High-purity tantalum-containing products, such targets for sputtering

 

The proposed high-purity metal containing tantalum and its alloys. Metal tantalum preferably has a purity of at least 9,995% and more preferably at least 99.999% availability. Also proposed metal tantalum and its alloys, or which have a grain size of about 50 microns or less, or texture, in which the (100) pole figure is the intensity of the Central peak is lower than about 15 random, or the logarithm of the relationship of the intensities of the (111):(100) center peak greater than about 4.0, or any combination of these properties. In addition, the proposed products and components made of metal tantalum, which include, but are not limited to, a target for sputtering, condenser capacity, resistive film layers, wire, etc., also Proposed a method of manufacturing a high-purity tantalum, which includes the stage of the interaction between salt containing tantalum with at least one compound capable of restoring this salt to the tantalum powder and the second salt in the reaction vessel. The reaction vessel or the lining of the reaction vessel and the stirrer or lining stirrers made of metal material having the same or higher pressure steam,native microstructure. 23 179 N. and Z. p. f-crystals, 11 tab., 15 table.

The invention relates to metals, in particular tantalum, and products made from tantalum, as well as to methods of obtaining and processing of tantalum.

In the industry for a number of reasons always wanted to get the metals of high purity. With respect to the tantalum more pure metals are particularly desirable due to the use of tantalum as a target for sputtering and its use in such electrical devices as capacitors. Therefore, impurities in the metal can have undesirable effect on the properties of products made from tantalum.

To obtain tantalum from its ore grind, and tantalum are extracted from milled ore using dissolution in acid and separating the density gradient of the acid solution containing the tantalum from the acid solution containing niobium and other impurities. Then the acid solution containing the tantalum, crystallized in salt, and then this contains the tantalum salt is introduced into the reaction with pure sodium in the reactor with stirrer, usually made of Nickel alloy, where a part of the Nickel alloy is tungsten or molybdenum. The reactor typically predstavlyayuschaya powder of tantalum. However, in this technology, the tantalum powder is contaminated by contact with different surfaces, for example, containing tungsten and/or molybdenum. Many impurities can escape during subsequent melting, with the exception of soluble refractory metals (e.g., Nb, Mo and W). These impurities usually difficult or impossible to remove, which does not allow to obtain high-purity tantalum product.

Consequently, there is a need to obtain high-purity tantalum products, which contain almost no impurities, obtained by the above described technology. In addition, it is desirable to obtain tantalum product having a higher purity, fine grain size and/or homogeneous texture. Such as a small grain size can be an important property for made of tantalum targets for sputtering because of small grain size can lead to improved uniformity of thickness of the applied spray film. In addition, other products containing tantalum with small grain size, it is possible to obtain improved uniformity of deformation and improved ability to deep drawing and extensibility, which is favorable for the manufacture of condenser tanks, Labasa tantalum products can improve the effectiveness of spraying (for example, higher velocity dispersion) and can increase the normal anisotropy (e.g., increased ability to deep drawing) in manufactured products.

The task of the invention to provide a tantalum product of high purity, having a fine-grained structure and/or homogeneous texture.

In addition, the object of the invention is the obtaining of goods, products and/or components containing high-purity tantalum.

Another objective is to provide a method for producing high-purity tantalum product, as well as products, products and/or components containing high-purity tantalum.

Additional features and advantages of the present invention partially shown in the following description, in part should be clear from the description or can be elucidated from studies of the implementation of the present invention. The objectives and other advantages of the present invention should be realized and attained by means of the elements and combinations specifically listed in the description and the attached claims.

To achieve these and other advantages in accordance with the present invention as it is implemented and described in detail below, this is positive for at least 99,999%. Metal tantalum preferably has a fine-grained structure and/or homogeneous texture.

Further, the invention relates to mixtures or alloys containing tantalum, where present in a mixture or alloy of tantalum has a purity of at least 99,995% and more preferably at least 99.999% availability. Alloy or mixture (e.g., at least present in the alloy or mixture of tantalum) also preferably has a fine-grained structure and/or homogeneous texture.

The invention relates also to a high-purity tantalum, suitable for use as a target for sputtering which has a fully recrystallized grain size with an average grain size of about 150 microns or less and/or having a primary texture type (111) mainly on the thickness of the tantalum and preferably through the entire thickness of the metal tantalum, and/or do not have a strong (100) texture zones in the thickness of the tantalum.

The present invention relates further to the plate or sheet made of the above-mentioned tantalum by free forming tantalum, processing machines in flat blanks for rolling (slabs), annealing slabs, rolling into a plate or sheet, and then annealing the plate or sheet. The final product, so is A.

The present invention relates to a target for sputtering comprising the above-described tantalum and/or alloy. The target for sputtering may also be formed by radial forging and subsequent processing of the circle to obtain blanks or "otter", which are then subjected to the rink to get the disks, which can then be machined and annealed.

The present invention relates further to the resistive films and capacitors comprising the above-described tantalum and/or alloys.

The present invention relates also to the products, components or products, which include at least partially above the tantalum and/or alloys.

In addition, the present invention relates to a method for producing the above-described tantalum, which includes interaction containing tantalum salt, pure sodium or other suitable salt in the reaction vessel or boiler with a stirrer, which are made or have a lining of metal or alloy, with the same or a higher vapor pressure, and tantalum, with a melting point of tantalum.

The present invention relates further to the processing of tantalum powder by melting powder of tantalum in the deep vacuum of 10-2mm RT. Art. Il is giving tantalum powder is carried out by electron beam melting.

The above brief description, and the subsequent more detailed description of the invention are only examples and explanations of the invention presented in the claims.

In Fig. 1(a-b)-11(a-b) presents charts and relevant data pertaining to changes in texture (the increment of thickness against confusion) and the logarithm relationship gradients (111):(100) (increment of thickness versus ln(111/100)) plates made of high-purity tantalum of the present invention.

The invention relates to metallic tantalum, having a purity of at least 99,995%. Preferably the metal tantalum has a purity of at least 99.999% availability and its purity may be in the range of from about 99,995% to about 99.999 percent or more. Other intervals include from about 99,998% to about 99.999 percent and from about 99,999% to about 99,9992%, and from about 99,999% to about 99,9995%. The present invention relates further to a metal alloy that includes high-purity metallic tantalum, such as a base alloy of tantalum or other alloy, which contains high-purity tantalum as one of the components of the alloy.

The impurities that may be present in high-purity tantalum, less than or equal to 0.005%, and they usually include stoimosti in tantalum, such as niobium, molybdenum and tungsten.

Metallic tantalum and its alloys containing the metal tantalum, preferably have a texture conducive to specific end uses such as sputtering. In other words, when the metal tantalum or alloy produce the target for sputtering having a surface, and then hold her sputtering, the metal texture of tantalum of the present invention provides a target for sputtering, which is easily deposited, and very few areas of the surface of the target for sputtering, if there is such resistance to sputtering. In addition, when the metal texture of tantalum of the present invention, the sputtering target for sputtering leads to a very homogeneous erosion of sprayed target, resulting in a deposited film, which is also homogeneous. Preferably, tantalum, with any clarity, but preferably a purity of at least about 99,995%, had a grain size of about 150 microns or less. Preferably, the metal tantalum was at least partially recrystallized, more preferably at least 80% of the metal tantalum was recrystallized, and even more preferably,Metallichesky tantalum was completely recrystallized.

