較
例として温度処理のしていない粉末は、図３ｂより明ら
かなように粒子形状が研磨剤特有の角張つた形状を示し
ていた。また、図４ｃより明らかなように８８０℃で処
理した粒子形状も、塊形状と角形状が混ざった形状を示
しており好ましくない、さらに図４ｄより明らかなよう
に１６００℃で処理した粒子形状は粒子径状が大きく不
均一に成るため好ましくない。As is clear from Table 1, the results of the quantitative analysis
It was confirmed that the obtained mixed inorganic powder of the Al2O3 component and the ZrSiO4 component had almost no impurities and was a highly pure powder. Further, as is clear from the X-ray diffraction in FIG. 2, in the mixed inorganic powder, in the X-ray peak pattern, a peak of alumina and zircon of the corundum crystal was clearly precipitated, and the two phases of the Al2O3 component phase and the ZrSiO4 component phase were observed. It was confirmed that it was composed of phases. As is clear from the results of the microscopic observation in FIG. 3A, it was confirmed that the shape of the particles had a lump shape and that the particles had a uniform particle size. As a comparative example, the powder that had not been subjected to the temperature treatment had an angular shape peculiar to the abrasive as shown in FIG. 3B. Further, as is clear from FIG. 4c, the particle shape treated at 880 ° C. also shows a mixed shape of a lump shape and a square shape, which is not preferable. Further, as apparent from FIG. 4d, the particle shape treated at 1600 ° C. It is not preferable because the particle size becomes large and non-uniform.
【００１８】[0018]
【実施例２】次いで、上記Ａｌ２Ｏ３成分とＺｒＳｉＯ
４成分の混合無機粉末を用い耐熱性のファインセラミッ
クスを試作した。実施例１で得られたＡｌ２Ｏ３成分と
ＺｒＳｉＯ４成分の混合無機粉末と新しいＡｌ２Ｏ３成
分粉末とＺｒＳｉＯ４成分粉末を用い表２の組成比率に
成るように、各々配合した。まず、７寸のアルミナ質製
のポットミルとジルコニア玉石を用い水と共に４８時間
の湿式混合を行い、その後、乾燥し、さらに５％溶液の
ＰＶＡ有機バインダーを５重量％（原料粉末１００に対
し）添加し乾式成形用の粉末を作成した、その後、直径
８cm、厚み２cmの円盤を圧力１トンで成形した、その
後、カンタルヒーターの電気炉を用い表２の各温度で焼
成し耐熱性のファインセラミックスを作り、その後、諸
特性を測定した。Embodiment 2 Next, the above Al2O3 component and ZrSiO
A heat-resistant fine ceramics was experimentally produced using a mixed inorganic powder of four components. The mixed inorganic powder of the Al2O3 component and the ZrSiO4 component obtained in Example 1, the new Al2O3 component powder and the ZrSiO4 component powder were blended so as to have the composition ratios shown in Table 2. First, wet mixing is performed for 48 hours with water using a 7-inch alumina pot mill and zirconia cobblestone, then dried, and a 5% solution of a PVA organic binder is added in an amount of 5% by weight (based on 100 of raw material powder). Then, a disk having a diameter of 8 cm and a thickness of 2 cm was formed at a pressure of 1 ton, and then fired at each temperature shown in Table 2 using an electric furnace of a Kanthal heater to obtain heat-resistant fine ceramics. After that, various characteristics were measured.
【００１９】[0019]
【表２】 [Table 2]
【００２０】表２から明らかなように、再生品そのまま
のＮＯ１試料では比重が４．１８と高く、熱膨張係数
５．５と小さく、ビ−カス硬度１３８０、曲げ強度５１
８０と著しく高い物性特性を示し良好な耐熱性セラミッ
クスであった。また、ＮＯ２〜ＮＯ４迄の試料は新たら
しいＡｌ２Ｏ３成分とＺｒＳｉＯ４成分を添加したもの
で、無添加のＮＯ１試料とほとんど特性値が同一であつ
た。また、ＮＯ６の試料は焼結温度を低下させる目的で
ＬｉＯ２の含有している天然の葉長石を２０Ｗｔ％添加
したもので焼結温度が１４００℃と著しく低下し、熱膨
張係数３．０と小さく、ビ−カス硬度１０５０、抗折力
４８４０と著しく良好な耐熱性セラミックスが得られ
た。また、ＮＯ７〜ＮＯ９迄の試料は酸化物や天然鉱物
等を添加したが、これらも良好な特性を示していた。As is clear from Table 2, the regenerated NO1 sample has a high specific gravity of 4.18, a small thermal expansion coefficient of 5.5, a viscous hardness of 1380, and a bending strength of 51.
