200940447 六、發明說明： 【發明所屬之技術領域】 本發明係關於一種機械特性優異’且具有平滑之表面 的燒結矽晶圓。 【先前技術】 矽半導體之製造步驟中，主要使用藉由單晶提拉所製 ❺ 造之晶圓。該單晶矽晶圓隨著時代發展而不斷變大，預計 在不久之將來會達到400mm以上。並且，為了確立半導體 製造製程中所必需之裝置及周邊技術，需要試驗用之所謂 之機械晶圓（mechanical wafer )。 一般而言，由於需要進行精度相當高之試驗，因此此 種機械晶圓需要具備與單晶碎之機械物性類似之特性。因 此’以往的實際情況是’儘管為試驗用亦直接使用可實際 使用之單晶石夕晶圓。但是，4〇〇mm以上之單晶石夕晶圓非常 ❿ 昂貴’因而需要特性與單晶矽類似之廉價晶圓。 另一方面’亦提出使用由矽之矩形或圓盤狀之板所構 成的濺鍍靶，作為此種半導體製造裝置之構成零件。目前 使用濺鍍法作為薄膜之形成方法，具有2極直流濺鍍法、 咼頻率濺鍍法、磁控濺鍍法等幾種濺鍍法，係利用各自特 有之濺鍍性質來形成各種電子零件之薄膜。 此滅鑛法係使作為陽極之基板與作為陰極之乾相對 向，在惰性氣體環境下，於此等基板與靶之間施加高電壓 而產生電場者，其係利用下述原理：施加電壓而產生電場 3 200940447 時電離之電子與惰性氣體相碰撞而形成電漿，該電漿中之 陽離子碰撞靶表面而將靶構成原子擊出，此飛出之原子附 著於對向之基板表面而形成膜》 提出有使用多晶之矽燒結體來作為此濺鍍靶，但是為 了提高成膜效率，要求此燒結體靶為厚度大且大型之矩形 或圓盤狀之靶。另外’亦提出使用此多晶之矽燒結體來作 為單晶矽晶圓之保持用板。 但是，多晶矽存在燒結性差、所獲得之產品的密度低 且機械強度低的主要問題。 根據上述情況’為改善上述矽燒結體之特性而提出如 下矽燒結體：該矽燒結體係於減壓下、丨2〇〇它以上且未達 石夕之炫點之溫度範圍内，對矽粉末加熱而使之脫氧，然後 進行壓縮成形並燒製而形成者，並且，將燒結體之結晶粒 徑設定為100μιη以下（例如，參照專利文獻1 )。 另一方面，於使用作為機械晶圓之情形時，最大課題 之一在於使多晶矽燒結體具備與單晶（非晶）矽晶圓同等 之平滑性。利用先前之技術難以使多晶矽晶圓具有與非晶 發晶圓相同程度之平滑性。 上述專利文獻1中所示之多晶矽燒結體存在下述問 題.其疋全無視表面之平滑性，另外，於厚度較薄例如為 5rmn以下之情形時，密度相對增大且強度亦提高但於超 過該厚度之情形時，密度仍然較低（未達99%)，隨之導 致機械強度劣化’無法製造大型之矩形或圓盤狀之靶。 根據以上狀況，本申請人先前曾提出一種平均結晶粒 200940447 徑為50μιη以下、；I；日m & 方法（參照專利文獻2、度為"％以上之錢結體及其製造 度高等許多優點，作是要：石夕燒結趙具有密度高、機械強 M ^ ^ ^ 仁是要未進一步對此等特性加以改善， 並且亦要求對矽燒妹 晋 嗯結體表面之平滑性加以改善。 專利文獻1 ·日本特許第3342898號 專利文獻2·日本特許第38 19863號200940447 VI. Description of the Invention: [Technical Field] The present invention relates to a sintered tantalum wafer having excellent mechanical properties and having a smooth surface. [Prior Art] In the manufacturing steps of germanium semiconductors, wafers fabricated by single crystal pulling are mainly used. The single crystal germanium wafer has grown larger with the development of the times and is expected to reach 400 mm or more in the near future. Further, in order to establish a device and a peripheral technology necessary for a semiconductor manufacturing process, a so-called mechanical wafer for testing is required. In general, such mechanical wafers need to have properties similar to those of single crystal shreds due to the need for relatively high precision tests. Therefore, the 'practical situation in the past' is the use of a single crystal wafer that can be used practically for the test. However, single crystal wadding wafers of 4 〇〇 mm or more are very expensive and require inexpensive wafers having characteristics similar to those of single crystal ruthenium. On the other hand, it has been proposed to use a sputtering target composed of a rectangular or disk-shaped plate as a component of such a semiconductor manufacturing apparatus. At present, sputtering is used as a method for forming a thin film, and has two kinds of sputtering methods such as a 2-pole DC sputtering method, a 咼 frequency sputtering method, and a magnetron sputtering method, and uses various unique sputtering properties to form various electronic parts. The film. In the ore-preserving method, a substrate serving as an anode is opposed to a cathode as a cathode, and in an inert gas atmosphere, a high voltage is applied between the substrate and the target to generate an electric field, and the following principle is applied: voltage is applied. When the electric field 3 200940447 is generated, the ionized electron collides with the inert gas to form a plasma, and the cation in the plasma collides with the surface of the target to strike the target constituent atom, and the flying atom adheres to the surface of the opposite substrate to form a film. It is proposed to use a polycrystalline sintered body as the sputtering target. However, in order to improve the film formation efficiency, the sintered body target is required to have a large-sized and large rectangular or disk-shaped target. Further, it has been proposed to use this polycrystalline tantalum sintered body as a holding plate for a single crystal germanium wafer. However, polycrystalline germanium has a major problem of poor sinterability, low density of the obtained product, and low mechanical strength. According to the above situation, in order to improve the characteristics of the above-mentioned tantalum sintered body, the following sintered body is proposed: the tantalum sintered body is in a temperature range of less than 〇〇2〇〇 and less than the peak of the shovel, and the tantalum powder The film is formed by deoxidation by heating, and then formed by compression molding and firing, and the crystal grain size of the sintered body is set to 100 μm or less (for example, see Patent Document 1). On the other hand, in the case of using as a mechanical wafer, one of the biggest problems is to make the polycrystalline tantalum sintered body have the same smoothness as that of a single crystal (amorphous) germanium wafer. It is difficult to make the polysilicon wafer have the same degree of smoothness as the amorphous wafer using the prior art. The polycrystalline tantalum sintered body shown in the above Patent Document 1 has the following problems: the ruthenium is completely ignored in the smoothness of the surface, and when the thickness is as small as 5 rmn or less, the density is relatively increased and the strength is increased but exceeded. In the case of this thickness, the density is still low (less than 99%), which in turn leads to deterioration of mechanical strength, and it is impossible to manufacture a large rectangular or disk-shaped target. According to the above situation, the applicant has previously proposed an average crystal grain of 200940447 with a diameter of 50 μm or less; I; day m & method (refer to Patent Document 2, degree "% or more of the money structure and its high degree of manufacture, etc. Advantages, the work is: Shi Xi Sinter Zhao has a high density, mechanical strength M ^ ^ ^ Ren is to further improve these characteristics, and also requires the improvement of the smoothness of the surface of the 矽 妹 晋 晋 晋 。. Patent Document 1 • Japanese Patent No. 3342898 Patent Document 2 • Japanese Patent No. 38 19863
【發明内容】 本發月係馨於上述狀況而完成者，目的在於提供—種 結=結’晶圓係即便為直徑較大者亦具備固 、、°晶圓，並且視需要具有與單晶矽同等之表 面粗糙度’且機械物性及平滑性與單晶矽同等或極其類似。 為了解決上述課題，本發明人發現藉由對燒結條件下 :夫、調節結晶粒徑且限制雜質含量，可獲得機械強度提 门之燒:。夕晶圓。並且，本發明人發現藉由對燒結條件下 工夫、調節結晶方位，可獲得具有與單晶梦相同程度之表 面平滑性的燒結矽晶圓。 本發明基於上述發現而提供： 1. 一種燒結矽晶圓，其特徵在於··其最大結晶粒徑為 2〇μΐη以下，平均結晶粒徑為Ιμιη以上、ι〇μπι以下，該晶 圓所含之矽氧化物之體積比率為〇 〇1%以上、〇 2%以下矽 碳化物之體積比率為0.01%以上、〇 15%以下’金屬矽化物 之體積比率為0·006%以下。 又，本發明提供： 5 200940447 2_如上述1之燒結矽晶圓，其中，當將晶圓表面劃分成 任意多個區塊’在各個區塊中測定平均粒徑時，各區塊之 平均粒徑的偏差為士5μιη以下。 又’本發明提供： 3.如上述1或2之燒結矽晶圓，其中，上述燒結矽晶圓 中，利用X射線繞射所測定之（220 )面的強度與（i丨η 面的強度之比⑴]為二1ιη0)7 以下，且（311)面的強度與（111)面的強度之比[1(311) /工（11 1 ) ( 2 )]為0.2以上、0.4以下； 4·如上述3之燒結矽晶圓，其中’利用χ射線繞射所 測定之除（ 220)面及（3⑴面以外之面的強度與（ιιι) 面的強度之比為0.2以下； 5.如上述3或4之燒結矽晶圓，其中，在上述燒結矽晶 圓面上所測定的（220)面之面方位強度比〇)與（311) 面之面方位強度比⑺，相對於在與該晶圓面垂直之面上 所測定的各強度比⑴，及（2)，，|(1)_(ι)ί為〇1 以下 ’ | ( 2 ) — ( 2) '|為 〇.〇5 以下。 又’本發明提供： 6.如上述1至5中任一 項之燒結矽晶圓，其係直徑為 400mm 以上去，日目士·&从 ^ 1 具有自該燒㈣晶圓採集多個試驗樣品 而測疋的下述（A)〜（c)的機械特性： (A) 利用三點彎曲法 9n, 7 2 无所求得的抗彎強度之平均值為 20kg/cm 以上、50kg/cm2 以下丨 ’ (B) 拉伸強度之平均值為2〇kg/cm2以下； 200940447 (C)維克氏硬度之平均值為800以上、1200以下。 ❹ 、上可提仏種即便為大型之圓盤狀燒結矽晶 圓亦可使強度顯著提高的燒結體晶圓，且可提供—種與 使用作為機械晶圓之單晶矽的機械物性類似之燒結矽晶 圓：而且，具有下述主要特徵：由於強度高，目而不會產 生裂縫或碎屑’即便是複雜之形狀亦可容易地加工形成， 可使良率大幅度提高，降低製造成本。並且，具有下述優 異效果：可提供-種視需要而具有平滑之表面的燒結石夕晶 圓’且可提供一種與使用作為機械晶圓之單晶碎之表面粗 糙度同等或極其類似的燒結石夕晶圓。 【實施方式】 本發明提供一種燒結矽晶圓，其最大結晶粒徑為2〇μιη 乂下平均結晶粒徑為1 μηι以上、1 Ομη!以下，該晶圓所含 之碎氧化物之體積比率為以上、以下，梦碳化物 # 之體積比率為0.01%以上、0.15%以下，金屬矽化物之體積 比率為0.006%以下。 另外’作為金屬石夕化物之對象之金屬的代表例，可列 舉鉬、鶴、鉻、鐘、鈦、鐵、鈦 '鎳等，但並不限於此等 金屬’包括所有以雜質之形態所包含之金屬矽化物。 