TWI303661B - Cerium-based abrasive and stock material therefor - Google Patents

Cerium-based abrasive and stock material therefor Download PDF

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TWI303661B
TWI303661B TW093112159A TW93112159A TWI303661B TW I303661 B TWI303661 B TW I303661B TW 093112159 A TW093112159 A TW 093112159A TW 93112159 A TW93112159 A TW 93112159A TW I303661 B TWI303661 B TW I303661B
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weight
rare earth
oxide
tre0
ratio
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TW093112159A
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Chinese (zh)
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TW200504189A (en
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Daisaku Kobayashi
Yoshitsugu Uchino
Hidehiko Yamasaki
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Mitsui Mining & Smelting Co
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1454Abrasive powders, suspensions and pastes for polishing
    • C09K3/1463Aqueous liquid suspensions
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/20Compounds containing only rare earth metals as the metal element
    • C01F17/206Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/20Compounds containing only rare earth metals as the metal element
    • C01F17/206Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • C01F17/224Oxides or hydroxides of lanthanides
    • C01F17/235Cerium oxides or hydroxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/30Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1409Abrasive particles per se
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/221Oxides; Hydroxides of metals of rare earth metal

Description

1303661 五、發明說明(1) 【發明所屬之技術領域】 本發明係有關於以夤 其原料。 飾為主成分的飾系研磨材料及 【先前技術】 鈽系研磨材料係對例如1303661 V. INSTRUCTION DESCRIPTION OF THE INVENTION (1) Technical Field of the Invention The present invention relates to a raw material thereof. Decorative abrasive material as a main component and [Prior Art] A pair of abrasive materials are, for example,

Cmonaz ite)精礦、中丽益放* 施粉碎、乾燥、、炉捧Ϊ 精礦等的礦石原料,通過實 (夂昭往門〇 &、粕碎(解碎)、分級等步驟來製造的 二二—183/96號公報、特開2002 —97457號公報、 人:辅 4949々號公報)。所列舉的原料中,氟碳鈽精礦 二鑭、鈥等稀土類元素及氟,係鈽系研磨材料之合 適的原料之一。 、例如氟碳鈽精礦的典型係全稀土類氧化物換算重量 乂下稱為TRE0)的重量比例為68〜73wt%左右、氟6wt%左 右、強熱減量(1 00 0。〇為20wt%左右。且TRE〇中,氧化鈽 Ce02#)係5〇wt%左右,氧化鑭(La2〇3等)係35紂%左右,氧 ^歛〇H〇3等)係丨丨奴%左右,氧化镨(Pr6〇ii等)係4以%左 然而,作為研磨材料,要求研磨到傷儘可能不會發生 等研磨特性優良之材料。且經過研磨步驟、效率良好地製 造製品,最好儘可能地縮短研磨步驟所需要的時間。這 樣’作為鈽系研磨材料要求研磨速度儘可能高(研磨值°大) 的材料。 而且’近年來鈽系研磨材料使用於光硬碟或磁硬碟用Cmonaz ite) concentrate, Zhongli Yifang* smashing, drying, and holding ore concentrates, etc., manufactured by real (Zhao Zhao to the threshold & mashing (smashing), grading, etc. Japanese Patent Publication No. 1982-96, JP-A-2002-97457, and People: Auxiliary 4949 No. Among the listed raw materials, the fluorocarbon quinone concentrate, such as lanthanum, lanthanum and the like, and fluorine are one of suitable raw materials for the lanthanum-based abrasive. For example, a typical ratio of total rare earth oxides of fluorocarbon strontium ore is TBA0), a weight ratio of about 68 to 73% by weight, about 6 wt% of fluorine, and a strong heat loss (100%. 〇 is 20% by weight). In the TRE, the cerium oxide Ce02#) is about 5〇wt%, the cerium oxide (La2〇3, etc.) is about 35%, the oxygen is 〇H〇3, etc.)镨 (Pr6〇ii, etc.) is 4% left. However, as an abrasive, it is required to polish the material to the extent that the damage is not as high as possible. Further, it is preferable to carry out the grinding step and efficiently manufacture the article, and it is preferable to shorten the time required for the grinding step as much as possible. Such a material as the lanthanide abrasive material requires a polishing rate as high as possible (grinding value is large). Moreover, in recent years, lanthanum abrasive materials have been used for hard disk or magnetic hard disk.

2169-6322-PF(N2).ptd 第8頁 1303661 五、發明說明(2) 玻璃基板、活性矩陣型LCD(Liquid Crystal Display)、 液晶TV用彩色過濾器、時鐘、桌上型電子計算機、相機用 LCD、太陽電池等的顯示用玻璃基板、LSI光罩用玻璃基板 或光學用透鏡等的玻璃基板、或者光學用透鏡等的研磨, 這些領域中,特別需要能進行更高精度的表面研磨、且研 磨速度更南的飾系研磨材料。 但是,習知的鈽系研磨材料之研磨中,會發生無法滿 足光硬碟或磁硬碟用玻璃基板等研磨所要求的研磨精度之 大刮傷。且,研磨開始後,隨著研磨的進行研磨速度會急 ϋ下降,研磨效率會急速降低。這樣,習知的鈽系研磨材 料無法充分地滿足上述這些領域的要求。 【發明内容】 發明所欲解決的課題 鑒於以上的問題點,本發明以提供備有刮傷的發生更 ^專的優良研磨特性、研磨速度更高的鈽系研磨 題0 "解決上述課題的第1發明之鈽系研磨材料,至少含有 mi化:及氧化鈦作為稀土類氧化物、並含有氧, 上,® #王稀土類虱化物換算重量(tre〇)為9〇討%以 虱化鈽佔TRE0之重量比例(Ce〇2/TRE〇)係 5〇wt%〜65wt%,氧化歛佔TRE〇i ⑽ 10wt%〜16wt%。 1夕KM2U3/TREO)係 若使用該飾系研磨材料,可以得到研磨刮傷發生少2169-6322-PF(N2).ptd Page 8 1303661 V. INSTRUCTIONS (2) Glass substrate, liquid crystal display (LCD), color filter for liquid crystal TV, clock, desktop computer, camera In the field of polishing such as a glass substrate for display such as an LCD or a solar cell, a glass substrate for an LSI mask, or an optical lens, or an optical lens, it is particularly necessary to perform surface polishing with higher precision. And the polishing rate is more south. However, in the polishing of the conventional lanthanum-based abrasive material, there is a possibility that the scratch of the polishing precision required for the polishing of the optical hard disk or the glass substrate for the magnetic hard disk cannot be satisfied. Further, after the start of the polishing, the polishing rate is rapidly lowered as the polishing progresses, and the polishing efficiency is rapidly lowered. Thus, conventional lanthanide abrasive materials do not adequately meet the requirements of these fields. DISCLOSURE OF THE INVENTION PROBLEM TO BE SOLVED BY THE INVENTION In view of the above problems, the present invention provides a bismuth-based grinding problem in which the polishing performance is improved and the polishing rate is higher. The bismuth-based polishing material according to the first aspect of the invention contains at least a mi: and a titanium oxide as a rare earth oxide and contains oxygen, and the weight of the ruthenium-based bismuth compound (tre 〇) is 9%. The weight ratio of strontium to TRE0 (Ce 〇 2 / TRE 〇) is 5 〇 wt% to 65 wt%, and the oxidation occupies TRE 〇 i (10) 10 wt% 〜 16 wt%. 1 K KM2U3/TREO) If you use this decorative material, you can get less abrasive scratches.

2169-6322-PF(N2).ptd 第9頁 13036612169-6322-PF(N2).ptd Page 9 1303661

五、發明說明(3) 的、所要求的高精度之研磨面(被研磨面)。且,可以防止 7磨開始後研磨速度之急遽下降,能夠更長時間地維持更 咼的研磨速度。這樣,備有優良研磨特性之理由並不明 ,可旎主要係因為增加了研磨材中的鈥(氧化鈥)比例。 f知的鈽系研磨材料,其TRE0中的氧化鈥之比例係5 〇wt% 左右,若使用這樣的鈽系研磨材料,如先前說明的,刮傷 會發生,研磨速度會急劇地降低之故。 研磨材料中 含有氟之 物等的各種 較簡單地研 上,若在 素之比例一 最有助於研 速度。且由 可以更確實5. The high-precision polished surface (the surface to be polished) required by the invention (3). Further, it is possible to prevent a sharp drop in the polishing speed after the start of the 7-grinding, and it is possible to maintain a longer polishing speed for a longer period of time. Thus, the reason for having excellent polishing characteristics is not clear, and it is mainly because the ratio of bismuth (yttria) in the abrasive is increased. The ratio of yttrium oxide in TRE0 is about 5 〇wt%. If such a lanthanum-based abrasive is used, as described earlier, scratches will occur and the polishing rate will be drastically reduced. . Various types of materials such as fluorine contained in the abrasive material are relatively simple to study, and if the proportion of the element is high, the speed is most favored. And can be more sure

鈽系研磨材料中,一般會根據TRE〇來研討 的稀土類元素之量。本發明之研磨材料這樣, 物i稀土類元素係以氧化物、氟氧化物或氟化 形態存在於研磨材料中,若使用TRE〇,可以比 討研磨材料中的稀土類元素量。 上述發明之研磨材料中,TRE0係90wt %以 9jwt %以上則更理想。研磨材料中各稀土類元 定時二TRE0的比例越高,即是稀土類氧化物中 磨的氧化鈽之比例增加,能夠確保更高的研磨 於雜質(刮傷發生的原因之一)的含有率降低, 地防止刮傷的發生。Among the lanthanum abrasive materials, the amount of rare earth elements generally studied according to TRE〇. In the abrasive material of the present invention, the rare earth element is present in the abrasive in the form of oxide, oxyfluoride or fluorination. When TRE is used, the amount of the rare earth element in the abrasive can be compared. In the abrasive material of the above invention, it is more preferable that the TRE0 is 90% by weight or more and 9% by weight or more. The higher the proportion of the rare earth elements in the abrasive material, the higher the ratio of the TRE0, the higher the proportion of the cerium oxide that is ground in the rare earth oxide, and the higher the content of the polishing in the impurity (one of the causes of the scratch). Reduce, and prevent the occurrence of scratches.

但=’ TRE0中的氧化鈽之重量比例(Ce02/TRE0)越高, 刮傷越谷易發生,若超過上述上限值,容易發生要求高精 度研磨的前述領域中無法容許的研磨刮傷。另一方面,若 該比例越低,如上述這樣,研磨速度會下降,若未滿上述 I限值’則無法確保充分的研磨速度。考慮到這兩方面, 氧化鈽佔TRE0的重量比例(Ce02/TRE0)更好的係However, the higher the weight ratio (Ce02/TRE0) of yttrium oxide in the =' TRE0, the more likely the scratch is to occur, and if it exceeds the above upper limit, it is likely to cause scratches which are not allowed in the above-mentioned field requiring high-precision polishing. On the other hand, if the ratio is as low as described above, the polishing rate is lowered, and if the above-mentioned I limit is not satisfied, a sufficient polishing rate cannot be ensured. Considering these two aspects, yttrium oxide accounts for a better ratio of TRE0 (Ce02/TRE0).

1303661 五、發明說明(4) 50wt%〜60wt% 〇 、且TRE0中的氧化鈥之重量比例(Nd2〇3/TRE⑻越高,研 f速度會下降’ 1超過上述上限值’ %無法_保充分的研 ^速,另方面,氧化鉉之比例越低,刮傷越容易發 生,若未滿上述下限值,容易發生要求高精度研磨的前述 領域中無法容許的研磨刮傷。因此若考慮到這兩方面,氧 化鈥佔TRE0的重量比例(Nd2〇3/TRE〇)較好的係 llwt% 〜15wt% ’12wt% 〜14wt% 則更理想。 ΐ上,發明之鈽系研磨材料,氧化鑭佔全稀土類氧化 ,換算重里之重;^比例(La2〇3/TRE〇)最好係22wt%〜3〇wt% 〇 氧化鑭之比例越高研磨速度會下降,若超過上述上限值, 則無法確保充分的研磨速度。氧化鑭之比例若增加,則相 對地二氧化鈽的比例會減少,研磨速度會下降。另一方 面氧化鑭之比例越低越容易發生刮傷,若未滿上述的下 限值’在要求高精度研磨的前述領域,容易發生無法容許 的研磨刮傷。考慮到這兩方面,氧化鑭佔,㈣比例更好 的係24wt%~28wt%。 .另外,作為上述發明之鈽系研磨材料,含有氧化镨, 氧=镨佔TRE0之重量比例…八/咖㈨更好的係I 〇wt%〜& Owt% 〇 從以上的5己載可知,研磨材料中不僅有鈽,鑭及鈦也 :助:研磨,鍚]或鈥的含有量會對研磨狀態產生差異。因 、、$研讨鑭或歛的含有量與研磨之間的關係,想到 了與上述第1發明不同的第2發明。1303661 V. INSTRUCTIONS (4) 50wt%~60wt% 〇, and the weight ratio of yttrium oxide in TRE0 (the higher the Nd2〇3/TRE(8), the lower the research f speed '1 exceeds the above upper limit'% cannot be _ In addition, the lower the ratio of yttrium oxide, the more likely the scratch is to occur, and if it is less than the above lower limit, it is easy to cause scratches and scratches that are not allowed in the above-mentioned field requiring high-precision polishing. In both respects, the weight ratio of cerium oxide to TRE0 (Nd2〇3/TRE〇) is preferably llwt% 〜15wt% '12wt% 〜14wt%, more preferably. 发明, the invention is an abrasive material, oxidized.镧 occupies the total rare earth oxidation, the weight of the weight of the weight; ^ ratio (La2 〇 3 / TRE 〇) is preferably 22wt% ~ 3 〇 wt% 〇 〇 镧 镧 镧 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨 研磨If the ratio of cerium oxide is increased, the ratio of cerium oxide will decrease and the polishing rate will decrease. On the other hand, the lower the proportion of cerium oxide, the more likely the scratch will occur. The above lower limit 'is required for high precision grinding In the above-mentioned field, it is easy to cause an unacceptable polishing scratch. Considering these two aspects, the cerium oxide accounts for a ratio of 24% by weight to 28% by weight, and the cerium-based abrasive material of the above invention contains cerium oxide. Oxygen = 镨% by weight of TRE0... Eight/Cai (9) Better I 〇wt%~& Owt% 〇 From the above 5 loads, there are not only enamel, bismuth and titanium in the abrasive material: help: grinding The content of 钖 or 鈥 varies depending on the state of polishing. The second invention which is different from the first invention described above is conceivable because of the relationship between the content of the sputum and the sputum.

1303661 五、發明說明(5) 即是,第2發明之錦系研磨材料 氧化鋼及氧化敍作為稀土類氧化物、並含有氟:特:、在 rrvo /T'RF'm # ^ 物換异重量(TRE0)之重量比例 (Ce02/TRE0)係45wt%〜7〇wt%,TRE〇 ^ ^ ^ ^ ^ ^ ^ 鈥(ΜΑ)之重量比例(L 〇 ^化綱(La2〇3)與乳化 中負化鑭盥备π从 3 2 3 )係J·4〜2.8。這樣,TRE〇 中乳化鑭/、乳化鉉之重量比例在 研磨材料中鑭之量鱼敍之晉#nff圍内之研磨材科, 性優良。々里。斂之里的千衡良好’其結果,研磨特 π η該ί日^ 研磨材料令,氧化鑭與氧化鉉之上述重量比 ,3 2 3)若太大或者太小,研磨速度會 確保充分的研磨速度。從這點出發,該重量比 j,…法 (La2 03 / Nd2 03 )在 1 · 6 〜2 · 6 則更理想。 另外’氧化鑭與氧化歛的總重量佔TRE〇之比例 人的r園合换’則氧化鋼與氧化敛的總重量之比例,其適 SHi ί °之所以要在該範圍内,係比例越高研磨 ' "a降,右超過上述上限值,則無法確保充分的研磨 ΐίί故。Ϊ化鑭之比例若增加,則相對地,氧化鈽的比 :二^路:結果研磨速度會下降。另一方面,該比例越 L越今易發生刮傷,若未滿上述的下限值,在古 二磨的前述領域,容易發生無法容許的研磨刮傷二g】二 這兩方面,上述比例((La2〇3 + Nd2〇3)/TRE〇)更好 " 30wt°/〇〜45wt〇/〇。 若綜合以上的研討内容,最好係如下的鈽系研磨材料 第12頁 2169-6322-PF(N2).ptd 1303661 五、發明說明(6) (第3發明)。即是,至少含有氧化鈽、氧化鑭及氧化鈥作 為稀土類氧化物、並含有氣’其特徵在於’全稀土類氧化 物換算重量(TRE0)為90wt %以上,氧化鈽佔TRE0之重量比 例(Ce02/TRE0)係45wt%〜70wt%,氧化鈥佔TRE0之重量比例 (Nd2 03 /TRE0)係 10wt%〜16wt%,TRE0 中氧化鑭(La2 03 )與氧化 鈥(Nd2 03 )之重量比例(La2 03 /Nd2 03 )係1 · 4〜2· 8。更進一步 說,這樣的研磨材料,氧化鈽佔TRE0之重量比例 (Ce02/TRE0)更好的係50wt%〜65wt%,氧化鑭佔TRE0之重量 比例(La2 03 /TRE0)更好的係22wt%〜30wt%,氧化鑭與氧化 欽的總重量佔TRE0之比例((La2〇3 + Nd2 03 )/TREO)更好的係 25wt%〜50wt% 〇1303661 V. INSTRUCTION OF THE INVENTION (5) That is, the galvanized abrasive material of the second invention is oxidized steel and oxidized as a rare earth oxide and contains fluorine: special: in rrvo /T'RF'm #^ The weight ratio of weight (TRE0) (Ce02/TRE0) is 45wt%~7〇wt%, the weight ratio of TRE〇^^^^^^^鈥(ΜΑ)(L 〇^化纲(La2〇3) and emulsification The negative negative preparation π from 3 2 3 ) is J·4~2.8. In this way, the weight ratio of the emulsified 镧/, emulsified enamel in the TRE〇 is in the abrasive material, and the amount of the sputum in the grinding material is excellent. 々里. The weight of the balance is good. The result is that the grinding material is π η. The grinding material makes the above weight ratio of cerium oxide to cerium oxide. If the ratio is too large or too small, the grinding speed will ensure sufficient Grinding speed. From this point of view, the weight ratio j, ... method (La2 03 / Nd2 03 ) is more desirable at 1 · 6 to 2 · 6. In addition, the ratio of the total weight of yttrium oxide to oxidized enthalpy to the ratio of TRE 人 is the ratio of the total weight of oxidized steel to the oxidized aggregate. The reason why SHi ί ° is within this range is High grinding ' "a drop, right above the above upper limit, can not ensure sufficient grinding. If the proportion of bismuth bismuth is increased, the ratio of yttrium oxide is relatively: two ways: the polishing rate will decrease. On the other hand, the higher the ratio, the more likely the scratch will occur. If the lower limit value is not exceeded, the above-mentioned field in the second mill will be prone to unacceptable polishing scratches. ((La2〇3 + Nd2〇3)/TRE〇) Better " 30wt°/〇~45wt〇/〇. In the case of the above discussion, it is preferable to use the following lanthanide abrasive materials. Page 12 2169-6322-PF(N2).ptd 1303661 V. Description of the invention (6) (3rd invention). That is, at least cerium oxide, cerium oxide, and cerium oxide are contained as a rare earth oxide and contain a gas, which is characterized in that the total weight of the rare earth oxide (TRE0) is 90% by weight or more, and the weight ratio of cerium oxide to TRE0 ( Ce02/TRE0) is 45wt%~70wt%, the weight ratio of cerium oxide to TRE0 (Nd2 03 /TRE0) is 10wt%~16wt%, and the weight ratio of lanthanum oxide (La2 03 ) to yttrium oxide (Nd2 03 ) in TRE0 ( La2 03 /Nd2 03 ) is 1 · 4~2· 8. Furthermore, in such an abrasive material, the weight ratio of cerium oxide to TRE0 (Ce02/TRE0) is preferably 50% by weight to 655% by weight, and the weight ratio of cerium oxide to TRE0 (La2 03 /TRE0) is more preferably 22% by weight. 〜30wt%, the total weight of cerium oxide and oxidized oxime in the ratio of TRE0 ((La2〇3 + Nd2 03 ) / TREO) is more preferably 25wt% ~ 50wt% 〇

