TW201111536A - Copper material for use in a sputtering target, and manufacturing method therefor - Google Patents

Abstract

Provided are a copper material for use in a sputtering target, said copper material comprising high-purity copper having a purity of at least 99.99%, and a manufacturing method therefor. X-ray diffraction peak intensities (I{111}, I{200}, I{220}, and I{311}) for surfaces on which sputtering is performed (surface {111}, surface {200}, surface {220}, and surface {311}) satisfy equation (1), and the diameters of crystal grains in the provided copper material are between 100 [mu]m and 200 [mu]m. (1) I{200}/(I{111}+I{200}+I{220}+I{311}) = 0.4

Description

201111536 VI. Description of the Invention: [Technical Field to Be Invented by the Invention] The present invention relates to a copper material and a method for producing the same as 贱(4). [Prior Art] In recent years, flat panel displays have been used in various sizes from small electronic devices such as mobile PCs (personal computers) and mobile phone terminals to large-scale televisions. In the liquid crystal display or organic EL (EleCtroluminescence) display classified as a flat panel display, in order to meet the requirements for high-speed rendering of high-quality and dynamic images, a thin film transistor has been developed for insertion into a pixel ( Thin Film The following is a TFT component and is currently becoming mainstream. Fig. 1 is a cross-sectional view showing a configuration of a TFT element of a liquid crystal display panel. In the TFT element, the scanning line 3 and the closing electrode 4 (the portion of the scanning line are provided on the glass substrate 2 as a function of performing 〇N/〇FF control of the TFT). The gate electrode is formed by covering with the insulating film 5 of tantalum nitride, and amorphous germanium (hereinafter referred to as a-Si) is sequentially formed on the insulating film 5 (μ*r*·, 豕 & >) Layer ό 4 hetero-P (phosphorus) a_Si layer 7, source-polar electrode 8 and 9. A protective film having a % of nitridation is formed by covering it, and an indium-doped indium (hereinafter referred to as an ITO (Indium Tin 0xide)) film is disposed in the pixel region. [. First, the scan line, the gate electrode, and the source-drain electrode are used,

High-melting-point metals such as Cr, aluminum and alloys thereof, etc. However, as the liquid crystal display is enlarged or squashed, the image display is uneven due to an increase in wiring length, signal delay, power loss, and the like. The problem is revealed. Therefore, 201111536 copper wiring with lower resistivity began to receive attention. When a copper wiring film is formed on the wiring of the TFT element, when the Cu film is directly formed on the glass substrate, the Cu wiring film is peeled off from the glass due to poor adhesion between the cu/glass interface. As a invention for solving the problem of the peeling, the techniques described in Patent Documents i to 3 and the like have been proposed. In Patent Document 1, a barrier layer having excellent adhesion to a glass substrate is formed by inserting a high melting point metal between a copper wiring and a glass substrate to suppress peeling. In Patent Documents 2 and 3, an oxide is formed on the interface between the copper wiring and the glass substrate by using a thick alloy formed by copper, and the alloy element is concentrated on the interface between the copper wiring and the glass substrate. These methods inhibit peeling. In the inventions of the patent documents 2 and 3, methods such as copper alloying have also been developed. However, in the industrial invention, as described in the patent document, Mo or Ti having good adhesion to glass is used as a map. The barrier layer 2 described in 丨 is formed under the copper wiring, thereby improving the peeling and forming a wiring of pure copper by sputtering. One of the important characteristics required in the step of forming the gate electrode of the TFT element is the in-plane uniformity of the wiring film. The uniformity of the film, that is, the difference in film thickness or the presence or absence of the unevenness, causes the capacitance in the TFT to become uneven, which adversely affects the display. In addition, in the TFT element manufacturing step, if there is a difference in film thickness or coarse clusters (particles, splashes, etc.), there is a disconnection and short wiring when the wiring electrode is formed by etching. Bad shackles. In the case of forming a pure steel film such as a semiconductor wiring by the steps of < (4), the sputtering target which can be made into a uniform wiring film of 9 and suppresses coarse clusters and suppresses disconnection failure can be used. Shan Shi* contains the technology. Yu Ming, a patent document 4 ~ " in the document of the 4th document, 'disclosed the following is difficult to record, by the non-nitrogen stone and hydrogen gas composition purity of 99 9999% or more copper As a substrate, it can be produced by solidifying and solidifying at an oxygen concentration of 〇1 ppm or less, and it is possible to obtain a poor disconnection rate and super (3) (10).

