200844052 九、發明說明： 【發明所屬之技術領域】 本發明係關於一種立方體狀氧化鎂粉末及其製法。 【先前技術】 氧化鎂（magnesia)，除耐火物以外，亦被利用作為各 種添加劑或電子零件用途、螢光體原/料、各種靶材原料、 超導體薄膜基底用原料、穿隨磁阻元件（tmr元件）用之隨 道位障原料1色電㈣示面板（PDp)用之保護膜原料、 或甚至PDP用結晶氧化鎮層之原料，為具有極為廣泛用 之無機材料，因而受到矚目。 ’、 ，例如，作為用以形成PDP用結晶氧化鎂層之原料的氧 :鎬’係要求初級粒子之形狀為立方體狀之高純度結晶粉 ’且各結晶之粒徑大、粒度分布狹窄、及分散性優異之 :化鎂粕末之製法’已知主要有以下方法：⑴使金屬 錢化之氣相法、⑺以熱分解溫度以 或碳酸鎂等前驅物進行燒成之n丨/對職化鎮 製得之塊加以粉碎。成之熱刀解法、及（3)將電炼法所 其粒===得高純度立方體狀之氧化鎂粉末，但 此外，^滿1心（參照專散獻！及非專利文獻υ。 淨之問題！ 表面會附著大量微粒，造成表面不乾 非僅由立^ # 彳體狀粒子與非立方體狀微粒，並 僅由立方體狀粒子構成之單分散粉末的問題。 200844052 以生產性更佳之熱分解法所製造之氧化鎂粉末，係具 有結晶粒子之角或稜邊帶圓之多角形形狀的粉末，且不易 製得較大之粒子。因此’會有吸附大氣中之二氧化碳或水 分等，而導致妨礙發揮氧化鎂原有特性的情況。再者，大 多僅能製得粒子互相凝集，分散性不佳之粉末。 為克服以上熱分解法之缺點，專利文獻2中記載有下 述兩種方法，亦即在將氣化铷M工、H 斤 ^ 、， 乳化物離子混合於氧化鎂前驅物或 氧化鎂之後予以燒成之方法，以及將氯化m容液與驗性 沉殿劑溶液混合後，不經洗淨，過濾後加以燒成之方法。 該文獻之實施例中，印恭古+与γΛ …』 σ己载有在乳氣流中實施前述燒成。藉 斤衣得之氧㈣結晶雖為立方體狀，但其粒徑僅在〇2 _左右’僅能製得粒子彼此凝集者（該文獻之圖2(A))。 專利文獻1 ··曰本特開平i — 號公報 專利文獻2 :日本特開2〇〇6— 36544號公報 非專利文獻1 :「材料」，昭和6 第川號，ρ·1157_1161 牛1月，弟36卷， 【發明内容】 本發明有藜於上述現爿 狀且平均% + Μ ^ 八、在於提供一種立方體 十々粒徑大的氧化鎂粉末及其製法。 本發明人等為解決上 果，發現/ u、、 覆進行各種研究後之結 化鎂粉末時，萨由在拉〜 ㈣仃燒成，製造氧 於一般燒成條k封化物離子存在Τ，且以異 ” 、才糸統貫施该燒成，可製造出習知製 6 200844052 法元全然法製得之立方體狀且平均粒徑在丨“叻以上之極 大的氧化鎂粉末，從而完成本發明。 ° 亦即，本發明係關於一種立方體狀氧化鎂粉末，其特 徵在於：以掃描型電子顯微鏡觀察之粒子形狀為立方體 狀，且以雷射繞射散射式（laser diffracU〇n s叫—咖e) 粒度分布測得之累積5〇%粒徑（〇5。)在i心爪以上。此處， 雷射繞射散射式粒度分布測得之累積1〇%粒徑⑴ = 90%粒徑(〜)之比以在1〇.〇以下較佳，B°ET、比表 面積以：0mVg以下較佳。又，純度以在99 9質量％以： 較佳。前述立方體狀氧化鎂粉末，較佳為藉由將氧化。鎂二 對於該前驅物總量有。·5〜3〇質量％之_化物： 子存在下，以封閉系統進行燒成來製得。 再者，本發明亦關於一種立方體狀氧化鎂粒子，其 徵在於：以掃描型電子顯微鏡觀察之粒子；體 ::立方體-邊之長度大於—又，亦關二 已3 °亥方體狀氧化鎂粒子之氧化鎂粉末。 μ再者，本發明亦關於一種氧化鎂粉末之製造方法，1 特徵在於：將氧化鎂前驅物在相對於該前驅物總量有- 貝1%之i化物離子存在下，以封閉系統進行 該氧化鎮前驅物較佳為驗性碳酸鎮、氫氧化鎂、或：： 混合物。 /寻之 根據本發明，可製得立方體狀且平均粒徑大的 ^末。於最佳狀況下，根據本發明可製造具有以下之 氧化鎮粉末，亦即⑴粒子形狀皆呈立方體狀、⑺平均二 200844052 :達1// m以上、(3)粒徑—致、(4)不含微粒，立方體狀結 曰曰之表面乾淨且平滑、(1)各個結晶粒均分離，分散性優異。 【實施方式】 本發明t氧化鎂粉末係初級粒+之形狀為立方體狀 者。該形狀可藉由掃描型電子顯微鏡確認。此外，「立方 體狀』非指具幾何學上意義之嚴格的立方體，如圖卜5， 係指藉由以目視觀察顯微鏡照片而可辨識出大致呈立方體 的形狀。由於本發明之氧化鎂粉末立方體狀之初級粒子不 會產生凝集，彼此分離，因此能具有分散性優異之性質。 本發明之氧化鎂粉末係平均粒徑大的粉末，具體而言， 以雷射繞射散射式粒度分布測得之累積5〇%粒徑⑴5Q)在 1 ·〇// m以上。具有此種大平均粒徑之立方體狀氧化鎂粉 末，係由本發明人等初次發現。該D5g以12//m以上較佳， 1.5 // m以上更佳。在本發明之製法的範圍内，可製得ο” ，致在2〇//m以下，或1〇//m以下之粉末。此外，〜係。 寺曰中值直徑，在粒度累積表中相當於50體積％之粒徑 )田以某粒控將粉體分成2組時，較大側與較小側呈等 量的粒徑。 再者彳欠初級粒子整體較大且不含微粉之觀點，本發 月之氧化鎂粉末，藉由BET法測得之比表面積較佳在 1 .〇m /§以下。更佳為4.0m2/g以下，再更佳為2.5m2/g以 下’知'佳為1 ·0 m2/g以下。 本卷明之氧化鎂粉末，較佳為，粒子形狀皆呈立方體 200844052 狀’微粒未附著於立方體狀結晶表面，該 因此，本發明夕与儿A、， 札乎五十滑。 虱化鎂粉末粒徑一致，亦即，叙八 狹窄者較佳，具體而言，以雷射繞射散射式粒声 之累積嶋徑㈤與累積90%粒徑(D二:二布二 係滿足1〇·〇以下者較佳。更佳為6.0以下，再更乂 1〇 以下。 1 丹更佳為4.5 0/、本毛明之乳化鎂粉末係高純度粉末，純度以99 9質曰 %以上較佳，99.99質量％以上更佳。 99.9貝！ 其-人，巩明本發明之氧化鎂粉末的製造方法。 施下11二：製造方法係根據熱分解法’本發明係藉由實 於，：…來製造氧化鎂粉末：將氧化鎂前驅物，在相： 於切驅物總量有。·5〜30 f量 對 以封閉系統進行離子存在下， 化鎂粉末。 了Ik具有上述諸特性之氧 前述氧化鎂前驅物只要為習知之埶 — 驅物即可，並無特別限定，可 /斤使用之則 酸鎮、破酸鎮、草酸鎂等。其中：由於：:：鎂、驗性碳 的特性優異，因此f聽鎂粉末 物較佳。 W軸、驗性碳_、及此等混合 若前述前驅物含有大量雜質， 形狀不會呈立方體狀，而有 之于聽鎮粉末的 此前驅物之雜質以較少為佳。且體而：狀的傾向’因 質量，係藉由熱分解法產4 j D，刖驅物所含之雜 量，較佳為不吁南化物 聽鎂時所殘留之雜質的合計 不她物離子在。.】質量％以下，更佳在。 200844052 質量％以下。 :述燒成係在ύ化物離子存在τ進行。㈣物離子， Πΐ化物離：、氣化物離子、漠化物離子、峨化物離 糸使用風化物離子。包含鹵化物離子之化合物的 等體例’可列舉鹽酸、氯化録、氯化納、氯化卸、氯化鎮 幽化物離子之存在量，係相對於氧⑽㈣㈣h 0.5〜30 f：t%之範圍。若幽化物離子之存在量過少， ^ ΓΓΓ揮本發明之效果，反之，若過多則氧化鎖之結晶 ”較佳在L0〜25質量％之範圍，更佳在10〜25 貝1 %之範圍。 :含齒化物離子之化合物，可直接為氧化鎂前驅物、 自於氧化鎂前驅物所含之雜質者、或為藉由溶液合 前=製氧化鎂前驅物時所產生之副產品、或為對氧化鎮 另外添加者、或亦可為在封閉式爐中之氣體環境氣 加例^作為氣體之氯化氫等者。又，亦可藉由洗淨 生7除去乳化鎮前驅物所含之亲隹質或調製氧化鎮時所產 中。J產σ口’再另添加於氧化鎮前驅物或氣體環境氣氛 2發明中氧化鎂前驅物，較佳為以溶液合成所製得者。 日士，當氧化鎂前驅物為鹼性碳酸鎂與氫氧化鎂之混合物 日：’在以溶液合成法調製該前驅物時，例如⑴混合氯化鎂 ^溶液與氫氧化納水溶液，以製得氫氧化錢液，⑺使該 液中之風乳化鎂之一部分碳酸化，以製得包含鹼性碳酸 10 200844052 i ^氧化鎂之漿液，（3)過濾該漿液，以製得驗性碳酸鎂 契風乳化鎮之混合物。於該混合物包含作為起始材料之氯 美或^產品之氯化納的氯化物離子。 ^述步驟⑴中，製得氫氧化镁漿液後，可藉由以水稀 車父佳為將該漿液之濃度調整至50〜l00g/L之範圍，更 仏為60〜9Gg/L之範圍。藉由降低漿液之濃度，可降低漿 液之粘度，用以使後續步驟（2)之碳酸化反應能均勻地進 行0 可述步驟（2)中，藉由將二氧化碳氣體吹入上述衆液， 使漿液中之氫氧化鎂的—部分碳酸化。此碳化反應之溫度 以40〜8G c較佳。在該溫度範圍’可迅速進行由氫氧化鎮 轉換成驗性碳酸鎂’且反應效率佳。再者，在該溫度範圍 内’可製得具有㈣效率優異之粒徑㈣性碳㈣ 化鎂的混合物。 〃礼 河述碳酸化反應所使用之二氧化碳氣體的使用量，係 ，為能使氫氧化職液中之氫氧化鎂的—部分轉換成驗性 石厌酸鎮，以供應驗性碳酸鎮與氫氧化鎮之混合物的量。具 體之二氧化碳氣體的使用量，係相對於氫氧域i莫耳:、 以0.2〜2.0莫耳當量較佳。在該範圍内，可以高效率製得 過濾㈣優異之驗性碳魏與氫氧化鎂的混合物。 产前述步驟（3)中，將前述步驟（2)所得之包含驗性碳酸錢 與風氧化㈣漿液加以過濾，而製得固體之驗性碳酸鎮斑 虱乳化鎂的混合物。由於該固態混合物含有氯化物離子:、 因此亦可不經洗淨將其直接乾燥後，進行後述之燒成 200844052 亦可使用適量之水將該混合物加以洗淨，藉此使塊狀物中 之風化物離子的量降低至適當程度後，再進行乾燥及炉 成。若充分進行洗淨，則由於氯化物離子之含量會過低， 而無法得到本發明之效果，因此必須藉由洗淨水之使用 =洗淨時間等來控制洗淨的程度。然而，亦可充分進行 子之化合物。 #另卜添加…化物離 =鎮前驅物為氯氧化鎮時，…溶液合成法調 厂〗：物，例如⑴混合氯化鎮水溶液與氫氧化鈉水溶 氫氧化鎂。該固態物含有作液， 之氯化納的氯化物離子為起始材料之氯化鎮或副產品 =步:⑴中，製得氫氧化㈣液後，藉由以水稀釋， =二之濃度較佳為調整至—g/L之範圍，更佳為 调登至60〜9〇2/T夕歆、， 、夜中夕& t 、、且較佳為再藉由熟化使該漿 液中之虱氧化鎂粒子成長。驻 率。#、f 1 ^ 稭此，可提升步驟（2)之過濾效 化條件，並無特別限定，只要在娜液下， ::保持-定時間即可。熟化溫度例…〇〜15〇。。左 右，：化時間為數分鐘〜數小時左右即可。 月1J述步驟（2)中，蔣：益、+、i 加$ 、述V驟（1)所得之氫氧化鎂的漿液 IS :寻固態之氣氧化鎂。由於該固態物含有氯化 :，口此以上述方式來處理該固態物即可。