而且,對研磨特性的提高進一步作了研討,得到以下 結果。即是,作為上述各發明之研磨材料,無論哪一種發 明之研磨材料,氟相對於全稀土類氧化物換算重量之重量 比(F/TRE0)最好在4· 〇wt%〜9· Owt %。氟的比例越高,研磨 面的狀態越粗糙,研磨特性會下降,若超過上述上限值, 在要求高精度研磨的前述領域,容易發生無法容許的研磨 面之粗链化。認為這是氟量過剩而產生強化學作用之結 果。另一方面,氟的比例越低,研磨速度會下降若未滿上 述下限值,則無法確保足夠的研磨速度。氟量少則產生有 助於研磨的化學作用小之故。且從這兩方面考慮、,氣相對 於TRE0之重I比(F/TRE0)在5· 〇wt%〜8· 〇wt %則更理想。且 含有氟之鈽系研磨材料中,稀土類元素的一部分(或者全 部)不是作為稀土類氧化物,而是作為氟氧化物或貌化物Further, the improvement of the polishing characteristics was further studied, and the following results were obtained. In other words, as the polishing material of each of the above inventions, the weight ratio of fluorine to the total rare earth oxide equivalent weight (F/TRE0) is preferably 4·〇wt% to 9·0 wt%. . The higher the ratio of fluorine, the coarser the state of the polishing surface, and the lower the polishing property. When the above-mentioned upper limit is exceeded, the above-mentioned field requiring high-precision polishing tends to cause unacceptable roughening of the polishing surface. This is considered to be the result of a strong chemical action caused by excess fluorine. On the other hand, the lower the ratio of fluorine, the lower the polishing rate. If the lower limit is not satisfied, a sufficient polishing rate cannot be ensured. When the amount of fluorine is small, the chemical action which contributes to the grinding is small. Considering these two aspects, the weight ratio of gas to TRE0 (F/TRE0) is more preferably 5·〇wt%~8·〇wt%. Further, in the fluorine-containing lanthanum-based abrasive, a part (or all) of the rare earth element is not used as a rare earth oxide but as a oxyfluoride or a surface oxide.

五、發明說明(7) =量=。;=?飾系研磨材料之全稀土類氧化物 稀土類氧化物,在貝元素換算成作為 ί材:r所謂的心 磨材料中的氟含有量。 、』里對象之鈽糸研 相對稀ίΐί!:之鈽系研磨材#,触與灶的總重量 t ^ ^0. 〇5wt% ,χ Τ *;b^U^h)/TREO) 或轴等的放射性物質最好疋儘因可為能飾地系少研磨因材料中所/β的处 ^i:o.〇r ,各發月之鈽系研磨材料,研磨材料番旦盥命 材料的TREO及氟含有量的總 :==磨 ^ t t) t ^ ^95wt^l 〇5wt ί t " t 1 } ^ 成會降低’若超過上述上限值,會形 法容許的粗糙研磨面之故。若該重量二 ;。另=過剩’ f生強化學作用,結果使研磨面變粗 ^ ,該重1比越低,研磨刮傷越容易發生,若 限!,則容易產生前述領域中無法容許的研: 之故装里比低的主要原®,認為是含有較多的雜質 旦ί宙ί易發生刮傷。若考慮到這兩方面,上述重 里比更好的係98wt%〜104wt%。 另外,對上述各發明之鈽系研磨材料,用义射線繞射 :析進行研討’得到以下這樣的結果。作為上述各發明之 鈽糸研磨材料’藉由使用Cu_Ka線或^“丨線作為χ射線 1303661 五、發明說明(8) 源之X射線繞射法測量,在2 0 (繞射角)=2 〇。〜3 〇。的範圍 出現的X射線繞射峰中,稀土類氟氧化物(Ln〇|?)之X射線繞 射峰強度中最強的X射線繞射峰強度,與氧化鈽(Ce〇2)之X 射線繞射峰強度中最強的X射線繞射峰強度之強度比 (LnOF/ Ce02)最好係 〇·4 〜0.7。 該X射線繞射峰強度比越大,越容易發生研磨刮傷, 若超過上述上限值,容易發生前述領域中無法容許的研磨 刮傷。另一方面,X射線繞射峰強度比越小,研磨速度會 下降’若未滿上述的下限值,則無法確保充分的研磨速 度。若考慮到這兩方面,X射線繞射峰強度比更好的係 0· 45〜0· 65 〇 ’、 且作為上述各發明之鈽系研磨材料,藉由使用Cu — Ka 線或Cu-K &線作為X射線源之X射線繞射法測量,在2 0(繞 射角)=24.2。±〇.5。的範圍出現的稀土類氟化物(1^^: X射線繞射峰強度中最強的X射線繞射峰強度,與氧化 X射線繞射峰強度中最強的X射線繞射峰強度之/強 ' 6/ Ce〇2)最好係在ο.】以下。這裡所指的稀土類氣"化物 anF3j,係例如含有稀土類氧化物的原料,在研磨材料製 造階段’對該原料實施氟化處理後所生成之物。 因此,該X射線繞射峰強度比超過上述上限 形,有由於焙燒不足,使稀土類氟化物未能轉換 Θ t化物,而作為稀土類氧化物殘留之情形,或者培燒雖 二!2=:匕物變成稀土類氟氧化物之轉換係有限 的乱相對於稀土類元素有過剩之故,而使稀土類氣化物V. Description of invention (7) = quantity =. ;=? All rare earth oxides of the abrasive materials. Rare earth oxides, which are converted into shellfish in terms of fluorine content in the so-called heart-grinding material. , "The object of the research is relatively thin ίΐί!: The 钸 is the abrasive material #, the total weight of the touch stove t ^ ^ 0. 〇 5wt%, χ Τ *; b ^ U ^ h) / TREO) or shaft It is best to use the radioactive material of the material to reduce the amount of the material in the material. The surface of the material is βi: o.〇r, the abrasive material of each month, and the material of the material. Total of TREO and fluorine content: ==磨^ tt) t ^ ^95wt^l 〇5wt ί t " t 1 } ^ The formation will decrease 'If the above upper limit is exceeded, the roughness of the rough surface will be allowed Therefore. If the weight is two; Another = excess 'f strong chemical action, the result is that the polished surface becomes thicker ^, the lower the weight ratio, the more likely the grinding scratches will occur, if any! It is easy to produce research that cannot be tolerated in the above-mentioned fields: The main original® which is low in the ratio of the inside is considered to contain more impurities. If these two aspects are considered, the above ratio is preferably 98% by weight to 104% by weight. Further, the ruthenium-based abrasive materials of the above-described respective inventions were subjected to the analysis of the diffraction of the right ray to obtain the following results. The crucible abrasive material of the above inventions is measured by X-ray diffraction method using a Cu_Ka line or a "twist line as a x-ray ray 1303661", the invention (8) source, at 20 (diffraction angle) = 2 〇.~3 〇. The X-ray diffraction peak in the range of X-ray diffraction peak intensity, the strongest X-ray diffraction peak intensity of rare earth oxyfluoride (Ln〇|?), and yttrium oxide (Ce强度 2) The intensity ratio of the strongest X-ray diffraction peak intensity (LnOF/ Ce02) of the X-ray diffraction peak intensity is preferably 〇·4 to 0.7. The larger the X-ray diffraction peak intensity ratio, the easier it is to occur. If the scratch is excessively exceeded, the above-mentioned upper limit value is liable to cause scratching which is unacceptable in the above-mentioned field. On the other hand, the smaller the X-ray diffraction peak intensity ratio, the lower the polishing rate, if the lower limit value is not exceeded. However, sufficient polishing speed cannot be ensured. If these two aspects are considered, the X-ray diffraction peak intensity ratio is better than 0·45~0·65 〇', and as the lanthanide abrasive material of each of the above inventions, X-ray diffraction method using a Cu-Ka line or a Cu-K & line as an X-ray source, at 20 (wound The angle of incidence = 24.2. The range of ± 〇.5. The rare earth fluoride (1 ^ ^: X-ray diffraction peak intensity of the strongest X-ray diffraction peak intensity, and the strongest oxidized X-ray diffraction peak intensity The intensity of the X-ray diffraction peak/strong '6/ Ce〇2) is preferably hereinafter. The rare earth gas referred to herein is a raw material containing a rare earth oxide, for example, in the grinding. In the material production stage, the material produced by the fluorination treatment is applied to the raw material. Therefore, the X-ray diffraction peak intensity ratio exceeds the above upper limit shape, and the rare earth fluoride cannot be converted into the ruthenium compound due to insufficient calcination. In the case of residual rare earth oxides, or the second generation of 2:2 =: the conversion of the rare earth oxyfluoride is limited, and the rare earth vaporization is excessive with respect to the rare earth element.

2169-6322-PF(N2).ptd 第15頁 1303661 五、發明說明(9) 殘留之情形。焙燒不足的研磨材料無法確保八 度,所以不合適。另一方面,經過充分焙燒、分,:磨速 的研磨材料,相對地含有較多的粗粒子(研^磨$而氣量過剩 因也並不適合。含有的氣量相對過剩的研=原 磨材料製造時的焙燒階段中,氟的化學作用&针/研 產生粗粒子(因研磨材料粒子之燒結過唐而士 & 曰 幻厌肉成為研磨刮傷 之原因)。且該研磨材料由於氟量相對地過剩,楊 焙燒後的粉碎或分級充分地降低了粗粒手,枯m 吏經過 1文用該研磨材 料之研磨中,研磨面會受到過剩的氟之化學作用, 生要求高精度研磨的前述領域中無法容許的研磨面之^ 化。 〒植 且用於上述峰強度比之計算的氧化鈽(Ce02)之X射線繞 射峰’指的是以鈽為主成分的稀土類氧化物 峰,係、在20=28.!。±1.〇。的範圍内出現的X射射線^射射 峰。 且這裡所謂的氧化鈽(Ce〇2)之X射線繞射峰強度,更具 體的,指的是以鈽為主成分的立方晶稀土類氧化物“ηχ〇/)' 之X射線繞射峰強度。Lnx〇y係通常15^γ/χ^2,鑑定^列 如Ce02、CeQ5NdQ 5 01 75、或CeusNdusOuu。但是,即使是2169-6322-PF(N2).ptd Page 15 1303661 V. INSTRUCTIONS (9) Residual conditions. An abrasive material that is insufficiently baked cannot be guaranteed to be octave, so it is not suitable. On the other hand, the abrasive material which has been sufficiently calcined, divided, and milled at a relatively high rate contains relatively large amount of coarse particles (it is not suitable for the excessive amount of gas and the amount of gas contained is excessively large. In the roasting stage of the time, the chemical action of fluorine & needle/grinding produces coarse particles (since the sintered material particles are sintered by Doners & 曰 厌 厌 成为 成为 成为 成为 成为 成为 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 Relatively excessive, the pulverization or classification after the roasting of the yang is sufficiently reduced by the coarse granules. In the grinding of the abrasive material, the polishing surface is subjected to the chemical action of excess fluorine, which requires high-precision grinding. In the above-mentioned field, the surface of the polished surface which cannot be tolerated is determined. The X-ray diffraction peak of cerium oxide (Ce02) which is used for the calculation of the peak intensity ratio described above refers to the rare earth oxide peak which is mainly composed of cerium. , X-ray radiation peak appearing in the range of 20=28.!.±1.〇. And the so-called X-ray diffraction peak intensity of cerium oxide (Ce〇2), more specific , refers to cubic thinning based on bismuth Based oxide "ηχ〇 /) 'of the X-ray diffraction peak intensity .Lnx〇y lines are usually 15 ^ γ / χ ^ 2, ^ column identified as Ce02, CeQ5NdQ 5 01 75, or CeusNdusOuu. However, even

Nc^Os/TREO小的研磨材料,也可能被鑑定為Ce—Nd —〇系化合 物之故’被推測為同時含有Ce或Nd以外的稀土類元素(La 等)之氧化物。從以上的所述可知,對於X射線繞射,氧化 飾(Ce〇2)之情形,與TREO中的Ce02指的是純粹的氧化鈽不 同,這裡可以不是純粹的氧化鈽。An abrasive material having a small Nc^Os/TREO may be identified as a Ce-Nd-lanthanide compound. It is presumed to contain an oxide of a rare earth element (La or the like) other than Ce or Nd. As apparent from the above, in the case of X-ray diffraction, the case of oxidized decoration (Ce 〇 2) is different from that of pure yttrium oxide in the case of Ce02 in TREO, and may not be pure yttrium oxide.

1303661 五、發明說明(10) 且上述各么明之鈽系研磨 下述值。即是,使用裡平均粒徑(心)使用 測量的鈽系研磨材料= 亂法粒度分布測量法所 容易發生研磨到傷若^ Λ粒徑(D5d )越大,越 =二,f的别述領域中無法容許的研磨刮傷。另一方面, 平均粒控(D )越小’研磨 ^ . #,M H # π t Y 會降,右未滿上述的下限 -二 的研磨速度。若考慮到這兩方面,平 均粒徑〇>50)更好的係〇.8"111〜1.4/^。 十 品隹作為上述各發明之飾系研磨材料’ΒΕΤ法比表 ® JJ^#2.〇m2/g.5.〇m2/g 、、=s下降,若超過上述上限值,則無法確保充分的研磨 1 ΐ之ί。另一方面,謝法比表面積越小,㉟容易發生 it,右未滿上述的下限值,容易發生要求高精度研磨的 刖述領域中無法容許的研磨刮傷。若考慮到這兩方面, ΒΕΤ法比表面積更好的係2. 5mVg〜4. OmVg。 接著’研討鈽系研磨材料用的原料。 蛛 ^述發明之鈽系研磨材料中,對於全稀土類氧化物換 算重K(TREO)之重量比為9〇wt %以上,氧化鈽佔TRE〇之比 例(Ce02/TRE0)係5〇wt%〜65wt%,氧化鈥佔TRE0之比例 (Nd2 03 /TRE0)係1 〇wt%〜1 6wt%之鈽系研磨材料(第1發明), 其原料(第4發明)係至少含有鈽、鑭及鈥作為稀土類元素 之飾系研磨材料用原料,其特徵在於,氧化鈽佔TRE0之重 第17頁 2169-6322-PF(N2).ptd 1303661 —1^———...... 五、發明說明(11) —- 量比例(Ce02/TRE0)係50wt%〜65wt%,氧化欽佔treo 日 比例(Nd203 /TRE0)係10wt%〜16wt%,轴與处的總重量m TRE0 之重量比((U + Th)/TRE0)在 0· 〇5wt〇/0 以下。 $ ; 該鈽系研磨材料用原料,伴隨著TRE〇中氧化鈽之比 (CeOz/TREO)的升高,製造出的研磨材料容易發生刮傷,若 超過上述上限值,容易發生要求高精度研磨的前述領域^ 無法容許的研磨刮傷。另一方面,氧化鈽之比例越低,製 造出的研磨材料之研磨速度會下降,若未滿上述下限值, 則難以確保充分的研磨速度。因此,若考慮到這兩方面, 氧化鈽佔TRE0之重量比例(Ce02/TRE0)更好的係 50wt%〜60wt%。一方面對氧化鈥之情形,其重量比例越 高’製造出的研磨材料之研磨速度會下降,若超過上述上 限值,則難以確保充分的研磨速度。另一方面,氧化敍之 比例越低,·製造出的研磨材料容易發生刮傷,若未滿上述 的下限值,容易發生要求高精度研磨的前述領域中無法容 許的研磨刮傷。因此,若考慮到這兩方面,氧化鈥佔TRE〇 之重量比例(Nd2 03 /TRE0)更妤的係llwt%〜15wt%, 12wt%〜14wt%則更理想。 且TRE0與轴及鉦的總重量之重量比((u + Th)/TRE〇)最 好在上述範圍内之理由,係鈾或钍等的放射性物質最好儘 可月b少之故。氟碳鈽精礦、獨居石精礦、中國複雜礦精礦 等的礦石(特別係獨居石精礦及中國複雜礦精礦),含有較 多的灶’不除去轴及鉦,直接作為研磨材料用原料使用並 不合適。因此’該重量比((u + Th)/TRE〇)在〇· 00 5wt%以下1303661 V. INSTRUCTIONS (10) The above-mentioned values are the following values. That is, using the measured average particle size (heart) using the measured lanthanide abrasive material = chaotic particle size distribution measurement method is prone to grinding to the injury if the Λ particle size (D5d) is larger, the more = two, f Unacceptable abrasive scratches in the field. On the other hand, the smaller the average grain size (D) is, the smaller the grinding rate is. #, M H # π t Y will fall, and the right is less than the lower limit of the above - two. If these two aspects are taken into consideration, the average particle size 〇 > 50) is better than 88 "111~1.4/^. Shipin 隹 is a material for the above-mentioned various inventions. The ΒΕΤ法比表® JJ^#2.〇m2/g.5.〇m2/g and =s are decreased. If the above upper limit is exceeded, it cannot be ensured. Fully grind 1 ί. On the other hand, the smaller the Xiefa specific surface area, the easier it is to generate 35, and the lower limit is not satisfied by the above, and it is easy to cause scratches and scratches that are not allowed in the field of high-precision polishing. 5mVg〜4. OmVg。 Having a better specific surface area of 2. 5mVg~4. OmVg. Next, we will discuss the raw materials for the abrasive materials. In the bismuth-based abrasive material of the invention, the weight ratio of the total rare earth oxide to the weight K (TREO) is 9 〇 wt% or more, and the ratio of cerium oxide to TRE ( (Ce02/TRE0) is 5 〇 wt%. ~65 wt%, the ratio of cerium oxide to TRE0 (Nd2 03 /TRE0) is 1% by weight to 1% by weight of the lanthanum-based abrasive (first invention), and the raw material (fourth invention) contains at least lanthanum, cerium and原料 As a raw material for a rare earth element, it is characterized in that yttrium oxide accounts for the weight of TRE0. Page 17 2169-6322-PF(N2).ptd 1303661 —1^———...... , invention description (11) --- quantitative ratio (Ce02 / TRE0) is 50wt% ~ 65wt%, oxidation of the proportion of treo day (Nd203 / TRE0) is 10wt% ~ 16wt%, the total weight of the shaft and the weight of m TRE0 The ratio ((U + Th)/TRE0) is below 0·〇5wt〇/0. $ ; The raw material for the abrasive material, with the increase in the ratio of cerium oxide (CeOz/TREO) in the TRE ,, the abrasive material is easily scratched, and if it exceeds the above upper limit, high precision is likely to occur. The aforementioned field of grinding ^ unacceptable abrasive scratches. On the other hand, the lower the ratio of cerium oxide, the lower the polishing rate of the produced abrasive, and if the lower limit is not satisfied, it is difficult to ensure a sufficient polishing rate. Therefore, in consideration of these two aspects, the weight ratio of cerium oxide to TRE0 (Ce02/TRE0) is preferably 50% by weight to 60% by weight. On the other hand, in the case of cerium oxide, the higher the weight ratio is, the polishing rate of the manufactured abrasive material is lowered, and if it exceeds the above upper limit, it is difficult to ensure a sufficient polishing rate. On the other hand, the lower the ratio of oxidized, the scratches to be produced are likely to be scratched, and if the lower limit is not satisfied, it is likely to cause scratches that cannot be tolerated in the above-described field requiring high-precision polishing. Therefore, in consideration of these two aspects, the weight ratio of cerium oxide to TRE ( (Nd2 03 /TRE0) is more preferably llwt% to 15% by weight, and 12% by weight to 14% by weight is more preferable. Further, the reason why the weight ratio of TRE0 to the total weight of the shaft and the crucible ((u + Th)/TRE〇) is preferably within the above range is that the radioactive material such as uranium or thorium is preferably as small as possible. Bastrite concentrate, monazite concentrate, complex ore concentrates in China (especially monazite concentrates and complex mineral concentrates in China), containing more stoves 'do not remove shafts and sputum, directly as It is not suitable to use the raw materials for the abrasive materials. Therefore, the weight ratio ((u + Th)/TRE〇) is less than 00 00 5 wt%

