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TW379158B - Method of manufacturing micro granule segregate for polishing - Google Patents

Method of manufacturing micro granule segregate for polishing Download PDF

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Publication number
TW379158B
TW379158B TW87117485A TW87117485A TW379158B TW 379158 B TW379158 B TW 379158B TW 87117485 A TW87117485 A TW 87117485A TW 87117485 A TW87117485 A TW 87117485A TW 379158 B TW379158 B TW 379158B
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Taiwan
Prior art keywords
dispersion
grinding
ultrafine
particles
polishing
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TW87117485A
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Chinese (zh)
Inventor
Yukihiko Karasawa
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Karasawa Fine Co
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  • Colloid Chemistry (AREA)

Description

五、發明說明(1) 【發明之詳細說 【發明之技術領 本發明係關於 也就是說,本發 性紀錄用媒體等 法’特別是關於 於層間絕緣膜和 細凹凸之平滑、 (CMP . Chem i ca 子分散體之製造 所謂具備有相當 磨用超微粒子分 【先前技術】 在半導體裝置 面相當精密地研 紀錄用媒體之表 磨用超微粒子分 導體之積體化之 發展。在呈多層 各層間之層間絕 體之製造作業中 得層間絕緣膜之 f作業中’也藉 疋,也必須對於 域】 —種研磨用超 明係關於一種 之表面之研磨 一種在半導體 金屬配線膜形 以及平坦加工 1 Mechanical 方法,並且, 良好之加工精 散體之製造方 微粒子分散體之製、生 用以研磨著半導體^方法; 用超微粒子分散裝置和磁 裝置之製造作;:之製造方 成後之具有大、而破使用 方面之化學機械之微 Polish)方法二研磨 還尤其是關於—種之4微产 度和無污染化之加=; 法。 叫 < 研 和磁性 磨成為 面之相 散體。 進步發 化之半 緣獏之 ,係對 表面, 由真空 該成膜 紀錄用 鏡面狀 當精密 特別是 展,半 導體裝 表面, 於層間 成為平 成膜用 後之具 媒體之 。在前 之研磨 ,在半 導體裝 置中, 成為平 絕緣膜 坦化。 手段, 有大小 製造方法中 述半導體裝 方法中,係 導體裝置中 置也正朝向 必須要使得 坦化,因此 ’進行著研 此外,在半 而形成金屬 疏密性之微 ’係將表 置和磁性 使用著研 ,隨著半 著多層化 該形成於 ,在半導 磨,而使 導體之製 配線,但 細凹凸,V. Description of the invention (1) [Details of the invention [Technical aspects of the invention] The present invention is about the method of the present invention for recording media, especially the smoothing of interlayer insulating films and fine unevenness, (CMP. The manufacture of Chem i ca sub-dispersions is so-called equipped with ultra-fine particles for grinding. [Previous technology] The development of the integration of ultra-fine particle conductors for surface grinding of recording media has been studied on the semiconductor device surface quite precisely. In the manufacturing operation of the interlayer insulation between the layers, the operation of the interlayer insulation film is also used, and it must also be used in the field. — A kind of polishing super-brightness is about the polishing of a surface and the shape and flatness of the semiconductor metal wiring film. Processing 1 Mechanical method, and the method of manufacturing fine dispersions of fine dispersions, producing and producing semiconductor dispersions; methods of manufacturing ultrafine particle dispersing devices and magnetic devices; Large and broken use of chemical mechanical micro-Polish) method 2 grinding is especially about-the kind of 4 micro-productivity and pollution-free The plus =; method. Called < Grind and magnetic mill to become a phase dispersion. The half of the progress is related to the surface, the mirror surface of the film is formed by vacuum. When the precision is particularly spread, the semiconductor is mounted on the surface, and it becomes the media after the flat film is used between the layers. In the previous grinding, in the semiconductor device, the flat insulating film became flat. Means, in the semiconductor manufacturing method described in the manufacturing method of large and small, the center of the conductor device is also oriented so that it must be frank. Therefore, 'researching and forming a micro metal density in half' is to place the surface and Magnetism is used in research, and it should be formed with semi-multilayering, and it will be polished in semiconducting to make the conductor wiring.

δ亥使用於化學機械式研磨方法中之超丑 使用顆粒研磨機、球f研麼嬙 μ 、子刀政體,係 Μ八” 磨機、和砂粒研磨機等之介暫樹 體型刀放機、卩及膠體型研磨機 :貝媒 波分散機’而進行著氧化石夕、氧化铭、音 鈦、乳化#、乳化猛、以及氧化鐵等之粒子之製 d?機械式研磨用超微粒子分散體,—般係使用 者該3有1二人粒子直徑10nm 〜100nm之相當微細用 粒子分散體。it且,將超微粒子粉體,分散於鹼性2微 性之水溶液中’但是’當在將超微 分二二 之表面之附近,會由:水u中;:r些超微粒子粉體 ^ a ^ 成〒之離子,而形成有電I- 重層,並且,也會使得漿體中之粒子之f電位 一 (zeta-P〇tential ),變成為比較小, :間…力’變得比較大,而產生有所謂之;:广拉 現象’以至於成為所謂胸m 右之凝集體(aggregate )之相當穩定之狀態。在目 :m ϊ m該成為化學機械式研磨用超微粒子分 散體之所要求之粒子直徑之中心粒子直徑,係為“Ο⑽〜刀δHai is used in chemical-mechanical grinding methods. It uses a particle grinder, a ball grinder, a knife body, a M-8 "mill, and a sand grinder.卩 and colloid-type grinding machine: Shell medium wave dispersing machine 'is used for the production of particles such as stone oxide, oxide, titanium, emulsified, emulsified, and iron oxide. D? Ultrafine particle dispersion for mechanical grinding -Generally, the user has a fairly fine particle dispersion with a particle diameter of 10nm to 100nm. It also disperses ultrafine particles in an alkaline 2 micron aqueous solution 'but' when the will Near the surface of the ultra-differential two or two, the ultra-fine particles ^ a ^ will form ions of 〒 in the water u, and an electric I- layer will be formed, and the particles in the slurry will also be made. The f-potential one (zeta-P0tential) becomes relatively small, and the "... force" becomes larger, and there is a so-called ": wide-pulling phenomenon", so that it becomes the so-called aggregate of the chest m. ) Is quite stable. In the head: m ϊ m should become chemical mechanical grinding The particle diameter of the center of the required particle diameter of the dispersion with ultrafine particles is "Ο⑽ ~ 刀