Integ coffee η, large integrated circuit) wiring. The wire breakage is reduced by reducing the amount of impurities in the copper material. Patent Document 5 discloses that a sputtering target having a recrystallized structure having an average crystal grain size of 8 μm or less and having a Vickers hardness of 100 or less is used in a copper having a purity of 99 995% or more. It inhibits the expansion of spattered particles and the formation of coarse clusters. Patent Document 6 discloses that the purity of the gas component is not more than 99.999%, and the peak intensity of the x-ray diffraction of the {1U} plane in the (tetra) plane is increased by 1{11 1}, and the average particle diameter is 250 μm. Hereinafter, the particle diameter variation by the position is made 20% or less, whereby the film thickness uniformity is good. Patent Document 7 discloses that the volume of crystals having a surface facing the {1] surface is 80% or more, and the crystals are uniformly distributed from the surface to the center, so that the copper atoms are splashed vertically. On the surface, a film can be formed deep in the vertical and horizontal grooves. In Patent Document 8, it is disclosed that in the copper 201111536 having a purity of 99.999% or more, the average crystal grain size is controlled to be 1 〇 〜 3 〇 from the claws, so that (11 丨), {200}, {220}, and { The amount of particles in each of the alignments is less than 5%, and has a random alignment, thereby achieving uniformity and minimum particle generation. In the prior invention, it has been possible to control the spattering of sputtered particles by controlling the composition, crystal grain size, strain, and crystal orientation, thereby controlling uniform film formation and suppressing coarse clusters. However, the size of a substrate such as a liquid crystal display for a large-sized television has been increasing, and in the seventh generation or the like, it has become a substrate size of more than 2 m such as l87 〇 mm > 2200 mm. In the sputtering step for forming a wiring, it is necessary to form a thin film on a large substrate. Even if the method described in the above patent document is used, the thickness of the formed wiring film becomes not large at each portion of the substrate. Problems such as the generation of uniform and coarse clusters become more apparent. Further, since the sputtering target itself is also increased in size, the metal structure tends to be uneven at each portion of the sputtering target, and the influence on the film thickness precision and the coarse cluster is increased. [PRIOR ART DOCUMENT] [Patent Document 1] Japanese Laid-Open Patent Publication No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. [Patent Document 4] Japanese Patent No. 3,971, 519, and Japanese Patent No. 3,997, 371, and Japanese Patent No. 3,997, 371. [Patent Document 8] Japanese Patent No. 3971 171, 201111536, 容内明发rk [Problems to be Solved by the Invention] The problem of the present invention is to provide a == material which is in the use of splashing When the wiring of the FT liquid crystal panel is made of the two large substrates, the particles are generated more uniformly than before, and it is difficult to cause a change in the frequency of generation of the particles during use. [Means for Solving the Problem] The inventors of the present invention have found that the alignment of the 'Όaa and the crystal grains are controlled within a specific range, and that they can be more uniformly used by appropriate use. The extrusion method for controlling the manufacturing method of the stalking organization can provide a copper material suitable for the production of a wiring film of a uniform sentence. The present invention is based on this insight. That is, the present invention provides: 〇) a copper material for a sputtering target, characterized in that it is composed of high-purity copper having a purity of 99.99% or more, and (1)I in the surface of the splashing surface, Tao The peak intensities of the 乂-ray diffraction of the face, the (10)} face, and the {311} face, that is, 1{111}, 1{200}, 1{220}, and 1{311} satisfy the following formula (1), and crystallize The particle size of the grain is 1〇〇~2〇〇4 1{200}/(1{1 11} + i{200} + 1{22〇} + 1{311 })> 〇(2)如如1 The copper material for sputtering target, which is obtained by hot extrusion of an ingot of high purity copper having a purity of 99% or more, and the extruded material is cooled by hot extrusion at 11°201111536; (3) If the splashing target of item (1) is hot-extruded from the 丨#" copper material's high-purity copper casting with a purity of 99.99% or more, it will be extruded. The material is cooled immediately after the hot extrusion, and then cold rolled to produce; (4) The copper material for the sputtering target of (1) is tied to 7 (eight) to 〖ο". (: the purity of the next pair is 99.99. More than % of high-purity copper ingots are hot extruded,