In addition, it is preferable that the metal tantalum had a fine texture. More preferably, the texture is such that the intensity peak of (100) according to any 5% of the increased thickness of the tantalum was less than about 15 random and/or had the natural logarithm (In) of the relationship of the intensities of the Central peaks (111): (100) by the same increment more than about -4,0 (i.e., values -4,0, -3,0, -2,0, -1,5, -1,0, and so on), or had (100) centroid intensity and attitude. The intensity of the Central peak is preferably from about 10 Rand to about 10 Rand, and more preferably from about 0 Rand to about 5 Rand. Other intervals (100) centroid intensity include, but are not limited to, from about 1 Rand to about 10 Rand and from about 1 Rand to about 5 Rand. In addition, the logarithm of the relationship of the intensity of the Central peak (111):(100) has a value from about -4,0 to about 15 and more preferably from about -1,5 of 7.0 to about. Other suitable intervals logarithm relationships include, but are not limited to, from about 1.0 to about 10.0 g, and from about -3,0 to about a 5.0. Most preferably the metal tantalum is required at least acousti (100) and the relationship growing centroid intensities of (111):(100). Method and equipment that can be used to characterize texture, described in the following works: Adams et al., Materials Science Forum, Vol. 157-162 (1994), PP. 31-42; Adams et al., Metallurgic Transactions A, Vol. 24 A, April 1993 No. 4, pp. 819-831; Wright et al., International Academic Publishers, 137 Chaonei Dajie, Beijing, 1996 ("Textures of materials: Proceedings of the Eleventh International Conference on Texture of Materials; Wright, Journal of Computer-Assisted Microscopy, Vol. 5, №3 (1993).

High-purity metallic tantalum according to the invention can be used in a number of areas. For example, high-purity metallic tantalum can be made the target for sputtering or the casing of the warhead ammunition to chemical energy, which include high-purity metal. High-purity metal can also be used for manufacturing a capacitor electrode or resistive film layer. Metal tantalum according to the invention can be used in any products or components that use normal tantalum, and methods of making various products or components containing conventional tantalum, can be equally used with the introduction of products or components of high-purity tantalum. For example, for the fabrication of targets for sputtering can be applied subsequent (additional) processing , the which can be used to obtain high-purity tantalum according to the invention, includes the refining process, the vacuum melting process and thermo-mechanical process. According to this method, or the operational cycle of the refining process includes a step of extracting the metal tantalum is preferably in the form of a powder containing tantalum ore, and preferably selected containing tantalum ore has a low content of impurities, particularly low content of niobium, molybdenum and tungsten. More preferably, the content of niobium, molybdenum and tungsten below about 10 h/m and most preferably less than 8 h/million This choice results in a more pure metallic tantalum. After the refining process used vacuum melting process for the removal of tantalum low-melting impurities, such as Alcide and transition metals, while tantalum is fully consolidated in a tight cast ingot. Then after this process can be used thermomechanical process which includes a combination of cold working and annealing tantalum, which further guarantees the preferred grain size and/or preferred texture, if desired.

with at least one agent (e.g., compound or element) that is able to restore salt to metallic tantalum and additionally may lead to the formation in the reaction vessel of another salt. The reaction vessel may be any vessel used for the reactions of metals, and must withstand the high temperatures of the order of from about 800With up to about 1200C. For the purpose of the present invention, the reaction container or lining of the reaction vessel, which come into contact with the containing tantalum salt and an agent capable of restoring salt to tantalum, made of a material having the same or higher pressure steam as tantalum, with a melting point of tantalum. The stirrer in the reaction vessel can be made of the same material and may be lined. The lining may be available only on those parts of the reaction vessel and the agitator that come in contact with salt and tantalum. Examples of such metal materials that can form the lining in the reaction vessel include, but are not limited to, materials based on metals, made of Nickel, chromium, iron, manganese, titanium, zirconium, Garr is in has the same or higher pressure steam as tantalum with a melting point of tantalum.

Preferably the metal is Nickel or an alloy based on Nickel, chromium or alloys based on chromium, or iron or an alloy based on iron. The lining on the reaction vessel and/or the mixer, if available, usually has a thickness of from about 0.5 cm to about 3 see Used, the thickness may be different. In the framework of the present invention is a multilayer lining is made from the same or different metal materials described above.

Salt containing tantalum, can be any salt containing tantalum, for example potassium tantalum fluoride. As for agent capable of restoring salt to tantalum, and the second salt in the reaction vessel, the agent is able to perform such a recovery is any agent that has the ability to lead to the restoration of containing tantalum salt to the metallic tantalum and other ingredients (such as salt or salts), which can be separated from the metal tantalum, for example, by dissolution of salt water or other water sources. Preferably, this agent is sodium. Other examples include, but are not limited to, lithium, magnesium, calcium, potassium, carbon, carbon monoxide, hydrogen ion is et a sodium fluoride. Details of the recovery process, which can be used in the present invention, in the light of this proposal, presented in Kirk-Othiaer, Encyclopedia of Chemical Technology, 3rdEdition, vol. 22, pp. 541-546, and U.S. patent 2.950.185, 3.829.310, 4.149.876 and 3.767.456. Additional details about the processing of tantalum can be found in U.S. patent 5.234.491, 5.242.481 and 4.684.399.

The above process may be included in a multi-stage method, which may begin with tantalum low purity, such as containing tantalum ore. One of the impurities, which may in substantial quantities to be present in the tantalum is niobium. Other impurities at this stage are tungsten, silicon, calcium, iron, manganese, etc. in More detail tantalum low purity can be cleaned by mixing tantalum low purity, which contains tantalum and impurities from the acid solution. Tantalum low purity, if it is presented in the form of ore must first be milled before being connected with acid solution. The acid solution should be capable of dissolving almost all of tantalum and all impurities, particularly when the mixing is carried out at high temperatures.

When the acid solution had sufficient time for the solution of fluid - solid, which usually must remove any undissolved impurities. Then, the solution clear liquid extraction. For contact with enriched tantalum solution can be used methylisobutylketone (MIBK), and to create a faction of tantalum can be added deionized water. By this time the concentration of niobium present in the containing tantalum fluid, usually below 25 h/million

Next, the liquid containing at least tantalum, provide an opportunity to crystallize in salt when using vats. Usually salt should be potassium tantalum fluoride salt, more preferably the salts is the K2TaF7. Then this salt is introduced into reaction with an agent capable of restoring salt to tantalum and the second salt, as described above. This connection should normally be clean sodium and the reaction should be carried out in the above-described reaction vessel. As mentioned above, by-products of the second salt may be separated from the tantalum by dissolving salt in the water source and the leaching of dissolved salts. At this stage, the purity of the tantalum is usually from up to 99,99 99,50%.