200844052 IX. DESCRIPTION OF THE INVENTION: TECHNICAL FIELD The present invention relates to a cubic magnesium oxide powder and a process for the preparation thereof. [Prior Art] Magnesia, in addition to refractory, is also used as various additives or electronic component applications, phosphor raw materials/materials, various target materials, raw materials for superconductor film substrates, and wear-through magnetoresistive elements ( The tmr element is used as a material for the protective material of the material (1) of the display panel (PDp), or a raw material for the oxidized town layer of the PDP, and is an inorganic material which is widely used. ', for example, oxygen as a raw material for forming a crystalline magnesium oxide layer for PDP: 镐' is a high-purity crystalline powder in which the shape of the primary particles is cubic, and the particle diameter of each crystal is large, the particle size distribution is narrow, and Excellent dispersibility: The method for preparing magnesium bismuth is known as follows: (1) a gas phase method in which a metal is made into a gas, and (7) a calcination at a thermal decomposition temperature or a precursor such as magnesium carbonate. The block made by the town was crushed. Into the hot knife solution, and (3) the high-purity cube-shaped magnesia powder obtained by the electro-refining method, but in addition, ^1 heart (refer to the special offer! and non-patent literature υ. The problem! The surface will adhere to a large number of particles, causing the surface to be dry. It is not only the problem of monodisperse powder composed of cubic particles and non-cubic particles, but only cubic particles. 200844052 More productive heat The magnesium oxide powder produced by the decomposition method is a powder having a polygonal shape of a corner of a crystal particle or a rounded edge, and it is difficult to produce a large particle. Therefore, it is possible to adsorb carbon dioxide or moisture in the atmosphere. In addition, in the case where the original characteristics of the magnesium oxide are impeded, the powders which are aggregated with each other and have poor dispersibility are often produced. In order to overcome the disadvantages of the above thermal decomposition method, Patent Document 2 describes the following two methods. That is, after the gasification 铷M work, the H ^ ^, the emulsion ions are mixed with the magnesium oxide precursor or the magnesium oxide, the method is fired, and the chlorinated m liquid is mixed with the test scent solution , After washing, filtering and then calcining. In the embodiment of the document, Inkang + and γ Λ 』 σ have been carried out in the milk stream to carry out the above-mentioned firing. The oxygen (4) crystal obtained by the jacket is It is a cubic shape, but its particle size is only about 〇2 _', and only particles can be agglomerated with each other (Fig. 2(A) of the document). Patent Document 1 曰本特开平i - No. Patent Document 2: Japanese Patent Laid-Open Publication No. Hei 2-6-36544 Non-Patent Document 1: "Materials", Showa 6 No. 1 Chuan, ρ·1157_1161 Niu January, 36 volumes, [Description of the Invention] The present invention is contrary to the present invention And the average % + Μ ^ 八 is to provide a magnesium oxide powder having a large particle size of a cubic cerium and a method for producing the same. The present inventors have found that, after solving the above results, it is found that / u, and coatings are subjected to various studies of the magnesiumated powder. , Sa is in the pull ~ (four) 仃 firing, the production of oxygen in the general burning of the k-seal ions in the presence of Τ, and the different, 糸 糸 施 施 该 该 该 该 , , , , , , , , , , , 2008 2008 2008 2008 2008 2008 2008 2008 2008 2008 2008 2008 2008 2008 2008 2008 The cube-like method and the average particle size of the magnesia powder above the 叻" The present invention has been completed. ° That is, the present invention relates to a cubic magnesium oxide powder characterized in that the shape of the particles observed by a scanning electron microscope is a cube shape and is laser-diffractive (laser diffrac U〇ns).叫—咖e) The cumulative particle size distribution measured by the particle size distribution (〇5.) is above the i-claw. Here, the cumulative diffraction particle size distribution measured by the laser diffraction scattering particle size distribution (1) = 90 The ratio of the % particle diameter (~) is preferably 1 Å or less, and the B ET and the specific surface area are preferably 0 mVg or less. Further, the purity is 99 9% by mass: preferably the aforementioned cubic magnesium oxide. The powder, preferably by oxidation, is present in the total amount of the precursor. · 5 to 3 〇 mass% of the compound: in the presence of a sub-unit, and fired in a closed system. Furthermore, the present invention also relates to a cubic magnesium oxide particle which is characterized by: a particle observed by a scanning electron microscope; a body: a cube-edge having a length greater than - and a Guan 2 having a 3 ° oxidized body oxidation Magnesium oxide powder of magnesium particles. Further, the present invention also relates to a method for producing a magnesium oxide powder, characterized in that the magnesium oxide precursor is subjected to a closed system in the presence of 1% of the ion of the precursor relative to the total amount of the precursor. The oxidized precursor is preferably an anatase