第5頁 五、發明說明(3) 20 0nm ’並且,其粒子分布範圍為1〇〇ηπι〜4〇〇n[n,因此, 就必須要藉由某些方法,而再一次地分散出前述之凝集體 (aggregate ) 〇 ,在僅使用授拌型分散機而再一次地分散出前述之化學機 ^式研磨用超微粒子分散體之凝集體(aggregate)之狀 悲下,即使進行著相當長時間之分散處理,也幾乎無法再 人地刀政出月ij述之凝集體(aggregate)。 例如在使用氧化矽粒子作為研磨劑用之化學機械式研磨 用超微粒子分散體之狀態下,於超純水中而溶解有氫氧化 鉀之鹼性溶液之中,混合入1 3〜25重量%之1次粒子直徑 30nm之氧化石夕’接著,在3〇〇〇『叩之條件下,對於前 述所彳于到=分散體’進行著1小時之高速度之攪拌處理, 並,,還藉由顆粒研磨機,而在1 40 0rpm之條件下,對於 =徑2mm之顆粒,進行著1小時之分散處理,以便於得到中 米子直k230nm、|占度6〜i〇mpa ·3之研磨用超微粒子 散體。 4 Ϊ使用者球體研磨機等之介質媒體型分散機之狀態下, I Ϊ子直徑而言’係可以得到中心粒子直徑2 0 〇ηιη左Page 5 V. Description of the invention (3) 200 nm 'and its particle distribution range is 100nm to 400nm [n, so it is necessary to disperse the aforementioned again by some methods Aggregate 〇, even if it is used for a long period of time, the aggregate of the aforementioned ultrafine particle dispersion for chemical machine ^ is once again dispersed using only a mixing type disperser. The decentralized treatment of time can hardly be done anymore. For example, in the state of ultrafine particle dispersion for chemical mechanical polishing using silicon oxide particles as an abrasive, in an alkaline solution in which potassium hydroxide is dissolved in ultrapure water, and mixed with 1 to 25% by weight The oxide particle with a particle diameter of 30 nm was then 'stirred at a high speed for 1 hour under the conditions of 3,000 Å', and, also, borrowed With a particle grinder, at 1 400 rpm, the particles with a diameter of 2 mm are dispersed for 1 hour in order to obtain neutron straight k230nm, and a 6 ~ i0mpa · 3 grinding. Ultrafine particle dispersion. 4 Ϊ In the state of a media-media disperser such as a user's sphere grinder, in terms of the diameter of the ’系, the diameter of the central particle can be obtained. 20 〇ηιη 左

Υ U π U ^超微粒子分散體,而就粒子分布範圍而言,則 U得到粒子公右 # J 散體,因此,:m5〇nm〜7°〇nm之研磨用超微粒子分 护,、丈不奋易仔到相當尖銳集中之粒度分布,同 ‘峰右斛$過相當長時間之處理的話,則介質媒體本身會 :生=之磨耗現象,以至於在半導體裝置之製造作業 甲,產生有污毕物,二 )木物’而很可能會污染到半導體裝置。Υ U π U ^ ultrafine particle dispersion, and as far as the particle distribution range is concerned, the particle public right # J dispersion is obtained, so: m50nm ~ 7 ° 〇nm grinding for ultrafine particle protection, Fenyizi has a very sharp and concentrated particle size distribution. If it is treated for a long time with the peak right, the medium itself will: wear phenomenon, so that in the semiconductor device manufacturing operations, there is contamination. (2) Wooden objects, and it is likely to contaminate semiconductor devices.

第6頁 五、發明說明(4) 此外’該藉由像前述這樣之方法而進行著分散處理之 微粒子分散體,係隨著經時變化,而在每一次之藥劑 ° 次中,其處理特性並不相同,以至於變成為並無_ ^ ^, 在之研磨結果’或者是在為了研磨1曰份之晶圓而供應著子 相當充分之研磨劑之漿體之所謂之D型槽之槽體内^ ^殺 有漿體,而導致會有所謂必須將漿體由槽體内排出至~外'"部 中而進行著漿體廢棄之問題產生。 因此,在日本專利特開平9_1 4 828 6號公報中,係提蟻有 所謂之「動態地進行著混合之方法」之方法,而該「動態 地進行著混合之方法」,係設置有氧化劑、研磨劑、以及 漿體用混合機,每一次皆相當少量地分散處理著前述之氧 化劑及研磨劑,然後,再將前述之分散處理過之氧化劑及 研磨劑,+施加在研磨面上,但是,該作為毁體用混合機, 係使用者該採用磁性攪拌子之磁性攪拌器,而該藉由磁性 攪拌器而得到之漿體之分散性,並不是很充分完全, 時’也無法避免所謂由於經時變化而使得粒子::隼, 結果生成粒徑比較大之粒子之現象發生。 〃、 【發明所欲解決之問題】 本發明之澤,係提供一種研磨用, 造方法,也就是說,本發明之研磨;2:粒子分散體之製 滑、以及平坦加工方面之化學機凹凸之平 ⑷Mechanieal PQlish)方法上之超微粒子之濕式Page 6 V. Explanation of the invention (4) In addition, the microparticle dispersion which is subjected to a dispersion treatment by a method such as the one described above, has a processing characteristic that changes with the passage of time, and in each of the medicaments ° times. It is not the same, so that it becomes no _ ^ ^, in the grinding result 'or in the so-called D-shaped groove of the slurry which is supplied with a sufficient abrasive for polishing a wafer of 1 part. There is a problem in the body that there is a slurry, which leads to the problem that the slurry must be discharged from the tank to the outside, and the slurry is discarded. Therefore, in Japanese Patent Laid-Open No. 9_1 4 828 6, there is a so-called "method for dynamically mixing" for raising ants, and the "method for dynamically mixing" is provided with an oxidizing agent, The abrasive and slurry mixers disperse and treat the aforementioned oxidants and abrasives in a relatively small amount each time, and then apply the aforementioned dispersed oxidants and abrasives to the abrasive surface, but, As a mixer for destroying the body, the user should use a magnetic stirrer with a magnetic stirrer, and the dispersibility of the slurry obtained by the magnetic stirrer is not sufficiently complete. Changes in time cause particles :: 隼, resulting in the generation of particles with relatively large particle sizes. 【[Problems to be Solved by the Invention] The present invention provides a method for grinding, that is, the grinding of the invention; 2: the smoothness of the particle dispersion, and the unevenness of the chemical machine in flat processing (Mechanieal PQlish) method wet method of ultrafine particles

II _II _

第7頁 五、發明說明(5) 超微粒子:氧化矽、 鈽 '氧化锰、以及氧 所提供之微粒子分散 散至1次粒子或者1次 定地製造出均一之微 求,而完全地並不會 子,以便於得到所謂 隨著半導體裝置之高 械式研磨處理中之所 度、高純度、比較狹 中心粒子直徑等之要 種也可以針對今後之 粒子分散體之製造方 此外,本發明之課 該並無混入有不純物 法,尤其是’本發明 經時變化現象比較小 分散體之製造方法。 氧化紹、 化鐵等之 體之製造 粒子附近 粒子分散 包含到該 均一性更 度積體化 要求之比 窄之粒子 求’因此 微細化之 法。 題,係為 之研磨用 之課題, 並且特性 氣化錯、 分散體之 方法’係 為止,並 體,此外 所規定之 高之微粒 等之進展 較高度、 之分布範 ’本發明 進展中之 提供一種 超微粒子 係為提供 相當穩定 二氧化鈦 製造方法 能夠使得 且,也可 ’還能夠 粒子直徑 子分散體 ’而配合 平滑、平 圍、以及 之課題, 要求的研 、氣化 ;本發明 微粒子分 以相當穩 配合著需 以上之教 。此外, 著化學機 坦化精密 比較小之 還提供—> 磨用超微 可以連續地製造出 分散體之製造方 一種所謂凝集等之 之研磨用超微粒子 【解決問題之手段】 本發明係為一種研磨用超微粒子分散體之製造方法’而 具備有以下所敘述之分散作業: 在研磨用超微粒子分散體之製造方法中,藉由對於該在 液體中而分散有研磨用超微粒子之懸浮液,進行著攪拌, 而除去所明之趨流性(t h i X 〇 t r 〇 p y )之後,接著,再對於Page 7 V. Description of the invention (5) Ultrafine particles: fine particles provided by silicon oxide, ytterbium manganese oxide, and oxygen are dispersed to one particle or one time to produce a uniform microfinger, but not completely In order to obtain the so-called high-purity, high-purity, relatively narrow center particle diameter, etc., which can be obtained in the high-mechanical polishing process of semiconductor devices, it can also be targeted at future manufacturers of particle dispersions. There should be no impure method, especially the method of making a dispersion with relatively small change over time in the present invention. Manufacturing of bodies such as oxides, iron, etc. Near particles Dispersion of particles Including the uniformity required to integrate more, the ratio of the particles is narrower. The problem is a problem for polishing, and the method of characteristic gasification error and dispersion is' so far, combined, and in addition, the progress of the prescribed high fine particles and the like is relatively high, and the distribution range is provided in the progress of the present invention. An ultrafine particle system is provided to provide a relatively stable titanium dioxide manufacturing method which can, and can also, "capable of particle diameter sub-dispersions" to cooperate with smooth, flat, and other issues, the required research and gasification; the fine particles of the present invention are divided into equivalent Stable cooperation with the above teaching. In addition, the chemical machine is relatively small and precise, and it also provides— > Ultrafine grinding mills can continuously produce dispersions. Manufacturers of so-called agglomeration and other ultrafine particles for grinding [Solution to the problem] The present invention is A method for producing a superfine particle dispersion for polishing is provided with the dispersion operation described below: In the method for producing a superfine particle dispersion for polishing, a suspension in which a superfine particle for grinding is dispersed in a liquid is provided. After stirring, remove the known flow tendency (thi X 〇tr 〇py), then, for

