TWI293991B - Sputtering target and method of manufacturing same - Google Patents

Description

1293991 _ 索号 911 sister welcomes one-fifth, invention description (1) Technical Field of the Invention The present invention relates to a method of sputtering and film formation. The ruthenium plating target used in the prior art [Prior Art] One of the conventional film forming methods is known as a reduced shovel method. The _ surface generally means that under the decompression, the inert gas in a plasma state is hit by a machine key (hereinafter referred to as "target"), and the splattered squid flying out from the target is attached to the energy. The method of forming a thin film on a substrate is utilized in the industry because of the 尨 L L knife or the original product and obtaining a high-performance film. In addition, in recent years, in the sputtering method, a reactive sputtering method in which sputtering is performed in a reactive gas, a magnetron sputtering method in which a magnet is formed on the back surface of the target, and a high-speed magnetization sputtering method is formed. In the thin film formed by such a sputtering method, in particular, at least one of & (I η 2〇〇 or tin oxide (Sn〇2) is mainly composed of indium (hereinafter referred to as " Since the film has a high visible light transmittance and a high chemical conductivity, it is widely used as a transparent conductive film and is widely used for a liquid crystal turning, a heat-generating film for glass anti-fogging, an infrared reflecting film, and the like.曰曰颂 骏 置 置 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成 形成The sandpaper in the front and back is made into a grinding method, and is produced by performing other shapes processing by other processing machines. Ding plane research However, if a sputtering target prepared in this manner is used to produce a film, the following problems will occur. Righteousness, high performance, in the beginning, in other words, when sputtering is performed, especially during sputtering.

314023 (Revised Edition)· ptc Page 8 1393991 _ Case No. 91121199_April Day Correction _ V. Inventive Note (2) An abnormal discharge (hereinafter referred to as an initial arc) is generated (hereinafter referred to as "arc i ng") ), which will damage the film formation stability, and will also produce powder. The particles will adhere to and deposit on the sputtering target to form a black deposit called "n 〇 d u 1 e". This attachment is one of the causes of the initial arc and will also induce the production of new particles. In addition, if the particles adhere to the film, the film properties deteriorate. Therefore, when using a new sputtering target, in order to avoid such problems, even if a new sputtering target is placed on the sputtering device, it is necessary to start from the start of sputtering, and no arc can be generated. The time between product manufacturing is performed in an idle operation, which hinders the improvement of productivity. It is known that such an arc or agglomeration is produced by grinding the surface of the target, and the smoother the lower the phenomenon occurs, the surface grinding target for the surface grinding is the mainstream. For example, an ITO sputtering target that attempts to prevent arcing or agglomeration by setting the target surface roughness within a predetermined range is as disclosed in Japanese Patent No. 2 7 5 0483, No. 3 1 5 2 1 0 8 It is disclosed in the bulletin and the like. However, in order to achieve such a predetermined surface roughness, after the sputtering target is produced, the rough grinding is performed by mechanical grinding to adjust the thickness, and then the fine grinding (grinding) must be performed in a stepwise manner to reach the target surface. Smoothing, resulting in increased manufacturing time and cost issues. In addition, even if the I TO dry has such a predetermined surface roughness, the initial arc cannot be effectively prevented, and it takes a long time to perform the dry operation from the time when the new sputtering target is placed on the sputtering apparatus. problem. Furthermore, such problems are exploiting other oxides, nitrogen other than I TO

314023 (Revised Edition).ptc Page 9 1393991 Revision No. 91121199 V. Inventions (3) Powder metallurgy method based on compounds, carbides, borides, etc.) The metal target will also be the same. The present inventors have been in the above situation, and after intensive research, the result is that the sputtering target produced by the mechanical grinding step may have a grinding powder or the like in the initial stage without surface, or due to thermal shock = Detachment produces powder particles, which are the main cause of arcing and agglomeration, as long as they are removed to prevent the formation of an initial arc. ° Α In addition, according to the results of the study by the inventors, it was found that the above-mentioned parts were separated from the surface layer by the thermal shock during sputtering to produce powder particles, and it was said that it was caused by 粗 : ^ rough seam degree. This is attributed to the mechanical grinding that causes the dry surface to produce fine cracks & i η _ hungry Wei Ling inside. Moreover, it is found that the existence of all the fine turtles is not the cause of arcing and agglomeration. Especially for the initial arc, there are subtle cracks of depth and length above a predetermined value, which are caused by the substantial elimination. Such fine cracking can effectively prevent the occurrence of an initial arc, and thus the present invention has been completed. Therefore, the object of the present invention is to provide a sputtering target which can prevent the initial arc generation and improve the initial stability of the ruthenium plating, and which can significantly improve the productivity at the time of film formation, and a method for producing the same. SUMMARY OF THE INVENTION The sputter coating of the present invention is subjected to a mechanical polishing step to perform a sputtering process on the sputtered surface of the target prior to shipment. In the sputtering target of the present invention, the integrated input power amount of the sputtering treatment applied to the sputtering surface of the sputtering target is preferably 〇·〇〇5Wh/cm^, especially 〇· 01 Wh/ The cm slave is better, and it is better. 02Wh/cm slave is better. The present invention is preferably used for sputtering of the above-mentioned sputtering target at the time of shipment.