2169-6322-PF(N2).ptd 第18頁 13036612169-6322-PF(N2).ptd Page 18 1303661

之原料更好,在〇· 〇〇〇5wt%以下之原料則更理想。 且氧化鑭佔TREO的重量比例(La^/TREO)最好係 2 2wt%〜30wt%。且該比例為24wt%〜28wt%則更理想。氧化鑭 之比例越低,焙燒時的氟放出量容易變大,若未滿上述下 限值,則會過分地容易放出,在焙燒時難以控制鈽系 材料中的氟量之故。 上述發明之研磨材料中,對於氧化鈽佔全稀土類氧化 物換算重量(TREO)之重量比例(Ce02/TRE0)係 45wt%〜7 0wt°/。,TREO中氧化鑭(La2 03 )與氧化鈦(Nd2〇3)之重 里比例(L a2 03 / N d2 03 )係1 · 4〜2. 8之鈽系研磨材料(第2發 明),作為其原料(第5發明)係至少含有鈽、鑭及鈥作為稀 土類元素之鈽系研磨材料用原料,其特徵在於,之重 量比例(Ce02/TRE0)係45wt%〜70wt%,TREO中氧化鑭與氧化 鈥之重量比例(La2 03 /Nd2 03 )係1· 4〜2· 8。 該鈽糸研磨材料用原料’若T R E 0中氧化鈽之重量比例 (Ce〇2/TREO)升高,製造出的研磨材料容易發生刮傷,若超 過上述上限值,容易發生要求高精度研磨的前述領域中 * ivfy 法容許的研磨刮傷。另一方面,氧化鈽之比例越低,製造 出的研磨材料之研磨速度會下降,若未滿上述下限值,則 難以確保充分的研磨速度。因此,若考慮到這兩方面,氧 化鈽佔TREO之重量比例(Ce02/TREO)更好的係 50wt%〜60wt%。且氧化鑭與氧化鈥之重量比例(La2 03 /Nd2〇3) 太大或太小,製造出的研磨材料之研磨速度會下降,無法 確保充分的研磨速度。因此,TREO中氧化鑭與氧化鈥之重The raw materials are better, and the raw materials below 5 wt% of 〇·〇〇〇 are more desirable. Further, the weight ratio of cerium oxide to TREO (La^/TREO) is preferably from 2 2% by weight to 30% by weight. Further, the ratio is preferably from 24% by weight to 28% by weight. The lower the ratio of cerium oxide, the larger the amount of fluorine released during firing, and the excessively low amount is likely to be excessively released, and it is difficult to control the amount of fluorine in the lanthanoid material during firing. In the abrasive material of the above invention, the weight ratio (Ce02/TRE0) of the cerium oxide to the total rare earth oxide equivalent weight (TREO) is 45 wt% to 70 wt%. The ratio of the weight ratio of lanthanum oxide (La2 03 ) to titanium oxide (Nd2〇3) in TREO (L a2 03 / N d2 03 ) is 1 / 4 to 2. 8 钸 abrasive material (second invention) as its The raw material (the fifth invention) is a raw material for an antimony-based polishing material containing at least lanthanum, cerium and lanthanum as a rare earth element, wherein the weight ratio (Ce02/TRE0) is 45 wt% to 70 wt%, and ruthenium oxide in TREO The weight ratio of cerium oxide (La2 03 /Nd2 03 ) is 1·4~2·8. When the raw material of the crucible polishing material is increased in weight ratio (Ce〇2/TREO) in the TRE 0, the produced abrasive material is likely to be scratched. If the above-mentioned upper limit value is exceeded, high-precision grinding is likely to occur. In the aforementioned field, the *ivfy method allows for abrasive scratches. On the other hand, the lower the ratio of cerium oxide, the lower the polishing rate of the manufactured abrasive material, and if the lower limit is not satisfied, it is difficult to ensure a sufficient polishing rate. Therefore, in consideration of these two aspects, the proportion of cerium oxide in the weight ratio of TREO (Ce02/TREO) is preferably 50% by weight to 60% by weight. Further, the weight ratio of cerium oxide to cerium oxide (La2 03 /Nd2 〇 3) is too large or too small, and the polishing rate of the manufactured abrasive material is lowered to ensure a sufficient polishing speed. Therefore, the weight of yttrium oxide and yttrium oxide in TREO

1303661 五、發明說明(13) 量比例(La2 03 /Nd2 03 )係1· 6〜2. 6則更理想。 且丁1^0與轴及鉦的總重量之重量比((1| + 1^)/1^£:〇)最 好在0· 0 5wt%以下。這是鈾或钍等的放射性物質最好儘可 能少的緣故。氟碳鈽精礦、獨居石精礦、中國複雜礦精礦 等的礦石(特別係獨居石精礦及中國複雜礦精礦),含有較 多的钍’不除去鈾及钍而直接作為研磨材料用原料使用並 不適合。因此,該重量比((U + Th)/TRE0)在0· 00 5wt%以下 之原料更好,在〇. 〇 〇 〇 5 w t %以下之原料則更理想。 且氧化鑭與氧化鈥的總重量佔TRE0之比例((La2 03 + N d2 03 ) / T R E 0 )最好係2 5 w t %〜5 0 w t %。該比例越低,培燒時的 氟放出量容易變大,若未滿上述下限值,則會過分地容易 放出,在焙燒時難以進行鈽系研磨材料中氟量的控制之 故。 另外,上述發明之研磨材料中,至少含有氧化鈽、氧 化鑭及氧化鈥作為稀土類氧化物、並含有氟之鈽系研磨材 料,全稀土類氧化物換算重量(TRE0)為90wt %,氧化飾你 TRE0之重量比例(Ce02/TRE0)係45wt%〜70wt%,氧化鈦佔 TRE0 之重量比例(Nd2 03 /TRE0)係 10wt%〜16wt%,TRE0 中氧化 鑭(La2 03 )與氧化鈦(Nd2 03 )之重量比例(La2 03 /Nd2 03 )係 1· 4〜2. 8之鈽系研磨材料(第3發明),作為其原料(第6發 明)’係至少含有鈽、鑭及鈥作為稀土類元素之鈽系研磨 材料用原料,其特徵在於,TRE0係90wt%以上,氧化鈽佔 TRE0之重量比例(Ce02/TRE0)係45wt%〜70wt%,氧化歛佔 TRE0 之重量比例(Nd2 03 /TRE0)係 10wt°/。〜16wt%,TRE0 中氧化1303661 V. Description of invention (13) The ratio (La2 03 /Nd2 03 ) is 1·6~2. 6 is more desirable. The weight ratio of (1) to the total weight of the shaft and the crucible ((1| + 1^)/1^£: 〇) is preferably 0. 0 5 wt% or less. This is because the radioactive material such as uranium or plutonium is preferably as low as possible. Bastrite concentrates, monazite concentrates, complex ore concentrates in China (especially monazite concentrates and complex mineral concentrates in China), containing more 钍' without removing uranium and plutonium The use of raw materials for abrasive materials is not suitable. Therefore, the weight ratio ((U + Th) / TRE0) is preferably 0. 00 5 wt% or less, and the raw material of 〇. 〇 〇 〇 5 w t % or less is more preferable. Further, the ratio of the total weight of cerium oxide to cerium oxide to TRE0 ((La2 03 + N d2 03 ) / T R E 0 ) is preferably 2 5 w t % 〜 5 0 w t %. The lower the ratio, the larger the amount of fluorine released during the calcination, and the more easily the above-mentioned lower limit is excessively released, and it is difficult to control the amount of fluorine in the lanthanum-based abrasive during baking. In addition, the polishing material of the above invention contains at least cerium oxide, cerium oxide, and cerium oxide as a rare earth oxide and a fluorine-containing cerium-based abrasive, and the total rare earth oxide conversion weight (TRE0) is 90% by weight. The weight ratio of your TRE0 (Ce02/TRE0) is 45wt%~70wt%, the weight ratio of titanium oxide to TRE0 (Nd2 03 /TRE0) is 10wt%~16wt%, and the lanthanum oxide (La2 03 ) and titanium oxide (Nd2) in TRE0 03) The weight ratio (La2 03 /Nd2 03 ) is a bismuth-based polishing material (third invention), and the raw material (the sixth invention) contains at least lanthanum, cerium and lanthanum as rare earths. The lanthanum-based material for the abrasive material is characterized in that the TRE0 system is 90% by weight or more, the cerium oxide accounts for the weight ratio of TRE0 (Ce02/TRE0) is 45 wt% to 70 wt%, and the oxidation ratio accounts for the weight ratio of TRE0 (Nd2 03 / TRE0) is 10wt ° /. ~16wt%, oxidation in TRE0

2169-6322-PF(N2).ptd 第 20 頁 1303661 五、發明說明(14) 鑭(La2 03 )與氧化鈥(Nd2 03 )之重量比例(La2 03 /Nd2 03 )係 1· 4〜2· 8。更進一步,這樣的原料,氧化鈽佔TRE0之重量 比例(Ce02/TRE0)係50wt%〜65wt%,氧化鑭佔TRE0之重量比 例(La2 03 /TRE0)係22wt%〜30wt%,氧化鑭與氧化鈥的總重量 佔TRE0 之比例((La2 03 + Nd2 03 )/TRE0) 25wt%〜50wt%則更理 想。且,該原料中,基於上述同樣的理由,TRE0與鈾及鉦 的總重量之重量比((U + Th)/TRE0)最好在〇.〇5wt%以下,在 0.005wt%以下之原料更好,在〇.〇〇〇5wt%以下之原料則更 理想。 上述發明之釗j系研磨材料用原料,無論任何一項發明 之原料’其中,氧化镨佔TRE0之重量比例(pr6〇n / TRE〇)最 好係2· 〇wt%〜8. Owt%。 且先前談到原料中所含的鈾或钍等的放射性物質,研 磨材料用原料之礦石中,除此以外,還較多地含有詞 (Ca)、鋇(Ba)、鐵(Fe)、磷(p)等元素。從這樣的含有多 種元素之礦石(原料)中製造出的研磨材料,較多地將這些 ^分作為雜質含有,若使用較多地含有這些雜質的研磨材 料’容易發生研磨刮傷,且研磨速度會下降。且若這些雜 質(特別係鐵)殘留於研磨面等,可能使研磨對象&特 性或=特性降低。從這點出*,關於上述原= = 任何項,作為本發明之鈽系研磨材料用原料及鈽系研磨 材料’ TREp與鈣、鋇、鐵、磷的總重量之重量比 ((Ca + Ba + Fe + P)/TRE〇)最好在 2.0wt% 以下,在 1〇wt% 以下 更好,在〇.5wt%以下則更理想,且作為其原料,該重量比2169-6322-PF(N2).ptd Page 20 1303661 V. INSTRUCTIONS (14) The weight ratio of lanthanum (La2 03 ) to yttrium oxide (Nd2 03 ) (La2 03 /Nd2 03 ) is 1·4~2· 8. Further, in such a raw material, the weight ratio of cerium oxide to TRE0 (Ce02/TRE0) is 50% by weight to 655% by weight, and the weight ratio of cerium oxide to TRE0 (La2 03 /TRE0) is 22% by weight to 30% by weight, cerium oxide and oxidation. The ratio of the total weight of the crucible to the TRE0 ((La2 03 + Nd2 03 ) / TRE0) is preferably from 25 wt% to 50 wt%. Further, in the raw material, for the same reason as described above, the weight ratio of TRE0 to the total weight of uranium and lanthanum ((U + Th) / TRE0) is preferably 5% by weight or less, and less than 0.005% by weight of the raw material. Well, it is more desirable to use less than 5% by weight of raw materials. The above-mentioned invention is a raw material for the abrasive material, in any one of the raw materials of the invention, wherein the weight ratio of cerium oxide to TRE0 (pr6〇n / TRE〇) is preferably 2·〇wt%~8. In addition to the radioactive materials such as uranium or thorium contained in the raw materials, the ore of the raw material for the abrasive material contains, in addition, the words (Ca), barium (Ba), iron (Fe), and phosphorus. (p) and other elements. The polishing material produced from such a multi-element ore (raw material) is often contained as an impurity, and if an abrasive containing a large amount of these impurities is used, polishing scratches are likely to occur, and the polishing speed is high. Will fall. Further, if these impurities (especially iron) remain on the polished surface or the like, the properties and properties of the object to be polished may be lowered. From this point, regarding the above-mentioned original == any item, as the raw material of the bismuth-based abrasive material of the present invention and the weight ratio of the lanthanide-based abrasive material 'TREp to the total weight of calcium, barium, iron, and phosphorus ((Ca + Ba) + Fe + P)/TRE〇) is preferably 2.0 wt% or less, more preferably 1 wt% or less, more preferably 〇 5 wt% or less, and as a raw material thereof, the weight ratio

1303661 五、發明說明(15) ((Ca + Ba + Fe + P)/TRE0)最好在 2.〇wt% 以下,在 l.Owt% 以下 更好,在0· 5wt%以下則更理想。 作為鈽系研磨材料用原料之製造方法,大致有以下這 樣的方法(原料之第1製造方法)。 、 首先’將氟礙鈽精礦等的精礦用硫酸分解法或鹼分解 法分解’經過分別沉澱或分別溶解等的處理,藉由減少· 除去轴、鼓、辦、鋇、鐵、磷等的雜質得到稀土類溶液。 並且调整所得的稀土類溶液之稀土類成分的組成(稀土類 組成调整)。其後,將組成經過調整的稀土類溶液與沉澱 劑(例如碳酸氫銨、碳酸銨、碳酸氫鈉、碳酸鈉、氨水、 草酸、草酸銨、草酸鈉、尿素等)混合,生成稀土類化合 物(例如碳酸鹽、鹼性碳酸鹽、一羥基碳酸鹽、氫氧化 物、草酸鹽等)的沉澱,將其過濾•水洗,得到本發明之 鈽系研磨材料用原料。 鈽系研磨材料用原料製造時,作為稀土類溶液(減少 :除去雜質後)之組成調整方法,有溶劑萃取法與添加 2。溶劑萃取法中’根據使用的方法也能一定程 稀土類元素以外的雜質。且也可 組合起來使肖。 也了以將溶劑卒取法與添加法 首先,說明溶劑萃取法。也丨丄 、 ^ 鈥之比例(Nd203 /TRE0)高的情· α,溶劑萃取前的溶液中 氧化欽之重量比aa2〇3/N(^二J該溶液中的氧化鑭與 法,可以列舉出以下;所:吏用的溶劑萃取 將鈦的-部分萃取至有機溶劑p疋’從稀土類水溶液 W之方法,或者將稀土類元素1303661 V. Inventive Note (15) ((Ca + Ba + Fe + P) / TRE0) is preferably 2. 〇 wt% or less, more preferably l.Owt% or less, and more preferably 0.45 wt% or less. As a method for producing a raw material for a lanthanum-based abrasive material, the following method (the first production method of the raw material) is roughly employed. First, 'the concentrate of the fluorine-contained concentrate or the like is decomposed by a sulfuric acid decomposition method or an alkali decomposition method, and the mixture is separately precipitated or separately dissolved, and the shaft, the drum, the handle, the crucible, the iron, the phosphorus, etc. are reduced and removed. The impurities give a rare earth solution. Further, the composition (rare earth composition adjustment) of the rare earth component of the obtained rare earth solution was adjusted. Thereafter, the composition of the adjusted rare earth solution is mixed with a precipitating agent (for example, ammonium hydrogencarbonate, ammonium carbonate, sodium hydrogencarbonate, sodium carbonate, ammonia, oxalic acid, ammonium oxalate, sodium oxalate, urea, etc.) to form a rare earth compound ( For example, a precipitate of a carbonate, an alkali carbonate, a monohydroxycarbonate, a hydroxide, an oxalate or the like is filtered and washed with water to obtain a raw material for the lanthanum abrasive of the present invention. When a raw material for a lanthanum-based abrasive material is produced, a method of adjusting a composition of a rare earth-based solution (reduced: after removing impurities) includes a solvent extraction method and addition. In the solvent extraction method, impurities other than rare earth elements can also be used depending on the method used. It can also be combined to make Xiao. The solvent extraction method and the addition method are also described first. First, the solvent extraction method will be described. Also, the ratio of 丨丄, ^ 鈥 (Nd203 / TRE0) is high, α, the weight ratio of oxidized oxime in the solution before solvent extraction is aa2 〇 3 / N (^二J 镧 镧 and the method in the solution, can be enumerated The following: a solvent extraction method for extracting titanium-portion to an organic solvent p疋' from a rare earth aqueous solution W, or a rare earth element