After the tantalum powder extracted from this reaction mixture, any impurities, including any antal may be fused in various ways, such as vacuum arc melting or electron beam melting. Typically, the vacuum in the melting time should be sufficient to remove from the extracted tantalum almost all present impurities so as to obtain a high-purity tantalum. Preferably the pressure above the molten tantalum is lower than the vapor pressure of metallic impurities, so that these impurities, such as Nickel and iron, evaporated. The diameter of the cast ingot has a sufficiently large as possible, preferably more than 24 see the Large diameter provides a large surface of the melt at the interface with the vacuum, which increases the speed of treatment. In addition, a large diameter ingot gives the possibility of increasing cold working, which is subjected to the metal during processing, which improves the properties of the final products. After the mass of molten metal solidifies, the resulting ingot must have the purity of 99,995% or higher and preferably 99,999% or higher. Electron-beam process is preferably carried out at a speed of melting from about 136 to about 363 kg/h, using from 20000 to 28000 In and from 15 to 40 and under vacuum of 110-3to 110-4to 110-6mm RT. Art. with regard to process VAR (vacuum arc remelting), then the rate of melting is preferably from 227 to 907 kg/h when using 25-45 In and from 12000 to 22000 And under vacuum of 210-2to 110-4mm RT. Art., and more preferably from 363 to 544 kg/h when using 30-60 In and from 16000 to 18000 And under vacuum of10-2to 110-4mm RT. Art.

The ingot of high purity tantalum can then be subjected to thermomechanical processing to obtain a product containing high-purity tantalum. Thin and preferably fully recrystallized grain structures and/or homogeneous texture to give the product through a combination of cold and/or hot working and intermediate annealing. The product of high-purity tantalum preferably has a thickness of homogeneous texture of mixed or primary (111) as determined by the orientational optical microscopy (pop), or other appropriate methods. As for thermomechanical treatment, the ingot may be subjected to processing by rolling and/elental has excellent fine grain size and/or uniform distribution. High-purity tantalum preferably has an average size of recrystallized grains is about 150 μm or less, more preferably about 100 μm or less, and more preferably about 50 μm or less. Intervals suitable average grain sizes include ranges from about 25 to about 150 microns, from about 30 to about 125 microns, and from about 30 to about 100 microns.

The obtained high-purity metal according to the present invention preferably contains 10 h/million or less metallic impurities and preferably 50 h/million, or less than About2, 25 h/million or less N2and 25 hours per million or less of carbon. If you want a purity level of about 99,995%, the resulting high-purity metal preferably contains about 50 h/million or less metallic impurities and preferably 50 h/million, or less than About2, 25 h/million or less N2and 25 hours per million or less of carbon.

As for the production of targets for sputtering of such ingot, can be used in the following ways. One variant of implementation, the target for sputtering, made of high-purity metallic tantalum, can be produced by mechanical or chemical cleaning of the surfaces of metal tantalum, which metalliseeritud, described below. Preferably the metal tantalum is a cross-sectional area with a diameter of at least 24,1 cm (9.5 inch) or more. The next stage includes a flat stamping of metallic tantalum in one or more slabs for rolling (slabs). Slab (slabs) is sufficiently deformed (strained) in order to achieve an almost uniform after recrystallization described later stage of annealing. Then the slab (slabs) annealed in vacuum and at a temperature sufficient to achieve at least partial recrystallization of the slab (slabs) for rolling. The preferred temperature and time of annealing are presented below in the examples. Then the slab (slabs) is subjected to cold or hot rolling, or both in perpendicular and parallel direction to the axis of the source metal tantalum (e.g., tantalum ingot) to form at least one plate. Then the plate is subjected to alignment (for example, flat rolling). Then the wafer is annealed for the last time at a temperature and for a period of time sufficient to obtain the average grain size equal to or smaller than about 150 microns, and textures, practically newly cleaned mechanically or chemically and molded in the target for sputtering, having any desired dimensions. Usually free stamping is carried out after the metal tantalum exposed to the air for a period of at least 4 hours at temperatures in the range from ambient temperature to about 370C. furthermore, preferably before cold rolling the workpiece to be rolled annealed at a temperature of, for example, from about 950With up to approximately 1500And over time, for example, from about 0.5 h to about 8 h to achieve at least partial recrystallization of metallic tantalum. Preferably cold rolling is a cross-rolling at ambient temperature, and the hot rolling is carried out at temperatures below about 370C.

As for annealing the tantalum plate, preferably, this annealing is a vacuum annealing at a temperature and for a time sufficient to achieve full recrystallization of metallic tantalum. The examples in this application are further preferred details relating to such processing.

Another method of processing a metallic tantalum target for racial ingot), where metallic tantalum has a sufficient starting cross-sectional area that allows the subsequent processing, as described above. The next stage includes a circular stamping metal tantalum in the at least one rod, where the rod has sufficient deformation in order to achieve an almost uniform recrystallization or after the stage of annealing, which is performed immediately after this stage, or after the stage of annealing before cold rolling. Then tantalum wire rod is cut into billets (in), and the surface mechanically or chemically cleaned. After this can be optional step of annealing to achieve at least partial recrystallization. Then the blanks are punched along the axis in the semis. This may again be an optional stage of annealing to achieve at least partial recrystallization. However, spend at least one of the optional stages of annealing or both stages. Then the semi-finished products are subjected to cold rolling in at least one plate. After that, the surface of the plate (plates) can be optionally cleaned mechanically or chemically. Then spend the final stage autigny zones, if not completely free of (100) textural zones. Usually circular stamping is carried out after the metal tantalum subjected to temperatures of about 370C or lower. Can be used at higher temperatures, which leads to an increase of surface oxidation. Preferably before stamping blanks billet is annealed. Additionally, the semi-finished products can be annealed prior to cold rolling. Usually the temperature of this annealing should be from about 900With up to about 1200C. in Addition, any annealing preferably is a vacuum annealing at a sufficient temperature and for a sufficient time to achieve recrystallization of metallic tantalum.

Preferably the target for sputtering, made of high-purity tantalum, have the following dimensions: thickness from about 0.2 cm to about 3.8 cm and a surface area of from about 45 to 7900 cm2.

High-purity tantalum preferably has a primary or mixed (111) texture and a minimum of (100) texture through the thickness of the target for sputtering and reasonably free from (100) textural zones.

Metal tantalum according izobreteniya. For example, a metal tantalum may be a component or part of components in integrated circuits, such as semiconductors or similar products. Can be used in the devices described in U.S. patent 5987635, 5987560, 5986961, 5986960, 5986940, 5986496, 5986469, 5986410, 5986320, 5986299, 5986294, 5985697 and 5982218, as well as other conventional devices, and each of these patents hereby incorporated in its entirety by reference. Metal tantalum may be present in any device, which typically use the technique of sputtering for the deposition of metal to form a component or sub-component of another device.

The present invention will be further clarified by the following examples which do not limit the invention.

EXAMPLES

Example 1

Numerous podprte recovered sodium powder tantalum technical skills, each weighing about 91-363 kg, were chemically analyzed for suitability for electron beam melting criterion 99,999% of The raw materials. Representative samples of each batch of powder was analyzed by the method of mass spectrometry glow discharge (♦); melting chose podprte powder having a total impurity content of niobium (Nb), molybdenum (Mo) and ve, in order to obtain a homogeneous 1814 kg basic lot powder, which was again analyzed by the method ♦ to confirm purity. Next, the powder was subjected to cold isostatic pressing in an unprocessed workpiece diameter approximately 14-16,8 cm, weighing nominally 136 kg each. Then extruded billet was degirolami by heating at 1450C for 2 hours in vacuum level of about 10-3-10-5mm RT. Art. For the operation of the workpiece covered tantalum sheets to prevent contamination of parts of the furnace.