314023 (Revised).ptc Page 10 1293991

Amendment 5. Inventive Note (4) A surface protective film is attached to the surface. Further, in the present invention, the sputtering target is preferably produced by a sintering method. ^ The Mingzhi splash target is made of indium oxide or contains an oxide (I TO) of one of the original meanings of indium oxide and tin oxide. ~ ΛΑ * t 明之贱 干 dry manufacturing method, it is best to use the target surface obtained by the sintering method AU _ SI, Μ 订 订 订 订 订 订 订 订 订 订The surface is sputtered. Ττη^ ^ When the 干 贱 贱 贱 贱 贱 属 属 I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I The obtained 1 το dry surface is subjected to mechanical grinding, and then r ♦ 2 2 f is first subjected to the treatment of the at least _ key surface of the 1 Τ〇. L Besch method] The following is specifically described for the present invention. By the machine I! : ί t the splash target, both the first and second aspects are manufactured by the stack grinding step.便 句 ::: The invention of the splash target is only the mechanical composition of the nitride, carbide, butterfly and other components of the main composition of the Tao Jing n〇 =: the target. Specifically, such a target may be, for example, at least one of φ or Ζηο as at least one of I η 2 〇 S S η 0 2 is mainly composed of eight, a component of (ΙΤ0), a ratio of 1η2〇3, Snf) 7 0 Knife (ΙΖ0), Ζη0-Α 1 20 3, Ιη20 3, bn02, ZnO, Al2〇3, Si09, Ta η μ a AIN, ς·Γ uwp 2 (4) 5, MS〇, NiO, Si3N4 , AIN, SiC, Mo, W, Cr, Ti, Zr, Hf ml by TTn^ ^ ^ Hf, Nb, Ta, A1, and the like. The 'ITCb贱 mine dry' in these is required to be sprayed efficiently by water, and

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IHM 314023 (Revised Edition) · ptc Case No. 9Π21199 1293991 Amendment 5, Invention Description (5): High initial stability, θ The first aspect of the present invention can be particularly effectively applied thereto. $ 悲 样 , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , (4) Various dry or wet methods are known for forming & sintering: when a metal-based target is produced by a sintering method (powder metallurgy method) which performs mechanical grinding, it can be cast after vacuum melting. Plastic addition = after the vacuum dissolution method of mechanical grinding, or H丨P (hot pressure compression, gentleman method, or CIP (cold pressure equalization sintering) method, then sintered, processed powder metallurgy The above dry method may, for example, be a CP (cold press) method, an HP (hot press) method, a Η IP (heat equal pressure sintering) method, etc. The c P method fills a mixed raw material powder into a forming mold, The molded body is formed into a molded body and fired (sintered) in an atmosphere or under oxygen gas. The HP method is carried out by simultaneously charging and heating the mixed raw material powder in a forming mold inside the furnace. Forming and sintering. HIP law will be mixed original The powder or the preliminary molded body is sealed in a metal foil such as y rubber or a metal foil which forms a covering even at a high temperature, and then inserted into a container, and isotropically applied through an inert atmosphere gas medium. The heating method is performed while applying pressure. /, The wet method is a filter molding method as described in Japanese Laid-Open Patent Publication No. 2 8 6 0 No. 2, which is a slurry molding method. A vacuum forming material is obtained by decompressing water to obtain a molded body, and a filter forming mold composed of a water-insoluble material is used. In the filter forming mold, the mixed raw material powder, ion-exchanged water, and organic additives are injected. of

314023 (Revised Edition) · ptc Page 12 Case No. Θ112119Θ The cookware is formed into an equal mechanical step, and the grinding step and the like are separated and shaped to produce agglomerates, which will result in a blow through the latter described. (6) Draining, drying and degreasing in the slurry after decompression, and then baking, and the appropriate temperature set in the above-mentioned respective methods is as described above, so that the raw material is after the molding, The target is processed to be smooth, and the planar grinding ore is applied at least by mechanical grinding in such a manner that adhesion to the substrate is adhered and deposited when the chain is removed from the surface by mechanical impact, which may normally occur with thermal shock during the grinding step. On the target, it is judged by the cause of the arc. Therefore, in the present invention, the sputtering target of the target plating is subjected to, for example, powder particles or thermal cracking at the time of sputtering to lower the initial arc. <First aspect of the present invention> i first 'produced after the sputtering of the first aspect of the present invention, and after the smashing of the target, the fine-grained fine-grain cutting mechanical grinding Because it is a sharp cut, the corrected moisture of the workpiece is ground to form a molded body, and the knot is formed. Preferably, the sintering temperature is matched and fired at a predetermined size. Changed. The initial film formed by the sudden formation of the powder is black. The new powder is mechanically ground. The specific treatment is easy to break off the knot, or in other words, the dry powder and the part. In the process of depositing, the adhering portion is formed by mechanically grinding the shape of the shaped body described later, and the surface of the target is formed, generally on the surface of the splash, or with the splashing of the powder, and then The removal of this by the electrician can be explained in one aspect. The key system is as described above according to the usual method, cracking or the use of a high-speed rotating abrasive sanding technology in the manufacturing process, so the contact with the blade between the matte should be