2169-6322-PF(N2).ptd 1303661 五、發明說明(16) 的幾乎全部萃取至有機溶劑後,使該有機溶劑與逆萃取用 的水溶液接觸,使敍的一部分殘留於有機溶劑中,而將其 他的大部分稀土類元素逆萃取至水溶液中之方法。藉由這 樣的方法來降低鈥之比例,調整成適合本發明之比例。相 反的,溶劑萃取前的溶液中歛之比例(Nd2 03 /TRE0)低的情 形’或該溶液中的氧化鑭與氧化歛之重量比(La2〇3/Nd2%) 大的情形所使用的溶劑萃取法,可以列舉出以下的方法。 即是,將鑭或鈽的一部分殘留於水溶液中,而將其他的稀 土類元素萃取至有機溶劑後,使之與逆萃取用的水溶液接 觸,將有機溶劑中萃取的稀土類元素之幾乎全部逆萃取至 水溶液之方法。藉由這樣的方法能提高鈥之比例,調整 適合本發明之比例。 、h且這裡所說明的各溶劑萃取法,作為有機溶劑使用了 越疋重稀土疋素越容易萃取之有機溶劑,也可能使用越 輕稀土元素越容易萃取之有機溶劑。且上述溶劑萃取 ^卒=驟或逆萃取步驟中,對象物質的萃取量或逆萃取 據所要的製造的研磨材料用原 料’等條件來適當地決定。 q之原 ^ ί ΐ對於添加法作說明。# 土類組成調整前的溶液 們盥ί 1二Nd2〇3」TREo)高的情形,或溶劑萃取前的氧化 二、;^ ί量比(La203 /Nd2 03 )小的情形所使用的添加 γ 有鑭或鈽等稀土類元素之化合物的大、々 液(例如,碳酸鹽、氫^ ^ ^ 的水溶 等的酸(鹽化物亦可m物紘^化物、乳化物等用鹽酸 jo /谷解所付的溶液),加以混合,2169-6322-PF(N2).ptd 1303661 5. After almost all of the organic solvent is extracted into the organic solvent, the organic solvent is brought into contact with the aqueous solution for reverse extraction, and a part of the residue is left in the organic solvent. A method of back-extracting most other rare earth elements into an aqueous solution. By such a method, the ratio of hydrazine is lowered to adjust to the ratio suitable for the present invention. Conversely, the ratio of the ratio of the solution before the solvent extraction (Nd2 03 /TRE0) is low or the solvent used in the case where the weight ratio of cerium oxide to oxidation is large (La2〇3/Nd2%) is large. The following methods can be mentioned as an extraction method. That is, a part of ruthenium or osmium is left in an aqueous solution, and other rare earth elements are extracted into an organic solvent, and then contacted with an aqueous solution for reverse extraction, and almost all of the rare earth elements extracted in the organic solvent are reversed. A method of extracting to an aqueous solution. By such a method, the ratio of bismuth can be increased, and the ratio suitable for the present invention can be adjusted. And each of the solvent extraction methods described herein, as the organic solvent, an organic solvent which is more easily extracted by the rare earth lanthanum cerium, and an organic solvent which is easier to extract with a lighter rare earth element may be used. In the solvent extraction step or the reverse extraction step, the extraction amount of the target substance or the reverse extraction is appropriately determined depending on conditions such as the raw material used for the desired abrasive material. The original q ^ ί ΐ for the addition method to explain. # The composition of the soil composition before adjustment 盥ί 1 2 Nd2 〇 3"TREo) high, or the oxidation before the solvent extraction, the amount of γ, the amount of (La203 / Nd2 03) is small, the addition of γ A large or sputum liquid of a compound having a rare earth element such as ruthenium or osmium (for example, an acid such as a carbonate or a hydrogen solution) (salt may also be a solution of a substance, an emulsion, or the like with a hydrochloric acid The solution), mixed,

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來降低鈦之比例’並調整成適合本發明之比例。相反 土類組成調,前的溶液中鈥之比例(Nd2〇3/TRE〇)低的情稀 形,或溶劑萃取前的氧化鑭與氧化鈥之重量比 α%〇3/Ν(12〇3)大的情形所使用的添加法,添加較多地含 鈥之化合物的水溶液,加以混合’來提高钕之比例,並調 整成適合本發明之比例。 且上述添加法中水溶液的添加量,根據所要的製造的 研磨材料用原料係哪一種發明之原料,等的條件來適當地 決定。 田 作為鈽系研磨材料用原料之製造方法,也有以下這樣 的方法(原料之第2製造方法)。 7 ^ ,如對製造上述發明之研磨材料,全稀土類氧化物換 算重量(TRE0)為90wt %以上,氧化鈽佔TRE0之重量比例 (Ce02/TRE0)係50wt%〜65wt%,氧化鈥佔TRE0之重量比例 (Nd2 03 /TRE0)係1 Owt%〜1 6wt%之鈽系研磨材料(第1發明) 時’首先作為研磨材料用原料之原料準備以下之物。具體 的,準備複數的鈾、钍、鈣、鋇、鐵、填等的元素之含有 率充分降低的、「Ce02/TRE0」或「Nd2 03 /TRE0」之值未必 在上述合適範圍内之物(例如,碳酸鹽、鹼性碳酸鹽、一 羥基碳酸鹽、氫氧化物、草酸鹽等)。且將這些複數的原 料(研磨材料用原料之原料)混合,並藉由調整鈽或歛之含 有率(混合步驟),來製造本發明之鈽系研磨材料用原料。 例如對製造上述發明之研磨材料,氧化鈽(Ce02)佔全 稀土類氧化物換算重量(TRE0)之重量比例(Ce02/TRE0)係To reduce the ratio of titanium ' and adjust to the ratio suitable for the present invention. On the contrary, the soil composition is adjusted, the proportion of bismuth in the former solution (Nd2〇3/TRE〇) is low, or the weight ratio of cerium oxide to cerium oxide before solvent extraction is α% 〇3/Ν (12〇3) In the case of a large-scale addition method, an aqueous solution containing a large amount of a compound containing ruthenium is added and mixed to increase the ratio of ruthenium and adjust to a ratio suitable for the present invention. In addition, the amount of the aqueous solution to be added in the above-mentioned additive method is appropriately determined depending on the conditions of the raw material of the raw material to be produced, and the like. Field As a method of producing a raw material for a lanthanum-based abrasive material, the following method (the second method for producing a raw material) is also available. 7 ^ , as in the manufacture of the abrasive material of the above invention, the total rare earth oxide conversion weight (TRE0) is 90 wt% or more, the weight ratio of cerium oxide to TRE0 (Ce02/TRE0) is 50 wt% to 65 wt%, and cerium oxide accounts for TRE0. When the weight ratio (Nd2 03 /TRE0) is 1% by weight to 6% by weight of the lanthanum-based abrasive (first invention), the following materials are prepared as raw materials for the raw material for the abrasive. Specifically, the value of "Ce02/TRE0" or "Nd2 03 /TRE0" whose value of the elements of uranium, thorium, calcium, strontium, iron, and the like is sufficiently reduced is not necessarily within the above-mentioned appropriate range ( For example, carbonates, basic carbonates, monohydroxycarbonates, hydroxides, oxalates, etc.). Further, these plural raw materials (raw materials for raw materials for polishing materials) are mixed, and the raw materials for the lanthanum abrasive materials of the present invention are produced by adjusting the content of the ruthenium or the entanglement (mixing step). For example, in the case of producing the above-described abrasive material, cerium oxide (Ce02) accounts for the weight ratio of the total rare earth oxide equivalent weight (TRE0) (Ce02/TRE0).

2169-6322-PF(N2).ptd 第24頁 1303661 五、發明說明(18) 45wt%〜70wt%,TRE0中氧化鑭(La2 03 )與氧化鈦(Nd2 03 )之重 量比例(1^2 03 /“2 03 )係1.4〜2.8之鈽系研磨材料(第2發明) 時,首先作為研磨材料用原料之原料準備了以下之物。具 體的,準備複數的鈾、钍、鈣、鋇、鐵、磷等的元素之含 有率充分降低的、「Ce02/TRE0」或「La2 03 /TRE0」之值未 必在上述合適範圍内之物(例如,碳酸鹽、驗性碳酸鹽、 一經基碳酸鹽、氫氧化物、草酸鹽等)。且將這些複數的 原料(研磨材料用原料之原料)混合,並藉由調整鈽或鈥之 含有率(混合步驟),來製造本發明之鈽系研磨材料用原 料0 另外,該第2製造方法所說明的混合步驟,只要在鈽 系研磨材料之製造的焙燒步驟之前進行即可。即是,該混 合步驟也可以在鈽系研磨材料用原料的製造步驟等階段進 行γ例如’對上述這樣的複數個原料(研磨材料用原料之 原料)分別進行粉碎、氟化處理後,再實施混合步驟也可 以。且作為用於混合的複數的原料(研磨材料用原料之原 料。)、’也可以係TRE0中1種類的稀土類氧化物之比例在99 Wt%以上的高純度之物。使用高純度的原料可以簡單地完 成組成之調整,但高純度的原料也係高價的。 、、以上對各種研磨材料用原料作了說明,也可以將鍛燒 j述研磨材料用原料所得的焙燒物(例如,鍛燒稀土類碳 =鹽、、鹼性碳酸鹽、一羥基碳酸鹽、氫氧化物、草酸鹽等 髀原斗所侍的氧化物、或該氧化物與其原料之間的中間 - 為本發明的鈽系研磨材料用原料。這裡所謂的研磨2169-6322-PF(N2).ptd Page 24 1303661 V. Description of invention (18) 45wt%~70wt%, weight ratio of lanthanum oxide (La2 03 ) to titanium oxide (Nd2 03 ) in TRE0 (1^2 03 / "2 03" When the 研磨-based abrasive material (the second invention) of 1.4 to 2.8 is used, the following materials are prepared as raw materials for the raw material for the polishing material. Specifically, a plurality of uranium, thorium, calcium, strontium, and iron are prepared. The content of "Ce02/TRE0" or "La2 03 /TRE0" whose content of phosphorus or the like is sufficiently lowered is not necessarily within the above-mentioned suitable range (for example, carbonate, carbonate, monobasic carbonate, Hydroxide, oxalate, etc.). Further, the raw material (the raw material of the raw material for the polishing material) is mixed, and the content of the crucible or the crucible (mixing step) is adjusted to produce the raw material for the crucible polishing material of the present invention. Further, the second manufacturing method The mixing step described may be carried out before the baking step of the production of the lanthanum abrasive. In other words, the mixing step may be carried out at the stage of the production step of the raw material for the lanthanum-based abrasive material, for example, γ, the pulverization and the fluorination treatment of the plurality of raw materials (the raw materials for the raw material for the polishing material) A mixing step is also possible. Further, it may be a raw material (raw material for a raw material for polishing materials) used for mixing, or 'a high-purity substance having a ratio of one type of rare earth oxide in TRE0 of 99 Wt% or more. The adjustment of the composition can be easily accomplished using a high-purity raw material, but the high-purity raw material is also expensive. Further, the raw materials for various polishing materials are described above, and the calcined product obtained by calcining the raw material for the polishing material (for example, calcined rare earth carbon=salt, alkaline carbonate, monohydroxycarbonate, or the like) may be used. The oxide of the hydrazine, such as a hydroxide or an oxalate, or the intermediate between the oxide and the raw material thereof - is a raw material for the bismuth-based abrasive material of the present invention.

2169-6322-PF(N2).ptd 第25 1303661 五、發明說明(19) 料指的是以其為原料製造研磨材料時,培燒步 中’不僅包含研磨材料製造之初期階段進行的粉:= 的原料’也包括鈽系研磨材料製造時、供給於 之原料(中間原料)。因此,以上所說明的對上述;j:: =巧料實施了粉碎處理及/或氟化處理之物,另外實施了 乾燥處理及/或粉碎處理之物,經過焙燒才成為鈽系研磨 材料之物(即研磨材料製造之焙燒步驟前之物),均系這裡 所謂的鈽系研磨材料用原料(中間原料)。 且上述各發明之鈽系研磨材料用原料及鈽系研磨材料 中,「F/TRE0」、「(u+Th)/TRE0」、 「(Ca + Ba + Fe+P)/TRE0」,係相對於研磨材料用原料及研 磨材料之全稀土類氧化物換算重量(TRE0)之「F」的重 量、「U + Th」的重量、「Ca + Ba + Fe + P」的重量之重量比, 而非「F」佔TRE0的重量、「U + Th」佔TRE0之重量、 「Ca + Ba + Fe + P」佔TRE0之重量。「TRE0」係不含有 「F」、「U + Th」、「Ca + Ba + Fe + P」的,「F」佔 TRE0 的重 量、「(U + Th)」佔TRE0之重量或「Ca + Ba + Fe + P」佔TRE0之 重量的比例基本上係0重量%。因此,在求取研磨材料用原 料及研磨材料之「F/TRE0」、「(U + Th)/TRE0」或 「(Ca + Ba + Fe + P)/TRE0」時,需要分別測量研磨材料用原 料及研磨材料之「TRE0(全稀土類氧化物換算重量)」 量 「F」的重量、「U + Th」的重量及「Ca + Ba + Fe + P」的重 用計算換算成「TRE0」lOOwt%。例如,研磨材料的2169-6322-PF(N2).ptd No. 25 1303661 V. INSTRUCTIONS (19) The material refers to the powder that is used in the initial stage of the manufacture of the abrasive material when the abrasive material is made from the raw material. The raw material of = also includes the raw material (intermediate raw material) supplied at the time of manufacture of the lanthanum abrasive. Therefore, the above-described; j:: = material is subjected to a pulverization treatment and/or a fluorination treatment, and a drying treatment and/or a pulverization treatment is carried out, and after firing, it becomes a lanthanide abrasive material. The material (that is, the material before the baking step in which the abrasive material is produced) is a raw material (intermediate raw material) for the lanthanide abrasive material herein. In the above-mentioned raw materials for the polishing material and the lanthanum-based polishing material, "F/TRE0", "(u+Th)/TRE0", and "(Ca + Ba + Fe+P)/TRE0" are relative. The weight ratio of the weight of "F", the weight of "U + Th", and the weight of "Ca + Ba + Fe + P" in terms of the weight of the total rare earth oxide of the raw material for the polishing material and the polishing material (TRE0) Non-"F" accounts for the weight of TRE0, "U + Th" accounts for the weight of TRE0, and "Ca + Ba + Fe + P" accounts for the weight of TRE0. "TRE0" does not contain "F", "U + Th", "Ca + Ba + Fe + P", "F" accounts for the weight of TRE0, "(U + Th)" accounts for the weight of TRE0 or "Ca + The ratio of Ba + Fe + P" to the weight of TRE0 is substantially 0% by weight. Therefore, when "F/TRE0", "(U + Th)/TRE0" or "(Ca + Ba + Fe + P) / TRE0" of the raw material for the polishing material and the polishing material is obtained, it is necessary to separately measure the polishing material. "TRE0 (full rare earth oxide conversion weight)" of the raw material and the abrasive material. The weight of the "F", the weight of "U + Th", and the reuse of "Ca + Ba + Fe + P" are converted into "TRE0" lOOwt. %. For example, abrasive materials

2l69>6322-PF(N2).ptd 第26頁 1303661 五、發明說明(20) 「TRE0」為90wt%,研磨材料的「F」為6.3wt%時,該研磨 材料的「F/TRE0」係 6.3(wt0/〇)/90.0(wt%)xl00(wt0/〇) = 7.0(wt%)。 【實施方式】 以下,對本發明之鈽系研磨材料的最佳實施形態作一 說明。 弟1實施形態 首先’準備了乳化稀土(印度產)。且其組成中全稀土 類氧化物換算重量(以下稱為TRE0)為46wt%、Ce02/TRE0為 50.3wt%,La2 03 /TRE0 為 23·7 wt%,Nd2 03 /TRE0 為 20.0wt°/〇, Pr60n/TRE0 為 5· 2wt%,(U + Th)/TRE0 為〇· 〇〇〇5wt% 未滿, (Ca + Ba + Fe + P)/TRE0為0.6wt%。且,該氯化稀土係,對氟 碳鈽精礦(印度產),按照順序實施粉碎,使用濃氫氧化納 水溶液之鹼分解(1 4 0 °C、3小時),將磷酸成分溶解至水溶 液中的熱水處理、過濾、使用pH調整成3.5〜4.0的鹽酸之 分別溶解(使稀土類元素溶解、並將鈾(U)、钍(Th)殘留於 氫氧化物沉澱中)、過濾、溶劑萃取、蒸發濃縮、放冷固 化之各步驟而得到的。 [施例】:使用準備好的氯化稀土來製造鈽系研磨材料用 原料(中間原料)。首先’將準備的氯化稀土與〇· lm〇1/L的 稀鹽酸混合•溶解來調製氯化稀土溶液,對調製的溶夜進 行過濾,對過濾後的溶液進行溶劑萃取。該溶劑萃取中,2l69>6322-PF(N2).ptd Page 26 1303661 V. Description of Invention (20) When "TRE0" is 90 wt% and the "F" of the abrasive is 6.3 wt%, the "F/TRE0" of the abrasive material is 6.3 (wt0 / 〇) / 90.0 (wt%) xl00 (wt0 / 〇) = 7.0 (wt%). [Embodiment] Hereinafter, a preferred embodiment of the bismuth-based abrasive material of the present invention will be described. Younger 1 embodiment First, an emulsified rare earth (made in India) was prepared. And the composition of the total rare earth oxide conversion weight (hereinafter referred to as TRE0) is 46wt%, Ce02/TRE0 is 50.3wt%, La2 03 /TRE0 is 23·7 wt%, and Nd2 03 /TRE0 is 20.0wt°/〇 Pr60n/TRE0 is 5.2 wt%, (U + Th)/TRE0 is 〇·〇〇〇5 wt%, and (Ca + Ba + Fe + P)/TRE0 is 0.6 wt%. Further, the rare earth chloride system is pulverized in the order of the fluorocarbon antimony concentrate (manufactured in India), and the phosphate component is dissolved in the aqueous solution by alkali decomposition (140 ° C, 3 hours) using a concentrated aqueous solution of sodium hydroxide. Hot water treatment, filtration, and dissolving separately using hydrochloric acid having a pH adjusted to 3.5 to 4.0 (dissolving rare earth elements and leaving uranium (U) and thorium (Th) in the hydroxide precipitate), filtering, solvent It is obtained by various steps of extraction, evaporation and concentration, and cooling and solidification. [Example]: A raw material (intermediate raw material) for a cerium-based abrasive material was produced using the prepared rare earth chloride. First, the prepared rare earth chloride is mixed with dilute hydrochloric acid of 〇·lm〇1/L to prepare a rare earth chloride solution, and the prepared solution is filtered, and the filtered solution is subjected to solvent extraction. In the solvent extraction,