藉此’即便是直徑為4〇〇mm以上之燒結矽晶圓，亦可 容易地使該晶圓之利用三點彎曲法所求得的抗弯i強度（弯 曲強度）之平均值為2〇kg/cm2以上、50kg/cm2以下，拉伸 強度之平均值為2〇kg/cm2以下’維克氏硬度之平均值為8〇〇 200940447 以上、1200以下。此亦係與單晶晶圓之機械特性—致之條 件。 '、 η·&二文付傲.藉由對上述 燒結矽晶圓之結晶粒徑加以調整，或對燒結矽晶圓所含之 本發明之燒結石夕 可分別單獨 以調整及操 矽氧化物、矽碳化物、金屬矽化物加以限制， 地使機械特性得到改善，藉由對兩者同時加 作，可更容易地實現機械特性之改善。 要提高上述機械特性時，結晶粒徑之微細化非常重 要。最大結晶粒徑超過20μιη，平均結晶粒徑未達“μ、超 過ΙΟμηι之燒結矽晶圓無法達成上述機械特性亦即"1^用三 點彎曲法所求得的抗彎強度之平均值為2〇kg/cm2 : 50kg/cm2’拉伸強度之平均值為2〇kg/cm2以下維克氏硬 度之平均值為800〜1200。 調整燒結矽晶圓之結晶粒徑之偏差，亦即將晶圓表面 劃分成任意多個區塊，在各個區塊中測定平均粒徑時各 區塊之平均粒徑的偏差為±5μιη以下亦為重要。其目的在於 實現晶圓組織之均一性，此係與上述機械特性之均一化直 接相關’可更有效地防止切口或裂縫。 另外’矽氧化物、矽碳化物、金屬矽化物之存在量亦 較為重要。於改善燒結矽晶圓之機械特性之意義上而言， 使該晶圓所含之矽氧化物之體積比率為〇 〇1%以上、 以下，矽碳化物之體積比率為〇〇1%以上、〇 15❶以下金 屬梦化物之體積比率為0·006%以下具有重大作用。 藉此’可使即便是直徑為·mm以上之燒結梦晶圓亦 200940447 更容易達成上述機械特性：該晶圓之利用三點彎曲法所求 得的抗t強度（f曲強度）之平均值為2〇kg/cm2以上、 5〇kg/cm2以下，拉伸強度之平均值為2〇kg/cm2以下，維克 氏硬度之平均值為800以上、1200以下。SUMMARY OF THE INVENTION The present invention is completed in the above-mentioned situation, and the purpose is to provide a seeding-junction wafer system having a solid, a wafer, and a single crystal, if necessary, even if the diameter is larger.矽Equivalent surface roughness' and mechanical properties and smoothness are equal or extremely similar to single crystal ruthenium. In order to solve the above problems, the inventors have found that mechanical strength can be obtained by sintering under the conditions of sintering, adjusting the crystal grain size, and limiting the impurity content. Xi wafer. Further, the inventors have found that a sintered tantalum wafer having the same surface smoothness as that of a single crystal dream can be obtained by adjusting the crystal orientation under sintering conditions. The present invention is based on the above findings: 1. A sintered tantalum wafer characterized in that the maximum crystal grain size is 2 〇μΐη or less, and the average crystal grain size is Ιμιη or more, ι〇μπι or less, and the wafer contains The volume ratio of the niobium oxide is 〇〇1% or more, 〇2% or less, and the volume ratio of the niobium carbide is 0.01% or more and 〇15% or less. The volume ratio of the metal telluride is 0.006% or less. Further, the present invention provides: 5 200940447 2 - The sintered tantalum wafer according to the above 1, wherein when the wafer surface is divided into any plurality of blocks 'the average particle diameter is measured in each block, the average of the blocks The deviation of the particle diameter is less than or equal to 5 μmη. Further, the present invention provides: 3. The sintered tantalum wafer according to the above 1 or 2, wherein the intensity of the (220) plane and the intensity of the (i) surface are measured by X-ray diffraction in the sintered tantalum wafer. The ratio (1)] is two or more, and the ratio of the strength of the (311) plane to the intensity of the (111) plane [1 (311) / work (11 1 ) (2)] is 0.2 or more and 0.4 or less; - the sintered tantalum wafer according to the above 3, wherein the ratio of the intensity of the (220) plane and the surface of the (3 (1) plane and the intensity of the (ιιι) plane measured by the x-ray diffraction is 0.2 or less; The sintered tantalum wafer of the above 3 or 4, wherein the plane orientation intensity ratio (〇) of the (220) plane measured on the surface of the sintered tantalum wafer and the surface orientation intensity ratio (7) of the (311) plane are relative to The intensity ratios measured on the vertical plane of the wafer surface (1), and (2),, |(1)_(ι)ί are 〇1 or less ' | ( 2 ) — ( 2) '|为〇.〇 5 below. Further, the present invention provides: 6. The sintered tantalum wafer according to any one of the above 1 to 5, wherein the diameter of the sintered tantalum wafer is 400 mm or more, and the Japanese meter has a plurality of wafers collected from the fired (four) wafer. The mechanical properties of the following (A) to (c) measured by the test sample: (A) Using the three-point bending method 9n, 7 2 The average value of the bending strength which is not obtained is 20 kg/cm or more and 50 kg/ Cm2 or less 丨' (B) The average value of tensile strength is 2〇kg/cm2 or less; 200940447 (C) The average value of Vickers hardness is 800 or more and 1200 or less. ❹ 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上 上Sintered tantalum wafer: Moreover, it has the following main features: because of its high strength, it does not cause cracks or debris. Even if it is a complicated shape, it can be easily formed, which can greatly improve the yield and reduce the manufacturing cost. . Moreover, it has the excellent effect of providing a sintered sacrificial wafer having a smooth surface as needed and providing a burning equivalent to or very similar to the surface roughness of a single crystal used as a mechanical wafer. Stone eve wafer. [Embodiment] The present invention provides a sintered tantalum wafer having a maximum crystal grain size of 2 〇μηη, an average crystal grain size of 1 μηι or more, 1 Ομη! or less, and a volume ratio of the broken oxide contained in the wafer. In the above and below, the volume ratio of the dream carbide # is 0.01% or more and 0.15% or less, and the volume ratio of the metal telluride is 0.006% or less. In addition, as a representative example of the metal which is a target of the metal ceramide, molybdenum, crane, chromium, bell, titanium, iron, titanium 'nickel, etc., but not limited to these metals' includes all of them in the form of impurities. Metal halide. Therefore, even in the case of a sintered tantalum wafer having a diameter of 4 mm or more, the average value of the bending i strength (bending strength) obtained by the three-point bending method of the wafer can be easily made 2 〇. Kg/cm2 or more and 50 kg/cm2 or less, the average value of the tensile strength is 2 〇kg/cm2 or less. The average value of the Vickers hardness is 8〇〇200940447 or more and 1200 or less. This is also due to the mechanical properties of the single crystal wafer. ', η·& 二文付傲. By adjusting the crystal grain size of the sintered germanium wafer, or the sintered stone of the present invention contained in the sintered germanium wafer can be separately adjusted and manipulated The physical properties, the niobium carbide, and the metal halide are limited, and the mechanical properties are improved. By simultaneously adding the two, the improvement of the mechanical properties can be more easily achieved. When the above mechanical properties are to be improved, it is important to refine the crystal grain size. The maximum crystal grain size exceeds 20 μm, and the average crystal grain size is less than "μ, and the sintered 矽 wafer exceeding ΙΟμηι cannot achieve the above mechanical properties, that is, the average value of the bending strength obtained by the three-point bending method is 2〇kg/cm2: 50kg/cm2' The average value of tensile strength is 2〇kg/cm2 or less. The average value of Vickers hardness is 800~1200. Adjusting the deviation of the crystal grain size of the sintered tantalum wafer is also the crystal The circular surface is divided into any number of blocks, and it is also important to measure the average particle diameter of each block when the average particle diameter is measured within each block to be ±5 μm or less. The purpose is to achieve uniformity of wafer structure. It is directly related to the homogenization of the above mechanical properties, which can prevent cuts or cracks more effectively. In addition, the presence of niobium oxide, tantalum carbide and metal telluride is also important to improve the mechanical properties of sintered tantalum wafers. In the above, the volume ratio of the tantalum oxide contained in the wafer is 〇〇1% or more, and the volume ratio of the tantalum carbide is 〇〇1% or more, and the volume ratio of the metal dreaming compound of 〇15❶ or less is 0. ·006% or less This makes it possible to achieve even the above mechanical properties even for sintered dream wafers with a diameter of more than mm and 200940447: the tensile strength (f-bend strength) obtained by the three-point bending method of the wafer The average value is 2〇kg/cm2 or more and 5〇kg/cm2 or less, and the average value of the tensile strength is 2〇kg/cm2 or less, and the average value of the Vickers hardness is 800 or more and 1200 or less.