1293991 _ Case No. 91121199_P Year (Monthly Revision _ V. Inventive Note (7) Force, a turtle will be produced on the surface of the target (especially for the surface for sputtering, hereinafter referred to as the "target surface") Crack. In this type of crack, the crack that can be observed from the surface is considered to be a grinding damage or a processing defect, but so far, no discussion has been made on the fine crack extending from the sputtering surface toward the inside. Although the degree of occurrence of the shape (depth, length, etc.), or the number of the fine cracks is different, as long as it is inevitably generated through a mechanical grinding step, the degree of occurrence will be adopted in the mechanical grinding step. In the first aspect of the present invention, attention is paid to the fine cracking of the abrasive article, and a microscopic crack can be provided to substantially eliminate the depth and length of a specific value or more. Cracking and effectively preventing the target from generating an initial arc. In other words, as mentioned above, the presence of all fine cracks does not cause the initial arc, but has a specific value or more. The existence of fine cracks in degrees and lengths is the cause of the initial arc. When the profile of the dry money surface is observed, the initial arc can be effectively prevented by substantially eliminating such specific fine cracks. Specifically, the sputtering target of the first aspect of the present invention is a sputtering target prepared by a mechanical polishing step, and substantially eliminates the depth of loss when the sputtering surface of the target is observed in a cross section. A fine crack of 5/zm or more and a length of 40/zm or more (preferably a depth of 1 〇//m or more and a length of 30//m or more). Here, the substantial elimination of fine cracking means that a fine turtle is applied to the target. The crack removal treatment does not find a fine crack with a depth and a length above the above specific value when the cross-section of the target is observed. In particular, it means that when the target is sputtered, In wide

314023 (revised edition).ptc page 141293991 _mt 91121199_β year & month correction __ five, invention description (8) in the degree direction, length 2 · 5mm range, no depth of more than 1 5 / zm and length Fine cracks of 40//m or more (preferably 1 〇//m or more and 30/zm or more in length). This is because even if there are fine cracks whose bead and length are lower than the above values, in this case, the fine crack itself will not cause arcing, and will not cause cutting with thermal shock during sputtering. Injury and the phenomenon of the source of the powder. More specifically, 'when the face is sputtered to observe the sputtered surface of the sputter target', no fine cracks of depth and length above the above specific value are found, even above 5/m and below 10 / m, and the number of fine cracks of length m or more and less than 30 / / m, in the width direction of the section, the average length of 2 · 5mm, preferably less than 5, especially in 3 is better It is better to be less than one. Of course, when the cross-section of the target sputter surface is observed, the depth is not more than 5# m and less than 1〇" m, and the length is more than 1〇〆m and less than 3X〇" fine crack, in other words 5毫米为0。 The number of the above-mentioned fine cracks, preferably in the width direction of the cross section, the average length of 2. 5mm is 0. However, if the number of cracks is 5 or less (preferably 3 or less, particularly preferably i or less), the initial arc can be effectively reduced without impeding the sputtering. Specifically, as a sub-microscope (SEM), the means for observing the cross-section of the target sputter surface is observed by a microscope such as an optical microscope, an electron microscope, or a scanning type. However, the ruthenium plating surface of & is as described above, and usually has fine irregularities due to the mechanical polishing step, and the setting of the deep cracking and long-term production of the above-mentioned fine cracking will cause a problem. So, in this book, ^ related