The extruded material is produced by cooling at a cooling rate of 5 『c/sec or more immediately after the hot extrusion; T (1) - a method for producing a copper material for a target for deplating, which is manufactured as in (1) (4) The method of using a copper material is characterized in that the method comprises the following steps: 埶 埶 高 高 删 删 删 删 删 高 9 9 9 高 高 9 高 高 9 高 高 高 纯度 纯度 纯度 纯度 纯度 纯度 纯度 纯度 纯度 纯度 纯度 纯度 纯度 纯度 纯度 纯度 纯度 纯度The cooling rate is cooled. [Effect of the Invention] According to the present invention, it is possible to provide a copper material which is suitable for being able to produce a uniform wiring film.士和amp; ηα 何抖 The copper material for the sputtering target of the present invention is more uniform than the previous one when the wiring is applied to the large substrate for the TFT liquid 曰 面板 panel. It is also difficult to cause a change in the frequency of generation of the particles during use. The above and other features and advantages of the present invention are set forth in the description of the appended claims. [Embodiment] The copper material for ore-killing of the present invention is a copper material composed of high-purity copper having a purity of 99.99% or more (hereinafter, simply referred to as "pure copper"), 8 201111536. The crystal orientation and crystal grain size are set to a specific range. When pure copper is recrystallized by annealing, it is easy to form a 丨丨丨" face, a {200} face, a {220} face, and a {311} face. Usually these are randomly aligned, but the inventors have found that The sputtering characteristics of the {200} plane are particularly excellent, and the peak intensities of the X-ray diffraction of the {111} plane, the {200} plane, the {220} plane, and the {311} plane are set to I{111. }, 1{2〇〇}, {22〇丨, and "3丨1}, although the ratio of 1{200} is 40% or more, that is, when the following formula (^) is satisfied, The sputtering characteristics, for example, the uniformity of the film thickness at the time of formation and the homogeneity of the film quality are excellent.

0 · 5 or more or more 'more preferably 0.7 to 0.9. When the degree of 1 degree is less than 〇.4, it is preferably 〇·4 or more, preferably

The a曰 alignment also affects the sputtering characteristics. The crystal grain size of the material is 1 〇〇 2 2 〇〇 claws, more preferably 120 〜 18 〇. The peak intensity of the ray diffraction is the diffraction surface of the surface where X is incident.