第8頁 五、發明說明(6) 月1J述之懸浮液’進行著加壓處理,並且,由相反之方向, 相互地導入前述之懸浮液,而使得該懸浮液之間’相互地 進行著衝撞,以便於分散開該懸浮液中之研磨用超微粒 子。 前述之研磨用超微粒子分散體之製造方法,其研磨用超 微粒子分散體’係為半導體平坦化用途之化學機械式研磨 用之分散體。 前述之研磨用超微粒子分散體之製造方法,其分散體係 為濃度5重量%以上、6 〇重量%以下之水性懸浮液。 此外’前述之研磨用超微粒子分散體之製造方法,在經 過所謂分散處理後,還具備有該用以分級出粒徑比較大之 粒子的分離作業。 【發明之實施形態】 〇 ^發明=研磨用超微粒子分散體之製造方法,係發現到 J •口著特疋之分散手段而進行著分散處理,可以得到 該呈高度分散狀態之超微粒子分散體。 也就疋忒’發現到:由於為了將研磨用超微粒子使用在 ^學機械式研磨之用途±,因此,在研磨用超微粒子之粉 f為水性懸洋液之時’該呈2次地凝集著超微粒子之凝 破㈣研Ϊ f為膠化,結* ’當藉由該使用著顆粒研磨機、 —:ft、以及砂粒研磨機等之介質之分散用裝置而相 懸浮液之時:必須要花費非常 1均自地八&二、子之^刀散作業上,同時,也無法得到所 明句勻也刀政成為相當微細粒子之分散體。Page 8 V. Description of the invention (6) The suspensions described in June 1J are subjected to pressure treatment, and the aforementioned suspensions are introduced into each other from opposite directions, so that the suspensions are mutually performed. Collision to facilitate dispersion of the grinding ultrafine particles in the suspension. In the aforementioned method for producing an ultrafine particle dispersion for polishing, the ultrafine particle dispersion for polishing 'is a dispersion for chemical mechanical polishing of semiconductor planarization applications. In the aforementioned method for producing a dispersion of ultrafine particles for grinding, the dispersion system is an aqueous suspension having a concentration of 5 wt% or more and 60 wt% or less. In addition, the aforementioned method for producing a dispersion of ultrafine particles for polishing further includes a separation operation for classifying particles having a relatively large particle size after a so-called dispersion treatment. [Embodiment of the invention] ○ ^ Invention = A method for producing a superfine particle dispersion for polishing, which is found by J. Orthogonal dispersion means and a dispersion process is performed to obtain the ultrafine particle dispersion in a highly dispersed state. . In other words, it was found that, in order to use the ultrafine particles for polishing in the application of mechanical mechanical polishing ±, when the powder f of the ultrafine particles for polishing is an aqueous suspension, it should be aggregated twice. Coagulation with ultrafine particles f is gelatinized, which means that * when the phase suspension is used by the dispersion device using a medium such as a particle grinder, —: ft, and a sand grinder: required It takes a lot of money to do all the work on the knife and knife, and at the same time, it is not possible to get the clear sentence and the knife into a dispersion of quite fine particles.

m 五、發明說明(7) 因此,在高度地分散荽升 在將粉體狀之研磨用超微粒^ ^ ^性懸汙液之别,也就是 後,為了防止所謂該呈21次地凝隹\性媒體混合在—起之 為膠化之現象發生,所卩,二?超微粒子之凝集體成 粉體狀之研磨用超微粒子與::3拌,而攪拌著前述之 去水性懸浮液之所具有之趨产,、之扣σ體’以便於除 L 上 > —,' 、· Ό生(t h 1 X 〇 t r 〇 p y ),缺德, 再相當向度地分散著前述之水性懸浮液。 .、'、後 此外,還發覌到以下所科十、 >、昍堂、S太直剎4* 敘述在美國專利第4 5332以號 ^料Η平第6 平第卜94 933號公報、或者日本專 利特開平第6-4,號公報中而用以作為高度分散之方 法.^於5亥懸/予者超微粒子之流體,進行著高壓處理,而 ΐ待:ΐί懸2超微粒子之流體,成為高壓狀態,接 該流體發生衝撞,而分散開超微粒子之方法; 形成於溝槽和板狀體間之流路中,使得該被加壓成為Ϊ壓 生著衝撞現象’ #著,由前述之溝槽和板 狀體兩者之溝槽之交點部開始,-直至該由形成於相反部 位之板狀體上之溝槽而組成之流路為止,流入前述之被加 壓成為高壓狀態之流體,而分散開超微粒子之方法;以 及,由該被設置於板狀體上之貫通孔之相互呈相反之方向 開始、’而在板狀體之中央部巾’使得該被加壓成為高壓狀 滤之"I!·體,發生著衝撞現象,而分散開超微粒子之等方 法;也就是說,在使用著前述之美國專利第45 3 325 4號說 明書、日本專利特開平第丨—9 4 9 3 3號公報、或者日本專利m V. Description of the invention (7) Therefore, the difference between highly dispersed powdered ultrafine particles for grinding ^ ^ ^ suspension suspension, that is, to prevent the so-called 21 times of condensation \ Sexual media mixed in-the phenomenon of gelation occurs, why? Aggregates of ultrafine particles are aggregated into powders. The ultrafine particles for grinding are mixed with :: 3, while agitating the aforesaid deaqueous suspension's production tendency, and deducting the sigma body to facilitate the removal of L > — — , ', · Health (th 1 X 〇tr 〇py), lack of virtue, and then dispersed the aforementioned aqueous suspension to a considerable degree. ., ', And later, also issued to the following department X, >, 昍 堂, S 太 直 刹 4 * described in U.S. Patent No. 4 5332 No. Η material flat No. 6 flat No. 94 933 Or in Japanese Patent Laid-Open No. 6-4, it is used as a highly dispersed method. ^ The fluid of the superfine particles in 5Hai / is subjected to high pressure treatment, and waits: ΐsuspend 2 superfine particles The fluid becomes a high-pressure state, and the fluid collides with the fluid to disperse the ultrafine particles. It is formed in the flow path between the groove and the plate-like body, so that the pressure is compressed and the collision phenomenon occurs. # 着, Starting from the intersection of the grooves of the aforementioned groove and the plate-like body,-until the flow path composed of the grooves formed on the plate-like body at the opposite position, flows into the above-mentioned and is pressurized to become A method of dispersing ultrafine particles in a fluid under a high pressure; and starting from the through holes provided in the plate-shaped body in opposite directions to each other, and 'the towel in the center of the plate-shaped body' makes the The pressure becomes the "I!" Body of the high-pressure filter. Opening the ultrafine particles and the like methods; that is, the use of the aforementioned U.S. Patent No. 4 453 325 instruction manual, Japanese Laid-Open Patent of Shu -9493 Publication No. 3, or Japanese Patent