carbonated, magnesium hydroxide, or:: mixture. / Looking for According to the present invention, it is possible to obtain a cube shape having a large average particle diameter. Under the optimal conditions, according to the present invention, the following oxidized town powder can be produced, that is, (1) the particle shape is cubic, (7) the average two 200844052: up to 1//m or more, (3) particle size-induced, (4) ) It does not contain particles, and the surface of the cubic crucible is clean and smooth. (1) Each crystal grain is separated and the dispersibility is excellent. [Embodiment] The shape of the primary magnesium oxide powder of the present invention is a cubic shape. This shape can be confirmed by a scanning electron microscope. In addition, "cube" does not refer to a geometrically rigid cube, as shown in Fig. 5, which means that a substantially cubic shape can be recognized by visually observing a microscopic photograph. Due to the magnesium oxide powder cube of the present invention. The primary particles of the form do not agglomerate and are separated from each other, so that they have excellent dispersibility. The magnesium oxide powder of the present invention is a powder having a large average particle diameter, specifically, a laser diffraction scattering particle size distribution. The cumulative particle size (1) 5Q) is 1 〇 / / m or more. The cubic magnesium oxide powder having such a large average particle diameter is first discovered by the present inventors, etc. The D5g is preferably 12/m or more. More preferably, it is 1.5 / m or more. Within the scope of the process of the present invention, a powder of 〇", which is less than 2 〇 / / m, or less than 1 〇 / / m can be obtained. In addition, ~ system. The median diameter of the temple is equivalent to 50% by volume in the particle size accumulation table. When the powder is divided into two groups by a particle control, the larger side and the smaller side have the same particle size. Further, in view of the fact that the primary particles are large and do not contain fine powder, the specific surface area of the magnesium oxide powder of the present month measured by the BET method is preferably 1. 〇m / § or less. More preferably, it is 4.0 m2/g or less, and more preferably 2.5 m2/g or less, and it is preferably 1. 0 m2/g or less. The magnesium oxide powder of the present invention preferably has a particle shape in the shape of a cube 200844052. The particles are not attached to the surface of the cubic crystal, and therefore, the present invention and the child A, are inferior. The particle size of the magnesium telluride powder is the same, that is, the stenosis is better, specifically, the cumulative diameter of the laser diffraction scattering particle sound (5) and the cumulative 90% particle size (D 2: 2nd cloth It is better to satisfy 1〇·〇. It is preferably 6.0 or less, and more preferably 1乂 or less. 1 Dan is better than 4.5 0/, and the emulsified magnesium powder of Benming is a high-purity powder with a purity of 99.9%. The above is preferable, and it is more preferably 99.99% by mass or more. 99.9 Å! The method for producing the magnesium oxide powder of the present invention is the same as the method of producing the magnesium oxide powder of the present invention. The following is a method for producing a magnesium oxide powder according to the thermal decomposition method of the present invention. ...to produce magnesium oxide powder: the magnesium oxide precursor, in the phase: the total amount of the cut-off material. · 5~30 f amount in the presence of ions in the closed system, magnesium powder. Ik has the above characteristics Oxygen The magnesium oxide precursor is not particularly limited as long as it is a known ruthenium-driver, and it can be used in acid town, acid-breaking town, magnesium oxalate, etc. Among them: due to:::magnesium, test carbon Excellent in characteristics, so it is better to listen to magnesium powder. W-axis, test carbon_, and these mixtures The precursor contains a large amount of impurities, and the shape does not have a cubic shape, and the impurities of the precursor of the powder of the town are less preferred. The tendency of the body: the shape is due to the quality, by thermal decomposition. 4 j D, the amount of impurities contained in the ruthenium drive, preferably the total amount of impurities remaining when the magnesium is not heard by the sulphate is not the mass of the ions. 】 mass% or less, more preferably. 