201111536 When the crystal grain size is small, the grain boundary is relatively large, but the atomic arrangement of the grain grain boundary is disordered, and the splashing degree of the element during sputtering is different from that in the grain, so the formed film is likely to become Not uniform. Further, in the case where the crystal grain size is large, a high energy is required for the target material to fly, and formation of coarse clusters such as simultaneous splashing of several target atoms is increased, and the formed film is liable to become uneven. . Further, in the present invention, the particle diameter of the crystal grains means an average particle diameter (particle size) measured based on JIS η 〇 5 〇 i (cutting method). Furthermore, it is presumed that the main reason for the excellent sputtering characteristics of the {200} surface is: When considering the atomic density of each surface in the FCC (Face-Centered Cubic) metal, the {11U surface is the most, and secondly { 2〇〇} has more faces, but the {111} face is the densest, so the energy required to make one atom fly is larger, and the best balance is {200} face. The method for producing the copper material for a sputtering target of the present invention is not particularly limited, and it is preferable to use hot extrusion as a manufacturing procedure for improving the orientation of the {200} plane. In the hot extrusion, it is preferred to set the heating temperature of the material to 7 〇〇 <»c or higher. When the temperature is lower than 700 C, dynamic recrystallization cannot be sufficiently produced in the extrusion, and it is difficult to obtain the relationship of the formula (1). Further, the upper limit of the heating temperature is not particularly limited, but since the melting point of pure copper is about 1 〇8〇t, so if it is too high, the small billet will partially melt and cannot be extruded. The hot extrusion temperature is preferably -900 ° C. The hot extrusion can be carried out using a conventional extruder and can be carried out at any pressure. The temperature of the material which is hot extruded is very high, and the crystal grains are usually coarsened and grown in a short time, and become $200 or more. In order to prevent this and make the particle size of the 201111536 crystal 1 〇〇~200 μηι, it is preferable to use 5 〇 by water cooling or the like immediately after extrusion (usually within 5 seconds after extrusion from the mold). Cool down at a cooling rate of 〇c / sec. The cooling rate is preferably 1 〇〇 / sec or more. The upper limit of the cooling rate is not particularly limited, but is usually about 3 Å/sec or less. Moreover, it is preferable to cool until the material becomes 2 〇〇t or less. The orientation of the crystal, that is, the crystal orientation indicated by the above formula (1) is the direction of processing during hot working (the metal flow varies depending on forging, rolling, and extrusion, and the direction is changed separately), and the processing ratio (amount) Various changes occur in temperature and the like. By processing by hot extrusion, "the above crystal aligning degree is controlled to satisfy the above formula (丨) prescribed by the present invention, and from the above dynamic recrystallization to the stage of grain growth, the knot:::large: determined . In addition to this, in order to fix the hot extruded structure, it is preferred to perform cooling immediately after the above extrusion. # The copper material of the present invention can be obtained by achieving these two points. In addition, in the case of hot forging, t corresponds to the size of the large-scale requirement in recent years to eliminate the cooling after forging: the uneven grain is not obtained, and the crystal grain structure of the uniform sentence cannot be obtained.辔-: outside' is to obtain the above crystal alignment or crystal grain a, and the purity of pure copper: I is contained in the electrolytic copper of the raw material for producing pure copper, and the impurities are also present in the cast bond of pure copper. If the impurities are two! The heat resistance of the material is increased. It is difficult to recrystallize and become difficult to obtain. Inch,,,. Crystal alignment. Yu Taigong, in the present invention, the purity of pure copper must be 99.99% or more preferably 99.99% or more. Further, the purity of the pure copper in the above-mentioned hot extrusion and the subsequent 7 portions is substantially unchanged. 11 201111536 As an excellent aspect of hot extrusion, it is possible to control the crystal grain size by the above-described crystal orientation or cooling rate with a small variation in the end and the width direction of the extruded material. The first steel target is manufactured by hot rolling, but since the hot rolling is gradually thinned by several passes to several dozen passes, a temperature drop occurs during rolling, and the temperature is lowered. It is easy to make a difference in the front end of the material. In addition, the temperature on both sides in the width direction is liable to lower due to heat dissipation. Further, the final water cooling is generally carried out from the one side of the rolled material into the water cooling zone, so that the difference between the front and rear ends is also likely to occur here. In the aspect of the hot extrusion, the extruded material is immediately cooled to form a (four) material, so that the difference in the length direction and the width direction of the cooling process does not occur. The temperature difference produced is a small temperature drop at the beginning of the extrusion and the end of the extrusion, but the processing time is shorter than that of the hot rolling': therefore, the amount of decrease is small, and the accumulation of processing heat is also generated, so the temperature difference Almost: Yes: For the problem. In this way, the material produced by hot extrusion has a small purity in the longitudinal direction and the width direction, and when the material is made into a large-sized display (four) material, it has a capacity to form a sputter film uniformly. The effect of the hot extrusion can be carried out by the step of cooling the material immediately after pressing the extruded material obtained by hot extrusion, and then cold rolling. Rolling 12 201111536 5 1~1 00 Hv (Vickers hardness). If the strain is too much, the target atoms will accumulate and spatter and increase the formation of coarse clusters, and the formed film tends to become uneven. 'It is desirable to have a hardness of 1 〇〇 Hv or less. It is also known that, in general, for oxygen-free copper (C1020), recrystallization or annealing is completely performed, and heat treatment at the lowest tensile strength is achieved (coffin) The hardness is 51~59 Hv ("Extension Copper Data Sheet (2nd Edition)", Japan Copper Association, March 31, 2009, 2nd edition, page 61), the lower limit of the hardness range Based on this value. In addition, the adjustment of the hardness is performed by cold working such as rolling, and the processing rate of cold working is suppressed to about 30% or less, whereby the upper limit of the preferable range of hardness can be made 1 〇〇Hv or less, which is simple. A copper material having a hardness of 5 i to 100 Hv is obtained. As described above, cold working is performed to adjust the hardness. The processing rate is 〇%, that is, the hardness under the state of complete annealing (coffin) is 51 to 59 Hv. If the processing rate is increased, the hardness is slowly increased, and the hardness is 1 时 when the processing rate is 3〇%.