第10頁 五、發明說明(8) =開=第6-4 726 4號公報中之所提議之藉由使得該被加壓 a為问壓狀態之流體,相互地發生著衝撞現象,以便於分 J開超微粒子之分散方法之狀態下,除了可以相當高度地 刀散開研磨用超微粒子分散體之外,同時,還能夠相當長 時間地維持著前述之分散特性。 並且,還具備有以下所敘述之特徵:在使用著顆粒研磨 機、球體研磨機、以及砂粒研磨體機等之分散用媒體之分 散方法中,會由於分散用媒體本身之破損以及磨耗等現 象.,而無法避士所謂異物之混入現象發生,但是,在使得 該被加壓成為高壓狀態之包含有研磨用超微粒子分散體之 流體’相互地發生著衝撞現象,以便於分散開超微粒子之 分散方法中,ϋ不會發生有所謂起因於分散用媒體之異物 混入現f發生,因在匕’即使是在半導體裝置之製造 而使用著前述之所得到之研磨用超微粒子分散體,不合 帶給半導體裝置,相當不良之影響。 s 圖1係為用以說明本發明之研磨用超 造作業之圖式。 丁刀政體之製 再調=業A中,將研磨用超微粒子與超純水、驗 化劑、I4之所要求之藥劑,混合在— 該在研磨作業中之所需要組成之懸更J :裝 業掉著前述之懸浮液乂二 流性(th1X〇tr〇py )。並且,在分散 云所明之趨 述之懸浮液之後,使得該懸浮液地中著加』著前 象,以便於分散開超微粒子。 也土生耆衝撞現Page 10 V. Explanation of the invention (8) = On = No. 6-4 726 No. 4 proposes that the fluids under pressure a are in a state of pressure collision with each other in order to facilitate In the state of dispersing the ultrafine particles in a divided manner, in addition to being able to disperse the ultrafine particle dispersion for grinding at a relatively high level, the aforementioned dispersion characteristics can be maintained for a long time. In addition, it also has the characteristics described below: In the dispersion method using a particle grinder, a ball grinder, and a sand grinder, the dispersion medium will be damaged due to the dispersion medium itself and abrasion. It is impossible to avoid the so-called foreign matter mixing phenomenon. However, the fluids containing the ultrafine particle dispersion for grinding which are pressurized to a high pressure state collide with each other to facilitate the dispersion of the ultrafine particles. In the method, the occurrence of so-called foreign matter caused by the dispersion medium does not occur. Since the ultrafine particle dispersion for grinding obtained above is used even in the manufacture of semiconductor devices, it is not suitable for Semiconductor devices have considerable adverse effects. s Fig. 1 is a diagram for explaining a superabrasive operation for polishing according to the present invention. Readjustment of the system of Ding Dao government = In industry A, the ultrafine particles for grinding, ultrapure water, test reagents, and I4 required agents are mixed in — the suspension of the required composition in the grinding operation J: The loading industry lost the aforementioned suspension (th1Xtrotropy). And, after dispersing the suspension of the cloud, the former phenomenon was added to the suspension so as to disperse the ultrafine particles. Peranakan rushes

五、發明說明 在分離作業D中,藉由離心分離等之方法,m分、級出前 f之所得到之研磨用超微粒子分散體之後,接著,在研磨 作業E中,使用著前述之研磨用超微粒子分散體。此外, 在研磨作業E巾,也可以使用著該並無經所謂分離作業 理過之研磨用超微粒子分散體。 而進行著相關之 首先,就本發明之方法中之攪拌作業 說明。 係使用該具備有2片或者4片之扇葉之攪拌機,作為本發 明之方法中之攪拌機用,接著,在扇葉及接液部,進行^ 聚四氟乙烯(polytetrafluoroethylene)等之惰性且穩 定之樹脂之被覆之完全處理,此外.,還使用著該並不會污 染到所謂研磨用超微粒子分散體之金屬離子。 當在製造著固形物濃度3 0重量%之研磨用超微粒子分散 體之狀態下而列舉出一實施例之時,係在6 8. 4 7 1 kg之超純 水中,溶解著1. 49 8kg之濃度2〇重量%之氫氧化鉀水溶 液’並且’還藉由該具備有50至l〇〇mm之扇葉之攪拌機, 以1500rpm之轉速’而攪拌著前述之溶解液,同時,在3〇 分鐘内,相當平均地投入30. 〇3kg之1次粒子直徑20〜3 〇nm 之煙燻過之氧化矽。 在投入全量之組成成分之後,使得攪拌機之旋轉數,成 為2000 rpm,而進行著15分鐘之攪拌作業,然後,在提升 則述之授拌機之旋轉數’成為3〇〇〇rpm,而進行著15分鐘 之攪拌作業之後’接著’在藉由高壓流體之衝撞現象而$分 散開研磨用超微粒子分散體之分散體製造裝置中,分散著V. Description of the invention In the separation operation D, the centrifugal separation method is used to obtain the ultrafine particle dispersion for grinding obtained in the fraction m and before f, and then, in the grinding operation E, the aforementioned grinding is used. Ultrafine particle dispersion. In the polishing operation E, the ultrafine particle dispersion for polishing which has not been subjected to the so-called separation operation may be used. And it is related. First, the stirring operation in the method of the present invention is explained. The agitator equipped with two or four blades is used as the agitator in the method of the present invention, and then, the blades and the liquid contact part are subjected to inert and stable polytetrafluoroethylene and the like The resin coating is completely treated, and metal ions that do not contaminate the so-called ultrafine particle dispersion for grinding are also used. 49. When an embodiment is listed in the state of producing a superfine particle dispersion for grinding with a solid concentration of 30% by weight, it is dissolved in 6 8. 4 7 1 kg of ultrapure water, 1. 49 8 kg of a potassium hydroxide aqueous solution having a concentration of 20% by weight, and 'the agitator provided with a fan having a blade of 50 to 100 mm at a speed of 1500 rpm' was used to agitate the above-mentioned dissolving solution. Within 0 minutes, 30. 3 kg of smoked silica having a primary particle diameter of 20 to 30 nm was put in fairly evenly. After putting in the full amount of the ingredients, the number of revolutions of the mixer was set to 2000 rpm, and the stirring operation was performed for 15 minutes. Then, the number of revolutions of the blender described in the lift was set to 3,000 rpm, and carried out. After 15 minutes of stirring operation, "continued" was dispersed in the dispersion manufacturing apparatus for dispersing the ultrafine particle dispersion for grinding by the collision phenomenon of the high-pressure fluid.