Ο 石夕氧化物為體積比率超過0.2%之量、矽碳化物為體積 比率超過0.15%之量、金屬矽化物為體積比率超過〇〇〇6% 之量的燒結矽晶圓，難以達成符合單晶晶圓之機械特性的 機械特性，亦即利用三點彎曲法所求得的抗彎強度之平均 值為20kg/cm2〜50kg/cm2，拉伸強度之平均值2〇kg/cm2以 下，維克氏硬度之平均值800〜12〇〇β矽氧化物之下限值的 體積比率未達0.01%、矽碳化物之體積比率未達〇 〇1%時並 =存在實際損害，但是會引起精製成本上升且並不有效 率，因而將其設定為下限值。金屬矽化物亦相同，但並不 特別設置下限值。總之，較佳為儘可能地小。 此種矽燒結體晶圓之機械強度高、富於加工性，因而 不僅可使用作為機械晶圓（或仿真晶圓（dummy wafer))， 亦可使用作為濺鍍靶或半導體製造裝置之托板等各種零 件。 本發明之燒結矽晶圓具有下述主要特徵：製作零件 時，燒結矽晶圓不會產生裂縫或碎屑，即便是複雜之形狀 亦可容易地加工形成，可大幅度提高良率，降低製造成本。 根據上述，本發明提供一種直徑為4〇〇mm以上的燒結 矽晶圓，此燒結矽晶圓之利用三點彎曲法所求得的抗彎強 度之平均值為2〇kg/cm2以上、5〇kg/cm2以下，拉伸強度之 9 200940447 平均值為20kg/cm2以下，維克氏硬度之平均值為800以上、 1200以下。先前並不存在具備此特性之直徑為4〇〇mm以上 之燒結矽晶圓。 另外，要求燒結矽晶圓具有與單晶矽之表面粗糙度同 等之表面粗糙度時，有效的是使利用X射線繞射所測定之 (220 )面的強度與（i丨丨）面的強度之比r ( 220 ) /1 ( 1 11 ) (1)]為0.4以上、0.7以下，且（311)面的強度與（iii) 面的強度之比[I ( 311) /1 ( 111) (2)]為0.2以上、0.4 以下。藉此’可使表面粗糙度（表面平均粗糙度）Ra在〇 〇2μιη 以下，甚至Ra可在0.01 μηι以下。與上述單晶矽之表面粗 糙度同等之表面粗糙度，係藉由調節燒結矽晶圓之結晶方 位而實現’偏離上述結晶方位的燒結矽晶圓無法具備與單 晶石夕同等之表面粗糖度。 但是容易理解’欲使燒結矽晶圓具有與單晶石夕之表面 粗糙度同等之表面粗糙度時，才需要達成此表面粗糙度， 當無此需要時，並不需要調整上述利用X射線繞射所測定 之面強度。 再者’具備上述結晶方位之燒結矽晶圓可同時使機械 特性提高。應當可理解，上述藉由調整結晶方位與限制雜 質來提高機械強度並不矛盾。 ” 因此，本發明可提供一種燒結矽晶圓，其具備與單晶 矽之表面粗糙度同等或極其近似之表面粗糙 9 人 亚即便 是直徑為40〇mm以上之燒結矽晶圓，亦具有如下機械特 性：該晶圓之利用三點彎曲法所求得的抗彎強声' V号曲強 200940447 • ,平句值為20kg/cm2以上、50kg/cm2以下，拉伸強度 之平均值為2〇kg/cm2以下，維克氏硬度之平均值為_以 、00以下。此係與單晶晶圓之機械特性一致之條件。 並且，本發明提供一種燒結矽晶圓，其利用χ射線繞 射所測定之除（220 )面及（3 i!)面以外之面的強度與（】i i ) 面的強度之比為0.2以下。 利用X射線繞射所測定之除（220)面及（311)面以 ❿夕卜，面方位，可列舉（400) A (331)。此等面方位由於 會損害平滑性，因而較佳為儘可能地少。 另卜較佳為，在上述燒結石夕晶圓面上所測定的（220) 面之面方位強度比⑴肖（3 1 i )面之面方位強度比（2 )， 相對於在與該晶圓面垂直之面上所測定的各強度比⑴， 及（2) ’ ’丨（1) — ( 1)，丨為（M以下，丨（2) — (2)，丨為 〇.〇5以τ。亦即，當石夕晶圓之面方位為均—時，可使燒結 石夕晶圓具有與單晶石夕晶圓共通之特性，因而較佳。 _ 。矽燒結體之製造方法’例如藉由於減壓下、n〇〇〜13〇〇 °C之範圍、難為未達12〇crc下，對利用喷射磨機將…以 上之高純度妙之粗粒加以粉碎而製造的石夕粉末進行供培而 使之脫氧’然後於12〇〇〜142(rc之範圍、壓力為雌大氣 壓以上進行腑處理，可製造如下燒結石夕晶圓：其最大結 晶粒徑為20μηι以下，平均結晶粒徑為1μιη以上、丨…爪以 下，且該晶圓所含之石夕氧化物之體積比率為〇〇ι%以上、 0.2%以下，矽碳化物之體積比率為〇 〇1%以上、〇 Η%以下， 金屬矽化物之體積比率為〇 〇〇6%以下。 200940447 於此情形時，可藉ώ估田古 粉末，採用師之脫妙粉末以及粉碎此 來調整“Ι ΗΙΡ處理之溫度及加屢條件， 調整”曰粒徑，可調節燒結條件，以使最大結晶粒徑為 以下，平均結晶粒徑為ΐμιη以上' 1〇㈣以下。上述 紐之條件中，未達12⑼。c 1力未達議大氣麼時同 樣地無法獲得高密度之石夕燒結體，同樣地，_時由於 超過S!之炼點，因而亦無法獲得高密度之石夕燒結體。可理 解上㈣培之主要制以使燒結原料脫氧，較佳為5小時Ο 夕 氧化物 oxide is a volume ratio of more than 0.2%, bismuth carbide is more than 0.15% by volume, and metal bismuth is a sintered ruthenium wafer having a volume ratio of more than 〇〇〇6%. The mechanical properties of the mechanical properties of the crystal wafer, that is, the average bending strength obtained by the three-point bending method is 20 kg/cm 2 to 50 kg/cm 2 , and the average tensile strength is 2 〇 kg/cm 2 or less. The volume ratio of the average value of Kelvin hardness of 800~12〇〇β矽 oxide is less than 0.01%, and the volume ratio of barium carbide is less than 1% and there is actual damage, but it will cause refining. The cost rises and is not efficient, so it is set to the lower limit. The metal halide is also the same, but the lower limit is not particularly set. In short, it is preferably as small as possible. Such a sintered ceramic wafer has high mechanical strength and is highly processable, and thus can be used not only as a mechanical wafer (or a dummy wafer) but also as a sputtering target or a semiconductor manufacturing apparatus. And other parts. The sintered tantalum wafer of the present invention has the following main features: when the part is produced, the sintered tantalum wafer does not generate cracks or debris, and even a complicated shape can be easily formed, which can greatly improve the yield and reduce the manufacturing. cost. According to the above, the present invention provides a sintered tantalum wafer having a diameter of 4 mm or more, and the average value of the bending strength of the sintered tantalum wafer obtained by the three-point bending method is 2 〇kg/cm 2 or more, 5 〇kg/cm2 or less, the tensile strength of 9 200940447 The average value is 20 kg/cm2 or less, and the average Vickers hardness is 800 or more and 1200 or less. A sintered tantalum wafer having a diameter of 4 mm or more having such characteristics has not previously existed. Further, when the sintered tantalum wafer is required to have the same surface roughness as that of the single crystal tantalum, it is effective to make the intensity of the (220) plane and the strength of the (i) plane measured by X-ray diffraction. The ratio r ( 220 ) /1 ( 1 11 ) (1)] is 0.4 or more and 0.7 or less, and the ratio of the strength of the (311) plane to the strength of the (iii) plane [I ( 311 ) / 1 ( 111 ) ( 2)] is 0.2 or more and 0.4 or less. Thereby, the surface roughness (surface average roughness) Ra can be made 〇 2 μηη or less, and even Ra can be 0.01 μηη or less. The surface roughness equivalent to the surface roughness of the above single crystal crucible is achieved by adjusting the crystal orientation of the sintered germanium wafer. The sintered germanium wafer which deviates from the above crystal orientation cannot have the same surface roughness as the single crystal stone. . However, it is easy to understand that it is necessary to achieve this surface roughness when the sintered tantalum wafer has the same surface roughness as that of the single crystal stone. When it is not necessary, it is not necessary to adjust the above-mentioned X-ray winding. The measured surface strength of the shot. Furthermore, the sintered tantalum wafer having the above crystal orientation can simultaneously improve the mechanical properties. It should be understood that the above is not contradictory by adjusting the crystal orientation and limiting the impurities to increase the mechanical strength. Therefore, the present invention can provide a sintered tantalum wafer having a surface roughness equal to or extremely similar to that of a single crystal tantalum. Even a sintered tantalum wafer having a diameter of 40 mm or more has the following Mechanical characteristics: The bending resistance of the wafer is determined by the three-point bending method. 'V No. 200940447 • The value of the flat sentence is 20kg/cm2 or more and 50kg/cm2 or less. The average tensile strength is 2 〇kg/cm2 or less, the average value of Vickers hardness is _, 00 or less. This is a condition consistent with the mechanical properties of the single crystal wafer. Moreover, the present invention provides a sintered tantalum wafer which utilizes χ-ray winding The ratio of the intensity of the surface other than the (220) plane and the (3 i!) plane measured by the shot to the intensity of the surface of (ii) is 0.2 or less. The (220) plane and (measured by X-ray diffraction) 311) The surface is in the form of a surface, and the surface orientation is (400) A (331). These surface orientations are preferably as small as possible because they impair the smoothness. The azimuth intensity ratio of the (220) plane measured on the wafer surface (1) the surface of the (3 1 i) plane The bit intensity ratio (2) is relative to each intensity ratio (1) measured on a plane perpendicular to the wafer surface, and (2) ' '丨(1) - (1), 丨 is (M or less, 丨( 2) — (2), 丨 is 〇. 