Hv. If the processing rate is too high, the hardness will exceed 100 Hv, which causes the above problem. It is cooled immediately after hot extrusion, and if necessary, the material produced by cold rolling, preferably a flat material, is processed to a target shape by any mechanical processing such as lathe processing, and is used for sputtering. . [Examples] Hereinafter, the present invention will be described in more detail based on examples, but the present invention is not limited to the examples. (Example 1) 13 201111536 An ingot having a diameter of 300 mm X and a length of 800 mm having a material of the purity shown in Table 1 was prepared as a small billet for hot extrusion. The pellet was heated to about 1 000 C and then extruded, and then the extruded material was immediately cooled at a cooling rate of about 100 C/sec for 20 seconds to obtain a plain plate having a thickness of 22 mm x 2 mm. Then, the above-mentioned plain plate is cold-rolled to produce a copper plate material for a sputtering target having a thickness of 2 〇 claw X width 200 mm×length of about 12 m (Ν), 再ο.Ι-Κι再者, n〇.h~ 15 is an example of the present invention, and n 〇 6 〜 1-8 is a comparative example in which the purity of copper is lower than that of the present invention. Further, as a prior art, a copper wire material for a flat wire is produced by using hot milk in a manufacturing process (5) as in (4). That is, the thickness of the purity of the material of the material is made... ah width (four) the length of the strip of the length of the town of mm, for a sniper. , -,, ..., rolling grain. The above ingot is heated to about 1 000 4 to make a ‘,, and rolled to produce a thickness of 23 melons and a width (4). The material cooling during the rolling is carried out by passing the material through the water-cooled zone after the final pass. Then, after planar cutting of the surface of the obtained plate, the thickness is 2 〇m by cold rolling, thereby producing a thickness of 2 G degrees Gmm, and then cutting the width of the edge plate (rolling) 贱 L mm x width 2GGmmx length about 丨21" The money is dried with copper material No. 1-9~1-1 1.