1303661 五、發明說明(21) 作為有機溶劑,使用了容易萃取重稀土類元素之萃取劑 (PC-88A :大八化學工業所製)與稀釋劑(zps〇L:出光石油 化學製),以液量比(萃取劑/稀釋劑)為1/2的比例混合所 得的溶液。且該有機溶劑與氯化稀土溶解液 (TRE0210g/L),以流量比(有機溶劑/氣化稀土溶解液)為 8/1之狀態,使其逆流多段接觸(30段),將稀土類元素萃 取至有機溶劑中。且該步驟中,與供用的有機溶劑之逆流 多段萃取之途中’添加了充分量的氫氧化鈉水溶液,使氯 化稀土溶液中的稀土類元素幾乎全部萃取出。其後,使含 有稀土類元素的有機溶劑與3mo 1 /L鹽酸水溶液,以流量比 (有機溶劑/鹽酸水溶液)為8 / 1 · 4之狀態,使之逆流多段接 觸(3 0段),將镨、鈥的一部分及比歛更容易被有機溶劑萃 取的稀土類元素(彭(Sm)至重稀土及記(γ))之大半殘留於 有機溶劑中,將鑭、鈽的大部分、镨及鈥的一部分逆萃取 至鹽酸水溶液中,得到稀土類溶液(精製液)。 溶劑萃取後’所得的稀土類溶液與碳酸氫銨水溶液 (、/儿澱劑)混合,生成稀土類碳酸鹽之沉澱後,使用離心分 離機過瀘、、洗淨(水洗),得到鈽系研磨材料用原料(中間 原料)之稀土類碳酸鹽。其組成,TRE0為44wt°/G。TRE0中的 各稀土類元素之重量比例與所得的鈽系研磨材料相同(參 照表1)。且F/TRE0 為0· lwt°/G 未滿、(u + Th)/TRE0 為〇· 〇〇〇5 wt% 未滿、(Ca + Ba + Fe + P)/TREO 為 〇.4wt% 未滿。 將這樣準備好的稀土類碳酸鹽(中間原料)與該原料重 量的2倍重量之純水混合,用濕式球磨機(使用直徑5mm的1303661 V. INSTRUCTIONS (21) As an organic solvent, an extractant (PC-88A: manufactured by Daiba Chemical Industry Co., Ltd.) and a diluent (zps〇L: manufactured by Idemitsu Petrochemical Co., Ltd.) which are easy to extract heavy rare earth elements are used. The resulting solution was mixed at a liquid ratio (extractant/diluent) of 1/2. The organic solvent and the rare earth chloride solution (TRE0210g/L) are in a state of flow ratio (organic solvent/gasified rare earth solution) of 8/1, and are subjected to countercurrent multi-stage contact (30 stages) to form a rare earth element. Extract into an organic solvent. Further, in this step, a sufficient amount of aqueous sodium hydroxide solution is added to the countercurrent multistage extraction of the organic solvent to be used, and almost all of the rare earth elements in the rare earth chloride solution are extracted. Thereafter, the organic solvent containing the rare earth element and the 3 mol / L hydrochloric acid aqueous solution were subjected to a countercurrent multi-stage contact (3 0 stage) in a flow ratio (organic solvent / aqueous hydrochloric acid solution) of 8 / 1 · 4 , A part of lanthanum, cerium, and rare earth elements (Pm (Sm) to heavy rare earth and γ) which are more easily extracted by organic solvents remain in the organic solvent, and most of lanthanum and cerium, A part of the rhodium was back-extracted into an aqueous hydrochloric acid solution to obtain a rare earth solution (refined liquid). After the solvent extraction, the obtained rare earth solution is mixed with an aqueous solution of ammonium hydrogencarbonate (or a precipitant) to form a precipitate of a rare earth carbonate, which is then dried by a centrifugal separator and washed (washed) to obtain a barium-based polishing. A rare earth carbonate of a raw material (intermediate raw material) for materials. Its composition, TRE0 is 44wt ° / G. The weight ratio of each rare earth element in TRE0 is the same as that of the obtained lanthanum-based abrasive (refer to Table 1). And F/TRE0 is 0·lwt°/G is not full, (u + Th)/TRE0 is 〇· 〇〇〇5 wt% is not full, (Ca + Ba + Fe + P)/TREO is 〇.4wt% full. The rare earth carbonate (intermediate raw material) thus prepared is mixed with 2 times by weight of pure water of the weight of the raw material, and a wet ball mill (using a diameter of 5 mm)

2169-6322-PF(N2).ptd 第28頁 1303661 五、發明說明(22) 氧化鍅球作為粉碎媒體)進行8小時的濕式粉碎,〜 料漿體。所得的粉碎品之DS()為〇· 8 V m。接著,所=到原 體添加10wt %的氫氟酸,調製漿體中的氟成分之 传的漿 (F/TRE0),將該漿體攪拌30分鐘(以下簡稱為氟*比 理)。氟化處理後的「F/TRE0」為8.〇wt%。且氟濃' 量使用了鹼熔融•溫水萃取·氟離子電極法。其X,的測 體成分沉澱,取出上層澄清液,添加純水進行^ 化^固 淨’將洗淨後的漿體用壓濾法過濾。且將所得的渡^ 140 °C乾燥48小時。另外,將所得的乾燥餅用樣品&磨 碎’將所得的粉碎品焙燒(焙燒溫度丨〇 〇 〇 〇c、焙燒時間^ 小時)。焙燒後,將所得的焙燒品用樣品磨機粉=:; 輪分級機(設定分級點於5# m)分級,得到鈽系研磨材料、。 置施例2、3 :這些的實施例中,在使含有稀土類元素的有 機溶劑與3mol/L鹽酸水溶液逆流多段接觸、將鑭等的稀土 類元素逆萃取至鹽酸水溶液的步驟中,有機溶劑與鹽酸水 溶液之流量比(有機溶劑/鹽酸水溶液)與實施例丨不同。且 實施例2中的流量比(有機溶劑/鹽酸水溶液)為8/1· 3,實 施例3中的流量比(有機溶劑/鹽酸水溶液)為8/1· 2。除此 以外的條件,與實施例1相同,省略了其說明。且實施例2 中所製造的稀土類碳酸鹽(中間原料)iTRE〇為46“。/◦,實 施例3中所製造的稀土類碳酸鹽(中間原料)之treq為43 wt%。且TRE0中的各稀土類元素之重量比例,無論哪一個 實施例’均與最終所製造的鈽系研磨材料相同(參照表2169-6322-PF(N2).ptd Page 28 1303661 V. INSTRUCTIONS (22) The cerium oxide ball is used as a pulverizing medium for 8 hours of wet pulverization, to slurry. The DS () of the obtained pulverized product was 〇·8 V m. Then, 10% by weight of hydrofluoric acid was added to the original body to prepare a slurry (F/TRE0) of the fluorine component in the slurry, and the slurry was stirred for 30 minutes (hereinafter referred to simply as fluorine* ratio). The "F/TRE0" after the fluorination treatment was 8. 〇wt%. And the fluorine concentration is measured by alkali melting, warm water extraction and fluoride ion electrode method. The X, the measured component is precipitated, and the supernatant liquid is taken out, and pure water is added for purification. The washed slurry is filtered by pressure filtration. The obtained ferment was dried at 140 ° C for 48 hours. Further, the obtained dried cake was ground with a sample & and the obtained pulverized product was fired (baking temperature 丨〇 〇 〇 〇 c, baking time ^ hours). After calcination, the obtained calcined product was classified with a sample mill powder =:; a wheel classifier (setting a classification point at 5 #m) to obtain a lanthanide abrasive material. Embodiments 2 and 3: In the examples, the organic solvent containing a rare earth element is contacted with a 3 mol/L hydrochloric acid aqueous solution in a countercurrent flow, and a rare earth element such as cerium is back-extracted to a hydrochloric acid aqueous solution, and an organic solvent is used. The flow ratio with the aqueous hydrochloric acid solution (organic solvent/hydrochloric acid aqueous solution) was different from that of the example. Further, the flow ratio (organic solvent/hydrochloric acid aqueous solution) in Example 2 was 8/1·3, and the flow ratio (organic solvent/hydrochloric acid aqueous solution) in Example 3 was 8/1·2. Conditions other than the above are the same as in the first embodiment, and the description thereof is omitted. Further, the rare earth carbonate (intermediate raw material) iTRE〇 produced in Example 2 was 46"/◦, and the treq of the rare earth carbonate (intermediate raw material) produced in Example 3 was 43 wt%. The weight ratio of each rare earth element, whichever embodiment is the same as the final lanthanide abrasive material (refer to the table)

2169-6322-PF(N2).ptd 第29頁 13036612169-6322-PF(N2).ptd Page 29 1303661

/TTRE0 為 〇· 〇〇〇5wt% 未滿、(Ca + Ba+Fe + P)/TRE0 為 0· 4wt% 未 滿0 1)。且無論哪一個實施例,F/TRE0為〇· lwt%未滿、(U+Th) 生較姐••作為原料準備了美國產的氟碳鈽精礦。且其組 成(重量比),TRE0 為70wt%、Ce02/TRE0 為49. 3wt%,/TTRE0 is 〇· 〇〇〇5wt% not full, (Ca + Ba+Fe + P)/TRE0 is 0·4wt% under 01). In either case, F/TRE0 is 〇·lwt% less than (U+Th), and the fluorocarbon strontium concentrate produced in the United States is prepared as a raw material. 3重量%, and its composition (weight ratio), TRE0 is 70wt%, Ce02/TRE0 is 49. 3wt%,

La2 03 /TRE0 為 34.0wt%,Nd2 03 /TRE0 為 ll.3wt%,Pr6〇u/TRE〇 為4· Owt%,F/TREO 為8· 0 wt%,(U + Th)/TRE0 為〇. lwt%, (Ca + Ba + Fe + P)/TRE0為6· 8wt%。將準備好的原料(氟碳鈽精 礦)與該原料重量的2倍重量之純水混合,用濕式球磨機 (使用直徑5 m m的氧化錯球作為粉碎媒體)進行8小時的濕式 粉碎,來得到原料漿體。且對於所得的原料漿體,按照^ 序,實施再漿化洗淨、過濾、乾燥、焙燒、粉碎、分&的 各步驟,來得到鈽系研磨材料。且再漿化洗淨後的各步驟 之條件與實施例1相同。 y於 例2、3 :這些的比較例中,使含有稀土類元素的有機 溶劑與3mol/L鹽酸水溶液逆流多段接觸、將鑭等的稀土類 元素逆萃取至鹽酸水溶液之步驟,其條件與實施例j不 同。比較例2中,有機溶劑與鹽酸水溶液之流量比(有機、、容 劑/鹽酸水溶液)為8/1· 6,且有機溶劑中的稀土類元素幾^ 乎全部逆萃取至鹽酸水溶液中,得到稀土類溶液(精製 液)。比較例3中的流量比(有機溶劑/鹽酸水溶液)為 8 /1 · 1。除此以外的條件與實施例1相同。且比較例2所製La2 03 /TRE0 is 34.0 wt%, Nd2 03 /TRE0 is ll.3 wt%, Pr6〇u/TRE〇 is 4·Owt%, F/TREO is 8.0 wt%, and (U + Th)/TRE0 is 〇 Lwt%, (Ca + Ba + Fe + P) / TRE0 is 6.8 wt%. The prepared raw material (Fluorocarbon concentrate) was mixed with 2 times by weight of pure water of the weight of the raw material, and subjected to wet pulverization for 8 hours using a wet ball mill (using a 5 mm diameter oxidized wrong ball as a pulverizing medium). To get the raw material slurry. Further, the obtained raw material slurry was subjected to steps of repulp washing, filtration, drying, calcination, pulverization, and separation to obtain a lanthanum-based abrasive. Further, the conditions of the respective steps after the repulp washing were the same as in the first embodiment. In the comparative examples of Examples 2 and 3, the organic solvent containing a rare earth element is subjected to a countercurrent multistage contact with a 3 mol/L hydrochloric acid aqueous solution, and a rare earth element such as ruthenium is back-extracted to a hydrochloric acid aqueous solution, and the conditions and implementation thereof are carried out. Example j is different. In Comparative Example 2, the flow ratio of the organic solvent to the aqueous hydrochloric acid solution (organic, solvent/hydrochloric acid aqueous solution) was 8/1·6, and the rare earth elements in the organic solvent were all back-extracted to the aqueous hydrochloric acid solution to obtain Rare earth solution (refined liquid). The flow ratio (organic solvent / aqueous hydrochloric acid solution) in Comparative Example 3 was 8 /1 ·1. The other conditions were the same as in the first embodiment. And made in Comparative Example 2

2169-6322-PF(N2).ptd2169-6322-PF(N2).ptd

1303661 五、發明說明(24) 造的稀土類碳酸鹽(中間原料)之TRE〇為42衬%,比較例3所 製造的稀土類碳酸鹽(中間原料)2TRE〇為46 wt%。且TRE〇 中的各稀土類元素之重量比例,無論哪一個實施例,均與 最終所製造的鈽系研磨材料相同(參照表丨)。且無論哪一 個實施例,F/TRE0 為(Klwt% 未滿、(u + Th)/TRE〇 為 〇〇〇〇5 wt% 未滿、(Ca + Ba + Fe + P)/TRE0 為 0.4wt% 未滿。 免轉例i_l.l •各實施例中,氟化處理之條件不同外,其他 用與實施例2相同的條件來製造鈽系研磨材料。且氟化處 理後的「F/TRE0」在實施例4為4· 〇wt%,實施例5為 5· 5wt%,實施例6為1 lwt%,實施例7為15wt%。 复施例8、9 :各實施例中,焙燒步驟之焙燒溫度不同以 外,其他用與實施例2相同的條件來製造鈽系研磨材料。 且焙燒溫度在實施例8為850 t:,實施例9為11〇〇。(:。 上述各實施例及各比較例所得的鈽系研磨材料,其 含有率、TREO、TRE0中的各稀土類氧化物之重量比例等= 如表1所示。且(0& + 6&砰4?)/1^肋在比較例1的研磨材 為6.2wt%,其他的研磨材料為〇4wt%未滿。 ’1303661 V. INSTRUCTION OF THE INVENTION (24) The TRE 造 of the rare earth carbonate (intermediate raw material) produced was 42% by lining, and the rare earth carbonate (intermediate raw material) produced in Comparative Example 3 was 46 wt%. Further, the weight ratio of each rare earth element in TRE〇 is the same as that of the finally produced lanthanum-based abrasive material (see Table 丨). In either case, F/TRE0 is (Klwt% is not full, (u + Th)/TRE〇 is 〇〇〇〇5 wt% less than, (Ca + Ba + Fe + P)/TRE0 is 0.4wt % is not full. Free example i_l.l • In each of the examples, the fluorination treatment was carried out under the same conditions as in Example 2, and the fluorination treatment "F/TRE0" was used. In Example 4, it was 4·〇wt%, Example 5 was 5·5 wt%, Example 6 was 1 lwt%, and Example 7 was 15 wt%. Compounds 8 and 9: In each of the examples, the calcination step The bismuth-based abrasive material was produced under the same conditions as in Example 2 except that the baking temperature was different. The baking temperature was 850 t in Example 8, and Example 9 was 11 Å. (: The above respective examples and The content of the lanthanum-based abrasive obtained in each of the comparative examples, the weight ratio of each of the rare earth oxides in TREO and TRE0, and the like are as shown in Table 1. (0& + 6 & 砰 4?) / 1 rib The abrasive of Comparative Example 1 was 6.2% by weight, and the other abrasive materials were 〇4% by weight.