Then degassed blanks were injected side in 1200 kW ED oven and subjected to drip melting speed 181,4 kg/h 25.4 cm copper crucible, cooled by water, under vacuum below 10-3mm RT. Art. After cooling, the resulting ingot of the first remelting turned, hung in the same furnace and subjected to remelting, using the same parameters melting ED. The second ingot remelting again turned and melted down for the third time, but in 30.5 cm crucible at a speed of melting 363 kg/h

With the side wall of the obtained ingot was sampled for chemical analysis by the method of mass spectrometry glow discharge (♦). The results confirmed that the linoma analysis with spark source K2TaF7contained 5 h/million or less of niobium. Concentrations of Mo and W were also analyzed by spectrographic determination, and these concentrations were below 5 h/million for Mo and below 100 h/million for W. In particular, K2TaF7has a concentration of Nb 2 h/million or below, the concentration of Mo is less than 1 h/million and the concentration of W is less than or equal to 2 h/million In each sample the total measured the content of Nb, Mo and W were below 5 h/million Analyzed four parties on 998 kg each.

One of the parties is transferred into the reactor KDEL, in which the used capacity of pure Nickel and stirrer Hastelloy x Hastelloy Stirrer X contained 9% Mo and 0.6% of W. Then the shaft and the blades of the stirrer were coated with Nickel coating thickness of 15.9 mm, using a welding plating all surfaces that come into contact with the reaction medium.

Used a standardized methodology sodium process except as stated below. The party was subjected to stirring in the presence of pure sodium to obtain a powder of tantalum. Then, the tantalum powder was washed with water and subjected to treatment with acid, then drying with steam and then sifting through 100 mesh.

Then a sample from each load represented by mass-spectral analysis of the glow discharge. In table.1 and 2 show the results of the analysis and the t obtained high-purity tantalum powder, suitable for electron beam melting in the wedge, and the purity order 99,999 can be obtained according to the technology shown in example 1.

Example 3

Used two different methodologies process. First used tantalum ingot 99,998% purity, which was subjected to three electron-beam refining to get the ingot nominal diameter of 30.5 see the Ingot was cleaned on the machine to a diameter of about 29,2 cm and then was heated in air to about 260C for 4-8 hours and Then the ingot was forged, cut and processed on the machines in the slabs (approximately 10.2 cm by 25.4 cm with a length of approximately 71,1 cm to 81,3 cm), and then subjected to acid cleaning solution of HF/HNO3/water. The slabs were annealed at 1050, 1150 and 1300With under vacuum 510-4mm RT. Art. for 2 h, and then subjected to cold rolling in the sheet thickness of 12.7 mm and 6.35 mm Such cold rolling was carried out, choosing a slab thickness of 10.2 cm, a width of 25.4 cm and a length of 76.2 cm and laminating it perpendicular to parallel to the axis of the ingot 5 mm for the passage width up to 78.7 see Then rolled plate parallel to the axis of the ingot 2.5 mm per pass to a thickness of 16.5 mm or 12.7 mm Both rolling issue is at 1.3 mm for the passage and then to 0.6 mm per pass with final finishing to the final mix in the plate 12.7 mm or plate 6.3 mm, using four finishing rolling mill. Then the plate was subjected to final annealing at temperatures 950-1150C.

An alternative method started with The 99.95%, which was subjected to three electron-beam refining in order to produce such an ingot, as described above, before forging. Then, the ingot was subjected to circular stamping using GFM rotary stamp, up to a diameter of 10.2 cm after multiple passes with about a 20% reduction in area per pass. From this intermediate pieces produced on the machine 4 bar (0 to 9.5 cm x length 17.8 cm) and 2 rod (marked a and b) were subjected to annealing at 1050Second, whereas the rods C and D were left neotaggenue. Then the rods were subjected to stamping draught in the semi-height of 6.35 cm, after which the semi-finished products a and C were annealed at 1050C. Then the semi-finished products were subjected to cyclic rolling to a thickness of about 10.2 mm, to obtain a disk with a diameter of approximately 35,6 see It carried out by multiple passes of 5 mm per pass to a thickness of approximately 13,3 mm, Then the disks were subjected to rolling to a thickness of about 12.7 mm multiple passes over the 2.5 mm per pass. Then the disks were subjected to cycle the 0,315 mm per pass, to get the disk thickness of about 10,2 mm and a diameter of about 35,6 see a Quarter of the disk is cut into four wedges and subjected to final annealing at temperatures 950-1100C. This technology are summarized in table.4.

Metallographic and texture analysis was performed on longitudinal sections of the plate material (measuring the bevel parallel to the final rolling direction) and radial sections stamped and laminated discs (measuring the bevel parallel to the radius of the disk).

METALLURGICAL ANALYSIS

The grain size and texture were determined along the longitudinal or radial directions of the samples taken, respectively, of the laminated plates and stamped and laminated disks. The grain size was determined using the method of ASTM E-112. The results of the experiments on annealing for products obtained by flat and circular processing shown respectively in table.3 and 4. Intermediate annealing has no significant influence on the grain size of the final product. In addition, for plates of finite grain size for tantalum with a thickness of 12.7 mm and 6.35 mm was comparable. It was found that the only variable that significantly affects the grain size of a material is the temperature of the load is to be placed according to ASTM gave the grain size of 6.5-7.0-samples taken from the product annealed at 1000 and 950C. However, each of these samples had evidence of the existence of elongated and/or supercriticality areas on the surface or close to it, and the depth of recrystallization was defined as 98-99%. For wafers annealed at 1050, 1100 and 1150With, the grain size according to ASTM was in the range from 5.3 to 3.7, and all samples were recrystallized 100%.

For disks made of circular processing for all the samples was recorded 100% recrystallization except drive annealed at 950With, which was recrystallized 99%. For disc samples annealed at 950, 1000 and 1050With, were identified respectively the grain size according to ASTM 7,1-7,2: 6.1 to 6.8 and 5.9 to 5.9 to. Annealing at 1100With gave the grain size according to ASTM 4.0 to 4.5.

For both processes the obtained results show that the size of the fully recrystallized grain 50 μm or less is achievable when using or rolling plate or stamping process billets at the preferred temperature of the final annealing from about 950 to about 1050C. Supercriticality what abucay on the machine.

Measurement technique textures: a limited number of samples (selected on the basis of metallurgical analysis) was used for texture analysis. Cut and polished samples prepared previously for metallurgical analysis, was used as texture samples after they were subjected to etching in a strong acid prior to determination of texture. As a method of texture analysis method was chosen orientational optical microscopy (pop) due to its unique ability to determine the orientation of individual grains within a polycrystalline sample. Conventional techniques, such as x-ray diffraction or neutron diffraction, may be unable to identify any localized variations of the texture on the thickness of the tantalum materials.

For the analysis of each texture sample is incrementally scanned electron beam (SEM) throughout its thickness; then the graph of the inverse scattering by Kikuchi generated for each of the measuring points, indexed, using the computer to determine the orientation of the crystals. For each sample created the primary data file containing orientation for each point in the matrix grid measurements. Such files from the distribution of orientation (FROH).