Regarding the N obtained in this way, the copper material 21 of the flat plate of the type 1 to 12 is moved according to the mode of Fig. 2, and the front end portion of the needle direction (the length of the extrusion (the end of the length) shown in the illustration of the long circle is shown. The center (end 1 ( 23 ), the center of the mountain ridge 0P ( 22 ) and the two parts (the center of the length) of the wide Tang (24)), the center of the length direction (26), the end 2 (27) direction Center portion (28) and both side portions (end 1 (29), end portions in the width direction of the end portion (25) and the side portions (end 1 and the rear end portion in the longitudinal direction of the extrusion (length 14 201111536 rear end)) In the total of 9 parts of 2 (30)), the crystal orientation distribution, crystal grain size, and hardness were investigated by the following method, and the longitudinal direction of the extrusion direction as shown in the explanatory view of the mode perspective view based on Fig. 3 Part (length front end) 31, the center portion (.length center) 32 in the longitudinal direction at the time of pressing, and the rear end portion (length rear end) 3 3 at the time of extrusion are cut into a diameter of 6 inches. For the circular plate, the sputtering characteristics were investigated by the following method. [1] Crystal orientation distribution regarding the crystal orientation in the copper material plate, Each part is made to have X-rays incident on the surface used as dry, and the intensity from each diffraction surface is measured. Compare the main ii}, {2〇〇), {22〇} and {31 i} faces. The diffraction intensity 'calculates the intensity ratio (crystal orientation) of the above formula (丨). Further, the conditions of the X-ray irradiation are: the type of the x-ray is CuK α i , and the tube voltage is 40 kv 'the tube current is 20 mA. [2] Crystal grain size Regarding the crystal grain size in the copper material sheet, it is used in the above-mentioned various parts, and the microstructure is observed on the surface used as a target, and based on JIS Η 〇5〇1 (cutting method) [3] The hardness in the hardness copper material sheet is measured on the surface used as a target, and is measured in accordance with JIS Z 2244 using a micro Vickers hardness tester. [4] The sputtering characteristics are shown in Fig. 3. The positions 31, 32, and 33 are cut from the obtained copper material plate by 6 inches (15 24 cm) and thickness 8 _, and are ground and 15 201111536 is used as a sputtering target. The effect of roughness, roughness is to grind all the maximum roughness Ra to 0.5~os μπι and make them consistent. Sputtering of the OA-1 bismuth glass substrate manufactured by Nippon Electric Glass Co., Ltd. with a thickness of 7·7 mm by a DC (Direct Current) magnetron sputtering device using the sputtering target prepared as described above A copper wiring having a thickness of 〇3 was formed. The sputtering conditions were such that the Ar gas pressure was set to 〇4 pa, and the discharge power was set to 12 W/cm2. Thereafter, heat treatment was performed in a vacuum of 3 Torr (rc, 3 〇 min). The film thickness of the copper wiring after the heat treatment is measured at a point of 1 point, and the range of the maximum film thickness and the minimum film thickness is ±7%, and 4 "good" is set. The results are shown in Tables 2 and 3. The inventive example satisfies any of the characteristics. In the case of N 6. i - 6 to i _ 8 of the comparative example, the crystal orientation, the entire region or the portion of the crystal grain (tetra) enthalpy deviated from the "defect" of the present invention. The previous example - "Benefit 2:" crystal orientation is outside the scope of the present invention in all of the examples. Further, although the crystal grain size is in the predetermined range of the present invention in the width direction, the crystal grain size at both ends is smaller than the center portion, and the tendency is such that the direction is not uniform, that is, the crystal grain size at the rear end is large. In comparison, the hardness also becomes uneven at the material width rt. According to the previous example, the splash characteristics are almost "not again 16 201111536 [Table i] Table 1

No. Material No. Copper purity (mass%) Manufacturing process Inventive Example 1-1 1 99.994 Hot extrusion 1-2 2 99.996 1-3 3 99.992 1-4 4 99.998 1-5 5 99.997 Comparative Example 1-6 6 99.958 Hot extrusion 1-7 7 99.929 1-8 8 99.976 1-9 1 99.994 Previous example 1-10 3 99.992 Hot rolling 1-11 5 99.997 [Table 2] Table 2