第12頁 五、發明說明(10) 以便於減少所謂之趨流性 研磨用超微粒子分敢體 (thixotropy ) 〇 接著,就藉由使田 製造方法之高壓流=者本發明之研磨用超微粒子分散體之 分散體之分散體势Ϊ f衝撞現象而分散開研磨用超微粒子 圖2係為用以說:/置’而進行著相關之說明。 體之某一例子之_ <本發明之分散體製造裝置之分散部本 分散體本部1,係& 散部,係在該形成右為装具備有分散部之分散裝置’而該分 片4以便於保持著前有f狀流路2、3之構件上而藉由填隙用 而形成之開口部6中^構件與相反部位上之構件5之間隔 體,發生著衝撞^ /該由溝狀之流路中而導入之流 此外,圖3係為用象以^明開研磨用超^粒子分散體。 他例子之圖式。乂5兒明本發明之分散體製造裝置之其 辟為用以說明本發明之分散體製造裝置之分散 《要素之圖 <,而圖3(B)係為用以顯示出本 體製造裝置之剖面圖。透過該形成有交差狀流 路16之中間板狀體17 ’而層積上該設置有流體之流入口 11、12之流入側板狀體13、以及該設置有溝狀貫通孔14之 出口側板狀體15,並且,由流入側板狀體13之入口處開 而流入該包含有超微粒子之流體,而在將流體 向’改變成為直角之後,接著,在該形成於溝槽 板狀體之間之流路中’衝撞著流體’然後,由前述之溝 槽和板狀體兩者之溝槽之交差點開始而一直至該由形成於Page 12 V. Description of the invention (10) In order to reduce the so-called thixotropy of ultrafine particles for flow-tightening grinding. Next, the high-pressure flow of the field manufacturing method is used to make the ultrafine particles for grinding of the invention. The dispersion potential of the dispersion Ϊ f colliding phenomenon and disperse the ultrafine particles for grinding Figure 2 is used to say: / set 'for related explanation. An example of a body _ < dispersion section of the dispersion manufacturing apparatus of the present invention, the dispersion section 1, is & the dispersion section, on the right side of the formation is a dispersion device provided with a dispersion section, and the slice is 4 In order to keep the f-shaped flow paths 2 and 3 in front, the gap between the ^ member in the opening 6 formed by the gap filling member and the member 5 on the opposite part is collided. The flow introduced in the groove-shaped flow path. In addition, FIG. 3 is a super particle dispersion for grinding by using an image. Schema of his example.乂 5The invention of the dispersion manufacturing apparatus of the present invention is used to explain the dispersion of the dispersion manufacturing apparatus of the present invention. "Elements < and Figure 3 (B) is used to show the main body manufacturing apparatus. Sectional view. Through the intermediate plate-like body 17 ′ having the intersecting flow path 16, the inflow-side plate-like body 13 provided with the fluid inlets 11 and 12 and the outlet-side plate-like shape provided with the groove-shaped through hole 14 are laminated. The body 15 is opened from the inlet of the inflow-side plate-shaped body 13 and flows into the fluid containing ultrafine particles. After changing the fluid to a right angle, the fluid is then formed between the grooved plate-shaped bodies. In the flow path, 'impinging on the fluid', then, starting from the intersection of the grooves of the aforementioned grooves and the plate-shaped body, the formation of the

五、發明說明(11) 相反部位之板狀辦L , ^ ^ ^ , 艰上之溝槽而組成之流路為止,流入前述 * H , I造出研磨用超微粒子分散體。 並且,圖4係A m 他之分散部本體之用圖以^說。明本發明之分散體製造裝置之其 圖4係為用以部; 分埒邾*舯々〜 出本發明之分散體製造裝置之流體之 刀敢部本體之立微面 鑽石等之硬度比* _。分散部本體21,係'藉由重疊著該由 分散部本體21,=之材料而組成之板狀體而構成的°在 + 〇 , 货、形成有2個之流入口 2 2,並且,在前述V. Description of the invention (11) The plate-shaped office L, ^ ^ ^ at the opposite part, flows through the channel formed by the difficult grooves, and flows into the aforementioned * H, I to create a superfine particle dispersion for grinding. In addition, Fig. 4 is a drawing of the main body of the dispersion part of A m and said. Fig. 4 shows the dispersion manufacturing apparatus of the present invention, and Fig. 4 is a part thereof; ; * 舯 々 ~ The hardness ratio of the standing faceted diamond of the blade body of the fluid of the dispersion manufacturing apparatus of the present invention * _. The dispersion unit main body 21 is formed by overlapping the plate-shaped body composed of the material of the dispersion unit main body 21, and the inflow port 2 is formed at + 〇, and, in Previously

之2個之流入口 22 $ I ,L 用iv心^ t 兩者’係形成有喷嘴’而該噴嘴’係被 州Μ渐減者小口部9。 „The two inflow inlets 22 $ I, L with iv heart ^ t both 'are formed with a nozzle', and the nozzle 'is a small mouth portion 9 which is gradually reduced by the state M. „

曰 .,,Z3之最小剖面積以及流路之剖面積。而 ι ’在衝才里著該g古A 准〜-mm 1 夂阿速度地通過小口部之固液混合相流而 丁者戶“礼化分散作業之後,而由流出口 24中,取出前 述之固液混合相户 , ^ Λ L。比起該設置有直線上之小口部之分散 ,θ像月』述這樣开〉狀之噴嘴,係可以防止住所謂由於固液 :合相流之接觸到壁面之接觸現象而導致之磨耗現象發 生。 係可以在冋壓容器内’藉著設置有該小於高壓容器内之 机體之流路而形成有直徑比較小之貫通孔且厚度比較薄之 板狀體,以便於形成圖4所示之分散體製造裝置。此外, 在圖4之裝置中,板狀體之貫通孔之中央’係朝向著板狀 體之側面,而連通有該垂直於板狀體之貫通孔上之流出用 通路,並且,該由乳化部之貫通孔之相互呈相反之方向而 供應過來之流體’係在板狀體之中央部,發生著衝撞現 象’以便於分散開研磨用超微粒子分散體。That is, the minimum cross-sectional area of Z3 and the cross-sectional area of the flow path. And ι 'in the red, the ggu A quasi ~ -mm 1 夂 A through the solid-liquid mixed phase flow in the small mouth at a speed and after the "ceremonial dispersion operation, and from the outflow port 24, take out the aforementioned The solid-liquid mixed phase, ^ Λ L. Compared to the nozzle with a small opening on a straight line, θ is opened like the above, it can prevent the so-called solid-liquid: combined phase flow contact. The abrasion phenomenon caused by the contact phenomenon to the wall surface can occur in the pressurized container by forming a flow path smaller than the body in the high-pressure container to form a through-hole with a relatively small diameter and a relatively thin plate. In order to form the dispersion manufacturing apparatus shown in Fig. 4, in the apparatus of Fig. 4, the center of the through hole of the plate-shaped body is toward the side surface of the plate-shaped body, and communicates with the perpendicular to the plate. The flow path for the outflow through the through-holes of the shape body, and the fluid supplied from the through-holes of the emulsified part in opposite directions to each other 'is in the central part of the plate-shaped body, and a collision phenomenon occurs' to facilitate dispersion. Superfine particle dispersion for grinding.

