…3/41… 3/41
五、發明說明（/ ) 【本發明之領域】 尤指— 可廣泛 硬式磁 、、本發明係、關紅氧化鈽改質粉體之製造方法 種通用於製作各種二氧化銻研磨漿料之製造方法 應用於各種研磨抛光製程，包括玻璃、光學鏡片 碟片或半導體製程中之研磨抛光等技術領域。 【本發明之背景】 習知<二氧化鈽粉體於水溶液中形成之研磨槳料，柘 易發生凝聚現象，形成較大難而快速沉降，造成研磨: 料懸浮於水溶液之時間短，即其穩定度不佳，進而大幅降 低研磨之研磨速率，且研磨批次間的不穩定性高。因此' 如何1展一種延長二氧化鈽粉體懸浮於水溶液漿料之時 間，使二氧化鈽粉體得以長時間穩定地分散於水溶液漿料 中’便成為一重要之研發課題。 於美國專利第6,343,976號中，曾提到改良二氧化鈽 粉體於水溶液中性質的方法，其乃將Ce〇2粉體加入含有 分散劑（dispersant)的水溶液中，藉由分散劑（水溶性 丙晞酸聚合物）改變溶液的性質，以改良二氧化鈽水溶液 漿料之性質，並未針對二氧化鈽粉體本身懸浮於水溶液之 穩定度做改善。 於美國專利第6,299,659號中則提到，將二氧化鈽粉 體進行表面改質，以改良其在水溶液中性質的方法，其乃 將一氧化鈽分散於水中後，再加入N - 3 -三甲氧基石夕丙基乙 二胺[N-3-(trimethoxysilyl) propylethylenediamine]，於 ^ --------β--------- (請先閱讀背面之注意事項再填寫本頁} 經濟部智慧財產局員工消費合作社印製 4V. Description of the invention (/) [Field of the invention] In particular-the method for manufacturing a wide range of hard magnetic, invented, and red dysprosium oxide modified powders, which are commonly used in the manufacture of various antimony dioxide slurry The method is applied to various grinding and polishing processes, including the technical fields of grinding and polishing in glass, optical lens discs, or semiconductor processes. [Background of the present invention] The conventionally known grinding paddle material of osmium dioxide powder in an aqueous solution is prone to agglomeration, which is difficult and rapid to settle, resulting in grinding: The time for which the material is suspended in the aqueous solution is short, that is, its Poor stability, which significantly reduces the grinding rate of grinding, and high instability between grinding batches. Therefore, 'how to show a way to extend the suspension time of the osmium dioxide powder in the aqueous slurry so that the osmium dioxide powder can be stably dispersed in the aqueous slurry for a long time' has become an important research and development issue. In U.S. Patent No. 6,343,976, a method for improving the properties of osmium dioxide powder in an aqueous solution has been mentioned, which is to add CeO2 powder to an aqueous solution containing a dispersant. The polymer of malonic acid) changes the properties of the solution to improve the properties of the osmium dioxide aqueous solution slurry, and does not improve the stability of the osmium dioxide powder itself suspended in the aqueous solution. In U.S. Patent No. 6,299,659, a method for surface modification of osmium dioxide powder to improve its properties in an aqueous solution is described. After dispersing osmium oxide in water, N-3 -trimethylamine is added. N- (trimethoxysilyl) propylethylenediamine, ^ -------- β --------- (Please read the precautions on the back before filling in this Page} Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs 4
A7 五、發明說明（3 ) 質的方法，:^所寺疋〈改良二氧化卸粉體在水溶液中性 ^、疋二氧化鈽粉體，使其延長懸浮於水 ==發明之方法，乃將二氧化錦粉體與切垸 二:在有機水溶液中反應’進行二氧化鈽粉體表面..改 長時間狀懸料水溶液之二氧化鈽粉 …發明人爰㈣此，杨積極發明之精神，巫思一種可 乂解决上述問通《「二氧化鈽改質粉體之製造方法 經研究實驗終至完成此項嘉惠世人之發明。 a 【本發明之概述】 訂 本發明《王要目的，係在提供二氧化錦改質粉體之製 造方法’俾能使二氧化卸粉體易於水中均勻分散，藉以延 =體之懸浮時間，使其不易產生❹而穩定^水溶液 本發明之另-目的，係在提供二氧化舞改質粉體之製 造方法，俾能應用於製作各種二氧化鈽相關之研磨聚料， 提供產業應用。 、為達成上述之目的，本發明之二氧化鈽改質粉體之製 造万法’其係將二氧化鈽粉體與一含錢（siiane)基的 偶聯劑化合物於有機水溶液中進行改質。將二氧化錦粉體 與-含石夕燒基的偶聯劑化合物於有機溶劑混合水溶液中進 行混合攪拌反應，使二氧化鈽與具有炫氧基之石夕化合物作 用，即可得經表面改質之二氧化鈽粉體。 I___6 5氏張尺度適用中國國家標準（CNS)A4規格⑽χ 297公爱丁 539741 經 濟 部 智 慧 財 產 局 員 工 消 費 合 作 社 印 製 A7 五、發明說明（今） ^本I月之有機溶劑，較佳的可為醇類或酮類，如甲 醇乙醇丙酉同等，其體積百分比為總體積之百分之五十 土百刀之九十九。本發明之含矽烷基的偶聯劑化合物可以 是一端含烷氧基另一端含極性官能基之化合物，如N-3_三 甲氧基矽丙基乙二胺◦本發明之二氧化鈽改質粉體之製造 万法，於該有機水溶液中尚可包括鹽類、無機物、有機金 屬化合物等物種。 由於本發明構造新穎，能提供產業上利用，且確有增 進功效，故依法申請發明專利。 【圖式簡單説明】 第1圖：係未經改質、經N-3-三甲氧基矽丙基乙二胺於水溶 液中改質及本發明之經]^_3_三甲氧基矽丙基乙二胺 於乙醇水溶液中改質之二氧化鈽粉體於水中之沉澱 變化隨時間之關係圖。 第2圖··係未經改質及本發明之經N _ 3 _三甲氧基矽丙基乙二 胺於乙醇水溶液中改質之二氧化鈽粉體其隨？