314023 (Revised Edition).ptc Page 151293991 Amendment No. 91121199 V. Description of invention (9) The definition of the depth and length of the fine crack is described below according to the figure. 0 In this specification, the so-called fine turtle The depth of the crack is, as in the third section, the cross section 3 in the direction of the target thickness, from the sputter surface 1 corresponding to the region where the fine crack 5 exists, and the top of the ridge line formed by the wearing surface 3, to the subtle The depth of the crack 5 is called the depth D. Okamoto is even more in this specification + 'The so-called fine crack length means the maximum distance l in the horizontal direction of the fine crack 5 of the section 3 as shown in Fig. 1. Further, the sputtering target according to the first aspect of the present invention may be a target which has substantially eliminated a fine crack of a depth of a predetermined value or more and a length. The surface roughness of the target sputtering surface (the arithmetic mean roughness of the roughness curve) Ra (measured according to JIS B0 60 1 C 1 994) may be ίο" m or more, or 5 // m or more, or 2 . 0 // m or more. Therefore, in the sputtering target of the first aspect of the present invention, in order to reduce the surface thick chain as is conventionally known, since the dry surface does not need to be slipped, the grinding step can be omitted. Make two twenty liters to make it productive. The production step, and of course the above, is further suitable for the present invention even when the Ra of the target is less than 1.0 m/m.质 在 在 获得 获得 获得 获得 获得 获得 获得 获得 ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( 已 已 已 已 已 已 已 已 已 已 已 已It is not found that ^, the aspect 'microcracking. Λ The above specific fine method to substantially eliminate such fine cracking (fine turtle), only to substantially eliminate the above-mentioned fine cracking of the 咭<

314023 (corrected version).ptc ° ' can be used to 1293991 -^^91121199 repair 5, invention description (10) What method. For example, the surface of the target grinding tool load or rotation speed, such as the weight of the target grinding, 16 lines strictly control the research, 铋 铋 * 丨 old + fine blanket, grinding, sputtering, laser processing, dry etching In the case of sand blasting, it is best to say that it is very good, / mine treatment, laser treatment, dry view, splashing sound:: 2 fine crack removal point 9' lifting target The sputtering method is performed by sputtering, and the method of = is specifically described as an example.仃# J?=Bei method for the above-mentioned fine crack disappearance (the removal of fine cracks:), when using bismuth plating, the method of sputtering; ϊ, 商告站, 埋埋: other restrictions ' ▼ Matching needs to be done == two. 4' If the splashing gas can be used in combination with the inert gas I# such as argon, it is preferable to set the gas pressure to is ι〇ιητ〇^. Furthermore, the integrated input power amount (Wh/cm2) at the time of sputtering (that is, the total power amount of the average target unit area to be input at the time) is preferably 〇i to aging for 10Wh/cm2, especially 〇· A range of 5 to 5 Wh/cm is preferred. When the integrated input power amount is within the above range, it is advantageous in terms of productivity required for the production of the sputtering target and productivity such as cost, in addition to the substantial fine cracking. Specifically, for example, in a sputtering device using a DC magnetron sputtering method, a target (which may be bonded to a wide plate) prepared by a mechanical grinding step is disposed, and then a sputtering gas of the above composition is used. Until the upper and & product = the amount of power input, the sputtering process is performed, and the money and dryness of the hair and the knife are obtained. When you obtain the dry surface when the sputter surface is observed in the cross section, the fine crack of the depth and length at a specific value has virtually disappeared.

1293991 V. Invention description (11) ~~~-^~t month ~~, the formation of the film ^', and the superior initial ^ effective to prevent the initial arc of the present invention - The β β device adopts the initial arc characteristic of the second = no system (such as the company name, transliteration), and enables the company to perform the film formation, and then the target of the above treatment can be used. :^h/Cm % Accumulated arc "When ^2?: The demining system of the input power is the first state of the invention, and the initial arc characteristics are better. The cumulative arc times are more than < The second aspect of the present invention is as follows: Secondly, the second aspect of the present invention which can be used in the second aspect of the present invention is: after the mechanical polishing is performed before the shipment from the splashing clock (four), it is reasonable. The sputtering surface of the plating surface is as described above, and the reason for the initial arc can be made by the cutting step, and the steel is coated with the sputtered surface of the sputtering target. Le Zhong-like & Α 〇 There is a powder, or a part that is easily separated from the thermal shock of the splash. By pre-sputtering the sputtering target ^2丄Α, ^ ^ < the sputtering surface itself is sputtered, and the micro-powder or the sputtering 溅 溅 Μ If the part that is more likely to be detached from the splatter is removed from the sputtered surface, the arc can effectively reduce the initial and other impacts, and the specific surface of the target surface can be removed even if it is detached. In the case of a depth value higher than the fine value generated by the recognition unit, the above-mentioned is a thermogravimetric polishing which is dependent on the micro-cracking and the fine-split key of the length, and whether or not there is a random turtle such as a micro-turtle from the first part of the present invention. crack.