五、發明說明(12) 即使是呈一體地形成有該進行著八 可以在板狀體之表面上,形成有所二:作業之板狀體,也 狀體之中央上之貫通孔開始而一直二:該形成於2片之板 之溝槽,並且,藉由重疊荖2h 至板狀體之側面上 以便於形成出該由前述:Γ通片孔 能夠藉由重疊著2片之板狀體之構件°之\出口 ’此外,還 部,以便於在對於分散部之各個形成出乳劃分散 溝槽之加工作業之時,办千而進行著貫通孔或者 狀之加工作業,因此,能夠非進行著各種任意形 裝置之製造作業。 易也進行著分散體製造 此外,使得該以相當 徑,小於該以相當高之壓力而:而5撞著流體之部分之直 同時,還使得該流體以古々IL入著流體之管路之直徑, 直線狀,並且,還# 田同之速度而通過之部分,成為 度,因此,能夠減少該 力以及流速之部分之長 大小,以便於提高該^ 體衝撞著器壁而損失之能量 在前述這些之分散刀散作業之構件之耐久性。 最為理想及良好。由^ 中’係以圖4所示之分散裝置, 係在分散裝置之内部中,圖2▲或者圖3所示之分散裝置中, 流體之流動方向,因’改變著該被加壓成為高壓狀態之 分散裝置之壁面,以11會由於流體衝撞到壁面而磨耗著 時,由於該用以決定,會有所§胃分散體之污染存在,同 壓力和流量之二次方^裝置處理能力之小口部半徑,係與 出大量之分散體之κ雜,例,所以,就會有所謂無法製造 叫雞存在著。 第〗5頁 五、發明說明(13) 此外,圖5係為用以說明喷嘴之剖面形狀以及固液混合 相流體中之固體粒子之存在狀態之圖式。在流入側和流出 側之間而形成有小口部之狀態下,管路之剖面積,係朝向 著小口部而漸減。如果說得更加具體一點,在圖5所示之 例子中,前述之流入側,係由大小1 m m之管路而形成的, 並且,在0.52mm之長度之間,管路之剖面積,係朝向著0. 3mm之小口部半徑而漸減。 結果,藉由小口部,而形成出該形成有所謂並無存在有 粒子之區域的境界粒子流線;在圖5之橫軸,係顯示出小 口部半徑成為1之狀態下之喷嘴長度,而在圖5之縱軸,係 顯示出小口部半徑成為1之狀態下之管路之直徑。比起喷 嘴之小口部,由於在出口側,係形成有所謂並無存在著粒 子之部分,因此,可以藉由在比起境界粒子流線而還更加 遠離開中心軸之位置上,形成出壁面,以便於防止所謂喷 嘴之磨耗現象發生。 此外,在本發明之研磨用超微粒子分散體之製造方法 中,可以藉由離心分離等之方法,配合著粒徑大小,而對 於該在分散作業中之所得到之分散體,進行著所謂之分級 作業。 雖然在分離作業中,係能夠使用著各種之裝置,但是, 例如在使用著離心分離裝置(柏格曼公司製、A VANT I HP-201型)而以轉速lOOOOrpm、離心力30000g之條件而進 行著連續處理之狀態下,其分離作業之處理前之粒度分布 區域,係為76nm〜339nm,然而,在實際上,其分離作業V. Description of the invention (12) Even if it is integrally formed, the surface can be formed on the surface of the plate-shaped body in two ways: the plate-shaped body that operates, and the through hole in the center of the body starts and continues. Two: The groove formed on the two-piece plate, and by overlapping 至 2h to the side of the plate-shaped body to facilitate the formation of the above-mentioned: Γ through-sheet hole can be overlapped by two plate-shaped body In addition, it is also provided to facilitate the processing of through-holes or shapes during the processing operation of forming the emulsion scatter grooves for each of the dispersion sections. Manufacturing of various arbitrary shaped devices is underway. Yi also carries out dispersion manufacturing. In addition, the diameter of the fluid is smaller than that of the fluid at a relatively high pressure: while the part hitting the fluid is straight, it also causes the fluid to flow into the pipeline of the fluid with GIL. Diameter, straight, and the part that passes through the speed of the field becomes degree. Therefore, the length of the force and the part of the flow velocity can be reduced, in order to increase the energy lost by the body crashing against the wall of the device. The durability of the components of the above-mentioned dispersion operation. Most ideal and good. From "^", the dispersion device shown in Fig. 4 is inside the dispersion device, and the flow direction of the fluid in the dispersion device shown in Fig. 2 ▲ or Fig. 3 is changed by 'pressurized to high pressure. When the wall surface of the dispersing device in the state is worn due to the impact of the fluid on the wall surface, due to the determination, there will be contamination of the gastric dispersion, which is the same as the pressure and flow rate. The small mouth radius is related to the κ complex that produces a large number of dispersions, for example, so there is a so-called chicken that cannot be manufactured. Page 5 5. Explanation of the invention (13) In addition, FIG. 5 is a diagram for explaining the cross-sectional shape of the nozzle and the existence state of solid particles in the solid-liquid mixed phase fluid. In a state where a small opening is formed between the inflow side and the outflow side, the cross-sectional area of the pipe gradually decreases toward the small opening. To be more specific, in the example shown in FIG. 5, the aforementioned inflow side is formed by a pipe with a size of 1 mm, and the cross-sectional area of the pipe is between 0.52 mm in length. It is gradually reduced toward a small mouth radius of 0.3 mm. As a result, the boundary particle flow line in which the so-called area where no particles exist is formed by the small mouth portion; the horizontal axis of FIG. 5 shows the nozzle length in a state where the small mouth portion radius is 1, and The vertical axis of FIG. 5 shows the diameter of the pipe in a state where the small mouth radius is 1. Compared with the small mouth of the nozzle, the so-called part without particles is formed on the exit side. Therefore, the wall surface can be formed at a position farther away from the central axis than the boundary particle flow line. In order to prevent the so-called nozzle wear phenomenon. In addition, in the method for producing the ultrafine particle dispersion for polishing of the present invention, the particle size can be adjusted by a method such as centrifugation, and the so-called dispersion obtained during the dispersion operation can be so-called Graded jobs. Although various devices can be used in the separation operation, for example, a centrifugal separation device (manufactured by Bergman, A VANT I HP-201) is used at a speed of 1000 rpm and a centrifugal force of 30,000 g. In the state of continuous processing, the particle size distribution area before the separation operation is 76 nm to 339 nm. However, in practice, the separation operation