As agreed, the orientation of the texture are described with respect to the normal to the sample coordinate system. Otherwise, pole figures "standardized" so that the origin is normal to the plate surface and the reference direction is the direction of rolling (or radial direction; similarly FROH always defined relative to the normal to the sample coordinate system. Terminology such as "(111) texture" means that the (111) atomic plane is predominantly oriented in parallel (and (111) pole is oriented along the normal to the surface of the plate. In the analysis of the orientation of the crystals was determined relative to the longitudinal direction of the sample. It was therefore necessary to transfer the data on the orientation of the longitudinal normal to the sample coordinate system, as part of the texture analysis. These problems were solved with the help of computer algorithms.

Card orientation of grains: according to the principles of representation of texture in the form of an inverse pole figure maps of orientation are the images of the microstructure in the sample, where each individual grain "painted" on its crystallographic orientation relative to the normal direction of the plate is passed along the longitudinal direction of the texture sample by OOM) were rotated 90around the transverse direction so as to align the axis of the crystals with the direction normal to the sample. Card orientation are used to detect the presence of textural relations or gradients across the thickness of the product; for tantalum card orientation showed that large elongated grains detected by optical microscopy, can be formed of several small grains with low-angle grain boundaries.

The results of the analysis texture: scanning the GMD was performed according to the thickness of each of the presented sample; sample plate 12.7 mm were made separate measurements for the upper and lower parts of the plates and their results are shown separately (see tab.5-15).

Map orientation was examined visually for the qualitative characteristics of the homogeneity of the texture on the thickness of the sample. In order to achieve a quantitative description of gradients, textures and textural relationships in the materials of the examples, the measurement data of the detector CRT divided into 20 subgroups, where each represented 5% increment of depth in the thickness of the sample. For each dataset, the first increment was calculated FROH, then determined numerically centroid of the intensity of (100) and (111), using known techniques. Used equipment and met the publication data in their entirety introduced by this reference. Then texture gradients described graphically by plotting a graph of the intensity of the (100) and (111), and the logarithm of the ratio (100):(111) as a function of the depth of the sample. These results are presented on figures from figures 1(a and b) to figure 11 (a and b).

Tantalum plate of great thickness showed a more homogeneous texture in thickness; the only sample that contained the texture area, was the sample obtained after annealing the slab at 1300And the final annealing at 1000C. In addition, the plate materials 12.7 mm also had relatively weak (more chaotic) texture, on the basis of pole figures and analysis FROH. Compared to a thick sheet 6.3 mm sheets had a gradient texture from weak to moderate and some manifestations of texture binding. In addition, the thin plate is shown in FROH more pronounced (111) texture and increased the peak of the (100) texture.

Greatest variability uniformity of texture and binding was detected in stamped and laminated disks. Unlike metallurgical properties on the texture stamped and laminated disks was influenced by the use of intermediate annealing. For drives a, b and C, each of which was manufactured with one or depending on the processing parameters) with weak, if it was binding. However, for a disk D, which is processed from ingot to finished disk without intermediate annealing, the final product contained less desirable strong texture gradients and distinct textural zones. In this way the disc, which was also stamped from notarianni blanks, but then annealed before cold rolling, also had a strong texture gradient and binding in the sample held a final annealing at 950C. To drive the increase in the temperature of the final annealing to 1100With acts downward gradient and destruction binding, but the increased intensity of the (100) texture component. These effects increase the temperature of the final annealing were also visible, although to a lesser extent as the other materials, disks, and plates of the plate.

From microstructural and textural studies can be made the following conclusions regarding the optimal technology of tantalum targets for the deposition of:

for flat processing annealing temperature of the slab is preferably not exceed 1150With (more preferably 1050C), and temperature �/chr/176.gif">C. the Obtained product is characterized by an average size of recrystallized grains is less than 50 μm, the incremental intensity (100) less than 15 Rand and the logarithm of the ratio of (111):(100) below -4,0;

for a circular processing of the workpiece is preferably annealed prior to stamping and rolling in the disk without using an intermediate annealing at the level of semi-finished products. The temperature of the final annealing is preferably equal 950-1100S and more preferably 1050C. the Obtained product is characterized by an average size of recrystallized grains is less than 50 μm, the incremental intensity (100) less than 15 Rand and the logarithm of the ratio of (111):(100) below -4,0.

Other implementation of the present invention should be clear to experts from consideration of the present description and described herein practice of the present invention. Have in mind that the present description and examples should be considered only as examples, and the scope and spirit of the invention presents the following claims.

Claims

1. Metal tantalum, characterized in that it has a purity of at least about 99,995% and the average grain size of about 150 microns or less.

2. Metal tantalum under item 1, characterized in that it is fully recrystallized.

3. Metal tantalum under item 1, characterized in that is at least partially recrystallized.

4. Metal tantalum under item 1, characterized in that it is recrystallized by 98% or more.

5. Metal tantalum under item 1, characterized in that it is recrystallized by 80% or more.

6. Metal tantalum under item 1, characterized in that it has a texture, for which a (100) pole figure is the intensity of the Central peak of less than about 15 random, or b) the logarithm of the relationship of the intensities of the (111):(100) center peak is more about -4,0, or C) both.

7. Metallic tantalum by p. 6, characterized in that the intensity of the Central peak is from about 0 Rand to about 15 random.

8. Metal Tanta is>/p>9. Metallic tantalum by p. 6, characterized in that the logarithm of the specified relation is from about -4,0 to about 15.

10. Metallic tantalum by p. 6, characterized in that the logarithm of the specified relation is from about -1,5 up to about 7.

11. Metallic tantalum by p. 6, characterized in that the intensity of the Central peak is from about 0 Rand to about 15 Rand and the logarithm of the specified relation is from about -4,0 to about 15.

12. Metal tantalum under item 1, characterized in that it has a purity of from 99,995% to about 99.999% availability.

13. Metal tantalum under item 1, characterized in that it is mostly fine and homogeneous microstructure.

14. Metal tantalum under item 1, characterized in that it has an average grain size from about 25 to about 150 microns.

15. Metallic tantalum by p. 14, characterized in that it has an average grain size from about 25 to about 100 microns.

16. Metallic tantalum by p. 15, characterized in that it has an average grain size from about 25 to about 75 microns.

17. Metal tantalum under item 1, characterized in that it has an average grain size of about 50 microns or less.

18. Metal tantalum, characterized in that it has a) the average grain size of about 50 microns or less, or (b) texture, DLI C) texture for which the logarithm of the relationship of the intensities of the (111):(100) center peak is more about -4,0, or combinations of these parameters a), b) and (C).

19. Metal tantalum under item 18, characterized in that it has an average grain size from about 25 to about 50 microns.

20. Metal tantalum under item 18, characterized in that the logarithm of the relationship of the intensities of the (111):(100) center peak is from about -4,0 to about 15.

21. Metallic tantalum by p. 20, characterized in that the logarithm of the specified relation is from about -1,5 up to about 7.

22. Metal tantalum under item 18, characterized in that it has a purity of at least 99,995%.

23. Metal tantalum under item 18, characterized in that it has a purity of at least 99.999% availability.

24. Metal tantalum under item 18, characterized in that it is fully recrystallized.

25. Metallic tantalum by p. 22, characterized in that it is fully recrystallized.

26. Metallic tantalum by p. 23, characterized in that it is fully recrystallized.

27. Metal tantalum under item 18, characterized in that it is recrystallized by 80% or more.

28. Metal tantalum under item 18, characterized in that the intensity of the Central peak FOSS least about 99,995%, the average grain size of about 150 microns or less and a uniform initial texture (111) throughout its thickness.