314023 (Revised Edition) · ptc Page 18 9112113⁄43⁄4 1293991 Amendment 5, Invention Description (12) Therefore, in the second aspect of the present invention, it is also preferable to perform sputtering on the sputtering surface of the sputtering target in advance. According to the first aspect of the present invention, a target which is finely cracked with a specific value or more and a substantial degree of cracking is formed. However, when such performance is not required, it is not necessarily limited to this. In other words, in the second aspect of the present invention, the integral input power amount for the sputtering treatment previously applied to the sputtering surface of the sputtering target is preferably at 0. 0 0 5Wh/cm^, especially 〇〇1Wh/cm^ is better, 〇2Wh/ci^ is better, especially for 〇^. 2 ; = quantity i: /Cm2) means the amount of dry splash before shipment. If the integral power of the average unit area is calculated, if the above-mentioned integration is performed on the 〇.〇〇5Wh/Cm^, it can effectively prevent the initial Ϊ = period electric soli characteristics. Preferably, since the surface does not need to be generated in a second, the user of the sputtering target performs the sea for film forming: operation, and the plating is directly performed by the machine and the thinning is performed efficiently. The productivity of film formation, in addition, the pre-execution of the win & system, if the sputtering condition of the normal strip; a treatment is not particularly limited to the amount of power input, the above-mentioned sputtering process is performed until the above product is reached. The present invention;:, can. , arc characteristics when using p 6 吋 target for sputtering

314〇23 (Revised Edition). Ptc No. 19 on page 19: In your sample, the upper limit of the amount of integrated input power is usually the time required for the manufacture of the target, the cost, etc. The initial electricity of the above target is taken at 10Wh/cm. 1293991 _ Case No. 91121199_Announcement of the Year of the Year - Amendment 5, Invention Description (13) · ~ _ ^ In the case of the case, the amount of integrated input power that is input until the arc generation interval is more than leap seconds (Wh/ Cm2) for evaluation. Specifically, when the ruthenium plating process is performed, the measuring device senses the arc using an arc counter (manufactured by Randmark® Technology Co., Ltd.), and uses the initial arc converging up to P6. The integrated input power amount up to the point where the interval between the arc and the next arc is equal to or greater than 1 sec. is evaluated. The smaller the value of the integrated input power amount, and the smaller the number of arc generations, the better the initial arc characteristics of the target. Furthermore, in the second aspect of the present invention, in order to perform a ruthenium plating treatment on the sputtering surface of the target, the surface roughness Ra of the sputtering target of the second aspect of the present invention is generally set to be larger than that of the mechanical polishing. After the initial value. Therefore, the Ra of the sputtering target of the second aspect of the present invention can also be set to be larger than the conventionally preferred 〇. 5 # m. Further, even in the case where the Ra of the target is 5% or less, it is of course also applicable to the second embodiment of the present invention. In addition, the surface roughness Ra in this specification means the arithmetic mean roughness of the roughness curve measured by J I S B 0 6 0 1 (199.4). More specifically, if the Ra value of the sputtering target according to the second aspect of the present invention is continued to be sputtered, it will be converged to a substantially constant value regardless of the initial value, from the viewpoint of productivity of the sputtering treatment. The Ra value of the sputtering target can be set in the range of 0 · 1 to 5 · 0 # m, and can also be set in the range of 〇 · 1 to 3 · 0 / / m. Further, in the second aspect of the present invention, the bell is sprayed on the sputtered surface; after the plating treatment, it is preferable to immediately attach the surface protective film to the tantalum surface. If the protective film is attached to the surface of the storage surface, impurities can be prevented from adhering and the gas can be adsorbed on the sputtering surface. The above surface protection film is for preventing adhesion of impurities and gas adsorption to the splash 1293991

^ At least the attached side of the protective film on the sputter surface can be dried as a whole. 5. Description of the invention On the surface of the money, it is attached. The film is adhered to the whole process. The thinner tree between the targets is on the target surface. In the case of pre-sintering, in the case of pre-sintering, tin is mainly used as a mechanical surface for the implementation of the splashing surface. -^^91121199 (14) Vacuum packaging method. ί中也=Resin film will be free of residual bubbles, this is more than: 匕褒 is because there is no special limit for film and grease film:; θ θ 2 is used for surface protection 'so it is better to use To prevent the transfer of the powder particles, the present invention relates to a resin film made of exfoliating granules. The method of manufacturing a sad sputtering target is to perform the target of the sputtering target of the second aspect; a 1 to remove the target (preferably to tl· LA, surface mechanical grinding, Straight in the 屮, the hair of the 2nd 贱 贱 施 施 施 施 施 施 溅 溅 溅 溅 溅 溅 溅 发明 发明 发明 发明 发明 发明 发明 发明 发明 发明 贱 贱 贱 贱 贱 贱 贱 贱 贱 贱 贱 贱 贱 贱 贱 贱 贱 贱 贱 贱 贱 贱For the Ting gentleman method, the surface is sputtered with 1 το obtained by indium oxide and oxidized grinding, and then treated in the second=2. Bebe' pre-deposited at least J Ϊ k The manufacturing method of the money plating dry, except for the ordering of the Tibetan key, the processing of the general sputtering target can be used.