第16頁 五、發明說明(14) 之處理前之粒度分布區域’係為76nm〜140nm,也就是 說’可以經過確認:並無存在有粒度14〇nm以上之粒子。 如果使用離心分離器的話’則可以按照所謂並不要求之上 限粒子直徑’而調整著離心分離器之旋轉速度。並且,比 較理想之離心力,係在丨0 〇 〇 〇 g〜6 〇 〇 〇 〇 g之範圍内。 、在本,明之研磨用超微粒子分散體之製造方法中,係可 ,使用著各種之高度比較大之研磨用粒子;如果列舉出一 =例f之時,則能夠列舉有以下所敘述之方法:藉由火焰 饱=軋化性'氣氛,而析出該包含有金屬成分之原料蒸氣之 燻法;或者,藉由固體膠質法而析出所謂研磨用粒子之 n'者,藉由像電滎之高溫生成之方法;或者,在粉 而配合著粒經之大小,以便於分級出研磨用粒 該作為研磨用超微粒子 士 乂 方法而製造出氧化矽、氧鋁 〗::戎措“述這些 鍺、氧化鈽、和氧化般Π、-乳化鈦、氧化鍅、氧化 混合物、以及氧化物以1 化物、&前述這些氧化物之 乂及乳化物以外之金屬化合物。 特別疋,在前述這此 氧化物,其純度係比 ’ 以㈢由電漿法而得到之 心以内之範圍中,並/ 次粒子直徑也是在10〜50 真圓。 且,粒子之形狀也最好是幾乎接近 並且’在分散體中, 絶等之鹼性物質、碘酸 類之物質β 係可以混合入氫氧化鉀、和氫氧化 鉀、以及過氧化氫水等之氧化劑之Page 16 V. Description of the invention (14) The particle size distribution area before treatment 'is 76nm ~ 140nm, that is, it can be confirmed that there are no particles with a particle size of 14nm or more. If a centrifugal separator is used, the rotation speed of the centrifugal separator can be adjusted in accordance with the so-called "no upper particle diameter requirement". In addition, the ideal centrifugal force is in the range of 0.001 g to 600 g. In the present method for producing ultrafine particle dispersions for polishing, it is possible to use a variety of relatively large particles for polishing; if one = example f is listed, the methods described below can be listed : Fumigation method in which the raw material vapor containing the metal component is precipitated by a flame-saturated = rolling 'atmosphere; or, n', which is a so-called abrasive particle, is precipitated by a solid colloid method, and is like The method of high-temperature production; or, the size of the granules is mixed with the powder to facilitate the classification of the grinding particles. As a method of grinding ultrafine particles, the silicon oxide and aluminum oxide are produced. , Osmium oxide, and oxidized titanium,-emulsified titanium, osmium oxide, oxidation mixture, and oxide compounds, and metal compounds other than the above-mentioned oxides and emulsions. In particular, the above-mentioned oxidation The purity ratio of the particles is within the range of the heart obtained by the plasma method, and the diameter of the secondary particles is also in the range of 10 to 50 true circles. Also, the shape of the particles should preferably be nearly close to each other and in In the dispersion, the absolute basic substances and iodic acid substances β are mixed with oxidants such as potassium hydroxide, potassium hydroxide, and hydrogen peroxide water.

第17頁 五、發明說明(15) "此外,本發明之研磨用超微粒子分散體中之研磨用超微 。粒子,其懸浮液之濃度,係最好為5重量%以上' 6 〇重量 义以下之水性懸浮液,若更加理想的話,則懸浮液之濃 度,最好為13重量%〜30重量%之水性懸浮液。當研磨用 超微胃粒子分散體中之研磨用超微粒子之懸浮液之濃度小於 5重1 %之時,則化學機械式研磨(CMp : ChemicalPage 17 V. Description of the invention (15) " In addition, the ultrafine particles for grinding in the ultrafine particle dispersion for grinding of the present invention. The concentration of the particles in the suspension is preferably an aqueous suspension of 5% by weight or more and 60% by weight or less. If it is more desirable, the concentration of the suspension is preferably 13% by weight to 30% by weight of water. suspension. When the concentration of the suspension of the ultrafine particles for grinding in the ultrafine gastric particle dispersion for grinding is less than 5 weight 1%, the chemical mechanical milling (CMp: Chemical

Mechanical Polish)中之金屬部份、也就是機械式研磨 特性,會變得比較小’ ϋ I ’在研磨用超微粒子分散體中 之研磨用超微粒子之懸浮液之濃度為6〇重量%以 則在固體成分濃度相當高之狀態下,而僅進行 7 磨處理’以致於化學式研磨作用,呈現出所謂降低:;見 i粒Ϊ並不適合作為研磨用超微粒子分散體中之研磨用超 該藉由本發明之方法而得到之分散體,係呈現出相冬古 度之分散現象,並且,其經時變化係相當地小, 田= ㈣月左右就會呈凝集沉-之時間: 車乂長之刀政體,该错由本發明之方法而得到之 可以使用到1年以上之長時間。 跃®,係 【實施例】 以下,列舉出本發明之實施例,而就本發 行說明。 心円谷,進 實施例1 在超純水中,添加入該作為pH值調整劑用之氫氧 以便於調製出ρ Η 11之驗性溶液。在前述之驗性溶液中钾 五、發明說明( ;16) 邊進行著 攪拌,一 邊投入 該煙燻過 之氧化矽, 以便於 分別 地調製出 所謂投入 量 12. 5 重量% 、 2 5重量% 、 以及5 0 重量 %之3種類之試料= ) 接著, 藉由圖3所示之具有對向型噴嘴之分散裝置( :杉 野機械公 司製高度 分析用 裝置(a 1 t i m i zer-sy stem ) HJP-2 5 0 28 ),在1 1 0 0 k g f / c m2之條件下,對於前述之 -試 料,分別 地進行著 1行程 (one-pas s )及2行程 (two- pass )之處理 次數,而 調製出 合計6個之分散體,並且,還藉 由雷射光 繞射式粒 度分布 測定裝置 (島津製作 所製、 SALD-2000A ),而 測定出 該分散體 中之超微粒 子之粒 徑和 粒徑分布 。將試料 之處理 條件以及 所得到之粒 子之特 性, 顯示於表1中。 【表1】 氧化物 處理壓力 通過 粒徑分布 中心粒徑 異 物 濃度( (kgf / 次數 範圍(n m) (nm) 重量% ) cm2) 12.5 1100 1 100-380 140 並未檢 測出 12.5 1100 2 80-300 130 並未檢 測出 25 1100 1 80-330 130 並未檢 測出 25 1100 2 70-300 125 並未檢 測出 50 1100 1 80-300 125 並未檢 測出 50 1100 2 65-280 120 並未檢 測出 接著, 藉著所謂 由分散 用裝置, 透過管路而 連結之 連續 式離心分離機(美國柏格曼公司製、AVANT I HP-20 1型The mechanical part of the mechanical polish), that is, the mechanical polishing characteristics, will become relatively small. The concentration of the suspension of the polishing ultrafine particles in the polishing ultrafine particle dispersion is 60% by weight. In the state where the solid content concentration is quite high, only 7 grinding treatments are performed, so that the chemical grinding effect shows a so-called reduction :; i granules are not suitable for grinding in the ultrafine particle dispersion for grinding. The dispersion obtained by the method of the invention exhibits the dispersion phenomenon of the ancient winter degree, and the change over time is relatively small, and the field will be agglomerated and settled around the time of the month: time Regimes, which are obtained by the method of the present invention, can be used for a long period of more than one year. [Exemplary Embodiments] Hereinafter, examples of the present invention will be listed and the present invention will be described. Heart pit valley, Example 1 In the ultrapure water, hydrogen and oxygen used as a pH adjusting agent were added to prepare a test solution of ρ Η 11. 5. In the aforementioned test solution, potassium V. Description of the invention (; 16) While stirring, the smoked silicon oxide is put in order to prepare the so-called input amounts of 12. 5 wt% and 25 wt%, respectively. And 3 types of samples of 50% by weight =) Next, a dispersing device having a facing nozzle as shown in FIG. 3 (: a 1 timi zer-sy stem by Sugino Machinery Co., Ltd.) HJP -2 5 0 28), under the condition of 1 100 kgf / c m2, for the above-sample, the number of processing times of one-pass (one-pas s) and two-pass (two-pass) are performed, A total of six dispersions were prepared, and the particle size and particle diameter of the ultrafine particles in the dispersion were measured by a laser light diffraction type particle size distribution measuring device (SALD-2000A manufactured by Shimadzu Corporation). distributed. Table 1 shows the processing conditions of the samples and the characteristics of the obtained granules. [Table 1] Oxygen treatment pressure through the particle size distribution center particle size foreign matter concentration ((kgf / frequency range (nm) (nm) weight%) cm2) 12.5 1100 1 100-380 140 No detected 12.5 1100 2 80- 300 130 not detected 25 1100 1 80-330 130 not detected 25 1100 2 70-300 125 not detected 50 1100 1 80-300 125 not detected 50 1100 2 65-280 120 not detected Next, a continuous centrifugal separator (manufactured by Bergman Corporation, AVANT I HP-20 1 type) connected by a so-called dispersing device through a pipeline.