No. Material No. Crystalline Alignment Crystal grain size (μηι) Length Front end Length Center length Rear end length Front end center - Pc degree Rear end 1 Center end 2 End 1 Center end 2 End 1 Center end 2 End 1 Center end 2 end 1 central end 2 end 1 central end 2 Inventive Example 1-1 1 0.7 0.6 0.6 0.5 0.6 0.6 0.6 0.5 0.5 160 160 160 160 160 150 160 150 150 1-2 2 0.6 0.6 0.7 0.6 0.7 0.6 0.6 0,6 0.6 160 170 170 170 170 160 160 170 170 1-3 3 0.7 0.8 0.7 0.8 0,7 0.7 0.7 0.8 0.7 140 140 130 130 130 140 140 140 130 1-4 4 0.6 0.6 0.6 0.7 0.6 0.6 0.6 0.7 0.6 180 180 170 170 180 180 180 180 180 190 1-5 5 0.8 0.8 0.7 0.7 0.8 0.8 0.8 0.8 0.8 150 150 160 150 150 160 140 150 160 Comparative Example 1-6 6 0.3 0.4 0.3 0.5 0.3 0.3 0.4 0.3 0.3 90 100 90 100 90 100 90 100 90 1-7 7 0.2 0.3 0.3 0.3 0.4 0.3 0.3 0.4 0.3 80 70 90 70 80 80 80 80 70 1-8 δ 0.3 0.4 0.4 0.3 0,4 0.5 0.4 0.5 0.3 100 110 110 100 110 100 90 110 90 1-9 1 0.3 0.3 0.2 0,2 0.3 0.2 0.3 0.1 0.2 120 150 110 130 170 130 150 180 140 1-10 3 0.3 0.2 0.3 0.2 0. 2 0.1 0.1 0.2 0.3 110 120 110 140 160 130 140 170 140 1-11 5 0.4 0.3 0.1 0.2 0.2 0.1 0.2 0.2 0.1 120 140 120 150 160 150 150 170 160 17 201111536 [Table 3] Table 3 Material Vickers hardness splash Features]> Jo. No. Length. Former length length Central length Rear length Length Central length Rear end 1 Center end 2 End 1 Center end 2 End 1 Center end? Front end 1-1 1 88 86 84 85 85 87 84 83 86 η Liang Liangfa 1-2 2 85 81 83 82 85 83 84 83 80 Liangliang Liangming li 3 84 88 89 85 86 89 82 87 91 η Good example 1-4 4 78 77 82 81 79 79 78 74 80 Liangliangliang lb 5 78 73 70 74 72 76 74 78 78 Liangliangliang ratio 1-6 6 100 89 97 92 81 88 84 75 86 Bad defects are better than 1- 7 7 122 110 123 104 92 101 86 79 84 Adverse defects 1-8 8 90 83 88 78 70 82 76 65 78 Good and bad first 1-9 1 110 99 107 102 91 98 94 85 96 Adverse bad 1 -10 3 132 120 133 114 102 111 96 89 94 Good and bad defects 1-11 5 100 93 98 88 80 92 86 75 88 Good defects (Example 2) Preparation of pure copper No. 1 in Example 1 The green compacts were extruded under the hot extrusion conditions A to I shown in Table 4. Conditions A to F are examples of the invention, and conditions G to I are comparative examples. Further, the adjustment of the heating temperature is performed by setting the furnace temperature of the heating furnace. Further, the cooling rate is performed by changing the amount of spray of the water-cooling belt. The obtained hot extruded material was cold rolled in the same manner as in Example ,, and a copper material for a sputtering target having a thickness of 20 mm x width of 200 mm x and a length of about m was produced. Further, the crystal orientation distribution, crystal grain size, hardness, and sputtering characteristics were investigated in the same manner as in Example 。. The results are shown in Tables 5 and 6. The copper material produced in the examples of the present invention satisfies any of the characteristics. The copper material produced in Comparative Example G had a crystal orientation within the range specified in the present invention, but the crystal grain size was less than 100 μm, and the sputtering property was partially inferior. The copper material produced in the comparative example had a crystal orientation of the predetermined range β ‘ of the invention of 18 201111536, but the crystal grain size exceeded 200 μm, and the sputtering bond characteristics were partially poor. In the case of the example I, the heating temperature is higher and local melting occurs in the heating furnace, and a "" is taken, and the extrusion is performed. [Table 4]