〇 5 is τ. That is, when the surface orientation of the Shi Xi wafer is uniform, the sintered shi wafer can have the characteristics common to the single crystal wafer. Therefore, it is preferable to use a jet mill, for example, by a method of manufacturing a sintered body of 矽, for example, by a range of n 〇〇 to 13 〇〇 ° C under reduced pressure, and it is difficult to use a jet mill. The high-purity coarse-grained coarse-grained granules are pulverized and prepared for deoxidation. Then, in the range of 12 〇〇 to 142 (the range of rc and the pressure is above the atmospheric pressure, the sputum can be produced as follows) Round: the maximum crystal grain size is 20 μm or less, the average crystal grain size is 1 μm or more, and the crest is equal to or less than the claw, and the volume ratio of the Osmanthus oxide contained in the wafer is 〇〇ι% or more and 0.2% or less. The volume ratio of the carbide is 〇〇1% or more and 〇Η% or less, and the volume ratio of the metal ruthenium is 〇〇〇6% or less. 200940447 In this case, you can use the ώ 古 古 古 古 powder, use the teacher's powder and smash to adjust the temperature and conditions of the Ι ΗΙΡ treatment, adjust the 曰 particle size, can adjust the sintering conditions, so as to maximize The crystal grain size is below, and the average crystal grain size is ΐμιη or more and is less than or equal to 12 (9). The condition of the above-mentioned neon is less than 12 (9). When the c 1 force does not reach the atmosphere, the high-density Shishi sintered body cannot be obtained in the same manner. Similarly, when _ exceeds the refining point of S!, it is impossible to obtain a high-density sinter sintered body. It is understood that the main process of (four) cultivating is to deoxidize the sintered raw material, preferably 5 hours.
左右’但由於其係根據原料之條# (品f)之不同而實施 者’因此非必要條件而是較佳條件。 另外，上述熱壓係進行1〇小時左右。較佳為進一步實 施3小時左右之HIP處理。長時間之HIp處理會導致晶粒 的粗大化，故不佳。但是，此等時間可根據處理條件作適 當變更’並不限於上述處理時間。 並且’藉由使用高純度之矽粉末以及粉碎此粉末，採 用烘焙之脫氧條件、HIP處理之溫度及加壓條件，可調整上 述雜質含量》 〇 而且’脫氧為重要，為了獲得微細結晶之矽燒結體， 必須充分地進行脫氧。將烘焙溫度設為1〇〇〇〜13〇〇°c、較 佳為未達1200。(：的原因在於，若未達1〇〇〇。(：則無法將氧充 分地去除。 氡之存在係助長直接形成矽氧化物之主要因素。另 外’若為1200°C以上，則會存在下述缺點：雖脫氧得以進 行，但頸縮（necking )(粉與粉相互緊貼之現象）増多， 12 200940447 . 熱壓時即便解除頸縮，粒度分布亦會出現不均，而且作業 時間變長。因此，須將上限溫度設為13〇(rc。 並且’藉由使用高純度之矽粉末以及粉碎此粉末，採 用烘焙之脫氧條件、HIP處理之溫度及加壓條件，可調整結 晶方位。亦即可獲得下述燒結矽晶圓：利用χ射線繞射所 測定之（220 )面的強度與（丨i丨）面的強度之比口（ 22〇 ) 71 ( U1) (丨）]為0.4以上、〇.7以下，且（311)面的 ❹ 強度與（n 1 )面的強度之比[I ( 3 11 ) /1 ( 111 ) ( 2)] 為0.2以上、〇.4以下。 [實施例] 以下，根據實施例來說明本發明。再者，以下實施例 係用以能夠容易理解發明者，本發明並不限於此等實施 例。亦即，基於本發明之技術思想之其他例或變形當然亦 包含於本發明。 (實施例1 ) φ 於減壓下且使脱度上升至1，對利用喷射磨機將 純度為6N之矽粗粒加以粉碎而獲得的矽粉末進行5小時烘 焙處理，使之脫氧。 接著，將溫度設為120(TC，同時將面壓設為2〇〇kgf/cm2 進行熱壓，然後，在溫度為12〇(rc、壓力為14〇〇大氣壓下 對其進行mP，獲得直徑為400mm之矽燒結體。並且，研 磨該矽燒結體而製成矽晶圓。 對於結晶粒徑及減少矽氧化物、矽碳化物及金屬矽化 物之雜質，可藉由使用高純度之㈣末及粉碎此粉末，採 13 200940447 用烘焙之脫氧條件、HIP處理之溫度及加壓條件，來調整上 述雜質含量。 實施例1之矽燒結體晶圓的平均結晶粒徑為邛爪，最 大結晶粒徑為16μιη，矽氧化物之體積比率為〇 16%、矽碳 化物之體積比率為〇·12%、金屬矽化物之體積比率小於 0.001% (金屬矽化物之量少，未達到分析水準）。測定此 燒結矽晶圓之機械強度。測定機械強度時，係自晶圓任意 地抽樣5點而獲得平均值。 其結果，所抽樣之5點的平均彎曲強度為31kg/cm2，5 點的平均拉伸強度為11 kg/cm2，5點的平均維克氏硬度為 1060，滿足作為機械晶圓所要求之特性。再者，將特性值 之小數點以後四捨五入。其結果示於表1。 如此’由於矽燒結體晶圓具有充分之強度，因而即便 使日日圓之直控增加至42〇min、440mm、460mm、480mm...... 時’亦不會產生裂縫或碎屑。 再者’可知由於當矽燒結體晶圓中混入有上述以外之 雜質時亦欠佳，因而係使用純度為6N之矽，但是只要純度 為N以上’則可無特別問題地加以使用β而且，只要純度 為5Ν以上，則亦不會對機械特性造成影響。 200940447 [表1] 最大 粒徑 μηι 平均 粒徑 μιη 氧化物 體積％ 碳化物 體積％ 矽化金屬 體積％ 抗彎強度 kg/cm2 拉伸強度 kg/cm2 維克氏 硬度 實施例1 16 5 0.16 0.12 <0.001 31 11 1060 實施例2 20 9 0.05 0.05 <0.001 37 16 830 實施例3 7 2 0.13 0.11 <0.001 47 14 1200 實施例4 14 4 0.20 0.03 <0.001 33 12 1060 實施例5 10 6 0.08 0.12 <0.001 31 16 1060 實施例6 15 5 0.10 0.12 <0.006 20 6 1080 實施例7 18 8 0.14 0.11 <0.002 22 6 970 © 表示所抽樣之5點的平均彎曲強度。 (實施例2-7) 與實施例 1相同地，於減壓下、1100〜1300°C ( 1100 °C、5小時）之範圍内，對純度為5N及6N之矽粉末進行 烘焙使之脫氧，接著，於1000〜1200°C之範圍、面壓為 200kgf/cm2以上之條件下對其進行熱壓，將藉此所獲得之矽 進一步於1200〜1300°C之範圍、壓力為1000大氣壓以上 (1400大氣壓）下進行HIP處理，藉此，製造如表1所示 之最大結晶粒徑為20μιη以下，平均結晶粒徑為1 μιη以上、 10μιη以下，矽氧化物之體積比率為0.01%以上、0.2%以下， 矽碳化物之體積比率為0.01 %以上、0.15%以下，金屬矽化 物之體積比率為0.006%以下之範圍的燒結矽。 再者，實施例2〜4中，與實施例1相同地使用6Ν之 矽，實施例5〜實施例7中使用5Ν之矽。 另外，將實施例2之熱壓溫度設為1100°C、HIP處理 之溫度設為1200°C，將實施例3之熱壓溫度設為1200°C、 15 200940447 HIP處理之溫度設為12〇(rc，將實施例4之熱壓溫度設為 1200°C、HIP處理之溫度設為13〇〇»c，將實施例5之熱壓 溫度設為11 〇〇°C ' HIP處理之溫度設為1200°C，將實施例 6之熱壓溫度設為uoot、HIP處理之溫度設為1200°C， 將實施例7之熱壓溫度設為12〇〇〇c、hip處理之溫度設為 1300〇C。 其結果同樣示於表1。如此表1所示，實施例2〜7之 矽燒結體晶圓的平均結晶粒徑為i〜1〇μηι，最大結晶粒徑 為20μιη以下，矽氧化物之體積比率為〇 〇1〜〇 2%、矽碳化 物之體積比率為〇·〇1〜015%、金屬矽化物之體積比率小於 0.006%，在本發明之範圍内。 並且，測定此燒結矽晶圓之機械強度。測定機械強度 時，係自晶圓任意地抽樣5點而獲得平均值。 任一者之利用三點彎曲法所求得的抗彎強度之平均值 均為20kg/cm2以上、5〇kg/cm2以下，拉伸強度之平均值均 為2〇kg/Cm2以下，維克氏硬度之平均值均為800以上、1200 以下，具有本發明之機械特性，可使用作為機械晶圓。 (實施例8 -1 〇 ) 其次，以實施例6為依據，將矽晶圓表面劃分成任音 多個區塊’在各個區塊中測定平均粒徑，冑察此時各區： 之平均粒徑的偏差。其結果示於表2。 根據上述平均粒徑之偏差之敎結果可知，為±5帥以 下之燒結矽B曰圓的該偏差越小，則越可提高機械特性。因 此可知，就提高矽晶圓之機械特性方面而言更佳為將上 200940447 述偏差抑制在±5μιη以下。 但是，應當可理解，此偏差之範圍只要在本發明之最 大結晶粒徑為20μιη以下，平均結晶粒徑為丨μιη以上、丨〇μιη 以下之範圍内，則並不會成為大問題。 另外’雖然此實施例8-1 〇之烘焙、HP條件、ΗΙΡ條件 與實施例6相同’但是並不為實施例6中所獲得之石夕燒結 體本身，因而可知由於燒結過程之變動，燒結體組織或特 性值會產生若干變動（偏差）。於此情形時，最大粒徑變 成16μηι，而且機械強度（抗彎強度、拉伸強度、硬度）亦 與實施例6稍有差異。但是，此差異並非本質差異實施 例6之再現性並未出現特別之問題。 [表2] 最大粒徑 μπι 平均粒徑 μιη 抗弩強度 kg/cm2 拉伸強度 kg/cm2 維克氏硬度 偏差 nm 實施例8 16 5 33 13 1090 1 實施例9 16 5 28 8 1030 5 實施例10 16 5 30 10 1050 -3 表示所抽樣之5點的平均彎曲強度。偏差表示平均粒徑之偏差。 氧化物、破化物、矽化金屬與實施例6相同，因而省略。 (比較例1 ) 使用純度為5Ν之矽，不進行烘焙（脫氧）處理，分別 選擇HIP之溫度與壓力’藉此製作平均結晶粒徑為3 μιη、 最大結晶粒徑為16μηι ’矽氧化物之體積比率為ο·。％、矽 碳化物之體積比率為〇.2%、且金屬矽化物之體積比率為 17 200940447 0.001%的燒結矽晶圓，以與實施例1相同之方式測定機械 強度。其結果示於表3。此機械強度之測定值係所抽樣之5 、 點的平均值。 如表3所示，寶曲強度為15kg/cm2，拉伸強度為 10kg/cm2，維克氏硬度為1320，並不滿足作為機械晶圓所 要求之彎曲強度、維克氏硬度。認為其原因在於不滿足本 發明之矽氧化物之體積比率為0·01 %以上、0.2%以下，妙碳 化物之體積比率為0.0 1 %以上、0.1 5%以下之條件。 ❹ [表3] 最大 粒徑 μηι 平均 粒徑 μιη 氧化物 體積％ 碳化物 體積％ 妙化金屬 體積％ 抗弩強度 kg/cm2 拉伸強度 kg/cm2 維克氏 硬度 比較例1 16 3 0.25 0.2 0.001 15 10 1320 比較例2 15 6 0.23 0.18 0.07 8 3 1150 比較例3 39 15 0.06 0.08 0.03 12 8 760 比較例4 25 10 0.12 0.13 0.04 19 11 820 比較例5 8mm 2mm 0.01 0.01 <0.001 8 5 780 表示所抽樣之5點之平均彎曲強度。比較例5係利用溶解法而製作 之砍晶圓’粒徑單位用mm表示。 ❹ (比較例2-5 ) 使用純度為5N之矽’分別選擇烘焙（脫氧）條件、HIP 之μ度與壓力（其中，僅比較例5利用溶解法進行製作）， 藉此’製作如表2所示之平均結晶粒徑為3〜15μιη、2mm， 最大結粒徑為15〜25 μιη、8mm，矽氧化物之體積比率為 〇.