200844052% by mass or less : The calcination system is carried out in the presence of cerium ions in the presence of telluride ions. (4) Ion ions, telluride ions: vapor ions, desert ions, and telluride ions are used in the form of halide ions. The hydrochloric acid, the chloride, the sodium chloride, the chlorination, and the chlorination of the sulphur ion are present in the range of 0.5 to 30 f: t% relative to the oxygen (10) (four) (four) h. If the amount of the scent ion is too small, ^ ΓΓΓ 本 本 本 本 本 本 本 本 本 本 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化 氧化Directly for magnesium oxide precursors, from The impurities contained in the magnesium precursor, or by-products produced by the solution before the formation of the magnesium oxide precursor, or added to the oxidation town, or may be the gas environment in the closed furnace As a gas hydrogen chloride, etc., it is also possible to remove the relatives contained in the emulsified town precursor by washing the raw material 7 or to prepare the oxidized town. Oxidation town precursor or gas atmosphere 2 In the invention, the magnesium oxide precursor is preferably prepared by solution synthesis. Japanese, when the magnesium oxide precursor is a mixture of basic magnesium carbonate and magnesium hydroxide: When the precursor is prepared by a solution synthesis method, for example, (1) mixing a magnesium chloride solution with an aqueous solution of sodium hydroxide to prepare a hydrogen peroxide solution, and (7) partially carbonating one of the emulsified magnesium in the liquid to obtain an alkaline solution. Carbonic acid 10 200844052 i ^ Magnesium oxide slurry, (3) The slurry is filtered to obtain a mixture of an experimental magnesium carbonate emulsified town. The mixture contains chloride ions of sodium chloride as a starting material or a product of sodium chloride. In the step (1), after the magnesium hydroxide slurry is obtained, the concentration of the slurry can be adjusted to a range of 50 to 100 g/L by the water thinner, and more preferably in the range of 60 to 9 Gg/L. By lowering the concentration of the slurry, the viscosity of the slurry can be lowered to uniformly perform the carbonation reaction of the subsequent step (2). In the step (2), the carbon dioxide gas is blown into the liquid. Partial carbonation of magnesium hydroxide in the slurry. The temperature of this carbonization reaction is preferably 40 to 8 Gc. In this temperature range ', it is possible to rapidly convert from hydrazine to magnesium carbonate, and the reaction efficiency is good. Further, a mixture of particle diameter (tetra) carbon (tetra)magnesium having excellent (iv) efficiency can be obtained in this temperature range. The amount of carbon dioxide gas used in the carbonation reaction of the Li River is to convert the magnesium hydroxide in the oxidizing liquid to a mineralized anaerobic town to supply the test carbonic acid and hydrogen. The amount of the mixture of oxidized towns. The amount of carbon dioxide gas used is preferably in the range of 0.2 to 2.0 mol equivalents relative to the hydroxide field. Within this range, it is possible to efficiently produce a mixture of (4) excellent inspective carbon and magnesium hydroxide. In the above step (3), the mixture of the test carbonated money and the wind-oxidized (tetra) slurry obtained in the above step (2) is filtered to obtain a solid mixture of the testable strontium carbonate and the emulsified magnesium. Since the solid mixture contains chloride ions, it can be directly dried without washing, and then calcined as described later. 200844052. The mixture can also be washed with an appropriate amount of water to weather the cake. After the amount of the ions is lowered to an appropriate level, drying and furnace formation are carried out. If the washing is sufficiently performed, the content of the chloride ions is too low, and the effect of the present invention cannot be obtained. Therefore, it is necessary to control the degree of washing by the use of washing water = washing time or the like. However, it is also possible to sufficiently carry out the compound. #其他卜添加...化化=When the town precursor is chlorine oxidation town, ...solution synthesis method factory::, for example, (1) mixed chlorination aqueous solution and sodium hydroxide water soluble magnesium hydroxide. The solid matter contains a liquid chloride, and the chloride ion of the sodium chloride is used as a chlorination town or a by-product of the starting material = step: (1), after the hydrogen (IV) solution is prepared, the concentration is reduced by diluting with water. It is better to adjust to the range of -g/L, and it is better to adjust to 60~9〇2/T, 夜, 夜夜& t, and preferably by aging to make the slurry Magnesium oxide particles grow. Resident rate. #,f 1 ^ The straw can improve the filtration efficiency of the step (2), and is not particularly limited as long as it is under the liquid, and it can be kept for a predetermined period of time. The curing temperature example...〇~15〇. . Left and right, the time is about a few minutes to several hours. In the step (2) of the month 1J, Jiang: Yi, +, i plus $, the slurry of the magnesium hydroxide obtained by the step (1) is IS: the solid gas magnesia is sought. Since the solid matter contains chlorination, the solid matter can be treated in the above manner.