Drinking spoons, as described above, 铱丄, J empty dissolution method, etc., so that the raw material ΐ mold method (powder smelting) for a long time to make the surface belt #玉 Mu for the target processing into a given size, usually after mechanical grinding Mechanical grinding such as two-face grinding. This _____^4 is connected to the bottom plate to form a sputtering target c.

1293991 Rev. 5, invention description (15) Grinding and grinding, generally adopting the method of plane grinding, etc., to form the flat surface of the above-mentioned forming process: b and rough grinding the surface, then Make the surface of the heart thousands, month, and stage the use of fine-grained matte, and apply (hereinafter also referred to as "grinding"), or perform grinding with glass beads, pearl beads, and wrong sand: The method of manufacturing the sputtering target, which is referred to as the second aspect of the invention, is subjected to mechanical polishing of the target surface as described above, and then at least the sputter surface of the target is previously sputtered before shipment. The sputtering target is produced by the treatment. The sputtering treatment can be carried out after the grinding, or after the fine grinding, after the sandblasting, and after the bottom plate, by using at least the splash surface. By sputtering, it is possible to remove the burrs or abrasive powder generated by the polishing or the spaces which are easily separated by thermal shock during sputtering, and as a result, the initial arc can be effectively reduced. Two-state Even if the surface is not subjected to mirror-like smooth polishing, and the blasting treatment with a fine particle size is performed without suppressing the surface roughness, a target which can reduce the initial arc and can effectively perform the sputtering treatment can be obtained. When the target of the second aspect of the present invention is used, the polishing step can be omitted, and the sputtering target can be formed by performing a sputtering treatment on the sputtering surface of the target. [Effect of the Invention] According to the first aspect It can produce fine cracked arcs, and the effective reduction of production is derived from the mechanical polishing, especially to reduce the initial arc.

314023 (Revised Edition)_ ptc Page 22 Case No. 91121199 1293991

Amendment 5. Inventive Note (16) Effect can significantly improve initial stability. In the first step, the production step can be simplified, and the polishing step is omitted. Further, the initial stability of the second off-arc arc according to the present invention is high: if the sum is second, the sputtering process can be effectively reduced, and the efficiency can be improved.曰 1 target. By using this sputtering target film. In addition, since it is possible to omit the productivity of grinding cattle and to form a thinness of the performance of the crucible and to achieve a low cost.因此" 'Therefore, it is also possible to simplify the grinding step. </ RTI> </ RTI> <RTIgt; </ RTI> <RTIgt; </ RTI> <RTIgt; </ RTI> <RTIgt; </ RTI> <RTIgt; The examples and comparative examples are as described in the column A1 &lt;Production of the target&gt; Example A 1 $ qu , the formula made to 3 and the comparative example A 1 used in the dyeing method. For example, the following is a mixture of In2 powder and Sn powder. Concurrent A 23 8^0 2=90: Zengwu. / Relatively poor ί conventional method for making 1T0 sintered body to form 钋j ratio relative initiality is 99.7 %. Bin into the target. This target of the dry material a plane grinding 鞑 wide:) 01·6 with 8 pieces, and placed in the joint surface (welding surface ^ then use # 170 diamond grinding tools on the sputtered surface ^2 to a8.) Double-sided grinding, to obtain a target team with a thickness of 6mm, in A1, &lt;fine crack removal treatment>

314023 (Revised Edition) ptc Page 23 1393991 Revision _91121199 V. Invention Description (17) The target Ν0·&amp;1&amp; a2 obtained in the above manufacturing example A1 is respectively soldered to a copper base plate and then mounted on the sputtering plate. The apparatus (Εχ_3〇13Μ, manufactured by Vacuum Instruments Industrial Co., Ltd.) was used to remove the sputtering treatment for fine cracking according to the following conditions. (money ore condition) sputtering method: DC magnetron sputtering treatment gas: A r treatment pressure: 3mTorr oxygen partial pressure · O.OZniTor'r input power: 3W/cm2 integral input power: l〇Wh/cm2 The surface roughness of the surface of the money of N 〇· a 1 and a 2 before and after the processing of money and money is based on JISB 0 6 0 1 (1 9 94) and the surface roughness test is made by SE 1 70 0 C. Measured according to the stylus radius: m, feed speed: 0_5mm/sec, cutoff: λ c 0.8mm, evaluation length: heart, piece. The results are shown in Table 1. &lt;Cross-section observation of Geba&gt; Using a grinding disc (manufactured by Okamoto Machine Co., Ltd.), the cutter was cut by a diamond #1 0 0 with a thickness of 1 mm of β 2 0 5111111 X, and the above-mentioned splash was strictly applied. No.al' is cut in the thickness direction. Next, using a grinding disc (manufactured by Okamoto Machine Co., Ltd.), the No. 3: 7 was polished by the #60 0 diamond wheel of 205 mm x 10 mm thickness with a +77 cut surface. # Next, single-sided grinding Machine (speed Peterfam company (company name "two 〇 1 translation" production), using GC# 1 0 0 0 free scrub, the above target N〇· ai