〇1〜0.25%、碎碳化物之趙積比率為〇 〇1〜〇 2%、且金屬Left and right 'but because it is implemented according to the difference of the raw material strip # (product f), it is therefore a non-essential condition but a better condition. Further, the above-mentioned hot press system is carried out for about 1 hour. It is preferred to further carry out the HIP treatment for about 3 hours. Long-term HIp treatment leads to coarsening of the crystal grains, which is not preferable. However, these times may be appropriately changed depending on the processing conditions' and are not limited to the above processing time. And 'by using high-purity bismuth powder and pulverizing the powder, using the deoxidation conditions of baking, the temperature of HIP treatment and the pressure conditions, the above impurity content can be adjusted 〇 and 'deoxidation is important, and 矽 sintering is performed for obtaining fine crystals. The body must be fully deoxygenated. The baking temperature is set to 1 〇〇〇 to 13 〇〇 ° c, preferably less than 1200. (The reason is that if it is less than 1 〇〇〇. (: The oxygen cannot be removed sufficiently. The presence of bismuth is the main factor that contributes to the direct formation of cerium oxide. In addition, if it is above 1200 °C, it will exist. The following disadvantages: Although deoxidation can be carried out, necking (the phenomenon that the powder and the powder are in close contact with each other) is high. 12 200940447 . Even if the necking is released during hot pressing, the particle size distribution will be uneven, and the working time will be Therefore, the upper limit temperature must be set to 13 〇 (rc.) and the crystal orientation can be adjusted by using high-purity bismuth powder and pulverizing the powder, using the deoxidation conditions of baking, the temperature of HIP treatment, and the pressure conditions. The following sintered tantalum wafer can also be obtained: the ratio of the intensity of the (220) plane measured by the x-ray diffraction to the intensity of the (丨i丨) plane (22〇) 71 (U1) (丨)] The ratio of the ❹ intensity of the (311) plane to the intensity of the (n 1 ) plane [I ( 3 11 ) /1 ( 111 ) ( 2)] is 0.2 or more and 〇.4 or less. [Examples] Hereinafter, the present invention will be described based on examples. Further, the following examples are intended to enable The present invention is not limited to the embodiments, and other examples or modifications based on the technical idea of the present invention are of course included in the present invention. (Example 1) φ is decompressed and desorbed The degree was raised to 1, and the tantalum powder obtained by pulverizing the coarse particles having a purity of 6 N by a jet mill was subjected to a baking treatment for 5 hours to deoxidize it. Next, the temperature was set to 120 (TC, and the surface pressure was set at the same time. Hot pressing was carried out for 2 〇〇kgf/cm 2 , and then mP was performed at a temperature of 12 Torr (pressure at a pressure of 14 Torr) to obtain a sintered body having a diameter of 400 mm. Further, the sintered body of the tantalum was polished. Made of germanium wafers. For crystal grain size and reduction of impurities of tantalum oxide, tantalum carbide and metal halide, by using high purity (4) and pulverizing the powder, 13 200940447 is used for baking deoxidation conditions, HIP The above-mentioned impurity content is adjusted by the temperature and the pressure conditions of the treatment. The average crystal grain size of the tantalum sintered body wafer of Example 1 is a paw, the maximum crystal grain size is 16 μm, and the volume ratio of niobium oxide is 〇16%.矽Carbide body The product ratio is 〇·12%, and the volume ratio of metal telluride is less than 0.001% (the amount of metal telluride is small, the analytical level is not reached). The mechanical strength of the sintered tantalum wafer is measured. When measuring the mechanical strength, the wafer is measured from the wafer. The average value of the 5 points sampled was 31 kg/cm2, the average tensile strength at 5 points was 11 kg/cm2, and the average Vickers hardness at 5 points was 1060. It satisfies the characteristics required as a mechanical wafer. Furthermore, the decimal point of the characteristic value is rounded off. The results are shown in Table 1. Thus, since the tantalum sintered body wafer has sufficient strength, cracks or chips do not occur even when the direct control of the Japanese yen is increased to 42 〇 min, 440 mm, 460 mm, 480 mm. In addition, it is known that when impurities other than the above are mixed in the sintered body wafer, the purity is 6N, but if the purity is N or more, β can be used without any problem. As long as the purity is 5 Ν or more, the mechanical properties are not affected. 200940447 [Table 1] Maximum particle size μηι Average particle size μιη Oxide volume % Carbide volume % Deuterated metal volume % Bending strength kg/cm2 Tensile strength kg/cm2 Vickers hardness Example 1 16 5 0.16 0.12 < 0.001 31 11 1060 Example 2 20 9 0.05 0.05 < 0.001 37 16 830 Example 3 7 2 0.13 0.11 < 0.001 47 14 1200 Example 4 14 4 0.20 0.03 < 0.001 33 12 1060 Example 5 10 6 0.08 0.12 <0.001 31 16 1060 Example 6 15 5 0.10 0.12 < 0.006 20 6 1080 Example 7 18 8 0.14 0.11 < 0.002 22 6 970 © represents the average bending strength of 5 points sampled. (Example 2-7) In the same manner as in Example 1, the powder having a purity of 5N and 6N was baked to deoxidize under a reduced pressure at a temperature of 1100 to 1300 ° C (1100 ° C, 5 hours). Then, it is hot-pressed under the conditions of a surface pressure of 200 kgf/cm 2 or more in the range of 1000 to 1200 ° C, and the crucible obtained therefrom is further in the range of 1200 to 1300 ° C and the pressure is 1000 atm or more. The HIP treatment was carried out under (1400 atm), whereby the maximum crystal grain size as shown in Table 1 was 20 μm or less, the average crystal grain size was 1 μm or more and 10 μm or less, and the volume ratio of the cerium oxide was 0.01% or more. 0.2% or less, the volume ratio of the niobium carbide is 0.01% or more and 0.15% or less, and the volume ratio of the metal telluride is 0.006% or less. Further, in Examples 2 to 4, 6 Ν was used in the same manner as in Example 1, and 5 Ν was used in Examples 5 to 7. Further, the hot pressing temperature of Example 2 was set to 1,100 ° C, the temperature of the HIP treatment was set to 1200 ° C, and the hot pressing temperature of Example 3 was set to 1200 ° C, and the temperature of the HIP treatment was set to 12 〇. (rc, the hot pressing temperature of Example 4 was set to 1200 ° C, the temperature of the HIP treatment was set to 13 〇〇»c, and the hot pressing temperature of Example 5 was set to 11 〇〇 ° C ' HIP processing temperature setting 1200 ° C, the hot pressing temperature of Example 6 was set to uoot, the temperature of the HIP treatment was set to 1200 ° C, the hot pressing temperature of Example 7 was set to 12 〇〇〇 c, and the temperature of the hip treatment was set to 1300. The results are also shown in Table 1. As shown in Table 1, the sintered crystal grains of Examples 2 to 7 had an average crystal grain size of i 〜1 〇μηι, and the maximum crystal grain size was 20 μm or less. The volume ratio of the substance is 〇〇1 to 〇2%, the volume ratio of ruthenium carbide is 〇·〇1 to 015%, and the volume ratio of metal ruthenium is less than 0.006%, which is within the scope of the present invention. The mechanical strength of the wafer. When measuring the mechanical strength, the sample is randomly sampled from the wafer to obtain an average value of 5 points. The average value of the bending strength obtained by the bending method is 20 kg/cm2 or more and 5 〇kg/cm2 or less, and the average tensile strength is 2 〇kg/cm 2 or less, and the average value of the Vickers hardness is 800 or more and 1200 or less, the mechanical properties of the present invention can be used as a mechanical wafer. (Embodiment 8.1) Next, based on the sixth embodiment, the surface of the ruthenium wafer is divided into a plurality of blocks. 