本發明之藉由轨分M 物離子存在下，日氣化鎮製法中，必須在函化 以封閉系統來進行氧化鎂前驅物之燒 12 200844052 成。本發明之封閉系統，係指大致密閉成使存在於進行燒 成之空間的氣體，實質上不會流出至外部，且實質上氣體 亦不會從外部流人之系、统，與開放在大氣或氧等環境氣氛 下，或一邊使該等氣流流動一邊進行之一般燒成方法不 同。本發明係藉由在封閉系統進行燒成，#鹵化物離子不 會飛散至外部，*留在進行燒成之容n巾，以充分參與氧 化鎂粉末之結晶成長過程，藉此製得平均粒徑極大之立方 體狀結晶粉末。 此封閉系統之燒成，例如可使用實質上無環境氣氛氣 體流出或流入的密閉式電爐，或置入可密閉之掛堝來進 行。燒成時之溫度可在600t〜 1400t左右，最佳在工細 C左右。若燒成時之溫度過高，則會有所製得之結晶產生 ::導致分散性變差的情況。燒成時間雖因溫度而異，但 ::1〜10小時左右。例如，當溫度在1200。。左右時， 产“雖I5小時左右。此外’為了進行燒成而升溫時之速 又.…特別限定，但以5〜1(TC /min左右即可。 5、1匕燒5時之環境氣氛’並無特別限定，可列舉例如大 :使:驅：二氬等，但較佳為大氣或氧環境氣氛，藉此 …斤3之雜質成為氧化氣體加以去除。 狀氧:==條;=之燒成，使平均粒徑大的立方體 法充分除去前但由於係在密閉下進行燒成，因此無 入燒成後之m物離子之化合物等雜質，而會混 混入量，以提古长降低该含有齒化物離子之化合物之 呵氧化鎂粉末之純度，本發明之製造方法， 13 200844052 較佳為在前述封閉系統之—次燒成後 進行第2：：欠燒成。 放糸統 4一次燒成’可為以一般開放系統所進行之 如可在大氣環境氣氛下，以 < *々 疋成例 Μ、々—^ * 衣兄氣氣氣體流動之燃氣 盧、或在氧氣流下之電爐等來 ...... 寻术進仃。二次燒成時之溫声、 =1、及爐内之氣體，只要能除去含有齒化物離子之二 =雜質即可，並無特別限定，㈣於結晶成長已以一二I ^成全部完成’因此二次燒成之時間相對較短亦可。 ”根據本發明之製法，可製得如圖4所示之具有極大粒 役之立方體狀氧化鎂粒子。該立方體狀粒子，以掃描型電 子顯微鏡觀察時，立方體—邊之長度係大於4#m。如此 既^又無微粒、且表面乾淨又平滑之立方體狀粒子，截至 :前為止尚未被提出過。在本發明之製法的範圍内，可製 ::方體-邊之長度在2一以下、或ΙΟ/zm以下之粒子。 包含該粒子之氧化鎂粉末亦屬本發明之範圍内者。 實施例 X下’雖揭示貫施例以進一步詳細說明本發明，但本 發明並非限定於此等實施例。 以下之實施例中，係依以下所示之順序來測量各種物 性等。 (〇掃描型電子顯微鏡（SEM)觀察法In the present invention, in the presence of the orbital M ion, in the daily gasification process, it is necessary to carry out the sintering of the magnesium oxide precursor in a closed system 12 200844052. The closed system of the present invention means a gas which is substantially sealed so as to be present in a space for firing, and does not substantially flow out to the outside, and substantially does not flow from the outside to the outside, and is open to the atmosphere. The general firing method is performed under an ambient atmosphere such as oxygen or while flowing the gas streams. In the present invention, by baking in a closed system, #halide ions do not scatter to the outside, and * remain in the firing chamber to fully participate in the crystal growth process of the magnesium oxide powder, thereby obtaining an average particle. A cubic crystal powder with a very large diameter. The firing of the closed system can be carried out, for example, by using a closed electric furnace in which substantially no ambient atmosphere flows or flows in, or by placing a sealable shackle. The temperature at the time of firing can be from about 600t to about 1400t, and the optimum is about C. If the temperature at the time of firing is too high, there is a case where the resulting crystal is produced :: causing the dispersibility to deteriorate. Although the firing time varies depending on the temperature, it is about 1:1 to 10 hours. For example, when the temperature is at 1200. . In the case of the left and right, the production is "about 5 hours. In addition, the speed of the temperature rise is particularly limited, but it is 5 to 1 (about TC / min.) 'It is not particularly limited, and for example, it is large: to drive: di-argon or the like, but it is preferably an atmosphere or an oxygen atmosphere, whereby the impurities of the pound 3 are removed as an oxidizing gas. Oxygen: == strip; In the case of firing, the cubic method having a large average particle diameter is sufficiently removed, but since it is baked in a sealed state, impurities such as a compound of m-ions after firing are not formed, and the amount is mixed to increase the length. The purity of the magnesium oxide powder of the compound containing the cation ion is reduced. The method of the present invention, 13 200844052, preferably performs the second:: under-burning after the secondary firing of the closed system. A single firing 'can be carried out in a general open system, such as in an atmospheric atmosphere, with a * 々疋 々疋 Μ 々 々 ^ ^ ^ 衣 衣 ^ ^ ^ ^ 衣 、 、 、 The electric furnace, etc. come to... Seek the technique and enter the 仃. The warm sound of the second firing, =1 The gas in the furnace and the gas in the furnace are not particularly limited as long as the impurity containing the tooth ions can be removed, and (4) the crystal growth has been completed in one or two times, so that the time for the secondary firing is relatively short. According to the method of the present invention, cubic magnesia particles having extremely large granules as shown in Fig. 4 can be obtained. The cube-like particles are observed by a scanning electron microscope, and the length of the cube-edge is larger than 4#m. The cube-shaped particles which are both fine and smooth, and have a clean and smooth surface have not been proposed until now. Within the scope of the method of the present invention, the length of the square-edge can be made: Particles of 2 or less or ΙΟ/zm or less. Magnesium oxide powder containing the particles is also within the scope of the present invention. The present invention will be described in further detail by way of example X, but the invention is not limited thereto. In the following examples, various physical properties and the like were measured in the order shown below. (〇 Scanning electron microscope (SEM) observation method