314023 (Revised).ptc Page 24 Case No. 91121199 1293991 % 曰

Month 5, invention description (18) Secondly, using a single-sided polishing machine (speeded by Peter Pem (company name)), using diamond grinding with an average particle size of 〇·1 # m, oblique μ 曰N 〇 · The cut section of a 1 is polished. % The cut profile of the above dry No. a 1 was produced using an optical microscope [Austrian Co., Ltd. (company name, transliteration), Βχ5〇-33p (attached to the spotlight, light observation). The results are shown in the table i. )]Into &lt;Evaluation of Initial Arc Characteristics&gt; Division: = Splashing treatment as a fine crack to go to the industrial company to produce X:, mining equipment (ΕΧ_3013Μ, vacuum equipment technology company (company name, sound dish visual state ( MAM Genesis) (Spark of Randmark. Sputtering at this time)) The results of sensing the reduction are shown in Table 1. ', /, arc sensing conditions are as follows. Junction (sputtering condition (ΜArc monitoring 玑 plating method processing gas processing pressure 1) 03⁄4 control money plating Ar ^ 3mTorr ^ Partial pressure: 0.02mT 〇rr Input power: 3W/Cm2 Integral torque sensor and power input amount: 5wh/cm2 &quot; 'conditions' sensing mode: energy

±JkMk2 Hard arc minimum time: 1 00// S

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Arc sensing voltage: 100V large-medium energy boundary: 50mJ Case number 91121199

1293991 V. INSTRUCTIONS (19) In addition to replacing 粑N〇· al and a2 with target No. a3 and a4, the integrated input power in the sputtering treatment conditions performed by the fine crack removal treatment is from 1 OWh/οιηϊ The text is 6Wh/cm, and the other κ^ modes are the same as the embodiment Α1. The results are shown in Table 1. Example A3 In addition to the target No. a5 and a6, Ν〇· al and a2 are replaced, and the integrated input power in the sputtering treatment conditions performed by the fine crack removal treatment is from the tooth, 1 0 W h / cm Except for 3 W h / cm, the remaining modes are as implemented A1. The results are shown in Table 1. , Comparative Example A1, and the fine turtle Example A1 was not executed. As a result, the other embodiments were as shown in Table 1, except that the targets No. a7 and a8 were substituted for No. a 1 and a2, and the split removal treatment was carried out. Table 1

No. The number of fine cracks (number)*^ Surface roughness Ra (μ, m) before splashing (crack removal treatment) Surface roughness Ra (μ m) after the money mirror (crack removal treatment) Arc generation Number of times (times) D^15 D^IO —^ 0^5 L^40 L^30 L^IO Example A1 _ al 0 0 0 1.1 1.3 - a2 Transfer 1.2 1.2 1 Example _ a3 0 0 1 1.1 1.1 - A2 a4 - one - 1.0 1.2 2 Example _ a5 0 0 3 1.1 1.1 - A3 a6 - • a 1.0 1.1 7 Comparative example ^ a7 5 8 10 1.1 - - A1 Γ a8 - - - 1.2 - 21

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Mi 911211flQ

π年士月 曰五, invention description (20) *.......D series fine crack depth U m) L series fine crack length (/ / m) Next, for the second embodiment of the present invention 1 He exemplified the following = In2 〇 powder and Sn0 powder according to In2 〇 3: Sn 〇 2 = 9 〇: line mixing, and according to the usual method of making IT 〇 sintered body to form 0 shells than the input material cut into "吋 size After that, the surface is polished by a flat surface (sputtering surface) and the surface of the sputtering is adjusted to 5 degrees. 二: 2 = row double-side grinding, grinding tool grinding, and VV Face::Different number of diamonds 1 wait No. bl to b4. In addition, instead of the sputtered surface, the 'grinding tool' is ground and the raw material of the alumina is used for sandblasting to obtain the target No. .b5. Reverse squirting / Saki-man's welding of these targets on a copper base plate, and then mounting them on a hand-made money mining device, and performing sputtering treatment under the following conditions: G贱 bond condition) sputtering method : DC magnetron sputtering process gas: Ar Processing pressure: 3mTorr Oxygen partial pressure: 0.03mTorr Input power: 1. 64W/cm2 At this time, the arc counter is used // Arc monitor y AM Genes is) (Landmark Technology Co., Ltd.), and the measurement conditions are set to: sensing mode: energy, arc sensing voltage · 100V, large-medium energy boundary: 5〇mj, hard arc minimum time: 1 0 0// s ' and perform arc sensing, the measured input power amount when the arc is closed up to the end of the arc (before the arc interval is more than leap seconds),