1303661 五、發明說明(25) [表1】 研磨材 研磨材 _中各稀土類氣化物之重量比例(ψ«) La2〇3/ F_) F/ U+TV 料之Μ 料之 Nd2〇3 +TRB0 TRBD TRBO 含有率 TRBO (wt%) (ψί%) (vt%) (wt%) (wt%) 002 Lai2〇3 Ρ^δΟιι Nd2〇3 b2〇3+Nja〇3 比較例1 6.1 87.8 48.3 34.6 4.0 11.3 45.9 3.06 93,9 6.9 0.10 itmn 6.6 94.0 50.3 23.7 5.2 20.0 43.7 1.19 100.6 7.0 <0.0003 實施例1 6.5 93.7 53.4 25.1 5.0 15.9 41.0 1.58 100.2 6.9 <i).0CO3 寶施例2 6.5 93.8 55,2 26.1 4,9 13,2 39.3 1.98 100.3 6.9 <0,0003 寶施例3 6.4 93.7 57.4 27.0 4.7 10.5 37.5 2.57 100.1 6.8 <0.0003 比較例3 6.4 93.9 59.4 28.0 4.9 7.1 35.1 3.94 100.3 6.8 <D.(XX)3 實施例4 3.0 %3 55.2 26.1 4.9 13.2 39.3 1.98 99.3 3.1 <Ω.(ΧΧ)3 寶施例5 4.4 95.4 552 26.1 4.9 13.2 39.3 1.98 99.8 4.6 <0.0003 實施例2 6.5 93.8 55.2 26.1 4.9 13.2 39.3 1.98 100.3 6.9 <0.0003 實施例6 8.2 92.5 55.2 26.1 4.9 13.2 39.3 1.98 100.7 8,9 <0.0003 實施例? 10.5 91.3 55.2 26.1 4.9 13.2 39.3 1.98 101.8 11.5 <0.0003 實施例8 6.7 93.7 55.2 26.1 4.9 13.2 39.3 1.98 100.4 7.2 <0.0003 實施例2 6.5 93.8 55.2 26.1 4.9 13.2 39.3 1.98 100.3 6.9 <D.CC03 寶施例9 6.3 93.8 55.2 26.1 4.9 13.2 39.3 1.98 100.1 6.7 <0.0003 使用各實施例及比較例所得的鈽系研磨材料,測量平 均粒徑(D5G)、BET法比表面積(BET)及繞射X射線強度 (Indensity)。且使用各實施例及比較例所得的鈽系研磨 材料進行研磨試驗,對研磨值(研磨速度)、所得的研磨面 之刮傷評價及附著性(洗淨性)作了評價。以下對測量方 法、研磨試驗方法、各種研磨特性之評價方法作說明。且 測量值及評價結果如其後的表2所示。1303661 V. INSTRUCTIONS (25) [Table 1] Abrasive material _ the weight ratio of each rare earth vapor (ψ«) La2〇3/ F_) F/ U+TV material Nd2〇3 + TRB0 TRBD TRBO Content rate TRBO (wt%) (ψί%) (vt%) (wt%) (wt%) 002 Lai2〇3 Ρ^δΟιι Nd2〇3 b2〇3+Nja〇3 Comparative Example 1 6.1 87.8 48.3 34.6 4.0 11.3 45.9 3.06 93,9 6.9 0.10 itmn 6.6 94.0 50.3 23.7 5.2 20.0 43.7 1.19 100.6 7.0 <0.0003 Example 1 6.5 93.7 53.4 25.1 5.0 15.9 41.0 1.58 100.2 6.9 <i).0CO3 Bao 2 Example 2 6.5 93.8 55, 2 26.1 4,9 13,2 39.3 1.98 100.3 6.9 <0,0003 Example 3 6.4 93.7 57.4 27.0 4.7 10.5 37.5 2.57 100.1 6.8 <0.0003 Comparative Example 3 6.4 93.9 59.4 28.0 4.9 7.1 35.1 3.94 100.3 6.8 <D (XX)3 Example 4 3.0 %3 55.2 26.1 4.9 13.2 39.3 1.98 99.3 3.1 <Ω.(ΧΧ)3 Bao Shi Example 5 4.4 95.4 552 26.1 4.9 13.2 39.3 1.98 99.8 4.6 <0.0003 Example 2 6.5 93.8 55.2 26.1 4.9 13.2 39.3 1.98 100.3 6.9 <0.0003 Example 6 8.2 92.5 55.2 26.1 4.9 13.2 39.3 1.98 100.7 8,9 <0.0003 Example? 10.5 91.3 55.2 26.1 4.9 13.2 39.3 1.98 101.8 11.5 <0.0003 Example 8 6.7 93.7 55.2 26.1 4.9 13.2 39.3 1.98 100.4 7.2 <0.0003 Example 2 6.5 93.8 55.2 26.1 4.9 13.2 39.3 1.98 100.3 6.9 <D.CC03 9 6.3 93.8 55.2 26.1 4.9 13.2 39.3 1.98 100.1 6.7 <0.0003 Using the lanthanide abrasive materials obtained in each of the examples and the comparative examples, the average particle diameter (D5G), the BET specific surface area (BET), and the diffraction X-ray intensity were measured ( Indensity). Further, the polishing test was carried out using the lanthanum-based abrasive materials obtained in the respective Examples and Comparative Examples, and the polishing value (polishing speed), the scratch evaluation of the obtained polished surface, and the adhesion (detergency) were evaluated. The measurement method, the polishing test method, and the evaluation methods of various polishing characteristics will be described below. The measured values and evaluation results are shown in Table 2 below.

2169-6322-PF(N2).ptd 第32頁 1303661 五、發明說明(26) 乎均粒徑(I )之測蕃 使用雷射繞射•散亂法粒度分布測量裝置((株)島津 製作所製:SALD-2 0 0 0A),測量鈽系研磨材料之粒度分 布,求得平均粒徑((D5():從小粒徑之側的累積體積 50%之粒徑)。 M.T法比表面積(BET):根據JIS R 1 626-1 996 (精細陶兗粉 體之氣體吸附BET法之比表面積測量方法)的「6 · 2流動法 之(3· 5) —點法」進行測量。這時,使用了載子氣體為氦 氣、吸附質氣體為氮氣之混合氣體。 X射線繞射測晉 使用X射線繞射裝置(Macscience(株)製、ΜΧΡ18),對 於鈽系研2材料進行X射線繞射分析,測量繞射χ射線強 度。本測量中,使用銅(Cu)靶,對Cu_K A線(照射Cu-K “ 線所得)之繞射X射線圖案中,繞射角(2 0)在2〇。〜3〇。内 出現的峰進行解析。且其他的測量條件係管電壓4〇kv、管 ,流150mA。、測量範圍20=5。〜8〇。、樣品寬度〇 〇2。、 f描速度4。/分。且,從所得的X射線繞射測量結果讀取 氧化飾(Ce〇2)的X射線繞射峰強度,鑭系氟氧化物(Ln〇F)之 X射線繞射峰強度及鑭系氟化物(LnFs )之X射線繞射峰強 度’求得各X射線繞射峰強度比(LnOF/ Ce02、LnF3/Ce02)。 研磨試驗2169-6322-PF(N2).ptd Page 32 1303661 V. Description of the invention (26) Measurement of the average particle size (I) using a laser diffraction/scatter method for particle size distribution measurement (Shimadzu Corporation) System: SALD-2 0 0 0A), measuring the particle size distribution of the lanthanide abrasive material, and obtaining the average particle diameter ((D5(): particle size of 50% of the cumulative volume from the side of the small particle size). MT specific surface area ( BET): It is measured according to JIS R 1 626-1 996 (the method of measuring the specific surface area of the gas adsorption BET method of fine ceramic powder) by the "6 · 2 flow method (3 · 5) - point method". A X-ray diffraction device (manufactured by Macscience Co., Ltd., ΜΧΡ18) was used for the X-ray diffraction measurement, and X-ray diffraction was performed on the X-ray diffraction. Shot analysis, measuring the intensity of the diffracted ray. In this measurement, a copper (Cu) target is used, and the diffraction angle (20) is in the diffracted X-ray pattern of the Cu_K A line (obtained by the Cu-K "line"). 2〇.~3〇. The peaks appearing inside are analyzed. Other measurement conditions are tube voltage 4〇kv, tube, flow 150mA. The circumference is 20=5.~8〇., the sample width is 〇〇2, and the f-drawing speed is 4/min. Moreover, the X-ray diffraction of the oxidized decoration (Ce〇2) is read from the obtained X-ray diffraction measurement result. Peak intensity, X-ray diffraction peak intensity of lanthanide oxyfluoride (Ln〇F) and X-ray diffraction peak intensity of lanthanide fluoride (LnFs)'s X-ray diffraction peak intensity ratio (LnOF/ Ce02) , LnF3/Ce02). Grinding test

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第33頁 1303661 五、發明說明(27) 作為研磨機,準備了研磨試驗機(HSP-21型、台東精 機(株)製)。該研磨試驗機係一邊將研磨材漿體供給於研 磨對象面,一邊用研磨墊片將研磨對象面研磨之機器,研 磨墊片使用聚氨酯製之物,該研磨試驗採用每1次(2 4小時 左右的研磨時間)交換成新品。作為研磨對象物,準備了 直徑6 5mm的平面板用玻璃。且將粉末狀的鈽系研磨材料粉 末與純水混合,調製固形成分濃度1 5 w t %之研磨材漿體 50L。使用該研磨材漿體來研磨平面板用玻璃的表面。本 研磨試驗中,以5升/分之比例供給研磨材漿體,並且循環 使用研磨材漿體。設定研磨墊片對研磨面的壓力係9. 8 kPa(100g/cin2) ’研磨试驗機的旋轉速度為i〇〇rpm。 研磨值(研磨速度)之評價 研磨開始3 0分鐘後,交換研磨對象之平面板用玻璃。 且交換的平面板用玻璃係測量完重量之玻璃。且平面板用 玻璃交換後進行10分鐘的研磨,求得因研磨引起的玻璃重 量之減少量,根據該數值來求得「研磨值1」。且使用比 較例1之研磨材料的研磨值為基準(1 0 〇 )。 最初的30分鐘與其後的10分鐘之總計40分鐘的;^冑、終 了後,交換成新的平面板用玻璃,進行23小時20分鐘(姨' 計24小時)之研磨,其後,交換成研磨對象之平面板用^ 璃。且交換的平面板用玻璃係測量完重量之玻璃。+ φ & 用玻璃交換後進行10分鐘的研磨,求得因研磨引起% i璃 重量之減少量,根據該數值來求得「研磨值2」。且^ _Page 33 1303661 V. INSTRUCTION OF THE INVENTION (27) As a grinding machine, a grinding tester (HSP-21 type, manufactured by Taitung Seiki Co., Ltd.) was prepared. This polishing tester is a machine that grinds a polishing target surface with a polishing pad while supplying a polishing slurry to a polishing target surface, and the polishing pad is made of a polyurethane material, and the polishing test is performed once every 2 hours (24 hours). The left and right grinding time) is exchanged for new products. As the object to be polished, a glass for a flat plate having a diameter of 6 5 mm was prepared. Further, the powdery cerium-based abrasive powder was mixed with pure water to prepare an abrasive slurry 50 L having a solid concentration of 15 w %. The abrasive slurry is used to polish the surface of the glass for a flat sheet. In the grinding test, the abrasive slurry was supplied at a rate of 5 liters/min, and the abrasive slurry was recycled. The pressure of the polishing pad to the polishing surface was set to 9.8 kPa (100 g/cin2). The rotational speed of the polishing tester was i rpm. Evaluation of polishing value (polishing speed) After 30 minutes from the start of polishing, the glass for the flat plate to be polished was exchanged. And the exchanged flat plates are measured with a glass system to measure the weight of the glass. Further, the flat plate was polished by glass for 10 minutes, and the amount of reduction in the amount of glass due to polishing was determined. From this value, "grinding value 1" was obtained. Further, the polishing value of the abrasive material of Comparative Example 1 was used as a reference (10 〇 ). In the first 30 minutes and the next 10 minutes, a total of 40 minutes; ^, after the end, exchanged into a new flat glass, 23 hours and 20 minutes (姨 24 hours) grinding, and then exchanged into The flat plate for grinding the object is made of glass. And the exchanged flat plates are measured with a glass system to measure the weight of the glass. + φ & After the glass exchange, the polishing was performed for 10 minutes, and the amount of reduction in the weight of the % i glass due to the polishing was determined, and the "grinding value 2" was determined from the value. And ^ _

2169-6322-PF(N2).ptd 第34頁 1303661 五、發明說明(28) 使用比較例1之研磨材料的研磨值1為基準(丨〇 〇 )來求得研 磨值2。 且根據「研磨值1」及「研磨值2」,求得「研磨值比 (研磨值2/研磨值1)」,使用「研磨值1」、「研磨值2」 及「研磨值比」來評價鈽系研磨材料之研磨值(研磨速 研磨刮傷之評價 r二將經過研磨的平面板用玻璃用純水洗 淨’對於在無塵狀態下乾燥後的研磨面進行刮傷評價1 傷之評價使用30萬勒克司的鹵燈作兔 ^ ^ ^ ^ ^ ^ ^」 為光源,用反射法觀察 ,田,、,、々田,士二、七 J揚之數目點數化,滿點 1 00點,以減點方式來評價。該刮傷評 LCD用的玻璃基板之精細研磨所要电认 T 文示《取 準。具艘的,在表2及表5中,◎未的非研磨精度為判斷基 適用於HD用· LCD用玻璃基板之精細」研表98 ,二上(非常 點未滿95點以上(適用於HD用· LCD用+ ’ υ」代表98 磨),「△」代表95點未滿90點以上(听=基板之精細研 LCD用玻璃基板之精細研磨),且「χ此使用於HD用· 用於HD用· LCD用玻璃基板之精細研^、。表90點未滿(不能 附荖性試驗 進行試驗。評價 察^用載片玻璃, 中, 浸潰 且對於研磨材之附著性(洗淨性) 首先將洗淨•乾燥後的光學顯微鏡觀2169-6322-PF(N2).ptd Page 34 1303661 V. Description of Invention (28) The grinding value 2 was determined using the polishing value 1 of the polishing material of Comparative Example 1 as a reference (丨〇 〇 ). Based on the "grinding value 1" and the "grinding value 2", the "grinding value ratio (grinding value 2 / polishing value 1)" is obtained, and the "grinding value 1", the "grinding value 2", and the "grinding value ratio" are used. Evaluation of the polishing value of the lanthanum-based abrasive material (Evaluation of the grinding speed of the polishing scratches, r2, Washing the polished flat glass with pure water), and scratching the polished surface after drying in a dust-free state 1 The evaluation uses a halogen lamp of 300,000 lux for rabbit ^ ^ ^ ^ ^ ^ ^" as the light source, and observes by reflection method, the number of points of Tian,,,, Putian, Shi Er, and Qi J Yang, full point 1 00 o'clock, evaluated by the point of reduction. The scratching of the glass substrate for the LCD is required to be electrically recognized by the T text. "The exact one. For the ship, in Tables 2 and 5, ◎ the non-grinding accuracy. In order to judge the basis, it is suitable for HD and glass substrates for LCDs. Table 98, 2 (very less than 95 points (applicable for HD, LCD + 'υ) stands for 98 grinding), "△" stands for 95 points or less is less than 90 points (listening = fine polishing of the glass substrate for the substrate), and "this is used for HD." The glass substrate for LCD is finely ground. The 90 points of the table are not full. (The test can not be carried out with the test. The evaluation is to use the carrier glass, and the adhesion to the abrasive material (detergency) will be Optical microscope after washing and drying

2169-6322-PF(N2).ptd 第35頁2169-6322-PF(N2).ptd第35页

1303661 五、發明說明(29) ------- 材聚體中,取出在5『c 一旦將其乾燥,其後浸潰於 ϋ純水的容器内,進行5分鐘的超音波洗淨。超音波洗 丄將從容器中取出的載片玻璃,用純水進行流水洗 淨,知到觀察對象之載片玻璃。其後用光學顯微鏡,觀察 載片玻璃表面上殘存的研磨材粒子之殘存量,來評價附著 性。具體的,表2及表5中,「〇」代表未觀察到研磨材粒 子之殘存’非常適用於精細研磨用,「△」代表觀察到少 許研磨材粒子之殘存,適用於精細研磨用,且「X」代表 觀察到非常多的研磨材粒子殘存,不適用於精細研磨用。1303661 V. INSTRUCTIONS (29) ------- In the polymer, take out 5 "c once it is dried, then pour it into a container of pure water, and perform ultrasonic cleaning for 5 minutes. . Ultrasonic washing The carrier glass taken out from the container was washed with pure water, and the carrier glass of the observation object was known. Thereafter, the residual amount of the abrasive particles remaining on the surface of the carrier glass was observed with an optical microscope to evaluate the adhesion. Specifically, in Tables 2 and 5, "〇" means that no residue of the abrasive particles is observed, which is very suitable for fine polishing, and "△" represents that a small amount of abrasive particles are observed, which is suitable for fine polishing, and "X" means that a large amount of abrasive particles remain observed, which is not suitable for fine grinding.

第36頁 1303661 五、發明說明(30) 【表2】 硏磨材料物性 X射線衍射峰強度 硏磨特性 〇50 〇m) BET (m2/g) UOF /Ce02 LnF3 /Ce02 研磨值1 研磨值2 研磨值比 刮傷評價 附著性評犢 比較例1 1.23 3.0 0.82 <0.10 100 23 0.23 Δ △ 比較例2 1.10 3.8 0.76 <0.10 107 32 0.30 Δ Δ 寳施例1 1.13 3.5 0.62 <0.10 122 82 0,67 0 0 實施例2 1.18 3.3 0,55 <0.10 138 107 0.78 ◎ 0 實施例3 1.20 3.2 0.48 <0.10 132 87 0.66 0 0 比較例3 1.22 3.0 0.33 <0.10 115 37 0.32 Δ △ 寳施例4 0.73 4.2 0.30 <0.10 88 62 0.70 ◎ Δ 實施例5 0.95 3.7 0.46 <0.10 119 88 0.74 ◎ 0 實施例2 1.18 3.3 0.55 <0.10 138 107 0.78 ◎ 0 實施例6 1.29 2.8 0.63 0.10 151 110 0.73 0 0 賨施例7 1.52 2.4 0.83 0.21 161 106 0.66 Λ Δ 實施例8 0,91 4.0 0,47 <0.10 113 S3 0.73 ◎ Δ 實施例2 1.18 3.3 0.55 <0.10 138 107 0.78 ◎ 0 實施例9 1.41 2.6 0.61 <0.10 154 111 0.72 0 0 如表2所示,實施例卜3的研磨材料,在研磨開始後不 久(30分鐘後)的研磨值(研磨值1)高,且長時間循環°使用 後也具有較高的研磨值(研磨值2) ’因使用而引起 值之下降比較小(研磨值比=〇· 66〜0· 78)。即是,u 研磨開始後急遽的研磨值(研磨速度)之胳你疋二可以防止 維持更高的研磨值。且實施例1〜3的研磨材料,我f間地 傷不易發生、不易附著於研磨面之優點。且,’有研磨刮 示,實施例的研磨材料,其全部研磨特柯 表2所 可丨王很良好,其中實Page 36 1303661 V. Description of invention (30) [Table 2] Physical properties X-ray diffraction peak intensity honing characteristics 〇50 〇m) BET (m2/g) UOF /Ce02 LnF3 /Ce02 Grinding value 1 Grinding value 2 Grinding value evaluation compared with scratch evaluation Comparative Example 1 1.23 3.0 0.82 <0.10 100 23 0.23 Δ △ Comparative Example 2 1.10 3.8 0.76 <0.10 107 32 0.30 Δ Δ Bao Example 1 1.13 3.5 0.62 <0.10 122 82 0,67 0 0 Example 2 1.18 3.3 0,55 <0.10 138 107 0.78 ◎ 0 Example 3 1.20 3.2 0.48 <0.10 132 87 0.66 0 0 Comparative Example 3 1.22 3.0 0.33 <0.10 115 37 0.32 Δ △ Bao Example 4 0.73 4.2 0.30 < 0.10 88 62 0.70 ◎ Δ Example 5 0.95 3.7 0.46 < 0.10 119 88 0.74 ◎ 0 Example 2 1.18 3.3 0.55 < 0.10 138 107 0.78 ◎ 0 Example 6 1.29 2.8 0.63 0.10 151 110 0.73 0 0 賨 Example 7 1.52 2.4 0.83 0.21 161 106 0.66 Λ Δ Example 8 0,91 4.0 0,47 <0.10 113 S3 0.73 ◎ Δ Example 2 1.18 3.3 0.55 <0.10 138 107 0.78 ◎ 0 Implementation Example 9 1.41 2.6 0.61 <0.10 154 111 0.72 0 0 As shown in Table 2, the abrasive material of Example 3, The polishing value (grinding value 1) is high shortly after the start of polishing (after 30 minutes), and also has a high polishing value (grinding value 2) after long-term cycle use. 'The decrease in value due to use is small (grinding) Value ratio = 〇 · 66~0· 78). That is, the sharp grinding value (grinding speed) after the start of the grinding can prevent the higher grinding value from being maintained. Further, in the polishing materials of Examples 1 to 3, the damage to the ground surface was difficult to occur, and it was difficult to adhere to the polished surface. And, there is a polishing scratch, the abrasive material of the example, which is all polished by the Turk Table 2, which is very good,