[Table 5] Table 5 Crystalline Alignment Crystallization pull (um) - length before i length center length back end County Yuqian Cheng Zaifu Φ 4? · End 1 Central end 2 End 1 Central End 7 End 1 Central end? Yesterday 1 Central end 2 end 1 towel 端 end?瑞1吗 7 Inventive Example A 0.6 0.5 0.6 0.6 0.6 0.7 0.5 0.6 0.6 17.0 no no 17,0 no P0 no no no B 0.6 υ.ί> 0.5 0.5 0.5 0.5 0.6 0.S 0 S 100 no no 110 110 100 110 100 HO (J 0.7 0.6 0.6 0.7 0.6 0.8 0.6 0.7 0.7 150 160 ISO 150 ISO 160 160 140 ISO D 0.7 υ.6 0.6 0.6 0.5 0.6 0.6 0.5 0,6 140 ISO iso ISO 140 140 1/10 140 140 E 0.5 0.6 0.5 0.5 0.5 0.6 0.6 0.6 0.6 180 190 180 170 m 180 170 190 180 F 0.6 U.7 0.6 0.6 0.5 0.5 0.5 06 06 170 170 170 180 180 17Π ικη 1 7Π ion Comparative Example G 0.4 0.5 0.5 0.5 0.4 0.5 0.4 0.4 04 ς〇Q〇100 q〇90 80 80 Η 0.6 0.6 0.5 0.6 0.5 0.7 0.6 0.6 0.5 240 240 710 ?? 0 740 ?40 ?40 7^0 I Can not squeeze the squeeze $ 19 201111536 [Table 6] Table 6 Vickers hardness sputtering characteristics length front end length central length rear end length length length end 1 central end 2 end 1 central end 2 end 1 central end 2 front end central rear end A 83 86 85 85 84 89 91 89 85 good η good invention B 101 103 97 103 98 97 104 100 101 good η good C 79 81 85 85 90 82 83 86 89 good η good example D 80 7 8 81 82 85 79 83 86 84 良良良 t 81 79 76 88 85 80 89 85 87 良良良 l· 80 76 85 84 91 76 83 89 90 良良ή Comparative example G 121 124 119 Ϊ27 123 116 125 ΈΓ 124 A bad HT 78 75 80 79 81 79 81 80 76 Good and bad, the invention and its implementation are described together, but as long as the current month does not specifically refer to $, in the description of the __ details The invention is not limited thereto, and a broad interpretation should be made without departing from the spirit and scope of the invention as set forth in the appended claims. This case is based on the application filed in Japan on August 28, 2009. Litto 2__198982 claims priority, and the contents of this case are referred to in the present specification as part of this specification. BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a cross-sectional view showing the structure of a TFT element in a liquid crystal display. _ 2 is an explanatory diagram of the sampling of the measurement test of the crystal orientation distribution in the embodiment. Fig. 3 is an explanatory diagram of sampling of a splash characteristic sample in the embodiment [Description of main component symbols] 20 201111536 1 TFT element 2 Glass substrate 3 Scanning line 4 Gate electrode 5 Insulating film of tantalum nitride 6 Amorphous layer 7 Phosphorus-doped amorphous germanium layer 8, 9 source-nothing electrode 10 protective film of tantalum nitride 11 tin-doped indium oxide film 12 barrier layer 21 copper material of flat plate 22 central portion of length direction direction when extruded 23 24 when the two sides of the length direction of the extrusion are pressed, the central portion of the length direction of the extrusion is 26 ' 27 when the two sides of the length direction of the extrusion are pressed. The width of the front end portion (length end) of the front end portion (length end) of the center portion 29, 30 is wide toward the center portion (length center) toward the center portion (length) Width of the center to the rear end (length rear end) to the rear end (length rear end) 21 201111536 31 Length of extrusion 32 Length of extrusion 33 Length direction of the front end of the extrusion (length front end In the direction Central part (length center) Direction rear end (length rear end) 22

Claims (1)

201111536 VII. Patent application scope: 1. A copper material for sputtering target, characterized by high-purity copper with a linear tonnage of 99.99% or more, in the surface of the sputtering surface 1 1 ··· face, surface , {22〇} face, and {311} face each ray diffraction = intensity, that is, [(1) small 叩 (9) 卟 卟 and 屮 (1) satisfy the following formula (1)), and the crystal grain size is 100~200 Ηηι ; ' 1{200}/(1{111} + 1{20〇} + 1{22〇} + 1{311})^〇4 〇)〇2·The copper material for shaft dry as claimed in the patent scope It is produced by hot-extruding an ingot of high-purity copper having a purity of 99.99% or more, and cooling the extruded material immediately after the hot extrusion. 3. The copper material for sputtering target according to the scope of patent application item i, which is subjected to hot extrusion of an ingot of high purity copper having a purity of 99.99% or more, and the extruded material is cooled immediately after the hot extrusion. Then, it is produced by cold rolling. 4. If the copper material for dry ore in the application for the scope of patent application is: 〇〇~U)5 (hot extrusion of high-purity copper ingot with a purity of 99 99% or more under TC, The extruded material is produced by cooling at a cooling rate of at least two seconds after the hot extrusion. μ 5.- A method for manufacturing a dry-plated copper material, which is required to be sprayed in the first item of the patent. A method for plating a copper material for a target is characterized in that it comprises the steps of: hot-squeezing high-purity copper having a purity of 99 99% or more under 700~]05 generations, immediately after hot extrusion of the extruded material Cool at a cooling rate of 50% or more. 23