'The average particle diameter was measured in each of the blocks, and the deviation of the average particle diameter of each zone at this time was observed. The results are shown in Table 2. According to the results of the above-mentioned deviation of the average particle diameter, it is found that it is ±5 or less. The smaller the variation of the sintered 矽B曰 circle, the more the mechanical properties can be improved. Therefore, it is better to improve the mechanical properties of the ruthenium wafer to suppress the variation of the above-mentioned 200940447 to ±5 μm or less. It is to be understood that the range of the deviation is not particularly large as long as the maximum crystal grain size of the present invention is 20 μm or less and the average crystal grain size is in the range of 丨μηη or more and 丨〇μηη or less. 8-1 Baking, HP The condition and the crucible condition are the same as in the case of the sixth embodiment. However, it is not the same as that of the Shishi sintered body obtained in the sixth embodiment. Therefore, it is understood that a certain variation (deviation) occurs in the sintered body structure or characteristic value due to the variation of the sintering process. In this case, the maximum particle diameter became 16 μm, and the mechanical strength (bending strength, tensile strength, hardness) was slightly different from that of Example 6. However, the difference was not the essential difference. The reproducibility of Example 6 did not appear particularly. [Table 2] Maximum particle size μπι Average particle size μιη Tensile strength kg/cm2 Tensile strength kg/cm2 Vickers hardness deviation nm Example 8 16 5 33 13 1090 1 Example 9 16 5 28 8 1030 5 Example 10 16 5 30 10 1050 -3 represents the average bending strength of the 5 points sampled. The deviation indicates the deviation of the average particle diameter. The oxide, the broken product, and the deuterated metal are the same as in the sixth embodiment, and thus are omitted. (Comparative Example 1) A crucible having a purity of 5 Å was used, and no baking (deoxidation) treatment was carried out, and the temperature and pressure of HIP were respectively selected to prepare an average crystal grain size of 3 μm and a maximum crystal grain size of 16 μηι '矽 oxide. The volume ratio is ο·. The mechanical strength was measured in the same manner as in Example 1 except that the volume ratio of %, 碳 carbide was 〇.2%, and the volume ratio of metal ruthenide was 17 200940447 0.001%. The results are shown in Table 3. The measured value of this mechanical strength is the average of the 5 points and points sampled. As shown in Table 3, the flexural strength was 15 kg/cm2, the tensile strength was 10 kg/cm2, and the Vickers hardness was 1320, which did not satisfy the bending strength and Vickers hardness required as mechanical wafers. The reason for this is that the volume ratio of the cerium oxide of the present invention is not more than 0. 01% or more and 0.2% or less, and the volume ratio of the sulphur carbide is 0.01% or more and 0.15% or less. ❹ [Table 3] Maximum particle size μηι Average particle size μιη Oxide volume % Carbide volume % Meticated metal volume % Antimony strength kg/cm2 Tensile strength kg/cm2 Vickers hardness comparison example 1 16 3 0.25 0.2 0.001 15 10 1320 Comparative Example 2 15 6 0.23 0.18 0.07 8 3 1150 Comparative Example 3 39 15 0.06 0.08 0.03 12 8 760 Comparative Example 4 25 10 0.12 0.13 0.04 19 11 820 Comparative Example 5 8mm 2mm 0.01 0.01 <0.001 8 5 780 The average bending strength of the 5 points sampled. Comparative Example 5 is a chopped wafer produced by a dissolution method. The particle size unit is expressed in mm. ❹ (Comparative Example 2-5) The baking (deoxidation) conditions, the HIP μ degree, and the pressure were respectively selected using a purity of 5 N (wherein only Comparative Example 5 was produced by a dissolution method), thereby making a preparation as shown in Table 2 The average crystal grain size shown is 3~15μηη, 2mm, the maximum knot particle size is 15~25μηη, 8mm, the volume ratio of cerium oxide is 〇.〇1~0.25%, and the ratio of the product of the broken carbide is 〇. 〇1~〇2%, and metal
1S 200940447 矽化物之體積比率小於0.001以及為0·001〜 0 07%的燒結 石夕晶圓’以與實施例丨相同之方式測定機械強度。 其結果同樣地示於表3。此機械強度之測定值係所抽樣 之5點的平均值。 如表3所示’平均抗弯強度變成8〜19kg/cm2，均不滿 足作為機械晶圓所要求之彎曲強度（平均抗彎強度為2〇〜 50kg/cm )，平均拉伸強度為3〜1 ikg/cm2並無特別問題， 但平均維克氏硬度在比較例1中為過高之132〇，另外，比 較例3及比較例5之平均維克氏硬度為過低之76〇與78〇， 並不滿足作為機械晶圓所要求之維克氏硬度（8〇〇〜丨2〇〇 )。 認為其原因在於，比較例2中矽氧化物、矽碳化物、 金屬矽化物之量均超過本發明之上限值。另外，於比較例3 及比較例4中，所含有之金屬矽化物之量非常多，均超過 本發明之上限值。另外，於比較例5中，由於係利用溶解 法來進行製作，因而結晶之最大粒徑及平均粒徑極大，導 致抗彎強度及維克氏硬度降低。 根據以上可知，比較例丨_5均不滿足本發明之條件，其 特性亦不充分。 ' (實施例1 1 ) 於本實施例U中’調整結晶方位，觀察表面粗趟度 於減壓下且使溫度上升纟職。c ’對利用喷射磨機將純 為6N之梦粗粒加以粉碎而獲得㈣粉末進行5小時供培 理使之脫I接著，將溫度設為1酬。c，同時將面麼設 200kgf/cm進行熱壓，接著，在溫度為12〇吖 < 19 200940447 大氣壓下對其進行HIP處理，獲得直徑為4〇〇mm之矽燒結-體。 · 於此情形時，使具有與實施例6同等之平均結晶粒徑、 最大結晶粒徑、矽氧化物之體積比率、矽碳化物之體積比 率、金屬矽化物之體積比率。亦即，矽燒結體晶圓之平均 結晶粒徑為5μιη、最大結晶粒徑為15μιη，矽氧化物之體積 比率為0.10%、矽碳化物之體積比率為〇12%、金屬矽化物 之體積比率小於0.006%。 另外，此實施例11中，烘焙、ΗΡ條件、ΗΙρ條件與實 〇 施例6相同。但是並非為實施例6中所獲得之矽燒結體本 身因而可知通常由於燒結過程之變動，燒結體組織或特 !·生值會產生右干變動（偏差），但此時卻並未確認到組織 或機械強度（抗彎強度、拉伸強度、硬度）與實施例6存 在差異。 對此實施例11之矽燒結體晶圓進行χ射線繞射，測 定、確認結晶面的強度。其結果，（22〇)面的強度與（ηι) 面的強度之比[1 ( 220) /I(m)]為〇 5，且（311)面的強 Ο 度與（111)面的強度之比[1(311) /1(111)]為03。此時 之表面粗糙度Ra為0.02,係與單晶矽晶圓同等之表面粗糙 度。其結果不於表4。 再者，本實施例11具有與作為具有代表性之實施例的 上述實施例6之矽燒結體晶圓同等的平均結晶粒徑、最大 結晶粒徑、亦即平均結晶粒徑為5μηι、最大結晶粒徑為 15μιη，因而表4中省略表示該等。以下，沿用實施例6或 20 200940447 • 實施例11之條件時，均同樣省略表示。 [表4] I (220) /1 (111) I (311) /1 (111) 表面粗縫度Ra( μιη ) 實施例11 0.5 0.3 0.02 實施例12 0.4 0.4 0.01 實施例13 0.4 0.2 <0.01 實施例14 0.4 0.3 0.01 實施例15 0.7 0.2 0.01 實施例16 0.7 0.4 0.01 實施例17 0.6 ] 0.4 0.01 I (220) /1 (iU) : (22〇)面的強度與（ιιι)面的強度之比 1(311)/1(^) : (311)面的強度與（η"面的強度之比 (實施例12-17 ) 本實施例中，與實施例丨丨相同地，改變條件而調整結 晶方位，觀察表面粗糙度。對於結晶方位之調整，可藉由 使用高純度之石夕、選擇烘培（脫氧）條件、分別選擇Hip ©之溫度與壓力，來任意加以調節，因而，藉此製作實施例 11之矽燒結體晶圓，並且研磨該矽燒結體晶圓而製成矽晶 圓。 與上述實施例1 1相同 於減壓下、1100〜130(TC< 範圍内，對純度為5N及6N之功从士“ N之矽粉末進行烘焙使之脫氧， 接著，於1200〜1420°C之銘囹 r p L之範圍、面壓為200kgf/cm2以上對 其進行熱壓，對藉此所獲得之砂推 更付之矽進—步於1200〜142CTC之 範圍、壓力為1000大氣壓以上 進仃HIP處理，藉此，製造 如表5所示之各種矽燒結體晶圓。 21 200940447 進一步對此等進行χ射線繞射，測定結晶面的強度。 ’ 其結果同樣示於表5。如該表5所示，（220 )面的強度與 (111)面的強度之比[I ( 220) /1 ( 11 1 )]為〇_4〜〇.7，且 (311)面的強度與（ill)面的強度之比U1)] 為0_2〜0.4。此時之表面粗糙度Ra為小於0.01及001〜 0.02 ’係與單晶矽晶圓同等之表面粗糙度。 (實施例18-20 ) 其次，以本發明之實施例丨丨為依據，對利用χ射線繞 射所測定之除（220 )面及（311)面以外之面的強度與（"丨）〇 面的強度之比為0.2以下之情形、與不為〇 2以下之情形進 行比較實驗。其結果示於表5。 如該表5所示，存在除（22〇)面及（311)面以外之 面時具有導致表面粗糙度增大之傾向，因而較佳為儘可能 地少。1S 200940447 The volume ratio of the telluride was less than 0.001 and the sintering strength of 0·001 to 0 07% was measured in the same manner as in Example 机械. The results are shown in Table 3 in the same manner. The measured value of this mechanical strength is the average of 5 points sampled. As shown in Table 3, the average bending strength becomes 8 to 19 kg/cm2, which does not satisfy the bending strength required for mechanical wafers (average bending strength is 2 〇 to 50 kg/cm), and the average tensile strength is 3 〜 1 ikg/cm2 has no particular problem, but the average Vickers hardness is 132 过 which is too high in Comparative Example 1, and the average Vickers hardness of Comparative Example 3 and Comparative Example 5 is too low 76 〇 and 78 〇, does not meet the Vickers hardness (8〇〇~丨2〇〇) required as a mechanical wafer. The reason for this is considered to be that the amounts of cerium oxide, cerium carbide, and metal cerium in Comparative Example 2 exceeded the upper limit of the present invention. Further, in Comparative Example 3 and Comparative Example 4, the amount of the metal telluride contained was extremely large, and both exceeded the upper limit of the present invention. Further, in Comparative Example 5, since the production was carried out by the