30. Metallic tantalum by p. 29, characterized in that it is fully recrystallized.

31. Metallic tantalum by p. 29, characterized in that is at least partially recrystallized.

32. Metallic tantalum by p. 29, characterized in that it is recrystallized by 98% or more.

33. Metallic tantalum by p. 29, characterized in that it is recrystallized by 80% or more.

34. Metallic tantalum by p. 29, characterized in that it has a purity of from 99,995% to about 99.999% availability.

35. Metal tantalum, characterized in that it has an average grain size of about 75 microns or less, and contains about 50 hours/million or less metallic impurities.

36. Metallic tantalum by p. 35, characterized in that it also contains 50 PM/m or less O2or 25 hours per million or less of N2or 25 hours per million or less of carbon, or combinations thereof.

37. Metallic tantalum by p. 35, characterized in that it contains 10 ppm or less of metal impurities.

38. Metallic tantalum by p. 37, characterized in that it also contains 50 PM/m or less O2or 25 hours per million or less of N2or redni grain size of about 50 microns or less.

40. Metallic tantalum by p. 35, characterized in that it has an average grain size from about 25 microns to about 75 microns.

41. Metallic tantalum by p. 35, characterized in that it is fully recrystallized.

42. Metallic tantalum by p. 35, characterized in that is at least partially recrystallized.

43. Metallic tantalum by p. 35, characterized in that it is recrystallized by 98% or more.

44. Metallic tantalum by p. 35, characterized in that it is recrystallized by 80% or more.

45. Metallic tantalum by p. 35, characterized in that it has a texture, for which a (100) pole figure is the intensity of the Central peak of less than about 15 random, or b) the logarithm of the relationship of the intensities of the (111):(100) center peak is more about -4,0, or C) both.

46. Metallic tantalum by p. 45, characterized in that the intensity of the Central peak is from about 0 Rand to less than about 15 random.

47. Metallic tantalum by p. 45, characterized in that the intensity of the Central peak is from about 0 Rand to about 10 Rand.

48. Metallic tantalum by p. 45, characterized in that the logarithm of the specified relation is eosine is from about 11.5 to about 7.

50. Metallic tantalum by p. 45, characterized in that the intensity of the Central peak is from about 0 Rand to less than about 15 random and the logarithm of the specified relation is more than about -4,0 to about 15.

51. Metal alloy, characterized in that it contains a metal tantalum according to any one of paragraphs.1, 3 and 6.

52. The target for sputtering, characterized in that it contains a metal tantalum any of paragraphs.1, 3, 6,18, 29 and 35.

53. Capacitor, characterized in that it contains a metal tantalum according to any one of paragraphs.1, 3,6, 18, 29 and 35.

54. A layer of resistive film, characterized in that it contains a metal tantalum according to any one of paragraphs.1, 3, 6, 18, 29 and 35.

55. The product, characterized in that it contains a metal tantalum according to any one of paragraphs.1, 3, 6, 18, 29 and 35.

56. Method of producing metal tantalum, having a purity of at least about 99,995% and the average grain size of about 150 microns or less, which includes interaction containing tantalum salt with at least one agent capable of restoring salt to tantalum and the second salt in the reaction vessel having a stirrer, wherein the reaction receptacle or the lining of the reaction vessel and the stirrer or the lining of the mixer is made of metal, the containing tantalum salt has a total content of Nb, Mo and W of less than about 10 hours/million

57. The method according to p. 56, characterized in that the containing tantalum salt contains calipered tantalum, and the agent contains sodium.

58. The method according to p. 57, wherein the second salt contains sodium fluoride and/or sodium chloride.

59. The method according to p. 56, characterized in that before the reaction, recovery containing tantalum salts spend getting acid solution containing the tantalum and impurities in the Department of density gradient acid solution containing the tantalum from the acid solution containing other impurities and crystallization containing tantalum acid solution for formation containing tantalum salt.

60. The method according to p. 59, characterized in that the tantalum and mixtures are milled ore containing tantalum and impurities.

61. The method according to p. 59, characterized in that the acid solution containing the tantalum and impurities, is formed by mixing the acid solution with crushed ore containing tantalum.

62. The method according to p. 56, wherein the reduction is conducted at temperatures from about 800With up to about 1100With under stirring.

63. The method according to p. 56, characterized in that stogo from the group includes Nickel, chromium, iron, manganese, titanium, zirconium, hafnium, vanadium, technetium, ruthenium, cobalt, rhodium, palladium, platinum, or any combination of them.

64. The method according to p. 63, wherein the metal is Nickel or an alloy based on Nickel.

65. The method according to p. 63, wherein the metal is chromium or an alloy based on chromium.

66. The method according to p. 63, wherein the metal is iron or an alloy based on iron.

67. The method according to p. 56, characterized in that it further comprises removing the tantalum by dissolving the second salt in the aqueous solution.

68. The method according to p. 67, characterized in that it further comprises melting the specified extracted tantalum in sufficient vacuum to remove virtually any present impurities from the extracted tantalum and production of high-purity tantalum.

69. The method according to p. 68, characterized in that the vacuum is 10-4mm RT. Art. or more.

70. The method according to p. 68, characterized in that the pressure above the melt extracted tantalum lower than the vapor pressure of almost all impurities.

71. The method according to p. 68, characterized in that the impurities are removed by evaporation of impurities.

72. The method according to p. 68, characterized in that the melting of the exercise of a put is the first remelting.

74. The method according to p. 68, wherein the high-purity tantalum allow to harden and is subjected to processing by rolling or stamping, or both.

75. A method of manufacturing a target for sputtering of the metal tantalum, having a purity of at least 99,995%, characterized in that it contains the stage at which (a) mechanically or chemically cleaned surface of the metal tantalum, which has a sufficient starting cross-sectional area for the implementation of stages b) to (g); (b) have a flat stamping of metallic tantalum in at least one workpiece to be rolled, with sufficient deformation to achieve an almost uniform recrystallization after annealing at stage d); (c) mechanically or chemically clean the surface of the specified at least one billet for rolling; d) annealed specified at least one billet for rolling at a sufficient temperature and for a sufficient time to achieve at least partial recrystallization of the billet for rolling; (e) carry out a cold or hot rolling to the specified at least one billet for rolling and in the perpendicular and parallel directions to the axis of shadnagar one plate; g) annealed specified at least one plate to obtain the average grain size of equal to or smaller than about 150 microns, and texture, almost free of (100) textural zones.

76. The method according to p. 75, characterized in that the metal tantalum has a purity of at least 99.999% availability.

77. The method according to p. 75, characterized in that the flat stamping is carried out after exposure of the metal tantalum on the air for at least about 4 hours at temperatures in the range from ambient temperature to about 1200C.

78. The method according to p. 75, wherein the cold rolling is a cross-rolling at ambient temperature, and the hot rolling is carried out at temperatures below about 370C.

79. The method according to p. 75, wherein the annealing of the plate is a vacuum annealing at a temperature and for a time sufficient to achieve recrystallization of metallic tantalum.