11變 化所量測之傑塔電位（Zeta p〇tential)圖。 ， 【圖號説明】 無 【發明詳細敘述】 ·, τ AW ^------------- (請先閱讀背面之注意事項再填寫本頁) 539741 A7 五、發明說明（6 ) 此外此含石夕之氨基型化合物的另一端，為一具極性之 氨基官能基，若將此經表面改質之化合物與水溶液混合， 因其氨基官能基為可溶於水之極性官能基，故非常容易與 水結合。因此可知，此含矽之氨基型化合物，其一端因含 矽之烷氧基’故可與二氧化鈽粉體結合，而另一端為含極 性之氨基g能基’故能與水結合，經由此兩者之作用可提 高二氧化鈽粉體分散於水中懸浮時間，進而增加此漿料之 穩定度。 裝 【較佳具體實施例之詳細説明】 訂. 本發明中所使用之一氧化鈽粉體、含石夕燒基的偶聯劑 化合物、有機溶劑以及水之取得及實驗進行中之製備為熟 悉此項技藝之人士所習知，於此不再贅述。 本發明之技術内容可以藉由以下之較佳具體實施例説 明，而有更佳之暸解。 * 复-施例1 (本發明之方法） 將2克之二氧化鈽粉體與i克之N-3-三甲氧基矽丙基 乙二胺[N-3-(trimethoxysilyl) propyiethylenediamine]於 含9 5 % (體積比）之1 〇 〇毫升乙醇水溶液中混合，即9 5毫 升乙醇加上5愛升純水，將此混合溶液置於超音波中震盪 10分鐘，爾後再將其於7 0°C下受熱1小時，將上述溶液之 沉殿物過濾後，以乙醇清洗之，再於8 5 °C乾燥，即可得本 發明之二氧化鈽改質粉體。A7 V. Description of the invention (3) Qualitative method: ^ Suo Si 疋 <Improved dioxide unloading powder is neutral in aqueous solution, 疋 钸 Dioxide powder, so that it is prolonged suspended in water == invention method, The reaction of bromide dioxide powder and cutting tincture: reaction in an organic aqueous solution to carry out the tincture of the hafnium dioxide powder surface .. Changing the long-time suspension solution of the hafnium oxide powder ... The inventor hereby, Yang actively invented the spirit Wusi can solve the above-mentioned question "" The manufacturing method of thorium dioxide modified powder has been researched and experimental until the completion of this invention that benefits the world. A [outline of the invention] It is to provide a manufacturing method of modified brocade powder, which can easily disperse the powder in the water, so as to prolong the suspension time of the body, making it difficult to produce tritium and stable. ^ Aqueous solution The purpose is to provide a manufacturing method of modified powder of titanium dioxide, which can be applied to the production of various abrasive aggregates related to dysprosium dioxide, and to provide industrial applications. In order to achieve the above purpose, the modified dysprosium dioxide of the present invention Manufacture of powder The method is to modify the osmium dioxide powder and a coupling agent compound containing a siiane group in an organic aqueous solution. The powder of the bromide dioxide and the coupling agent compound containing a shiyanaki group are modified. The mixed stirring reaction is carried out in a mixed aqueous solution of an organic solvent, so that the osmium dioxide can react with the stone compound with oxo, and the surface-modified osmium dioxide powder can be obtained. I_6 The 5's scale is applicable to Chinese national standards (CNS ) A4 Specification ⑽χ 297 Public Eding 539741 Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs A7 Printed on the Invention (Today) ^ The organic solvent of this month, preferably alcohols or ketones, such as methanol ethanol propylene酉 Equivalent, its volume percentage is fifty-nine hundred ninety-nine percent of the total volume. The silane-containing coupling agent compound of the present invention may be a compound containing an alkoxy group at one end and a polar functional group at the other end, For example, N-3_trimethoxysilylethylenediamine ◦ The method for manufacturing the rhenium dioxide modified powder of the present invention may include species such as salts, inorganic substances, and organometallic compounds in the organic aqueous solution. Because the invention has a novel structure, can provide industrial use, and indeed has an enhanced effect, it applies for an invention patent in accordance with the law. [Simplified illustration of the figure] Figure 1: The N-3-trimethoxysilicone has not been modified. Modification of