The material exhibited remarkably high physical properties of 80 and was a good heat-resistant ceramic. Further, the samples from NO2 to NO4 were obtained by adding a new Al2O3 component and a ZrSiO4 component, and had almost the same characteristic values as the NO1 sample without addition. The sample of NO6 was prepared by adding 20 Wt% of natural feldspar containing LiO2 for the purpose of lowering the sintering temperature. The sintering temperature was remarkably reduced to 1400 ° C., and the thermal expansion coefficient was small to 3.0. A remarkably good heat-resistant ceramic having a high viscous hardness of 1050 and a bending force of 4840 was obtained. Further, oxides, natural minerals and the like were added to the samples of NO7 to NO9, but these also showed good characteristics.
【００２１】[0021]
【発明の効果】以上から明らかなように本発明によれ
ば、Ａｌ２Ｏ３成分とＺｒＳｉＯ４成分の混合物を主体
とするシリコンウエハ研磨廃液をフィルターで研磨剤成
分と溶液に固液分離し、Ａｌ２Ｏ３成分とＺｒＳｉＯ４
成分の混合物を主体とする固形分を水に分散させ篩いに
より粗い異物を除去し、その後、湿式分級機により研磨
剤と珪素に分離し、再度、固形分を水に分散させたの
ち、磁力で鉄分を除去し、その後、９００〜１５５０℃
の温度範囲で熱処理を施こし、その後、粉砕処理した混
合無機粉末の作成方法によれば、従来研磨廃棄物として
処理されていた使用済みの研磨剤をファインセラミック
ス用の原料として再生することが可能に成り、安価で新
しいＡｌ２Ｏ３成分とＺｒＳｉＯ４成分の混合無機粉末
を得る効果がある。そして、得られた混合無機粉末は安
価で安定した品質の無機粉末であるという効果を有す
る。また、廃棄処理が必要な使用済み研磨剤廃棄物を大
幅に減少することが出来るため産業上多大な利点があ
り、環境保全技術としてもすぐれている、さらに廃棄物
処理に要するムダなコストを削減することも出来る。As is clear from the above, according to the present invention, a silicon wafer polishing waste liquid mainly composed of a mixture of an Al2O3 component and a ZrSiO4 component is solid-liquid separated into an abrasive component and a solution using a filter, and the Al2O3 component and the ZrSiO4 component are separated.
The solid content mainly composed of the mixture of components is dispersed in water and coarse foreign substances are removed by sieving.After that, the abrasive and silicon are separated by a wet classifier, and again, the solid content is dispersed in water, and then the magnetic force is applied. Remove iron, then 900-1550 ° C
According to the method of preparing a mixed inorganic powder that has been subjected to heat treatment in the temperature range of, and then pulverized, it is possible to recycle used abrasives that were conventionally treated as polishing waste as raw materials for fine ceramics And has the effect of obtaining an inexpensive new mixed inorganic powder of an Al2O3 component and a ZrSiO4 component. And the obtained mixed inorganic powder has the effect of being an inexpensive and stable quality inorganic powder. In addition, there is a great industrial advantage because the used abrasive waste that needs to be disposed of can be greatly reduced, and it has excellent environmental protection technology. Furthermore, it reduces unnecessary waste processing costs. You can do it.
【図１】本発明に係る研磨廃液からファインセラミック
ス用のＡｌ２Ｏ３成分とＺｒＳｉＯ４成分の混合無機粉
末作成方法の一例を示す工程図である。FIG. 1 is a process diagram showing an example of a method for preparing a mixed inorganic powder of an Al2O3 component and a ZrSiO4 component for fine ceramics from a polishing waste liquid according to the present invention.
【図２】混合無機粉末のＸ線回折図。FIG. 2 is an X-ray diffraction diagram of a mixed inorganic powder.
【図３】混合無機粉末の顕微鏡写真（ａ） 未処理混合無機粉末（比較例）の顕微鏡写真（ｂ）FIG. 3 is a micrograph of a mixed inorganic powder (a) A micrograph of an untreated mixed inorganic powder (comparative example) (b)
【図４】８８０℃で温度処理した混合無機粉末の顕微鏡
写真（ｃ） １６００℃で温度処理した混合無機粉末の顕微鏡写真
（ｄ）FIG. 4 is a micrograph of the mixed inorganic powder subjected to the temperature treatment at 880 ° C. (c). A micrograph of the mixed inorganic powder subjected to the temperature treatment at 1600 ° C. (d).