dissolution method, the maximum particle diameter and the average particle diameter of the crystal were extremely large, resulting in a decrease in the bending strength and the Vickers hardness. From the above, it can be seen that the comparative example 丨5 does not satisfy the conditions of the present invention, and its characteristics are also insufficient. (Example 1 1) In the present Example U, the crystal orientation was adjusted, and the surface roughness was observed under reduced pressure and the temperature was raised. c' was obtained by pulverizing pure 6N dream coarse particles by a jet mill to obtain (4) powder for 5 hours for conditioning to remove I, and then setting the temperature to 1 liter. c. At the same time, the surface was set to 200 kgf/cm for hot pressing, and then HIP treatment was carried out at a temperature of 12 〇吖 < 19 200940447 at atmospheric pressure to obtain a ruthenium sintered body having a diameter of 4 〇〇 mm. In this case, the average crystal grain size, the maximum crystal grain size, the volume ratio of the cerium oxide, the volume ratio of the cerium carbide, and the volume ratio of the metal cerium compound are obtained in the same manner as in the sixth embodiment. That is, the average crystal grain size of the tantalum sintered body wafer is 5 μm, the maximum crystal grain size is 15 μm, the volume ratio of niobium oxide is 0.10%, the volume ratio of niobium carbide is 〇12%, and the volume ratio of metal telluride. Less than 0.006%. Further, in this Example 11, the baking, the enthalpy conditions, and the ΗΙρ conditions were the same as those of the embodiment 6. However, it is not the sinter body itself obtained in Example 6, and it is therefore known that the sintered body structure or the special value of the sintered body changes due to the fluctuation of the sintering process, but the right dry variation (deviation) is not observed at this time. The mechanical strength (bending strength, tensile strength, hardness) was different from that of Example 6. The tantalum sintered body wafer of Example 11 was subjected to x-ray diffraction to measure and confirm the strength of the crystal face. As a result, the ratio of the intensity of the (22 〇) plane to the intensity of the (ηι) plane [1 (220) / I(m)] is 〇5, and the strength of the (311) plane and the strength of the (111) plane. The ratio [1(311) /1(111)] is 03. The surface roughness Ra at this time was 0.02, which was equivalent to the surface roughness of the single crystal germanium wafer. The results are not shown in Table 4. Further, the present embodiment 11 has an average crystal grain size, a maximum crystal grain size, that is, an average crystal grain size of 5 μm, and maximum crystal crystallization, which is equivalent to the tantalum sintered body wafer of the above-described Example 6 as a representative embodiment. The particle diameter was 15 μm, and thus the appearance is omitted in Table 4. Hereinafter, the conditions of the embodiment 6 or 20 200940447 • the eleventh embodiment are also omitted. [Table 4] I (220) /1 (111) I (311) /1 (111) Surface roughness Ra (μιη) Example 11 0.5 0.3 0.02 Example 12 0.4 0.4 0.01 Example 13 0.4 0.2 <0.01 Example 14 0.4 0.3 0.01 Example 15 0.7 0.2 0.01 Example 16 0.7 0.4 0.01 Example 17 0.6 ] 0.4 0.01 I (220) /1 (iU) : (22〇) the strength of the face and the strength of the (ιιι) face Ratio 1(311)/1(^) : ratio of the intensity of the (311) plane to the intensity of the (η" plane (Embodiment 12-17) In the present embodiment, the conditions are changed as in the embodiment The crystal orientation is observed, and the surface roughness is observed. The adjustment of the crystal orientation can be arbitrarily adjusted by using a high-purity stone, selecting a baking (deoxidizing) condition, and selecting the temperature and pressure of the Hip, respectively. The tantalum sintered body wafer of Example 11 was produced, and the tantalum sintered body wafer was polished to form a tantalum wafer. The purity was in the range of 1100 to 130 (TC<; 5N and 6N work from the "N 矽 矽 powder baking to deoxidize, then, at 1200 ~ 1420 ° C Ming 囹 rp L range, surface It is hot pressed at 200kgf/cm2 or more, and the sand obtained by this is further increased. The process is carried out in the range of 1200 to 142 CTC, and the pressure is 1000 atmospheres or more, and the HIP treatment is carried out, thereby manufacturing as shown in Table 5. Various tantalum sintered body wafers are shown. 21 200940447 Further, the X-ray diffraction is performed to measure the strength of the crystal face. The results are also shown in Table 5. As shown in Table 5, the strength of the (220) plane The ratio of the intensity to the (111) plane [I (220) /1 (11 1 )] is 〇_4 to 〇.7, and the ratio of the strength of the (311) plane to the strength of the (ill) plane is U1)] 0_2 to 0.4. The surface roughness Ra at this time is less than 0.01 and 001 to 0.02' is the same as that of the single crystal germanium wafer. (Examples 18-20) Next, the embodiment of the present invention is According to the method, the ratio of the intensity of the surface other than the (220) plane and the (311) plane measured by the x-ray diffraction to the intensity of the ("丨) 〇 plane is 0.2 or less, and the ratio is not 〇2 or less. In the case of the comparative experiment, the results are shown in Table 5. As shown in Table 5, there is a cause table when there are faces other than the (22〇) face and the (311) face. It tends to increase the roughness, and thus is preferably as small as possible.
再者，對於單晶矽晶圓而言，晶圓面與垂直於晶圓面 之面的特性之間基本上不存在差異。因此較佳為：燒結矽 亦同樣，其所測定的（220 )面之面方位強度比（1)及（311) 面之面方位強度t“2) ’肖在垂直於#晶圓面之面上所測 定的各強度比⑴，及⑺，之差，亦即丨⑴—⑴，丨為 0.1以下’ I ( 2) — ( 2) ’丨儘可能地小。於該意義上而言， 將〇·〇5以下作為容許範圍。表中雖未加以表示，但可:認 本案實施例1 - 1 〇均在此範圍内。 22 200940447 [表5] I (XYZ) /1 cun 表面粗糙度Ra (μιη) 實施例18 0.2 0.02 實施例19 0.1 0.01 實施例20 0.05 <0.01 I (XYZ) /1 (111):表示除（220)面及（311)面以外之面 的強度與（111)面的強度之比。 於本實施例11-17中，藉由調整結晶方位，而使得表面 ® 粗糙度Ra達到與單晶矽晶圓同等之表面粗糙度，且利用三 點彎曲法所求得的抗彎強度之平均值均為2〇kg/cm2以上、 50kg/cm2以下，拉伸強度之平均值均為2〇kg/cm2以下維 克氏硬度之平均值均為800以上、12〇〇以下，具有本發明 之機械特性，具備可使用作為機械晶圓之條件。如此可確 認，藉由調整面方位而獲得之矽燒結體晶圓同時具有充 之強度。 (比較例6) 鲁❹純度為5N之石夕，與實施们i相同地分別選擇供 焙（脫氧）條件、HIP之溫度與壓力，藉此製作表6所示之 燒結矽晶圓。於此情形時，對此矽燒結體晶圓進行χ射線 繞射，測定結晶面的強度。其結果，（22〇 )面的強度與（i丨丄） 面的強度之比[I( 220) /1 ( 11 1 )]為〇3,且（311)面的強 度與（111)面的強度之比[I(311) /I( lu)]為〇卜並且， 表面粗糙度Ra稍粗大化至〇.04μιη，。 此並不具備作為機械晶圓所要求之小於〇〇2μιη之表面 粗糙度Ra’因而並不充分滿足作為機械晶圓所要求之特 23 200940447 性。認為此特性降低之原因在於不滿足本發明之下述條 件，即，利用X射線繞射所測定之（220 )面的強度與（111 ) 面的強度之比[I ( 220) /1 ( 11 1 )]為0.4以上、0.7以下， 且（311)面的強度與（111)面的強度之比[1(311)/1(111)] 為0.2以上、0.4以下。 [表6] I (220) /1 (111) I (311) fl (111) 表面粗縫度Ra (μπι) 比較例6 0.3 0.1 0.04 比較例7 0.2 0.1 0.06 比較例8 0.8 0.1 0.09 比較例9 0.3 0.5 0.05 比較例10 0.2 0.2 0.05 I ( 22 0 ) /1 ( 1 1 1 ) : ( 220 )面的強度與（1U )面的強度之比 (311)/1(111) : (311)面的強度與（111)面的強度之比 (比較例7) 其次，利用溶解法製作5N之矽錠（sincon ing0t )，對 此矽錠進行切割而精加工成矽晶圓。對此鑄造矽晶圓進行χ 〇 射線繞射’與實施例11相同地測定結晶面的強度。其結果 同樣示於表6。 如表6所不，（220)面的強度與（11㈠面的強度之 比[I ( 220 ) /1 ( ιιη Λ， „ ^ )]為0.2’且（311)面的強度與（lu) 面的強度之比[I ( 3 1 Π π广！】，、Λ (111)]為0.1。並且’表面粗輪 度Ra粗大化至0.06μιη，。 此並不具備作為機械晶圓所要求之小於G.G2pm之表面 24 200940447 .粗糙度Ra，並不滿足作為機械晶圓所要求之特性。與比較 例1相同地’認為此特性降低之原因在於不滿足本發明之 下述條件，％ ’利用X射線繞射所測定之（22〇)面的強度 與（111)面的強度之比[1 ( 220) /1 ( 1 1 1 )]為04以上、 0.7以下，且（311)面的強度與（lu)面的強度之比[ι(3ιι) /1 ( 111)]為 0·2 以上、〇.4 以下。 (比較例8-10) 使用純度為5Ν〜6Ν之矽，分別選擇烘焙（脫氧）條件、 © ΗΙΡ之溫度錢力’藉此進行表6所示之χ射線繞射，與 實施例1相同地測定矽結晶面的強度。其結果示於表6。 