第19頁 五、發明說明(17) ),並且,還利用所謂2 . 8公升/分鐘、轉子之旋轉數 6000rpm、離心力18000g 和 lOOOOrpm、以及離心力 30000g 之2種方法,而對於前述之所得到之分散體,連續地進行 著處理,並且,將其處理之結果,顯示於表2中。 【表2】 氧化物 處理壓力 通過次數 6000rpm之 lOOOOrpm 之 濃度( (kgf / 粒徑分布 粒徑分布 重量% ) cm2 ) (nm) (nm) 12. 5 1100 1 100-180 100-140 12.5 1100 2 80-180 80-140 25 1100 1 80-180 80-140 25 1100 2 70-180 70-140 50 1100 1 80-180 80-140 50 1 100 2 65-180 65-140 【發明之效果】 就正如 以上所敘述的,藉由本發明之方 法,整理調整出 化學機械式研磨用 超微粒子分散體之粒徑 ^則能夠付到粒 度分布範圍比較狹窄並且呈水性之高純度之均勻之超微粒 子分散體 ,以至於在半導體製造作業中, 於層間絕緣膜等 之氧化膜及金屬配線膜之平滑、平坦化處理中,可以發揮 出相當大之效果。 【圖式之簡單說明】 圖1係為用以說明本發明之研磨用超微粒子分散體之製 造作業之圖式。Fifth, invention description (17)) on page 19, and two methods of so-called 2.8 liters / minute, rotor rotation number 6000 rpm, centrifugal forces 18000 g and 1000 rpm, and centrifugal force 30,000 g are also used. The dispersion was continuously processed, and the results of the processing are shown in Table 2. [Table 2] Concentration of oxide treatment pressure passing times 6000rpm to 1000rpm ((kgf / particle size distribution particle size distribution weight%) cm2) (nm) (nm) 12. 5 1100 1 100-180 100-140 12.5 1100 2 80-180 80-140 25 1100 1 80-180 80-140 25 1100 2 70-180 70-140 50 1100 1 80-180 80-140 50 1 100 2 65-180 65-140 [Effect of the invention] Just like As described above, by the method of the present invention, the particle size of the ultrafine particle dispersion for chemical mechanical polishing can be adjusted to adjust the uniform ultrafine particle dispersion with a narrow particle size distribution range and high purity in the water. So that during the semiconductor manufacturing operation, a considerable effect can be exerted in the smoothing and planarizing treatment of the oxide film and the metal wiring film such as the interlayer insulating film. [Brief description of the drawings] Fig. 1 is a drawing for explaining the manufacturing operation of the ultrafine particle dispersion for polishing of the present invention.

第20頁 五、發明說明(18) 圖2係為用以說明本發明之分散體製造裝置之分散部本 體之某一例子之圖式。 圖3係為用以說明本發明之分散體製造裝置之其他例子 之圖式。 圖4係為用以說明本發明之分散體製造裝置之其他之分 散部本體之圖式。 圖5係為用以說明喷嘴之剖面形狀以及固液混合相流體 中之固體粒子之存在狀態之圖式。 【元件編號之說明】 A :調製作業 B :攪拌作業 C :分散作業 D :分離作業 E :研磨作業 1 :分散部本體 2 :溝狀之流路 3 :溝狀之流路 4 :填隙用片 5 :相反侧之構件 6 :開孔部 11 :流體之流入口 12 :流體之流入口 13 :流入侧板狀體 14 :溝狀貫通孔Page 20 V. Description of the invention (18) FIG. 2 is a diagram for explaining an example of the dispersion part body of the dispersion manufacturing apparatus of the present invention. Fig. 3 is a diagram for explaining another example of the dispersion manufacturing apparatus of the present invention. Fig. 4 is a diagram for explaining another main body of the dispersion part of the dispersion manufacturing apparatus of the present invention. Fig. 5 is a diagram for explaining the cross-sectional shape of a nozzle and the existence state of solid particles in a solid-liquid mixed-phase fluid. [Description of component numbers] A: Preparation operation B: Stirring operation C: Dispersion operation D: Separation operation E: Grinding operation 1: Dispersion unit body 2: Groove-shaped flow path 3: Groove-shaped flow path 4: For gap filling Sheet 5: Opposite member 6: Opening section 11: Fluid inflow port 12: Fluid inflow port 13: Inflow-side plate-like body 14: Channel-shaped through hole

第21頁Page 21

第22頁Page 22

Claims (1)

六、申請專利範圍 1. 一種研磨用超微粒子分散體之製造方法,其特徵為, 係具備有以下所敘述之分散作業: 在研磨用超微粒子分散體之製造方法中,藉由對於該在 液體中而分散有研磨用超微粒子之懸浮液,進行著攪拌, 而除去所謂之趨流性(t h i X 〇 t r 〇 p y )之後,接著,再對於 前述之懸浮液,進行著加壓處理,並且,由相反之方向, 相互地導入前述之懸浮液,而使得該懸浮液之間,相互地 進行著衝撞,以便於分散開該懸浮液中之研磨用超微粒 子。 2. 如申請專利範圍第1項之研磨用超微粒子分散體之製 造方法,其中研磨用超微粒子分散體,係為半導體平坦化 用途之化學機械式研磨用之分散體。 3. 如申請專利範圍第1項之研磨用超微粒子分散體之製 造方法,其中分散體係為濃度5重量%以上、6 0重量%以 下之水性懸浮液。 4. 如申請專利範圍第1至3項中任一項之研磨用超微粒子 分散體之製造方法,其中在經過所謂分散處理後,還具備 有該用以分級出粒徑比較大之粒子的分離作業。6. Scope of patent application 1. A method for manufacturing a superfine particle dispersion for grinding, characterized in that it comprises the following dispersing operations: In the method for manufacturing a superfine particle dispersion for grinding, The suspension in which the ultrafine particles for grinding are dispersed is stirred, and the so-called flow tendency (thi X 〇tr 〇py) is removed. Then, the suspension is subjected to a pressure treatment, and, The aforementioned suspensions are introduced from each other in opposite directions, so that the suspensions collide with each other so as to disperse the ultrafine particles for grinding in the suspension. 2. The manufacturing method of the ultrafine particle dispersion for polishing as described in the first patent application range, wherein the ultrafine particle dispersion for polishing is a dispersion for chemical mechanical polishing of semiconductor planarization applications. 3. The manufacturing method of the ultrafine particle dispersion for grinding as described in the scope of patent application item 1, wherein the dispersion system is an aqueous suspension having a concentration of 5 wt% or more and 60 wt% or less. 4. The manufacturing method of the ultrafine particle dispersion for grinding according to any one of claims 1 to 3, wherein after the so-called dispersing treatment, it is further provided with the separation for classifying particles with a relatively large particle size. operation. 第23頁Page 23
TW87117485A 1998-10-22 1998-10-22 Method of manufacturing micro granule segregate for polishing TW379158B (en)

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