80. A method of manufacturing a target for sputtering of the metal tantalum, having a purity of at least 99,995%, characterized in that it contains the stage at which (a) mechanically or chemically cleaned surface of the metal tantalum, have ampuku metallic tantalum in the at least one rod, and the specified at least one rod has sufficient deformation to achieve an almost uniform recrystallization after annealing at stage d) or stage (f); (c) cut the rod blanks and carry out mechanical or chemical cleaning of the surfaces of the workpieces; d) if necessary, annealed billet to achieve at least partial recrystallization; (e) stamp of the workpiece along the axis of the semi-finished products; (f) if necessary, annealed semi-finished products to achieve at least partial recrystallization; (g) carry out cold rolling semi-finished products in at least one plate; (h) if necessary, mechanically or chemically clean the surfaces indicated at least one plate; (i) annealed specified at least one plate to obtain the average grain size of equal to or smaller than about 150 microns, and texture, almost free from the (100) textured areas, while the annealing is conducted at least at the stage d) or f), or at both these stages.

81. The method according to p. 80, characterized in that the metal tantalum has a purity of at least 99.999% availability.

82. The method according to p. 80, characterized in that the circular stamping is conducted after metallicheskaya fact, before stamping the workpiece is annealed.

84. The method according to p. 80, characterized in that prior to cold rolling semi-finished annealed.

85. The method according to p. 80, characterized in that the annealing is a semi-vacuum annealing at a sufficient temperature and for a sufficient time to achieve recrystallization.

86. Tantalum component for spraying, characterized in that it has an average grain size of about 150 microns or less and a uniform initial texture (111) through the entire thickness of the component.

87. Tantalum component for spraying on p. 86, characterized in that it is a target for sputtering.

88. Tantalum component for spraying on p. 86, characterized in that it contains 50 PM/m or less metallic impurities.

89. Tantalum component for spraying on p. 86, characterized in that it also contains 50 PM/m or less O2or 25 hours per million or less of N2or 25 hours per million or less of carbon, or combinations thereof.

90. Tantalum component for spraying on p. 86, characterized in that it contains 10 h/m or less metallic impurities.

91. Tantalum component for spraying on p. 90, characterized in that it also contains 50 PM/m or less O2or 25 hours/million or mine, characterized in that it contains tantalum, having a purity of at least 99,50%.

93. Tantalum component for spraying on p. 86, characterized in that it contains tantalum, having a purity of at least 99.99 percent.

94. Tantalum component for spraying on p. 86, characterized in that it contains tantalum, having a purity of at least 99,995%.

95. Tantalum component for spraying on p. 86, characterized in that it contains tantalum, having a purity of at least 99.999% availability.

96. Tantalum component for spraying on p. 86, characterized in that it has a purity of from 99,995% to about 99.999% availability.

97. Tantalum component for spraying on p. 86, characterized in that it is fully recrystallized.

98. Tantalum component for spraying on p. 86, characterized in that is at least partially recrystallized.

99. Tantalum component for spraying on p. 86, characterized in that it is recrystallized by 98% or more.

100. Tantalum component for spraying on p. 86, characterized in that it is recrystallized by 80% or more.

101. Tantalum component for spraying on p. 86, characterized in that it further comprises a support plate.

102. Tantalum component for restylene is the first component to spray on p. 86, characterized in that the average grain size is from about 25 to about 50 microns.

104. Tantalum component for spraying on p. 86, characterized in that the average grain size is about 125 microns or less.

105. Tantalum component for spraying on p. 86, characterized in that the average grain size is about 100 μm or less.

106. Tantalum component for spraying on p. 105, characterized in that it contains tantalum, having a purity of at least 99,50%.

107. Tantalum component for spraying on p. 105, characterized in that it contains tantalum, having a purity of at least 99.99 percent.

108. Tantalum component for spraying on p. 105, characterized in that it contains tantalum, having a purity of at least 99,995%.

109. Tantalum component for spraying on p. 105, characterized in that it contains tantalum, having a purity of at least 99.999% availability.

110. Tantalum component for spraying on p. 105, characterized in that it is fully recrystallized.

111. Tantalum component for spraying on p. 105, characterized in that is at least partially recrystallized.

112. Tantalum component for spraying on p. 105, characterized in that one is m, what is recrystallized by 80% or more.

114. Tantalum component for spraying on p. 105, characterized in that it has a purity of from 99,995% to about 99.999% availability.

115. Tantalum component for spraying on p. 105, characterized in that it further comprises a support plate.

116. Tantalum component for spraying, characterized in that it has a uniform primary texture (111) through the entire thickness of the component.

117. Tantalum component for spraying on p. 116, characterized in that it is a target for sputtering.

118. Tantalum component for spraying on p. 116, characterized in that it contains tantalum, having a purity of at least 99,50%.

119. Tantalum component for spraying on p. 116, characterized in that it contains tantalum, having a purity of at least 99.99 percent.

120. Tantalum component for spraying on p. 116, characterized in that it contains tantalum, having a purity of at least 99,995%.

121. Tantalum component for spraying on p. 11 b, characterized in that it contains tantalum, having a purity of at least 99.999% availability.

122. Tantalum component for spraying on p. 116, characterized in that it is fully recrystallized.

123. Tantalum component for spraying on p. 116, on which audica fact, what is the average grain size of about 75 microns or less and a homogeneous mixed texture (111) throughout its thickness, practically free of (100) textural zones.

125. Tantalum component for spraying on p. 124, characterized in that it is a target for sputtering.

126. Tantalum component for spraying on p. 124, characterized in that it contains tantalum, having a purity of at least 99,50%.

127. Tantalum component for spraying on p. 124, characterized in that it contains tantalum, having a purity of at least 99.99 percent.

128. Tantalum component for spraying on p. 124, characterized in that it contains tantalum, having a purity of at least 99,995%.

129. Tantalum component for spraying on p. 124, characterized in that it contains tantalum, having a purity of at least 99.999% availability.

130. Tantalum component for spraying on p. 124, characterized in that it is fully recrystallized.

131. Tantalum component for spraying on p. 124, characterized in that is at least partially recrystallized.

132. Tantalum component for spraying on p. 124, characterized in that it is recrystallized by 98% or more.

133. Tantalum component for spraying on p. 124, one by p. 124, characterized in that the average grain size is about 50 microns or less.

135. Tantalum component for spraying on p. 124, characterized in that the average grain size is from about 25 to about 50 microns.

136. Tantalum component for spraying on p. 124, characterized in that it further comprises a support plate.

137. Tantalum component for spraying, characterized in that it has a mixed texture (111)-type throughout its thickness, practically free of (100) textural zones.

138. Tantalum component for spraying on p. 137, characterized in that it is a target for sputtering.

139. Tantalum component for spraying on p. 137, characterized in that it has an average grain size of about 150 microns or less.

140. Tantalum component for spraying on p. 137, characterized in that it has an average grain size from about 100 microns or less.

141. Tantalum component for spraying on p. 137, characterized in that it has an average grain size of about 50 microns or less.

142. Tantalum component for spraying on p. 137, characterized in that it contains tantalum, having a purity of at least 99,50%.

143. Tantalum component for spraying on p. 137, wherein stergia fact, that contains tantalum, having a purity of at least 99,995%.

145. Tantalum component for spraying on p. 137, characterized in that it contains tantalum, having a purity of at least 99.999% availability.