ethylenediamine in aqueous solution and the present invention] ^ _3_ Precipitation change of rhenium dioxide powder modified with trimethoxysilylethylenediamine in aqueous ethanol solution over time. Fig. 2 is the unmodified osmium dioxide powder modified by N_3_trimethoxysilylethylenediamine in an ethanol aqueous solution without modification and the present invention. Tower potential (Zeta p〇tential) map., [Illustration of drawing number] None [Detailed description of the invention] ·, τ AW ^ ------------- (Please read the precautions on the back before filling (This page) 539741 A7 V. Explanation of the invention (6) In addition, the other end of the amino compound containing Shi Xi is a polar amino functional group. If this surface modified compound is mixed with an aqueous solution, its amino group The functional group is a polar functional group which is soluble in water, so it is easy to bind with water. Therefore, it can be known that one end of the silicon-containing amino-type compound can be combined with osmium dioxide powder because of the silicon-containing alkoxy group, and the other end is polar amino group energy-containing group, so it can be combined with water. The effect of the two can increase the suspension time of the osmium dioxide powder dispersed in water, thereby increasing the stability of the slurry. [Detailed description of the preferred embodiment] Order. It is familiar to obtain one of the osmium oxide powder, the coupling agent compound containing sulphuric acid group, organic solvent and water in the present invention and the preparation in the experiment. Those skilled in the art are familiar with it and will not repeat it here. The technical content of the present invention can be better understood by describing the following specific embodiments. * Compound-Example 1 (method of the present invention) 2 g of osmium dioxide powder and 1 g of N-3- (trimethoxysilyl) propyiethylenediamine were contained in 9 5 % (Volume ratio) mixed with 100 ml of ethanol aqueous solution, that is, 95 ml of ethanol plus 5 liters of pure water, this mixed solution was placed in an ultrasonic wave for 10 minutes, and then it was again at 70 ° C After being heated for 1 hour, the sanitary matter of the above solution was filtered, washed with ethanol, and then dried at 85 ° C to obtain the modified hafnium dioxide powder of the present invention.
本紙E度適用中國規格⑵〇 1297公釐Y 五、發明說明（rj ) _比較.创」.（美國專利第6,299,659號之方法） 將2克之二氧化鈽粉體與1克之ν_3·三甲氧基石夕丙基 乙二胺[N-3-(trimeth〇XySilyl)propylethylenediamine]於 100毫升純水中混合，將此混合溶液置於超音波中震盪1〇 分鐘，爾後再將其於7(rc下受熱i小時，將上述溶液之沉 澱物過濾後，以純水清洗之，再於85〇c乾燥，即可得表面 改質之二氧化鈽粉體。 二鈽粉藏於水溶液之況降奢腠 取男她例1之二氧化鈽改質粉體、比較例丨之二氧化鈽 改質粉體與未改質之二氧化鈽粉體各2克，置於含1〇〇毫 升蒸餾水 < 量筒内，經混合均勻後，量取其隨時間變化之 懸浮局度，所得結果如第i圖所示。由圖中顯示，靜置i 〇 天後，實施例1之二氧化鈽改質粉體僅發生些許沉澱現 象反之，比輪例1之一氧化鈽改質粉體，則於約2小時就 發生統聚現象，因而形成較大顆粒而沉澱◦另外，未改質 之二氧化鈽粉體，則於不到1〇分鐘内就快速地發生凝聚現 象’亦形成較大顆粒而沉澱。 一般產生沉澱愈多即代表懸浮穩定度不佳且混合效果 差，故本實驗可證實經本發明方法處理後，所得之表面改 質一乳化鈽粉體，其於水中可有效地延長粉體之懸浮時 間，進而提高其於水溶液之穩定度。The paper E degree applies to the Chinese standard 1 〇1297 mm Y V. Description of the invention (rj) _ comparison. Chuang ". (U.S. Patent No. 6,299,659 method) 2 g of osmium dioxide powder and 1 g of ν_3 · trimethoxy stone N- (trimeth〇XySilyl) propylethylenediamine] was mixed in 100 ml of pure water, and the mixed solution was placed in an ultrasonic wave for 10 minutes, and then heated at 7 (rc). After i hours, the precipitate of the above solution was filtered, washed with pure water, and then dried at 85 ° C to obtain a surface-modified osmium dioxide powder. The second osmium powder was stored in an aqueous solution, and it was