使用掃描型電子顯微鏡（產品名：jSM — 5410，JEOL ^ )以拍攝SEM組成像，來觀察粒子形狀及測量立方體 狀氧化鎂一邊之長度。 14 200844052 (2) 雷射繞射散射式粒度分布測量法 使用雷射繞射散射式粒度分布測量裝置（產品名： HIRA，日機裝製），以測量累積10%粒經（D士累積5〇 %粒徑（D50)、及累積90%粒徑（〇9〇)。 ”、 (3) B E T比表面積測量法 使用比表面積測量裝置（產品名：Ma_bi2ia， Mountech製），藉由氣體吸附法測量比表面積。 (4) 氧化鎭之純度測量法 氧化鎂之純度’係由100質量％減去所測得之雜質量 之合计後之值。 、 (5) 氧化鎂之雜質量測量法 氧化鎮之雜質量（Si、A卜Ca、Fe、V、Cr、Mn、Ni、 Zn、B' Zi*、Cu、Na、K、Cl)，係使用ICP發光分析裝置（產 品名· SPS— 1700，Seiko Instruments 製），將試料溶解於 酸後加以測量。 (6) 氧化鎮别驅物之鹵化物量測量法 氧化鎂前驅物之鹵化物量，係藉由lcp發光分析裝置 (產品名· SPS - 1700，Seiko Instruments 製）來測量。 實施例1 使氫氧化鈉（NaOH)水溶液與氯化鎂（MgCl2)水溶液反 應’以製得氳氧化鎂（Mg(OH) J漿液。以離子交換水將該 氫氧化鎂漿液稀釋至漿液濃度為75g/L，一邊以1〇〇〜 15 0rpm之速度攪拌經稀釋之氧化鎂漿液3〇l，一邊吹入水 瘵氣’以將液溫調整至60°c。其次，一邊將液溫保持於6〇 15 200844052 °C，一邊以lOL/min之流量，由槽下部將c〇 2濃度100容 量％之二氧化碳氣體吹入3小時（0.8莫耳當量），使一部分 轉換成鹼性碳酸鎂。 接著，過濾此漿液，並以離子交換水20L對所製得之 塊狀物進行水洗。此後，以乾燥機在l2(rc下將該塊狀物 乾燥10小時，以製得前驅物。由X射線繞射分析之結果 可知，前驅物係氫氧化鎂與鹼性碳酸鎂（化學式：4MgC03 · Mg(〇H) 2 · 8仏0 及 4MgC〇3 · Mg(〇H)2 · 4H20)之混合物。 此時，對上述前驅物所含之氯化物離子含量進行測量後， 為3質量％。 其次，將此氫氧化鎂與鹼性碳酸鎂之混合物的前驅物， 在大氣環境氣氛下以無環境氣氛氣體流出流入之封閉式電 爐，以升溫速度6°C /min加熱至12〇〇t：，並以同溫度保持 5小時，藉此進行燒成以形成氧化鎂粉末。並且在2氣環 兄氣氛下，以有環境氣氛氣體流出流入之燃氣爐，以12〇〇 °C對其進行再燒成i小時。s !係顯示以掃描型電子顯微 鏡（15，_倍）對所製得之氧化鎮粉末進行觀察的結果1 觀察之結晶形狀大致全部為立方體狀，粒子形狀極為一 致。又’立方體狀結晶之-邊大約在1//m左右，由D9G/D ，小可知為粒度分布極窄之粉末。與後述之圖9二： 曰曰表面未附著有微粒，結晶表面平滑且乾淨。再者，各個 立方體狀結晶粒彼此充分分離。 實施例2A scanning electron microscope (product name: jSM-5410, JEOL ^) was used to take a SEM image to observe the particle shape and measure the length of the cubic magnesium oxide side. 14 200844052 (2) Laser diffraction scattering particle size distribution measurement method using laser diffraction scattering particle size distribution measuring device (product name: HIRA, Nikkiso) to measure cumulative 10% grain (D-Cumulative 5 〇% particle size (D50), and cumulative 90% particle size (〇9〇).”, (3) BET specific surface area measurement method using specific surface area measuring device (product name: Ma_bi2ia, manufactured by Mountech), by gas adsorption method The specific surface area is measured. (4) The purity of yttrium oxide is measured by the purity of magnesium oxide minus 100% by mass of the measured impurity mass. (5) Magnesium oxide mass measurement method oxidation town The impurity mass (Si, A, Ca, Fe, V, Cr, Mn, Ni, Zn, B' Zi*, Cu, Na, K, Cl) is an ICP luminescence analyzer (product name · SPS-1700, (Seiko Instruments), after the sample is dissolved in acid, it is measured. (6) The amount of halide of the oxidized township precursor is measured by the lcp luminescence analyzer (product name · SPS-1700, Measured by Seiko Instruments. Example 1 Making sodium hydroxide (NaOH) water The liquid is reacted with an aqueous solution of magnesium chloride (MgCl 2 ) to obtain a magnesium oxyhydroxide (Mg(OH) J slurry. The magnesium hydroxide slurry is diluted with ion-exchanged water to a slurry concentration of 75 g/L, and the side is at 1 Torr to 150 rpm. Stir the diluted magnesium oxide slurry 3 〇l while blowing water 瘵 gas to adjust the liquid temperature to 60 ° C. Secondly, while maintaining the liquid temperature at 6 〇 15 200844052 ° C, while lOL / min The flow rate was blown into the lower part of the tank by carbon dioxide gas having a concentration of 100% by volume of c〇2 for 3 hours (0.8 mol equivalent), and a part was converted into basic magnesium carbonate. Next, the slurry was filtered and ion-exchanged water was used for 20 L. The obtained cake was washed with water. Thereafter, the cake was dried in a dryer at 12 ° for 10 hours to obtain a precursor. As a result of X-ray diffraction analysis, the precursor was magnesium hydroxide. a mixture with basic magnesium carbonate (chemical formula: 4MgC03 · Mg(〇H) 2 · 8仏0 and 4MgC〇3 · Mg(〇H) 2 · 4H20). At this time, the chloride ion contained in the above precursor After the content was measured, it was 3% by mass. Secondly, this magnesium hydroxide was alkaline. The precursor of the mixture of magnesium and magnesium is heated to 12 〇〇t: at a heating rate of 6 ° C / min in a closed electric furnace flowing in an ambient atmosphere without ambient atmosphere, and maintained at the same temperature for 5 hours. This was fired to form a magnesium oxide powder, and it was re-fired at 12 ° C for 1 hour in an atmosphere of a gas atmosphere in an atmosphere of a gas atmosphere. The s ! shows the results of observing the obtained oxidized powder by a scanning electron microscope (15, _ times). 1 The crystal shape observed was almost all cube-shaped, and the particle shape was extremely uniform. Further, the side of the cubic crystal is about 1//m, and D9G/D is small, and it is known that the particle size distribution is extremely narrow. Fig. 9: which will be described later: The surface of the crucible is not attached with particles, and the crystal surface is smooth and clean. Further, each of the cubic crystal grains is sufficiently separated from each other. Example 2