314023 (Revised).ptc Page 27 1393991 ^ ^ _tE 91121199_/3 years (month, day _ correction _ five, invention description (21) continue to perform sputtering process until the integral input power is 〇. 1Wh/cm 2 The results are shown in Table 2. The surface roughness Ra of the sputtering surface of the target before the sputtering treatment was measured according to JIS B 0 0 0 1 (1 9 94), and the results are as shown in Table 2. The surface roughness meter is based on SE 1 7 0 0 (manufactured by Otaru Research Institute), semi-pinch according to stylus: 2// m, feed speed: (K5mm/sec, cutoff: λ c (K8mm, evaluation length) : 4mm condition, measurement. Table 2 sample No. Density (%) Density (g/cm3) Pre-treatment technology surface sugar degree m) Integrated input power (Wh/cm2) 1! Electric bow melon generation (times) 12 bl 99.1 7.09 035 0.0100 261 b2 99.5 7.12 1.38 H 0.0120 1 -1119 b3 1 99.1 7.09 1.01 0.0073 740 Μ 99.3 7.10 0.79 0.0091 __83 b5 99.6 7.13 2.47 0.0064 1052

314023 (revised edition).ptc

1 1 ··· The amount of integrated input power when the arc generation interval is 10 seconds or longer * 2 · The number of arc generations when the arc generation interval is 1 〇 or more Example B 2 Stripping from a hand-spraying device The sample used in Example B 1 was subjected to vacuum packaging and allowed to stand for 1 day. Then, the sample was taken out from the vacuum package and mounted on the above-mentioned hand-made sputtering apparatus, and the enthalpy plating treatment was carried out in accordance with the full-key condition of Example B1 in accordance with the integral input power amount of Example B1 until it became 5 Wh/ Up to cm 2 . Further, as in the example B1, the measurement of the surface roughness Ra before the sputter treatment was performed. The results are shown in Table 3. 1293991 sharp hidden (10) V. Description of invention (22) Sample No. 3 No. 积分 Integral input power (Wh/cm2) Sub-Lin _ front surface. Tree level Ra (/zm) Integrated input power (Wh/ Cm2)" Number of arc generations (times) *2 bl 0.1 0.37 0.0004 2 b2 0.1 1.35 0.0009 2 b3 0.1 1.09 0.0005 3 b4 0.1 0.81 0.0009 4 b5 0.1 2.48 0.0004 2 * 1 ···The arc generation interval is more than 10 seconds The amount of integrated input power* 2 ···· The number of arc generations when the arc generation interval is 10 seconds or longer is known from the third table. If the sputtering process is performed, the arc after the sputtering will be closed. Faster, the number of arcs is also reduced, and has superior initial arc characteristics. Example B 3 The sample used in Example B2 was stripped from the hand-sputtering apparatus and then mounted, as in Example B1. The antimony conditions were matched with the integrated input power of Example B 1 and Example B 2, and sputtering treatment was performed until it became 6 Wh/cm 2 . As a result, no arc interval was generated for each target of less than 1 〇. Arc. In addition, as in Example B 1, the surface before the sputter treatment Roughness Ra measurement. The results are shown in Table 4.

314023 (Revised Edition).ptc Page 29 1139991 «91121199 Beta Year 6 Introduction Revision 5, Invention Description (23) Table 4 Sample No. Pre-Integrated Input Power (Wh/cm2) Surface 灭 before the plating treatment Rough integral input power (Wh/cm2)*! Number of arc generations (times)*2 bl 5.0 2.01 0 0 b2 5.0 1.74 0 0 b3 5.0 2.23 0 0 b4 5.0 2.92 0 0 b5 5.0 2.36 0 0 * 1 ··· The amount of integrated electric power when the arc generation interval is 10 seconds or more * 2 · The number of arc generations when the arc generation interval is 10 seconds or more [Industrial Applicability] The sputtering target of the present invention is effective It reduces the generation of the initial arc and is therefore suitable as a target for sputtering and film formation.

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Claims (1)

Public 12 (4) No. 91121199 Office Year 々曰 Amendment _ VI. Application for iTIEll 1. A method of manufacturing a sputtering target, which is to mechanically grind the target surface, and then pre-spray at least the sputtering surface of the target before shipment. The plating treatment, and the integral input power amount of the key-off treatment applied to the 贱 key surface of the 丨贱 key is 0.005 to 10 Wh/cm2. 2. The method of producing a sputtering target according to the first aspect of the invention, wherein the target is a target obtained by a sintering method. 3. A method for producing an ITO sputtering target, which is a mechanical polishing of an I TO light surface obtained by sintering a raw material containing indium oxide and tin oxide as a main component, and secondarily pre-drying this I TO before shipment At least the sputtered surface is sputtered, and the integrated input power of the sputtering treatment applied to the sputtered surface of the sputter target is 0.05 to 10 Wh/cm2. 314023 (Revised).ptc第32页