2169-6322-PF(N2).ptd 第37頁 1303661 五、發明說明(31) ---- 方也例2之研磨材料的研磨特性最優良。與此相對,比較例 1〜3的研磨材料,研磨值2顯著降低,因使用而使研磨力急 遽降低t研磨值比=〇· 23〜0· 32)。且發現有容易發生研磨刮 傷、並容易附著於研磨面之問題。 因此’根據表1所示的資料,對各實施例與比較例研 討後,得出以下結論。 】研 作為鈽系研磨材料,TRE0最好在9〇wt%以上,92wt%以 上則更理想。氧化鈽佔TRE〇之重量比例(Ce〇2/TRE〇)最好係 wt %以上。且從各實施例與比較例2得知,作為鈽系研磨 材料,氧化敍佔TRE0之重量比例(Nd2 03 /TRE0)最好係16wt% 以下。^外,從各實施例與比較例3得知,作為鈽系研磨 材料,氧化敍佔TRE0之重量比例(Nd2 03 /TRE0)最好係至少 1 0 w t %以上。 作為鈽系研磨材料,氧化鑭佔TRE〇之重量比例 (La2 03 /TRE0)最好係 3〇 wt% 以下。 且用別的觀點來比較各實施例與比較例之資料(表】) 知知,作為鈽系研磨材料,氧化鑭(1^〇3)與氧化鈥(Nd2〇〇 之重量比例(La2〇3/Nd2〇3)最好係ΐ· 4以上(各實施例與比較 例2之比較),2· 8以下(各實施例與比較例1、3之比較)。 另外作為鈽系研磨材料,氧化鑭及氧化鈥的總重量佔 TREO 之比例((La2〇3 + Nd2〇3)/TRE〇)最好係 25奴%〜5〇紂%。比 較實施例2及實施例4〜7得知,作為鈽系研磨材料,氟含有 量相對於TREO之重量比(F/TRE0)最好在4〇wt%〜9〇奴%。 且作為鈽系研磨材料,鈾及鉦的總重量相對於TRE〇之2169-6322-PF(N2).ptd Page 37 1303661 V. INSTRUCTIONS (31) ---- The abrasive material of Example 2 has the best polishing characteristics. On the other hand, in the polishing materials of Comparative Examples 1 to 3, the polishing value 2 was remarkably lowered, and the polishing force was suddenly lowered by the use of the t-grinding ratio = 〇· 23 to 0·32). Further, it has been found that there is a problem that polishing scratches are likely to occur and adhesion to the polished surface is liable to occur. Therefore, based on the data shown in Table 1, after the respective examples and comparative examples were studied, the following conclusions were obtained. 】 As a lanthanide abrasive material, TRE0 is preferably at least 9 〇 wt%, more preferably 92 wt% or more. The weight ratio of cerium oxide to TRE ( (Ce 〇 2 / TRE 〇) is preferably more than wt%. Further, from each of the examples and the comparative example 2, it is preferable that the weight ratio of the oxidized phase to the TRE0 (Nd2 03 /TRE0) is 16% by weight or less as the lanthanum-based abrasive. Further, from each of Examples and Comparative Example 3, it is preferable that the weight ratio of the oxidized phase to TRE0 (Nd2 03 /TRE0) is at least 10 w % or more as the lanthanum-based abrasive. As the lanthanide abrasive material, the weight ratio of cerium oxide to TRE ( (La2 03 /TRE0) is preferably 3 〇 wt% or less. And comparing the data of each of the examples and the comparative examples (Table) by other viewpoints, knowing that as a lanthanide abrasive material, the weight ratio of yttrium oxide (1^〇3) to yttrium oxide (Nd2〇〇 (La2〇3) /Nd2〇3) is preferably ΐ·4 or more (comparison of each example with comparative example 2), and 2·8 or less (comparison of each example with comparative examples 1 and 3). Further, as a lanthanum abrasive, oxidation The ratio of the total weight of cerium and cerium oxide to TREO ((La2〇3 + Nd2〇3)/TRE〇) is preferably 25% to 5% by weight. Comparing Example 2 and Examples 4 to 7, it is known that As the lanthanide abrasive material, the weight ratio of fluorine content to TREO (F/TRE0) is preferably from 4% by weight to 9% by weight. And as the lanthanide abrasive material, the total weight of uranium and lanthanum is relative to TRE〇 It

13036611303661

重量比((U + Th)/TRE0)最好在0.05wt%以下。日 ,0 t 丨 且比較實施例 1〜3與比較例1〜3得知,上述X射線繞射峰強度比(Ln〇F/ 五、發明說明(32)The weight ratio ((U + Th) / TRE0) is preferably 0.05 wt% or less. Day, 0 t 且 and Comparative Examples 1 to 3 and Comparative Examples 1 to 3, the X-ray diffraction peak intensity ratio (Ln 〇 F / V, invention description (32)

Ce02)最好係〇· 4〜〇. 7。 另外,從各實施例可得知,研磨材料粒子之平均粒和 (D5Q )最好係0 · 7 // m〜1 · 6 // m,BET法比表面積最好係 2.0m2/g〜5.0m2/g。 '、 如表2所示,實施例2及實施例4〜7的研磨材料Ce02) is best for 〇·4~〇. 7. Further, it can be understood from the respective examples that the average particle size (D5Q) of the abrasive particles is preferably 0 · 7 // m to 1 · 6 // m, and the specific surface area of the BET method is preferably 2.0 m 2 /g to 5.0. M2/g. ', as shown in Table 2, the abrasive materials of Example 2 and Examples 4 to 7.

磨值1高,且具有較高的研磨值2,因使用而引起的研磨值 之降低比較小(研磨值比=〇 · 6 6〜0 · 7 8 )。即是,I ,、,⑭L 防jr. 磨開始後急遽的研磨值(研磨速度)之降低,更長時間地維 持更高的研磨值。但是實施例4的研磨材料與實施例2等相 比’其研磨值1及研磨值2稍低’且有少量附著性。這是因 為與實施例2等相比,TRE0量與氟量之重量比(F/treD〇) 小,且X射線繞射峰強度比(LnOF/Ce〇2)小之故。實施例7 研磨材料與實施例2等相比,研磨刮傷較容易發生,且有 少量附著性。這是因為與實施例2等相比,χ射線繞射峰 度比(1^(^/〇6〇2或11^3/〇6〇2)大之故。 另外,如表2所示,實施例2、8及9的研磨材料,其研 磨值1高,且研磨值2也相對較高,因使用而引起的研磨值 之降低相對小(研磨值比=0.72〜〇 78)。即是,可以防止 磨開始後急遽的研磨值(研磨速度)之降低,更長時間地維 研磨冑。其結果可知,使用本發明之研磨材料用 原料研磨材料時,若焙燒溫度為⑽^匚〜12〇〇c>c(85〇t 1100 C更好),可以製造研磨值(研磨速度)之下降少(研The grinding value is 1 high and has a high grinding value of 2, and the reduction in the grinding value due to use is relatively small (grinding value ratio = 〇 · 6 6 to 0 · 7 8 ). That is, I , , and 14L prevent jr. The sharpening of the grinding value (grinding speed) after the start of the grinding is performed, and the higher grinding value is maintained for a longer period of time. However, the polishing material of the fourth embodiment has a slightly lower adhesion value than the second embodiment and the polishing value of 1 and the polishing value 2, and has a small amount of adhesion. This is because the weight ratio of the TRE0 amount to the fluorine amount (F/treD〇) is smaller than that of the second embodiment and the X-ray diffraction peak intensity ratio (LnOF/Ce 〇 2) is small. Example 7 The abrasive material was more likely to be scratched than the Example 2 and the like, and had a small amount of adhesion. This is because the krypton ray radiance ratio is larger than that of the second embodiment (1^(^/〇6〇2 or 11^3/〇6〇2). In addition, as shown in Table 2, The abrasive materials of Examples 2, 8 and 9 have a high polishing value of 1 and a relatively high polishing value of 2, and the decrease in the polishing value due to use is relatively small (grinding value ratio = 0.72 to 〇78). In addition, it is possible to prevent the sharpening of the polishing value (polishing rate) after the start of the grinding, and to maintain the polishing of the crucible for a longer period of time. As a result, it is understood that when the material for polishing the raw material of the present invention is used, the baking temperature is (10)^匚~12. 〇〇c>c (better than 85〇t 1100 C), can produce a small decrease in the grinding value (grinding speed)

1303661 ........ 五、發明說明(33) 磨值比大)的研磨材料。 蓋^實施形熊 接著,將碳酸鈽、碳酸鑭、碳酸镨、碳酸鈥分別鍛燒 (焙燒)後,加以混合來調製原料,使用所調製的原料來製 造鈽系研磨材料之實施例及比較例加以說明。 首先,準備了高純度的碳酸鈽(TREO : 45wt%、 Ce02/TRE0 : 9 9· 9wt% 以上)、碳酸鑭(TREO : 45wt%、1303661 ........ V. Description of invention (33) Abrasive material with a larger grinding ratio. After the cap is formed, the barium carbonate, the barium carbonate, the barium carbonate, and the barium carbonate are calcined (calcined), and then mixed to prepare a raw material, and the prepared raw material is used to produce a tantalum-based abrasive. Explain. First, high-purity cesium carbonate (TREO: 45wt%, Ce02/TRE0: 9.99% by weight or more) and strontium carbonate (TREO: 45wt%,

La2 03 /TRE0 : 99· 9wt% 以上)、碳酸镨(TREO : 45wt%、 Pr60u/TRE0 ·· 99· 9wt% 以上)、碳酸鈦(TREO : 45wt0/〇、La2 03 /TRE0 : 99·9wt% or more), strontium carbonate (TREO: 45wt%, Pr60u/TRE0 ··99· 9wt% or more), titanium carbonate (TREO: 45wt0/〇,

Nd2 03 /TRE0 : 99· 9w t%以上),分別進行鍛燒(焙燒)。鍛燒 溫度係6 0 0 °C、鍛燒時間1 2小時。且經過鍛燒,得到碳酸 鈽鍛燒品(TREO : 83wt%、Ce02/TRE0 : 99· 9wt°/。以上、強熱 減量:17wt%)、碳酸鑭鍛燒品(TREO : 85wt°/〇、Nd2 03 /TRE0 : 99· 9w t% or more), respectively, calcination (baking). The calcination temperature is 60 ° C and the calcination time is 12 hours. And calcined to obtain a barium carbonate calcined product (TREO: 83 wt%, Ce02/TRE0: 99·9 wt ° / above, strong heat loss: 17 wt%), barium carbonate calcined product (TREO: 85 wt ° / 〇,

La2 03 /TRE0 : 99· 9wt%以上、強熱減量:i5wt%)、碳酸镨鍛 燒品(TREO : 86wt%、Pr60n/TRE0 : 99· 9wt% 以上、強熱減 量:14wt%)、碳酸鈥鍛燒品(TRE〇 : 82wt%、Nd2〇3/TREO : 9 9· 9wt%以上、強熱減量:18wt%)。 且將這樣所得的各鍛燒品混合,調製以下說明的各實 施例及比較例所使用鈽系研磨材料(中間原料)。各實施例 及比較例=使用鈽系研磨材料(中間原料)之組成如表3所 不。且將這些混合後調製的中間原料5種類之(u+T"/TRE〇 之重量比均為〇· 〇〇〇5wt%未滿,(Ca + Ba + Fe + p)/TRE〇之重量 比為0 · 1 w t %未滿。La2 03 /TRE0 : 99·9wt% or more, strong heat loss: i5wt%), barium carbonate calcined product (TREO: 86wt%, Pr60n/TRE0: 99·9wt% or more, strong heat loss: 14wt%), barium carbonate Calcined product (TRE〇: 82wt%, Nd2〇3/TREO: 9.99% by weight, strong heat loss: 18% by weight). Each of the calcined products thus obtained was mixed to prepare a lanthanum-based abrasive (intermediate raw material) used in each of the examples and comparative examples described below. Each of the examples and comparative examples = the composition of the lanthanum-based abrasive (intermediate raw material) is as shown in Table 3. And the weight ratio of (u+T"/TRE〇) of the intermediate materials prepared by mixing these are all 〇·〇〇〇5wt% underfill, and the weight ratio of (Ca + Ba + Fe + p)/TRE〇 0 · 1 wt % is not full.

1303661 五、發明說明(34) [表3】 TTffiO 稀土類氯化物乏重量土例iwt%) La2〇3/ Nd2〇3 CeOa Laa〇3 PreOli Nd203 Laa〇3+ Nda〇3 比較例6 55.0 32.0 5.0 8.0 40.0 4.00 實施例10 55.0 29.0 5.0 11,0 40.0 2,64 寳施例11 55.0 27.0 5.0 13.0 40.0 2.08 實施例12 55.0 25.0 5.0 15.0 40.0 1.67 比較例7 55.0 22.0 5.0 18.0 40.0 1.22 比較例8 43.0 34.5 4.5 18,0 52.5 1.92 實施例13 46.0 33.0 4.0 17.0 50.0 1,94 賨施例14 68.0 19.0 4.0 9.0 28.0 2.11 比較例9 72.0 16.5 3.5 8.0 24.5 2,06 實施例1 0〜1 4及比較例6〜9 : 將調製的鈽系研磨材料用原料(中間原料=稀土類碳酸 鹽鍛燒品(混合品))與該原料重量的2倍重量之純水混合, 用濕式球磨機(使用直徑5mm的氧化锆球作為粉碎媒="進 行8、小時的濕式粉碎,來得到原料漿體。所得的粉碎品 ho為0· 8 "m。且對所得的漿體實施氟化處理者 處理相同)。氟化處理後的「F/TRE〇」為8· 〇 、 :固體成分沉澱’取出上層澄清液,添加純水°進行y ’ 洗淨,將洗淨後的漿體用壓濾法過濾。且 聚化 按照順序實施乾燥、培燒、粉碎、分級 + =過據品 系研磨材料。另外,乾燥以後的各步驟之ς = ^得到鈽 相同。 y /、實施例1 上述實施例1 〇〜14及比較例6〜9所得的飾备 氟含有率、TREO、TRE0中的各稀土類元素磨材料之 ^重量比例等值1303661 V. INSTRUCTIONS (34) [Table 3] TTffiO rare earth chloride-doped soil example iwt%) La2〇3/ Nd2〇3 CeOa Laa〇3 PreOli Nd203 Laa〇3+ Nda〇3 Comparative Example 6 55.0 32.0 5.0 8.0 40.0 4.00 Example 10 55.0 29.0 5.0 11,0 40.0 2,64 Bao Shi Example 11 55.0 27.0 5.0 13.0 40.0 2.08 Example 12 55.0 25.0 5.0 15.0 40.0 1.67 Comparative Example 7 55.0 22.0 5.0 18.0 40.0 1.22 Comparative Example 8 43.0 34.5 4.5 18,0 52.5 1.92 Example 13 46.0 33.0 4.0 17.0 50.0 1,94 Example 14 68.0 19.0 4.0 9.0 28.0 2.11 Comparative Example 9 72.0 16.5 3.5 8.0 24.5 2,06 Example 1 0 to 1 4 and Comparative Example 6 to 9 : The raw material for the prepared lanthanum abrasive material (intermediate raw material = rare earth carbonate calcined product (mixed product)) is mixed with 2 times by weight of pure water of the raw material, using a wet ball mill (using a zirconia having a diameter of 5 mm) The ball was subjected to wet pulverization for 8 hours as a pulverization medium = ", and the raw material slurry was obtained. The obtained pulverized product ho was 0·8 " m. The obtained slurry was subjected to the same treatment as the fluorination treatment). "F/TRE〇" after the fluorination treatment is 8· 〇 , : solid component precipitation 'The upper layer clear liquid is taken out, pure water is added, y ' is washed, and the washed slurry is filtered by pressure filtration. And the polymerization is carried out in the order of drying, simmering, pulverizing, and grading. In addition, the ς = ^ of each step after drying is the same. y /, Example 1 The contents obtained in the above Examples 1 to 14 and Comparative Examples 6 to 9 The fluorine content, the ratio of the weight ratio of each of the rare earth element grinding materials in TREO and TRE0

2169-6322-PF(N2).ptd 第41頁 1303661 五、發明說明(35) 如表4所示。且這些研磨材料之(Ca + Ba + Fe + P)/TRE0重量 比為0 . 1 w t %未滿。 【表4】 V VV V W S' V V V ' 研磨材 枓之氟 含有辛 (wt%) 研磨材 枓之 (wt%) TREO中各稀土類氧化物之重量比例 (wt%) Laa〇3/ Nd2〇3 F(wt%) 十 TREO (wt%) F/ TREO (wt%) U十TV TREO (wt%) Ce02 Lai2〇3 PreOn Ndb〇3 La2〇3+ Nd203 比較例6 6.4 94.1 55.0 32.0 5.0 8.0 40 4.00 100.5 6.8 <0.0003 實施例10 6.2 94.2 55.0 29.0 5.0 11.0 40 2.64 1C0.4 6.6 心腦 實施例11 6.5 94.3 55.0 27.0 5.0 13.0 40 2.08 100.8 6.9 <0.00)3 實施例12 6.4 94.2 55.0 25.0 5.0 15.0 40 1.67 100.6 6.8 <0.0003 比較例? 63 94.0 55.0 22.0 5.0 18,0 40 1.22 ICO,3 6.7 ^).0CO3 比較例8 7,0 93.2 43.0 34.5 4,5 18,0 52.5 1.92 100,2 7,5 <0.0003 實施例13 6,7 93.6 46.0 33.0 4.0 17.0 50.0 1.94 ICO,3 7.2 <0.003 實施例14 6.0 94.5 68.0 19.0 4.0 9.0 28.0 2.11 100.5 6.3 <0.0003 比較例9 5.7 94.5 72.0 16.5 3,5 8.0 24,5 2.06 100.2 6.0 ^).C003 使用各實施例及比較例所得的鈽系研磨材料,測量平 均粒徑(D5Q)、BET法比表面積(BET)及繞射X射線強度 (I n d e n s i t y )。且使用各實施例及比較例所得的鈽系研磨 材料進行研磨試驗,對研磨值(研磨速度)、所得的研磨面 之刮傷評價及附著性(洗淨性)作了評價。測量方法及試驗 方法如先前說明的。且測量值及評價結果如表5所示。2169-6322-PF(N2).ptd Page 41 1303661 V. Description of invention (35) As shown in Table 4. And the weight ratio of (Ca + Ba + Fe + P) / TRE0 of these abrasive materials is 0. 1 w t % is not full. [Table 4] V VV VWS' VVV 'The fluorine content of the abrasive material 辛 (wt%) The weight of the abrasive material (wt%) The weight ratio of each rare earth oxide in the TREO (wt%) Laa〇3/ Nd2〇3 F(wt%) Ten TREO (wt%) F/ TREO (wt%) U Ten TV TREO (wt%) Ce02 Lai2〇3 PreOn Ndb〇3 La2〇3+ Nd203 Comparative Example 6 6.4 94.1 55.0 32.0 5.0 8.0 40 4.00 100.5 6.8 <0.0003 Example 10 6.2 94.2 55.0 29.0 5.0 11.0 40 2.64 1C0.4 6.6 Cardio-cerebral Example 11 6.5 94.3 55.0 27.0 5.0 13.0 40 2.08 100.8 6.9 <0.00) 3 Example 12 6.4 94.2 55.0 25.0 5.0 15.0 40 1.67 100.6 6.8 <0.0003 Comparative example? 63 94.0 55.0 22.0 5.0 18,0 40 1.22 ICO,3 6.7 ^).0CO3 Comparative Example 8 7,0 93.2 43.0 34.5 4,5 18,0 52.5 1.92 100,2 7,5 <0.0003 Example 13 6,7 93.6 46.0 33.0 4.0 17.0 50.0 1.94 ICO,3 7.2 <0.003 Example 14 6.0 94.5 68.0 19.0 4.0 9.0 28.0 2.11 100.5 6.3 <0.0003 Comparative Example 9 5.7 94.5 72.0 16.5 3,5 8.0 24,5 2.06 100.2 6.0 ^). C003 Using the lanthanum-based abrasive materials obtained in the respective Examples and Comparative Examples, the average particle diameter (D5Q), the BET specific surface area (BET), and the diffraction X-ray intensity (I ndensity) were measured. Further, the polishing test was carried out using the lanthanum-based abrasive materials obtained in the respective Examples and Comparative Examples, and the polishing value (polishing speed), the scratch evaluation of the obtained polished surface, and the adhesion (detergency) were evaluated. The measurement method and test method are as described previously. The measured values and evaluation results are shown in Table 5.