１……フィルター ２……分散槽 ３……篩 ４……ポンプ ５……湿式分級機 ６……排水処理機 ７……除鉄機 ８……電気炉 ９……粉砕機 DESCRIPTION OF SYMBOLS 1 ... Filter 2 ... Dispersion tank 3 ... Sieve 4 ... Pump 5 ... Wet classifier 6 ... Drainage treatment machine 7 ... Iron remover 8 ... Electric furnace 9 ... Pulverizer
───────────────────────────────────────────────────── フロントページの続き (72)発明者 多木 宏光 宮崎県宮崎市大字島之内7078番地２ Ｆターム(参考） 3C047 FF08 GG14 4D004 AA50 BA10 CA04 CA09 CA10 CA12 CA13 CA22 CB09 DA03 DA06 4D071 AA01 AA02 AA46 AA65 AB61 AB62 CA03 DA15 DA20 ────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Hiromitsu Taki 7078-2, Shimanouchi, Oaza, Miyazaki City, Miyazaki Prefecture 3C047 FF08 GG14 4D004 AA50 BA10 CA04 CA09 CA10 CA12 CA13 CA22 CB09 DA03 DA06 4D071 AA01 AA02 AA46 AA65 AB61 AB62 CA03 DA15 DA20
Claims (2)
合物を主体とする研磨廃液をフィルターで無機成分と溶
液に固液分離し、前記Ａｌ２Ｏ３成分とＺｒＳｉＯ４成
分の混合物を主体とする固形分を水に分散させ篩いによ
り粗い異物を除去し、その後、湿式分級機により無機成
分と珪素に分離し、再度、固形分を水に分散させたの
ち、磁力で鉄分を除去し、その後、９００〜１５５０℃
の温度範囲で熱処理を施こし、その後、粉砕することを
特徴としたＡｌ２Ｏ３成分とＺｒＳｉＯ４成分の混合無
機粉末の作成方法1. A polishing waste liquid mainly composed of a mixture of an Al2O3 component and a ZrSiO4 component is solid-liquid separated into an inorganic component and a solution with a filter, and a solid mainly composed of a mixture of an Al2O3 component and a ZrSiO4 component is dispersed in water. The coarse foreign matter is removed by sieving, then the inorganic component and silicon are separated by a wet classifier, the solid content is again dispersed in water, and then the iron content is removed by magnetic force.
A method for preparing a mixed inorganic powder of an Al2O3 component and a ZrSiO4 component, characterized by performing a heat treatment in the temperature range described above and then pulverizing the mixture.
４成分の混合無機粉末の粒子形が塊形状を有する事を特
徴とした混合無機粉末2. Regenerated Al2O3 component and ZrSiO
Mixed inorganic powder characterized in that the particle shape of the four-component mixed inorganic powder has a lump shape
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|---|---|---|---|
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|---|---|---|---|
| JP01283299A JP3437106B2 (en) | 1999-01-21 | 1999-01-21 | Method for preparing mixed inorganic powder of Al2O3 component and ZrSiO4 component from polishing waste liquid and mixed inorganic powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012187652A (en) * | 2011-03-09 | 2012-10-04 | Univ Of Tokyo | Method for separating aluminum oxide and zircon from slurry composition containing aluminum oxide and zircon |
| WO2013141225A1 (en) * | 2012-03-19 | 2013-09-26 | 株式会社 フジミインコーポレーテッド | Polishing material for lapping and method for manufacturing substrate using same |
| CN111185464A (en) * | 2020-02-04 | 2020-05-22 | 绵竹市金坤化工有限公司 | Method and system for recycling zirconium oxide |
-
1999
- 1999-01-21 JP JP01283299A patent/JP3437106B2/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012187652A (en) * | 2011-03-09 | 2012-10-04 | Univ Of Tokyo | Method for separating aluminum oxide and zircon from slurry composition containing aluminum oxide and zircon |
| WO2013141225A1 (en) * | 2012-03-19 | 2013-09-26 | 株式会社 フジミインコーポレーテッド | Polishing material for lapping and method for manufacturing substrate using same |
| CN111185464A (en) * | 2020-02-04 | 2020-05-22 | 绵竹市金坤化工有限公司 | Method and system for recycling zirconium oxide |
| CN111185464B (en) * | 2020-02-04 | 2021-10-22 | 绵竹市金坤化工有限公司 | Method and system for recycling zirconium oxide |
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