除了將水洗步驟之離子交換水的使用量變更為1 〇L 16 200844052 外，係以與實施例1相同的順序，製得鹼性碳酸鎂與氫氧 化鎂之混合物的前驅物，並且製得氧化鎂粉末。其中 二 述前驅物所含之氯化物離子的含量為8質量y。 一 圃Z係顯 示以掃描型電子顯微鏡（15,000倍）對所製得之氧化鎂粉末 進行觀察的結果。若與實施合"相較，則立方體狀結：之 一邊變大至約Ι^ΑΠΙ左右。 實施例3 ，除了未實施水洗步驟外，係以與實施例i相同的順序， 製得驗性碳酸鎂與氫氧化鎂之混合物的前驅物，並且製得 氧化镇粉末。纟中，前述前驅物所含之氯化物離子的含量 為14質量％。圖3係顯示以掃描型電子顯微鏡。5，_倍) =所製得之氧化鎖粉末進行觀察的結果。若與實施例工相 又’則立方體狀結晶之一邊變大至約2"㈤左右。 實施例4 除了將水洗步驟之# $上 、，⑽ <離子父換水的使用量變更為30L， 亚將6N鹽酸以離子夺 你+ 又換水稀釋成約1 〇倍後添加於水洗 後、乾燥前之塊狀物以冰 制π 外’係以與實施例1相同的順序， 衣侍鹼性碳酸鎂與氫4 _ 鎮之混合物的前驅物，並且製得 虱化鎮粉末。其中，前二 Α ^ ⑺建珂驅物所含之氯化物離子的含量 為20質量％。圖4係_ — 1 對辦制〜 〜肩不以掃描型電子顯微鏡（1 5,000倍） 對所製得之氧化鎂粉 —译i , 進仃觀察的結果。立方體狀結晶之 邊達到大約4am Λ 子。 ^ ’形成極大之立方體狀氧化鎂粒 貫施例5 17 200844052 使氫氧化鈉（NaOH)溶液與氯化鎂（MgCl2)溶液反應， 以製付氫氧化鎂（Mg(〇H) J漿液。以離子交換水將該氫氧 化鎂水液稀釋至漿液濃度為75g/L，一邊以$⑼〜 之度授拌t稀釋之氧化鎂漿液3 ，一邊以高壓鋼將液 /皿保持於i 15 c，進行工小時水熱反應（hydr〇thermal reason)。接著，過濾此漿液，並以離子交換水3〇l對所 製得之塊狀物進行水洗。此後，以乾燥機在12 t下將該 塊狀物㈣10小時，以製得前驅物。此時，對上述前驅 物所含之氯化物離子含量進行測量，為丨質量％。其次， 在大氣環境氣氛下以無環境氣氛氣體流出流入之封閉式電 爐，以升溫速度6°C/min將此前驅物加熱至12〇〇χ：，並以 同溫度保# 5小時’藉此進行燒成，產生氧化鎂粉末。並 且在大氣環境氣氛下，以有環境氣體流出流人之燃氣爐， 以1200。(：對其進行再燒成i小時。 " J τ _ 5係顯不以掃描型電 子顯微鏡（15,_倍）對所製得之氧化_末進行觀察的結 果。所觀察到之結晶形狀大致全部皆為立方體狀，粒子形 狀極為一致。又，立方體狀結晶之一邊大約在〇 5以爪^ 右，由〜/〜較小可知係粒度分布範圍極為狹窄之 ： 比較例1 ^ 隊了在大氣環境下 =梅’係以與實施例1同樣方式，製得:化二爐 圖6係顯示以掃描型電子顯微鏡(15，_倍) :鎂粉末進行觀察的結果。所製得之氧化复：曰乳 未成長成立方體狀，再者，粒徑亦小且各粒子產生凝：。亚 18 200844052 比較例2A precursor of a mixture of basic magnesium carbonate and magnesium hydroxide was prepared in the same order as in Example 1 except that the amount of ion exchange water used in the water washing step was changed to 1 〇 L 16 200844052, and oxidation was obtained. Magnesium powder. The precursor ion contains a chloride ion content of 8 mass y. A 圃Z series shows the results of observation of the obtained magnesium oxide powder by a scanning electron microscope (15,000 times). If compared with the implementation, the cube-shaped knot: the side becomes larger to about Ι^ΑΠΙ. Example 3, except that the water washing step was not carried out, a precursor of a mixture of magnesium carbonate and magnesium hydroxide was obtained in the same order as in Example i, and an oxidized powder was obtained. In the crucible, the content of the chloride ion contained in the precursor is 14% by mass. Figure 3 shows a scanning electron microscope. 5, _ times) = the result of observation of the prepared oxidized lock powder. If it is working with the embodiment, then one side of the cubic crystal becomes larger to about 2" (five). Example 4 In addition to changing the amount of #10上上, (10) < ion parent water change to 30L in the water washing step, the 6N hydrochloric acid was diluted with ions and diluted to about 1 〇 times, and then added to the water after washing and before drying. The cake was made of ice in the same order as in Example 1, and a precursor of a mixture of basic magnesium carbonate and hydrogen was used, and a powder of eucalyptus was obtained. Among them, the content of chloride ions contained in the first two Α ^ (7) building materials is 20% by mass. Figure 4 is the result of the observation of the prepared magnesium oxide powder (1 5,000 times) against the prepared magnesium oxide powder. The edge of the cubic crystal reaches approximately 4am Λ. ^ 'Forming a maximal cubic magnesium oxide granules Example 5 17 200844052 A sodium hydroxide (NaOH) solution is reacted with a magnesium chloride (MgCl 2 ) solution to make a magnesium hydroxide (Mg(〇H) J slurry. The water is diluted with water to a slurry concentration of 75 g/L, and the diluted magnesium oxide slurry 3 is fed at a rate of $(9)~ while the liquid/dish is kept at i 15 c with high-pressure steel. Hour hydrothermal reaction. Then, the slurry was filtered, and the obtained cake was washed with ion-exchanged water 3 〇l. Thereafter, the cake was dried at 12 t in a dryer. (4) 10 hours to obtain a precursor. At this time, the chloride ion content contained in the precursor is measured as % by mass. Secondly, in a closed atmosphere furnace which flows into the atmosphere without ambient atmosphere in an atmospheric atmosphere. The precursor was heated to 12 〇〇χ at a heating rate of 6 ° C/min, and was fired at the same temperature for 5 hours to produce magnesium oxide powder, and in an atmospheric atmosphere, to have an environment. The gas flows out of the gas furnace of the person, with 1200 (: It was re-fired for 1 hour. " J τ _ 5 shows the result of observation of the obtained oxidation_end by a scanning electron microscope (15, _ times). Generally, all of them are in the shape of a cube, and the shape of the particles is extremely uniform. Moreover, one side of the cubic crystal is about 〇5 to the right of the claw, and the smaller than ～~~, the range of particle size distribution is extremely narrow: Comparative Example 1 ^ Team In the same manner as in the first embodiment, the atmosphere was measured in the same manner as in Example 1. Fig. 6 shows the results of observation by a scanning electron microscope (15, _ times): magnesium powder. : The milk does not grow into a cube shape, and the particle size is also small and the particles are condensed: U 18 200844052 Comparative Example 2