2169-6322-PF(N2).ptd 第42頁 1303661 五、發明說明(36) 【表5】 研磨材料物性 X射線衍射峰強度 研磨特性 D50 BET LnOF LnF3 研磨值1 研磨值2 mm 舌丨 附著麵 〇m) (m2/g) /CeOa /Ce〇2 比較例6 1.15 3.9 0.83 <0.10 111 33 0.30 Δ Δ 實施例10 1.19 3.6 0.65 <0.10 128 87 0.68 〇 〇 實施例11 1.24 3.5 0.53 <0.10 140 110 0.79 〇 實施例12 1.25 3.5 0.48 <0.10 131 88 0.67 〇 〇 比較例7 1.29 3.0 0.32 <DA0 116 37 0.32 Δ Δ 比較例8 0.99 4.3 ο.ω <0.10 85 26 0.31 Δ X 實施例13 1.04 4.0 0.59 <0.10 98 68 0.69 @ Δ 實施例14 1.33 2.5 0.49 135 90 0.67 〇 Δ 比較例9 1.37 2.2 0.42 <0.10 142 92 0,65 X Δ 如表5所示,各實施例的研磨材料,未使用狀態的研 磨值(研磨值1 )高,且使用完畢狀態也具有較高的研磨值 (研磨值2 ),因使用而引起的研磨值之降低比較小(研磨值 比=〇· 6 7〜〇· 7 9)。且各實施例的研磨材料有研磨刮傷不易 發生、不易附著於研磨面之優點。且實施例丨〇〜丨4中,實 施例11之研磨材料的研磨特性最優良。與此相對,各比較 例的研磨材料,研磨值2顯著降低,因使用而使研磨值(研 磨速度)急遽下降(其中比較例9除外)。且發現有容易發 研磨刮傷、並容易附著於研磨面之問題。 7知且對於表4所示的資料’比較各實施例與比較例8、9 ^二乂作為飾系研磨材料,氧化鈽佔TRE0之重量比例 例6 1 7 ^Ε〇)最好係45Wt%〜7〇Wt%。且比較各實施例與比較 仔知’作為鈽系研磨材料,氧化鈥佔TRE〇之重量比2169-6322-PF(N2).ptd Page 42 1303661 V. INSTRUCTIONS (36) [Table 5] Physical properties X-ray diffraction peak intensity Abrasive properties D50 BET LnOF LnF3 Grinding value 1 Grinding value 2 mm Tongue attachment surface 〇m) (m2/g) /CeOa /Ce〇2 Comparative Example 6 1.15 3.9 0.83 <0.10 111 33 0.30 Δ Δ Example 10 1.19 3.6 0.65 <0.10 128 87 0.68 〇〇Example 11 1.24 3.5 0.53 < 0.10 140 110 0.79 〇 Example 12 1.25 3.5 0.48 <0.10 131 88 0.67 〇〇Comparative Example 7 1.29 3.0 0.32 <DA0 116 37 0.32 Δ Δ Comparative Example 8 0.99 4.3 ο.ω <0.10 85 26 0.31 Δ X Implementation Example 13 1.04 4.0 0.59 <0.10 98 68 0.69 @ Δ Example 14 1.33 2.5 0.49 135 90 0.67 〇Δ Comparative Example 9 1.37 2.2 0.42 <0.10 142 92 0,65 X Δ As shown in Table 5, the examples of the examples The abrasive material has a high polishing value (grinding value 1) in an unused state and a high polishing value (grinding value 2) in the used state, and the reduction in the polishing value due to use is relatively small (grinding value ratio = 〇) · 6 7~〇· 7 9). Further, the abrasive materials of the respective examples have the advantage that the polishing scratches are less likely to occur and are less likely to adhere to the polished surface. Further, in Examples 丨 to 4, the polishing material of Example 11 had the most excellent polishing properties. On the other hand, in the polishing material of each comparative example, the polishing value 2 was remarkably lowered, and the polishing value (grinding speed) was drastically lowered by use (excluding Comparative Example 9). Further, it has been found to be problematic in that it is easily scratched and scratched and easily adhered to the polished surface. 7 know and for the data shown in Table 4 'Comparative Example and Comparative Example 8, 9 ^ 乂 as the decorative material of the decorative system, the weight ratio of cerium oxide to TRE0 Example 6 1 7 ^ Ε〇) is preferably 45Wt% ~7〇Wt%. And comparing the various examples and comparisons, as the lanthanide abrasive material, the weight ratio of cerium oxide to TRE 〇

13036611303661

五、發明說明(37) 例(Nd2 03 /TRE0)最好係i〇wt%〜16wt%。且如表5所示,作為 鈽系研磨材料,X射線繞射峰強度比(LnOF/Ce〇2)最好係 0· 4〜0· 7。 ' 且用別的觀點比較表4所示的各實施例與比較例之資 料得知,關於TRE0中的氧化鑭(1^2〇3)與氧化鈦(制2%)之貝重 里比例(L 〇3 / N dg 〇3 ) ’從實施例與比較例7之比較可知,最 好係1 · 4以上,從各實施例與比較例6之比較可知,最好係 2.8以下。且從實施例13、14可知,若調整氧化鑭盥化、 鈥之重量平衡,氧化鉉佔TRE〇之重量比例(Nd2〇3/TRE 9 w t %〜1 7 w t %也能得到較實用的研磨材料。 產業上的可利性 如以上說明的,本發明夕姑么 少,且能長蚌Η维括古:f鈽系研磨材料’刮傷發生 系研磨材料,彳以用更短的時門!^右使用本發明之鈽 附著少的高品質研磨面。即是::二刮傷少、%磨材料的 用於光硬碟或磁硬碟用破璃其拓=據本發明,可以提供適 表面研磨性能之領域的鈽系;^材:磨等、要求高精度的V. INSTRUCTIONS (37) The example (Nd2 03 /TRE0) is preferably i 〇 wt% 〜 16 wt%. Further, as shown in Table 5, as the lanthanum abrasive, the X-ray diffraction peak intensity ratio (LnOF/Ce 〇 2) is preferably 0·4 to 0·7. ' And comparing the data of each of the examples and the comparative examples shown in Table 4 from another point of view, the ratio of the bismuth oxide (1^2〇3) to the titanium oxide (2%) in TRE0 is known (L). 〇3 / N dg 〇3 ) ' From the comparison between the examples and the comparative example 7, it is preferable that the ratio is 1/4 or more. From the comparison between the respective examples and the comparative example 6, it is preferable that the ratio is 2.8 or less. It can be seen from Examples 13 and 14 that if the weight balance of oxidized cerium and lanthanum is adjusted, the weight ratio of cerium oxide to TRE ( (Nd2 〇 3 / TRE 9 wt % 〜 1 7 wt % can also be obtained by practical grinding. Industrial Applicability As explained above, the present invention has few eves, and can be long-lasting: the f-type abrasive material 'scratch-generating abrasive material, and the shorter time gate !^ The right side uses the high-quality polished surface with less adhesion of the present invention. That is: two less scratches, a % abrasive material for the optical hard disk or a magnetic hard disk, and the glass can be provided according to the present invention. Suitable for the field of surface grinding performance; ^ material: grinding, etc., requiring high precision

1303661 圖式簡單說明1303661 Simple description of the schema

2169-6322-PF(N2).ptd 第45頁2169-6322-PF(N2).ptd第45页

Claims (1)

1303661 _ 案號93112159_77年7月/4日_修疋不__ 六、申請專利範圍 • 1 · 一種錦系研磨材料,至少含有氧化鈽、氧化鋼及氧 化鈥作為稀土類氧化物、並含有氟,其特徵在於,全稀土 類氧化物換算重量(TRE0)為90wt%以上,氧化鈽佔全稀土 類氧化物換算重量之重量比例(Ce02/TRE0)係50wt%〜 65wt%,氟相對於全稀土類氧化物換算重量之重量比 (F/TREO)係5.0wt%〜8.0wt%,以及氧化歛佔全稀土類氧化 物換算重量之重量比例(Nd2 03 /TRE0)係10wt%〜16wt%。 2 .如申清專利範圍弟1項所述的釗5糸研磨材料,其 中,氧化鑭佔全稀土類氧化物換算重量之重量比例 (La2 03 /TRE0)係22wt%〜30wt%。 3 · —種鈽系研磨材料,至少含有氧化鈽、氧化鑭及氧 化鈦作為稀土類氧化物、並含有氟,其特徵在於,氧化鈽 佔全稀土類氧化物換算重量(TRE〇)之重量比例((^〇2/1^£:〇) 係4 5wt %〜7 0 wt%,氟相對於全稀土類氧化物換算重量之重 ,比(J/TRE0)係5.〇wt%〜8.0wt%,以及全稀土類氧化物換 算重量中氧化鑭α〜〇3)與氧化歛(Nd2〇3)之重量比例 (L a2 〇3 / N 己2 03 )係 1 · 4 〜2 · 8。 4.如申请專利範圍第3項所述的飾系研磨材料,其 中,氧化鑭與氧化鈥的總重量佔全稀土類氧化物換算重量 之比例((La2 03 +Nd2 03 )/TRE0)係 25wt% 〜50wt%。 、 5·如申請專利範圍第丨或3項所述的鈽系研磨材料,立 中,鈾與钍的總重量相對於全稀土類氧化物換算 重 量比((U+Th)/TRE0)在〇· 05wt% 以下。 里 6·如申請專利範圍第丨或3項所述的鈽系研磨材料,其1303661 _ Case No. 93112159_77 July/4 _Repairing __ VI. Patent application scope • 1 · A korea abrasive material containing at least cerium oxide, oxidized steel and cerium oxide as rare earth oxides and containing fluorine It is characterized in that the total rare earth oxide conversion weight (TRE0) is 90% by weight or more, and the weight ratio of cerium oxide to the total rare earth oxide equivalent weight (Ce02/TRE0) is 50% by weight to 655% by weight, and fluorine is relative to the total rare earth. The weight ratio of the oxide-based weight (F/TREO) is 5.0% by weight to 8.0% by weight, and the weight ratio of the oxidized weight to the total weight of the rare earth oxide (Nd2 03 /TRE0) is 10% by weight to 16% by weight. 2. The 钊5糸 abrasive material according to the patent scope of claim 1, wherein the weight ratio of cerium oxide to the total weight of the rare earth oxide (La2 03 /TRE0) is 22% by weight to 30% by weight. 3 - a lanthanum-based abrasive material containing at least cerium oxide, cerium oxide, and titanium oxide as a rare earth oxide and containing fluorine, characterized in that cerium oxide accounts for the weight ratio of the total rare earth oxide equivalent weight (TRE 〇) ((^〇2/1^£:〇) is 4 5wt %~7 0 wt%, the weight of fluorine relative to the total rare earth oxide, the ratio (J/TRE0) is 5.〇wt%~8.0wt %, and the weight ratio of yttrium oxide α~〇3) to oxidized (Nd2〇3) in the conversion weight of the total rare earth oxide (L a2 〇3 / N hex 2 03 ) is 1 · 4 〜 2 · 8. 4. The decorative abrasive according to claim 3, wherein the total weight of cerium oxide and cerium oxide is in proportion to the total weight of the rare earth oxide ((La2 03 + Nd2 03 ) / TRE0) is 25 wt. % ~ 50wt%. 5. If the lanthanide abrasive material described in the third or third paragraph of the patent application, the weight of the total weight of uranium and thorium relative to the total rare earth oxide ((U+Th)/TRE0) is at 〇 · Below 05wt%. 6) The lanthanide abrasive material as described in claim 3 or 3, 13036611303661 :’精由使用Cu-κ α線或Cu-K a 1線作為X射線源之χ射線 繞射法測量,在2 0 (繞射条、一 9 n。 q n。λα — b 、 植 k %射角)- 2 0〜3 0的乾圍出現的χ射綠 :、峰中,稀土類氟氧化物(Ln〇F)之义射線繞射峰強度、、、 =強的X曰射線繞射峰強度,與氧化鈽(Ce〇2)之χ射線繞射峰 5度中取強的X射線繞射峰強度之強度比(Ln〇F/Ce〇2)係〇 〜0 · 7 〇 · 4 7·如申請專利範圍第i或3項所述的鈽系研磨材料,其 中,研磨材料粒子之平均粒徑(D係〇· 7 〜l 6 。 ^、 8 ·如申請專利範圍第1或3項所述的鈽系研磨材料,复 中’ BET法比表面積係2· 〇m2/g〜5. 〇ffl2/g。 9 · 一種如申請專利範圍第1項所述之鈽系研磨材料用 的鈽系研磨材料用原料,至少含有氧化鈽、氧化鑭及氧化 鈦作為稀土類氧化物,其特徵在於,氧化鈽佔全稀土類氧 化物換算重量之重量比例(Ce〇2/TRE〇)係5〇¥1:%〜65对%,氟 相對於全稀土類氧化物換算重量之重量比(F/TRE〇)係未滿 〇 · 1 wt % ’以及氧化鈥佔全稀土類氧化物換算重量之重量比 例(Nd2〇3/TREO)係1 〇wt%〜16wi;%,鈾與钍的總重量相對於全 稀土類氧化物換算重量之重量比((u + Th)/TRE〇)在〇· 〇5wt% 以下。 1 0 · —種如申請專利範圍第3項所述之鈽系研磨材料用 的鈽系研磨材料用原料,至少含有氧化鈽、氧化鑭及氧化 敍作為稀土類氧化物,其特徵在於,氧化鈽佔全稀土類氧 化物換算重量之重量比例(Ce〇2/TRE〇)係45wt%〜70wt%,氟 相對於全稀土類氧化物換算重量之重量比(F/TRE〇)係未滿: 'The fine is measured by the χ ray diffraction method using the Cu-κ α line or the Cu-K a 1 line as the X-ray source, at 20 (the diffraction bar, a 9 n. qn. λα — b , plant k %射射) - 2 0~3 0 The dry circle appears in the dry green:, in the peak, the rare earth oxyfluoride (Ln〇F) ray diffraction peak intensity, ,, = strong X ray diffraction The peak intensity, the intensity ratio of the X-ray diffraction peak intensity which is strong in the χ-ray diffraction peak of cesium oxide (Ce〇2) (Ln〇F/Ce〇2) is 〇~0 · 7 〇· 4 7. The lanthanide abrasive material according to the invention of claim i or 3, wherein the average particle diameter of the abrasive particles (D system 〇·7 〜1 6 . ^, 8 · as claimed in claim 1 or 3 The lanthanum-based abrasive material described in the above section, the BET specific surface area system 2·〇m2/g~5. 〇ffl2/g. 9 · A lanthanide abrasive material as described in claim 1 The raw material for the lanthanum polishing material contains at least cerium oxide, cerium oxide, and titanium oxide as a rare earth oxide, and the cerium oxide accounts for the weight ratio of the total rare earth oxide (Ce〇2/TRE〇). 〇 1:% to 65% by weight, the weight ratio of fluorine to the total rare earth oxide equivalent weight (F/TRE〇) is less than 1·1 wt% 'and the weight ratio of cerium oxide to the total weight of the rare earth oxide (Nd2〇3/TREO) is 1 〇wt%~16wi;%, the weight ratio of the total weight of uranium and lanthanum to the weight of all rare earth oxides ((u + Th)/TRE〇) at 〇· 〇5wt The raw material of the lanthanum-based abrasive material for the lanthanum-based abrasive material according to the third aspect of the patent application, which contains at least cerium oxide, cerium oxide and oxidized cerium as a rare earth oxide, characterized in that The weight ratio of the cerium oxide to the total weight of the rare earth oxide (Ce〇2/TRE〇) is 45 wt% to 70 wt%, and the weight ratio of fluorine to the total weight of the rare earth oxide (F/TRE〇) is not full 2169-6322-PF3(N2).pt 第47頁 1303661 案號 93112159 气?年气月丨心曰 修正 六、申請專利範圍 0. 1 w t %,以及全稀土類氧化物換算重量中氧化鑭與氧化鈥 之重量比例(La2 03 / Nd2 03 )係1 · 4〜2 · 8。 (11 2169-6322-PF3(N2).ptc 第48頁2169-6322-PF3(N2).pt Page 47 1303661 Case No. 93112159 Gas? Amendment of the year of the month, the application of the patent range of 0.1% by weight, and the weight ratio of lanthanum oxide to yttrium oxide in the conversion weight of the total rare earth oxide (La2 03 / Nd2 03 ) is 1 · 4~2 · 8 . (11 2169-6322-PF3(N2).ptc第48页
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