如表6所示，（220 )面的強度與（111)面的強度之 比[I ( 220 ) /1 ( 1 1 1 )]在比較例8中為〇 8，比較例9中為 0·3，比較例10中為〇·2，且（31 i )面的強度與（i i i )面 的強度之比[I (311) /I(iii)]在比較例8中為〇1，比較 例9中為0·5，比較例1〇中為〇 2。並且，比較例8、比較 例9、比較例10之表面粗糙度Ra分別粗大化至0.09μιη、 響 〇·05μηι、0.05μπι，。 此並不具備作為機械晶圓所要求之小於〇 〇2μπι之表面 粗糙度Ra，並不滿足作為機械晶圓所要求之特性。與比較 例1相同地’認為此特性降低之原因在於不滿足本發明之 下述條件’即’利用X射線繞射所測定之（22〇 )面的強度 與（111)面的強度之比[I ( 220) /1 ( in)]為0.4以上、 0.7以下，且（311)面的強度與（iU)面的強度之比卩（311) /1 (111)]為 0.2 以上、〇·4 以下。 25 200940447 [產業上之可利用性] 本發明可獲得一種燒結體晶圓，其即便為大型之圓盤 狀燒結矽晶圓，亦具有與單晶矽類似之機械物性、且強度 顯著提高，另外，本發明可提供一種視需要具有與單晶矽 之表面粗糙度極為類似之平滑表面的燒結矽晶圓，因而作 為機械矽晶圓而言極為有用。而且，由於此種矽燒結體晶 圓之機械強度高’因而亦可使用作為濺鍍靶或半導體製造 裝置之各種零件。 【圖式簡單說明】 無 【主要元件符號說明】 無 Ο 26Furthermore, for a single crystal germanium wafer, there is substantially no difference between the characteristics of the wafer face and the face perpendicular to the wafer face. Therefore, it is preferable that the sintered crucible has the same plane orientation intensity ratio (1) and the surface orientation intensity t(2) of the (311) plane, which is perpendicular to the surface of the # wafer surface. The difference between the intensity ratios (1) and (7) measured above, that is, 丨(1)-(1), 丨 is 0.1 or less 'I (2) - (2) '丨 is as small as possible. In this sense, 〇·〇5 is the allowable range. Although not shown in the table, it can be said that the examples 1 - 1 are all within this range. 22 200940447 [Table 5] I (XYZ) /1 cun Surface roughness Ra (μιη) Example 18 0.2 0.02 Example 19 0.1 0.01 Example 20 0.05 <0.01 I (XYZ) /1 (111): indicates the strength of the surface other than the (220) plane and the (311) plane and (111) The ratio of the strength of the face. In the present embodiment 11-17, by adjusting the crystal orientation, the surface roughness Ra is equal to the surface roughness of the single crystal germanium wafer, and is obtained by the three-point bending method. The average value of the flexural strength is 2〇kg/cm2 or more and 50kg/cm2 or less, and the average tensile strength is 2〇kg/cm2 or less. 800 or more and 12 inches or less have the mechanical characteristics of the present invention, and can be used as a condition of a mechanical wafer. Thus, it has been confirmed that the tantalum sintered body wafer obtained by adjusting the plane orientation has a sufficient charging strength. Example 6) The rhodium purity was 5N, and the baking (deoxidation) conditions and the temperature and pressure of the HIP were selected in the same manner as in the example i to prepare the sintered tantalum wafer shown in Table 6. In this case, The 矽 sintered wafer was subjected to χ-ray diffraction to measure the strength of the crystal face. As a result, the ratio of the intensity of the (22 〇) plane to the strength of the (i丨丄) plane [I(220) /1 (11 1)] is 〇3, and the ratio of the intensity of the (311) plane to the intensity of the (111) plane [I(311) / I(lu)] is 〇 and the surface roughness Ra is slightly coarsened to 〇.04μιη This does not have the surface roughness Ra' required for mechanical wafers less than 〇〇2μηη and thus does not fully satisfy the requirements of the mechanical wafers. The reason for this characteristic reduction is that this is not satisfied. The following conditions of the invention, that is, the strongness of the (220) plane measured by X-ray diffraction The ratio of the intensity of the (111) plane [I (220) /1 (11 1 )] is 0.4 or more and 0.7 or less, and the ratio of the intensity of the (311) plane to the intensity of the (111) plane [1 (311) / 1(111)] is 0.2 or more and 0.4 or less. [Table 6] I (220) /1 (111) I (311) fl (111) Surface roughness Ra (μπι) Comparative Example 6 0.3 0.1 0.04 Comparative Example 7 0.2 0.1 0.06 Comparative Example 8 0.8 0.1 0.09 Comparative Example 9 0.3 0.5 0.05 Comparative Example 10 0.2 0.2 0.05 I ( 22 0 ) /1 ( 1 1 1 ) : ratio of the strength of the ( 220 ) plane to the strength of the (1U ) plane ( 311)/1(111) : ratio of the strength of the (311) plane to the strength of the (111) plane (Comparative Example 7) Next, a 5N niobium ingot (sincon ing0t) was produced by a dissolution method, and the niobium ingot was cut. Finished into a wafer. The cast tantalum wafer was subjected to χ ray diffraction. The strength of the crystal face was measured in the same manner as in Example 11. The results are also shown in Table 6. As shown in Table 6, the ratio of the intensity of the (220) plane to the intensity of the (11 (one) plane [I (220) /1 ( ιιη Λ, „ ^ )] is 0.2' and the intensity of the (311) plane and the (lu) plane The ratio of the intensity [I ( 3 1 Π π wide!], Λ (111)] is 0.1. And 'the surface roughness Ra is coarsened to 0.06 μιη. This does not have the required minimum as a mechanical wafer. Surface 24 of G.G2pm 200940447. Roughness Ra does not satisfy the characteristics required as a mechanical wafer. The same reason as in Comparative Example 1 is that the characteristic is lowered because the following conditions of the present invention are not satisfied, % 'utilization The ratio of the intensity of the (22 〇) plane measured by the X-ray diffraction to the intensity of the (111) plane [1 (220) /1 (1 1 1 )] is 04 or more and 0.7 or less, and the strength of the (311) plane The ratio of the intensity to the (lu) surface [ι(3ιι) /1 (111)] is 0·2 or more and 〇.4 or less. (Comparative Example 8-10) Using a purity of 5 Ν to 6 矽, respectively, baking is selected. The (deoxidation) conditions and the temperature of ΗΙΡ 钱 借此 进行 进行 进行 进行 χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ χ The ratio of the intensity of the (220) plane to the intensity of the (111) plane [I (220) /1 (1 1 1 )] is 〇8 in Comparative Example 8, and 0.3 in Comparative Example 9, in Comparative Example 10 〇·2, and the ratio of the intensity of the (31 i ) plane to the intensity of the (iii) plane [I (311) / I(iii)] is 〇1 in Comparative Example 8, and 0. 5 in Comparative Example 9. In Comparative Example 1, 〇2 was obtained, and the surface roughness Ra of Comparative Example 8, Comparative Example 9, and Comparative Example 10 was coarsened to 0.09 μm, 〇·05 μηι, and 0.05 μπι, respectively. The surface roughness Ra required for the wafer of less than μ2 μm does not satisfy the characteristics required as a mechanical wafer. The same reason as in Comparative Example 1 is that the decrease in the characteristic is that the following conditions of the present invention are not satisfied. That is, the ratio [I (220) /1 (in)] of the intensity of the (22 〇) plane measured by the X-ray diffraction to the intensity of the (111) plane is 0.4 or more and 0.7 or less, and the (311) plane The ratio 卩(311) /1 (111)] of the strength to the intensity of the (iU) plane is 0.2 or more and 〇·4 or less. 25 200940447 [Industrial Applicability] The present invention can obtain a sintered body wafer. It is a large disk-shaped sintered tantalum wafer, which also has mechanical properties similar to that of single crystal germanium, and the strength is remarkably improved. In addition, the present invention can provide a smoothing similar to the surface roughness of a single crystal germanium as needed. The sintered silicon wafer on the surface is extremely useful as a mechanical germanium wafer. Further, since such a sintered body has a high mechanical strength, it is possible to use various parts as a sputtering target or a semiconductor manufacturing apparatus. [Simple diagram description] None [Key component symbol description] None Ο 26