除了將水洗步驟之離子交換水的使 外，孫l、2 每a /丨1 j 里改變為50L ，係以"目同的順序’製得驗性碳 卜 化鎂之混合物的前驅物，並且製 …、虱軋 兀侍虱化鎂粉末。豆义 述前驅物所含之氯化物離子的含量為〇1 /、别 :不以“型電子顯微鏡(15，_倍)對所製：: ^進行觀察的結果。所製得之氧化鎮粉末其結晶：未= 成立方體狀，再者，粒徑亦小且各粒子產生凝隼。 、 比較例3 ^In addition to the ion exchange water in the water washing step, Sun 1 and 2 are changed to 50 L per a / 丨 1 j , and the precursor of the mixture of the amorphous magnesium carbide is prepared in the same order. And make ..., rolling 兀 兀 虱 magnesium powder. The content of the chloride ion contained in the precursor of the bean is 〇1, and the result is not observed by the "electron microscopy (15, _ times) of the product:: ^. The obtained oxidized powder Its crystal: not = cubic, and the particle size is also small and each particle produces coagulation. Comparative Example 3 ^
Che使：1質量％左右雜質之氫氧化鎂(Tateh。 m^InduStriesCo.，Ltd.製，純度 99 質量％，初級粒 仏〇.3〜〇.以m’比表面積3〇〜4〇m2/g)，作為氧化鎮 驅物。氯含量為〇·5質量％。其 ' ，、人在大虱％境氣氛下， 。:'核境氣氛氣體流出流入之封閉式電爐，以升溫速度6 議將此虱乳化鎂加熱至12〇〇t，並以同溫度 :下猎：m，產生氧化鎂粉末。並且在大氣環境氣 ” ，1有％境氣氛氣體流出流入之燃氣爐，以⑽ 其進行再燒成！小時。圖8係顯示以掃描型電子顯微鏡 (15,000倍）對所製得之氧化鎂粉末進行觀察的結果。在包 含1質量％左右雜質且Mg〇純度較低時，所製得之氧化 鎂雖產生粒子成長，但結晶形狀非為立方體。 比較例4 圖9係顯示以掃描型電子顯微鏡（15,〇〇〇倍）對市售之 以氣相法製造之氧化鎂粉末進行觀察的結果。雖含有立方 19 200844052 體狀結晶 非乾淨。 但同時大篁附著有微細之微粒狀結晶 表面並 比較例5 圖1〇係顯示以掃描型電子顯微鏡（15,000倍）對市隹 氧化鎂粉末進行觀察的結果。結晶非為立方體狀，再:之 粒徑亦小且各粒子產生凝集。 ’ 表1及表2 _;每》,, ·、、、貝不貫施例1〜5及比較例 粉末之物性值及雜暫曰 入摊貝ϊ的測量結果。 [表1] 貫施你丨1 _實施例2 _ 99.9 實施例3 99.9 實施例4 實施例5 MgO(質量％) 99 Q 99.9 99.99 SEM照片 目視形狀 立方體 ^__ 立方體 立方體 立方體 立方體 SEM照片 粒徑(//m) 1 1.5 2 4 0.5 D10(//m) 0.54 0.75 2.31 3.48 0.32 D50(//m) 1.50 2.41 5.31 6.13 1.05 D90("m) --- 3.07 4.0 9.74 1055 1.90 D%/ D10 5.7 5.3 4.2 To 5.9 比表面積(m2/g) 2.36 0.93 0.80 4.73 20 200844052 [表2]Che: Magnesium hydroxide of about 1% by mass of impurities (Tateh. m^InduStries Co., Ltd., purity 99% by mass, primary granules. 3~〇. with m' specific surface area 3〇~4〇m2/ g), as an oxidized town drive. The chlorine content was 〇·5% by mass. Its ',, people in the atmosphere of the big 虱%,. : 'The closed atmosphere of the nuclear atmosphere gas flowing into the furnace, heating the bismuth emulsified magnesium to 12 〇〇t at a heating rate of 6 and at the same temperature: hunting: m, to produce magnesium oxide powder. And in the atmospheric atmosphere, 1% of the atmosphere gas flows out into the gas furnace, and (10) it is re-fired! Hours. Figure 8 shows the magnesium oxide produced by scanning electron microscope (15,000 times) As a result of observation of the powder, when the impurities were contained in an amount of about 1% by mass and the purity of Mg oxime was low, the obtained magnesium oxide produced particle growth, but the crystal shape was not cubic. Comparative Example 4 FIG. 9 shows scanning electrons. Microscope (15, 〇〇〇倍) The results of observation of commercially available magnesium oxide powders produced by gas phase method. Although containing cubic 19 200844052, the crystals are not clean. However, at the same time, the large particles are attached with fine particulate crystal surface. Comparative Example 5 Fig. 1 shows the results of observation of a magnesite powder by a scanning electron microscope (15,000 times). The crystals were not cubic, and the particle size was small and the particles were aggregated. 1 and Table 2 _; Each,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,, _Example 2 _ 99.9 Example 3 9 9.9 Example 4 Example 5 MgO (% by mass) 99 Q 99.9 99.99 SEM photo visual shape cube ^__ Cube cube cube cube SEM image size (//m) 1 1.5 2 4 0.5 D10(//m) 0.54 0.75 2.31 3.48 0.32 D50(//m) 1.50 2.41 5.31 6.13 1.05 D90("m) --- 3.07 4.0 9.74 1055 1.90 D%/ D10 5.7 5.3 4.2 To 5.9 Specific surface area (m2/g) 2.36 0.93 0.80 4.73 20 200844052 [ Table 2]
SEM照片 目視形狀 , 立方體、 非立方體#立謂非立謂崎A量非立方體SEM photo visual shape, cube, non-cube #立立非立相崎 A quantity non-cube
本發明之立方體狀氧化鎮粉末，係適用作為添加劑、 填充材、電子零件用原料、醫藥品、研究室之試劑、各種 乾材原料、超導體薄膜基底膜用原料、tmr元件用隨道位 障原料、卿用保護膜原料、PDP用結日日日氧化鎂層 【圖式簡單說明】 鎮粉末的電子顯微鏡照 鎮粕末的電子顯微鏡照 鎂粉末的電子顯微鏡照 圖1，係實施例1製得之氧化 片 片 片 圖2，係實施例2製得之氧化 圖3，係實施例3製得之氧化 圖4，係實施例 製传之氧化鎂粉末的電子顯微 鏡照 21 200844052 片 片 圖5,係實…製得之氧化鎮粉末的電子顯微鏡照 片0 圖6,係比較例1製得之氧化鎂粉末的電子 顯微鏡照 圖 片 ，係比較例2製得之氧化鎂粉末 的電子顯微鏡照 圖 ，係比較例3之氡化糕伞v 士 魏鎂&末的電子顯微鏡照片。 圖9，係比較例4之氧化锃和* 礼化鎂私末的電子顯微鏡照片。 圖10，係比較例5之氧介赵私士 ^ 鎂叔末的電子顯微鏡照片。 明 主要元件符號說 22The cubic oxidized town powder of the present invention is suitable as an additive, a filler, a raw material for electronic parts, a pharmaceutical, a reagent for a laboratory, various dry materials, a raw material for a superconductor film base film, and a material for a tmr element. The protective film raw material and the PDP use day and day magnesium oxide layer [simple description of the figure] The electron microscopy of the powder of the town powder is taken as the electron microscope of the magnesium powder. FIG. 2 is an oxidation diagram prepared in Example 2, which is an oxidation diagram prepared in Example 3, and is an electron microscope photograph of the magnesium oxide powder produced in the example 21 200844052. Electron micrograph of the oxidized powder prepared by the method of Fig. 6 is an electron micrograph of the magnesium oxide powder obtained in Comparative Example 1, and is an electron microscope photograph of the magnesium oxide powder obtained in Comparative Example 2. An electron micrograph of the end of the saponin v weiwei magnesium & Figure 9 is an electron micrograph of the sputum oxide and * liquefied magnesium in Comparative Example 4. Fig. 10 is an electron micrograph of the oxygen-containing smear of Magnesium. The main component symbol says 22