146. Tantalum component for spraying on p. 137, characterized in that it is fully recrystallized.

147. Tantalum component for spraying on p. 137, characterized in that is at least partially recrystallized.

148. Tantalum component for spraying on p. 137, wherein is recrystallized 98% or more.

149. Tantalum component for spraying on p. 137, characterized in that it is recrystallized by 80% or more.

150. Tantalum component for spraying on p. 137, characterized in that it further comprises a support plate.

151. Deposited by sputtering a film of tantalum obtained by sputtering tantalum component for dispersion according to any one of paragraphs.86, 116, 124 and 137.

152. A method of manufacturing a tantalum component for spraying of metallic tantalum, characterized in that it contains the stage at which (a) mechanically or chemically cleaned surface of the metal tantalum, which has sufficient initial size of the cross is re one billet for rolling, with sufficient deformation to achieve an almost uniform recrystallization after annealing at stage d); (c) mechanically or chemically clean the surface of the specified at least one billet for rolling; (d) annealed specified at least one billet for rolling at a sufficient temperature and for a sufficient time to achieve at least partial recrystallization of the billet for rolling; (e) carry out a cold or hot rolling to the specified at least one billet for rolling and in the perpendicular and parallel directions to the axis of the source metal tantalum to form at least one plate; (f) align the specified at least one plate; (g) annealed specified at least one plate to obtain the average grain size of equal to or smaller than about 150 microns, and texture, almost free of (100) textural zones.

153. The method according to p. 152, characterized in that the tantalum component for spraying is a target for sputtering.

154. The method according to p. 152, characterized in that the metal tantalum has a purity of at least 99,50%.

155. The method according to p. 152, characterized in that the flat perature in the range from ambient temperature to about 1200C.

156. The method according to p. 152, wherein the cold rolling is a cross-rolling at ambient temperature, and the hot rolling is carried out at temperatures less than about 370C.

157. The method according to p. 152, wherein the annealing of the plate is a vacuum annealing at a temperature and for a time sufficient to achieve recrystallization of metallic tantalum.

158. The method according to p. 152, characterized in that the metal tantalum is in the ingot.

159. The method according to p. 152, characterized in that the metal tantalum is in the strand nominal diameter of 30.5 see

160. A method of manufacturing a component for spraying of metallic tantalum, characterized in that it contains the stage at which (a) mechanically or chemically cleaned surface of the metal tantalum, which has a sufficient starting cross-sectional area for the implementation of stages b) - i); (b) have a circular stamping metal tantalum in the at least one rod, and the specified at least one rod has sufficient deformation to achieve an almost uniform recrystallization after annealing at stage d) or stage, if necessary, annealed billet to achieve at least partial recrystallization; e) stamp of the workpiece along the axis of the semi-finished products; (f) if necessary, annealed semi-finished products to achieve at least partial recrystallization; (g) carry out cold rolling semi-finished products in at least one plate; (h) if necessary, mechanically or chemically clean the surfaces indicated at least one plate; (i) annealed specified at least one plate to obtain the average grain size of equal to or smaller than about 150 microns, and texture, almost free of (100) textural zones, when the annealing is conducted at least at the stage d) or f), or at both these stages.

161. The method according to p. 160, wherein the specified component for spraying is a target for sputtering.

162. The method according to p. 160, characterized in that the metal tantalum has a purity of at least 99,50%.

163. The method according to p. 160, characterized in that the circular stamping is carried out after the metal tantalum subjected to temperatures of about 370Or less.

164. The method according to p. 160, characterized in that prior to stamping the workpiece is annealed.

165. The method according to p. 160, characterized in that prior to cold rolling semi-finished products otsegolation temperature and for a sufficient time to achieve recrystallization.

167. The method according to p. 160, characterized in that the metal tantalum is in the ingot.

168. The method according to p. 160, characterized in that the metal tantalum is in the strand nominal diameter of 30.5 see

169. A method of manufacturing a component for spraying, characterized in that it contains a circular stamping metal tantalum in the at least one rod; annealing at least one rod; punching at least one rod in at least one material; annealing at least one of the material; rolling at least one of the material; subsequent annealing.

170. The method according to p. 169, wherein the specified component for spraying is a target for sputtering.

171. The method according to p. 169, characterized in that the stamping is axial.

172. The method according to p. 169, characterized in that the rolling is a cold-rolling.

173. The method according to p. 169, characterized in that the metal tantalum is in the ingot.

174. The method according to p. 169, characterized in that the metal tantalum is in the strand nominal diameter of 30.5 see

175. A method of manufacturing a component for spraying, characterized in that it contains stamping; rolling the specified metal tantalum; annealing the specified metal tantalum.

176. The method according to p. 175, wherein the specified component for spraying is a target for sputtering.

177. The method according to p. 175, wherein the specified component to spray does not have a (100) texture zones.

178. The method according to p. 175, wherein the specified component for spraying has a homogeneous mixed or homogeneous primary texture (111) throughout its thickness.

179. The method according to p. 175, characterized in that the radial stamping gives a compression deformation of about 88% or the equivalent reduction of the area of about 8.5:1.

180. The method according to p. 175, characterized in that the stamping after radial forging imparts a compression deformation of about 64%.

181. The method according to p. 175, characterized in that the rolling deformation gives a compression of about 84%.

182. The method according to p. 175, characterized in that the annealing after said rolling is carried out at a temperature of 950-1050C.

183. The method according to p. 175, characterized in that the metal tantalum is in the ingot.

184. The method according to p. 175, characterized in that the metal tantalum Narodism, it contains a flat stamping metal tantalum; annealing the specified metal tantalum; rolling the specified metal tantalum to plate or sheet; annealing the specified plate or sheet to obtain a metal tantalum, having (100) textural zones.

186. The method according to p. 185, wherein the specified component for spraying is a target for sputtering.

187. The method according to p. 185, characterized in that it further comprises the alignment of the specified metal tantalum after the last annealing and then another annealing.

188. The method according to p. 185, characterized in that the flat stamping gives a compression deformation of about 62% or an equivalent decrease in the area of approximately 3:1.

189. The method according to p. 185, characterized in that the rolling deformation gives a compression of about 87%.

190. The method according to p. 185, characterized in that the rolling deformation gives a compression of about 94%.

191. The method according to p. 185, wherein the annealing of said plate or sheet is carried out at a temperature of 950-1050°C.

192. The method according to p. 185, characterized in that the metal tantalum is in the ingot.

193. The method according to p. 185, characterized in that the metal is to be placed, characterized in that it contains a combination of cold and/or hot working of metal tantalum and process annealing to obtain a homogeneous mixed or homogeneous primary texture (111) through the entire thickness of the metal tantalum.

195. The method according to p. 194, wherein the specified component for spraying is a target for sputtering.

196. The method according to p. 194, characterized in that the cold and/or hot processing includes processing the specified metal tantalum rolling and/or forging.

197. The method according to p. 194, characterized in that the metal tantalum has a purity of at least 99,50%.

198. The method according to p. 194, characterized in that the metal tantalum has a purity of at least 99.99 percent.

199. The method according to p. 194, characterized in that the metal tantalum has a purity of at least 99,995%.

200. The method according to p. 194, characterized in that the metal tantalum has a purity of at least 99.999% availability.

201. The method according to p. 194, characterized in that the metal tantalum is in the ingot.

202. The method according to p. 194, characterized in that the metal tantalum is in the strand nominal diameter of 30.5 see

 

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