extravagantly obtained. Men's and hers Example 1 modified osmium dioxide powder, Comparative Example 丨 modified osmium dioxide powder and unmodified osmium dioxide powder 2 g each, placed in 100 ml distilled water < measuring cylinder After the mixture is evenly mixed, the suspension locality that changes with time is measured, and the result is shown in Figure i. As shown in the figure, after standing for 〇 days, the modified thorium dioxide powder of Example 1 is only On the contrary, a slight precipitation phenomenon occurred. The modified powder of thoron oxide, which was one of Round Example 1, was developed in about 2 hours. Larger particles are formed and precipitated due to the aggregation phenomenon. In addition, the unmodified osmium dioxide powder quickly aggregates in less than 10 minutes. 'Large particles are formed and precipitated. Generally, precipitation occurs. The more it means that the suspension stability is poor and the mixing effect is poor, so this experiment can confirm that after the treatment of the method of the present invention, the resulting surface is modified with an emulsified powder, which can effectively prolong the suspension time of the powder in water. Improve its stability in aqueous solution.
本紙張尺錢时關 539741 A7 B7 五、發明說明（7 ) 輿水泫该 pH> _化 私未改質之二氧化鈽粉體與實施例1之二氧化鈽改質 粉體各配成5 wt%之混合水溶液，將此混合溶液置於超音 波中震盪15分鐘，爾後以硝酸（HN〇3)及氫氧化鉀（κ〇Η) 調配pH値，量測ρΗ為3.5至ρΗ*1〇 5之傑塔電位隨？11之 變化。 如第2圖所示，本實施例丨之二氧化鈽改質粉體於ρΗ 為3 .5至pH為10.5之傑塔電位均呈現正電位値，表示經改 質·^二氧化鈽粉體表面帶正電荷；反之，未改質之二氧化 鈽粉體，僅於pH為3.5至PH為8.5呈現正電位値，而於pH 8·5以後反而呈現負電位。故此實驗結果證實本發明所得 之表面改質二氧化鈽粉體，可改變粉體表面所帶之電荷， 使改質（二氧化鈽粉體可適用於較寬廣之範圍。 综上所陳，本發明無論就目的、手段及功效，在在均 顯示其迥異於習知技術之特徵。惟應注意的是，上述H 施例僅係為了便於説明而舉例而已，本發明所主張之權利 範圍自應以申請專利範圍所述為準，而非僅限於上 例。 請 1先 閱 讀 背 面 1之 注 意 事 1 項 再| m 填 W 寫 本 裝 頁 i 經濟部智慧財產局員工消費合作社印剩衣 11 本紙張尺度_㈣國家標準（CNS〉A4規袼（21G X 297^7The paper rule is 539741 A7 B7 V. Description of the invention (7) The pH of the water is not modified, and the modified osmium dioxide powder of Example 1 and the modified osmium dioxide powder of Example 1 are each composed of 5 wt. % Mixed aqueous solution, the mixed solution was placed in an ultrasonic wave for 15 minutes, and then pH 値 was adjusted with nitric acid (HN03) and potassium hydroxide (κ〇Η), and the measured ρΗ was 3.5 to ρΗ * 105. The Jetta potential follows? 11 changes. As shown in FIG. 2, the modified osmium dioxide powder of this embodiment 丨 has a positive potential 値 at the ρ 杰 3.5 to pH 10.5, indicating that the modified 钸 钸 钸 powder The surface is positively charged; on the other hand, the unmodified osmium dioxide powder shows a positive potential only at pH 3.5 to pH 8.5, but it shows a negative potential after pH 8 · 5. Therefore, the experimental results confirm that the surface-modified osmium dioxide powder obtained by the present invention can change the charge on the surface of the powder, so that the modification (the osmium dioxide powder can be applied to a wide range. In summary, this, Regardless of the purpose, means, and effect of the invention, the invention shows its characteristics that are quite different from the conventional technology. However, it should be noted that the above-mentioned H embodiment is merely an example for the convenience of explanation. Please refer to the scope of the patent application, not just the above example. Please read the note 1 on the back 1 and then | m fill in this page and install the page i the Ministry of Economic Affairs Intellectual Property Bureau staff consumer cooperatives printed leftover clothes 11 pieces of paper Standards_㈣National Standards (CNS> A4 Regulations) (21G X 297 ^ 7