Classifications

• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
  • H01J37/32—Gas-filled discharge tubes
  • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
  • H01J37/3411—Constructional aspects of the reactor
  • H01J37/3414—Targets
  • H01J37/3426—Material
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
  • H01J37/32—Gas-filled discharge tubes
  • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
  • H01J37/3411—Constructional aspects of the reactor
  • H01J37/3414—Targets
  • H01J37/3426—Material
  • H01J37/3429—Plural materials
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
  • C22C27/04—Alloys based on tungsten or molybdenum
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
  • B22F3/12—Both compacting and sintering
  • B22F3/14—Both compacting and sintering simultaneously
  • B22F3/15—Hot isostatic pressing
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
  • B22F3/24—After-treatment of workpieces or articles
• • C—CHEMISTRY; METALLURGY
  • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
  • C22C—ALLOYS
  • C22C1/00—Making non-ferrous alloys
  • C22C1/04—Making non-ferrous alloys by powder metallurgy
  • C22C1/045—Alloys based on refractory metals
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
  • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
  • C23C14/14—Metallic material, boron or silicon
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
  • H01J37/32—Gas-filled discharge tubes
  • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
  • H01J37/3488—Constructional details of particle beam apparatus not otherwise provided for, e.g. arrangement, mounting, housing, environment; special provisions for cleaning or maintenance of the apparatus
  • H01J37/3491—Manufacturing of targets
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
  • B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
  • B22F2003/185—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers by hot rolling, below sintering temperature
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
  • B22F3/24—After-treatment of workpieces or articles
  • B22F2003/248—Thermal after-treatment
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F2201/00—Treatment under specific atmosphere
  • B22F2201/01—Reducing atmosphere
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F2301/00—Metallic composition of the powder or its coating
  • B22F2301/20—Refractory metals
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B22—CASTING; POWDER METALLURGY
  • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
  • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
  • B22F2998/10—Processes characterised by the sequence of their steps
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
  • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
  • C23C14/34—Sputtering
  • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
  • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy

Definitions

• the invention relates to a sputtering target containing molybdenum (Mo) and at least one metal from the group (tantalum, niobium), wherein the average content of the at least one metal from the group (tantalum, niobium) 5 to 15 at% and the Mo Content 2 80 at%, and a method for producing a sputtering target.
• Mo molybdenum
• the average content of the at least one metal from the group (tantalum, niobium) 5 to 15 at% and the Mo Content 2 80 at% and a method for producing a sputtering target.
• Sputtering also called sputtering, is a physical process in which atoms are released from a sputtering target by bombardment with high-energy ions and then transferred to the gas phase.
• Sputtering targets containing the molybdenum and the metals tantalum (Ta) and / or niobium (Nb) are known, for example, from EP0285130A1
• JP2002327264A JP2005307226A or WO2015061816A1.
• Molybdenum-based sputtering targets containing the metals tantalum and / or niobium are used, for example, for the production of electrode layers for thin-film transistors or contact layers for touch panels.
• HIP hot isostatic pressing
• gases such as oxygen contained in the powder mixture can not or only partially escape and it can lead to the formation of undesirable oxides in the structure (the microstructure) of the sputtering target.
• the size of the middle hot isostatic pressing (HfP) manufacturable sputtering targets is limited by the size of the available HIP equipment. This limitation is even more pronounced when HIP is taken directly from the powder mixture, since the volume shrinkage can be about 50 to 70%.
• a production over HIP has further the disadvantage that thereby almost no homogenization of the alloying elements occurs. Also, the diffusion may be hindered by oxides, for example.
• Solid solution hardening is greatly reduced. This, in turn, drastically limits the production of large-format flat targets as well as tubular targets of greater length.
• Tube targets with a greater length but in addition have a fine-grained and homogeneous structure to produce.
• the object of the present invention is therefore to provide a sputtering target which fulfills the requirements described above and / or does not have the deficiencies described above.
• Layer thickness distribution can be produced and that does not tend to local smears by Are processes.
• the sputtering target should have a uniform sputtering behavior. Under even
• Sputtering behavior is understood to mean that the individual grains or the individual regions of the sputtering target can be removed at the same speed, so that during the sputtering process no
• Relief structure arises in the area of the sputtered surface.
• the sputtering target should be as large as possible, that is, it should be possible to provide large areas or long tubes.
• a further object of the present invention is to provide a preparation path which allows the manufacture of a sputtering target having the aforementioned properties in a simple and process-constant as well as cost-effective manner.
• a sputtering target according to the invention contains molybdenum and at least one metal from the group (tantalum, niobium), the average content of the metal from the group (tantalum, niobium) being 5 to 15 at% and the molybdenum content s being 80 at%.
• the sputtering target has at least the following
• An average content of the at least one metal from the group (tantalum, niobium) below 5 at% represents less of a challenge for the microstructure of the target since sputtering targets with such low contents can be more easily homogenized and also easier to transform (lower Solid solution strengthening).
• the corrosion and etching behavior of one of a sputtering target with a tantalum and / or niobium content of less than 5 at% is still not sufficiently favorable.
• a tantalum and / or niobium content of more than 15 at% is not desired since this no longer leads to a further optimization of the corrosion or etching behavior of a layer deposited by a corresponding sputtering target.
• the average content of the metal from the group (tantalum, niobium) of 5 to 15 at% a favorable combination of good corrosion and
• microstructure is to be understood as the microstructure of the sputtering target, which is determined in a simple manner and familiar to a person skilled in the art by means of a metallographic grinding and the
• the matrix denotes a very molybdenum-rich phase in which particles of a tantalum and / or niobium-rich phase are embedded.
• the matrix surrounds these particles and forms one
• the matrix has an average molybdenum content of greater than or equal to 92 at%, which by means of EDX (energy dispersive
• X-ray spectroscopy energy dispersive X-ray spectroscopy
• the molybdenum content is greater than or equal to 95 at%.
• a higher molybdenum content means in most cases also a lower content of tantalum and / or niobium in the matrix, which in turn is accompanied by a lower solid solution hardening and thus better formability. This makes it easier to produce larger-area sputtering targets or tube targets of greater length.
• the embedded particles in the matrix have a mixed crystal composition of at least one metal from the group (tantalum, niobium) and molybdenum, wherein the average molybdenum content is greater than or equal to 15 at%.
• Several crystallographic grains - separated by grain boundaries - can be present in one particle.
• mixed crystal is meant a solid solution of at least two elements which form a common crystal structure.
• the mean molybdenum content of the particles is determined by EDX as the mean of 5 point analyzes. An average molybdenum content of the particles greater than or equal to 15 at% has proven to be particularly positive for the
• the structure of the sputtering target is thus at least two-phase, but it may also contain other additional phases, such as oxides or pores therein. However, the proportion of such further phases should be as low as possible, since these have a negative effect on the
• Sputter in particular its homogeneity, may have.
• oxides may favor the occurrence of localized arcs.
• the average molybdenum content of the particles is preferably greater than or equal to 20 at%, even more preferably greater than or equal to 25 at%, since therewith a further
• the molybdenum content of the particles does not exceed a value of 50 at%. With a molybdenum content of less than or equal to 50 at%, the combination is only minor
• a sputtering target according to the invention more preferably has no or essentially no elemental metal from the group (tantalum, niobium).
• a sputtering target according to the invention preferably has a forming texture.
• a forming texture results from a forming process, such as a rolling, forging or extrusion process.
• a forming process the khstafiographischen grains present in the sputtering target, preferably in the same or similar orientation to
• a forming texture also remains in an annealing treatment after the forming process, for example, a recovery or recrystallization annealing.
• a sputtering target which has a forming texture shows a further improved, more homogeneous sputtering behavior, since the erosion rate of the crystallographic
• Orientation of the individual grains depends. It is particularly advantageous if both the matrix and the particles which are present in a sputtering target according to the invention have the following dominant orientations: a. In forming direction: (110)
• the rolling direction in a rolling process or the direction of the feed in a radial forging process is understood as the "normal direction", ie the direction during a rolling process the surface normal or in a radial forging process, the radial direction.
• the intensity is greater than 1.5 times, preferably 2 times, the background intensity.
• the reshaping texture is determined by SEM (scanning electron microscope) and EBSD (electron backscatter diffraction). The sample is installed at an angle of 70 °. The incident The primary electron beam is inelastically scattered at the atoms of the sample. If some electrons strike grid surfaces in such a way that the
• Kikuchi pattern all angular relationships in the crystal and thus the
• the particles in a sputtering target according to the invention have an average aspect ratio of greater than or equal to 2, even more preferably greater than or equal to 3, very particularly preferably greater than or equal to 5.
• the average aspect ratio can easily at a
• Grain growth of the matrix can be reduced or contained.
• the average distance between the particles perpendicular to the deformation direction is less than or equal to 250 ⁇ m, preferably less than or equal to 150 ⁇ m, more preferably less than or equal to 100 ⁇ m, even more preferably less than or equal to 50 ⁇ m is.
• the mean distance between the particles also correlates essentially with the maximum mean grain size of the matrix.
• the matrix in a sputtering target according to the invention has at least partially a recrystallized structure.
• a recrystallized structure is created by the degradation of lattice defects
• Recrystallization form new grains. At least partially recrystallized may therefore mean that the matrix is partially still in the formed state, partially recovered (rearrangement of lattice defects), partially recrystallized or completely recrystallized. A recrystallized structure still shows the previously introduced forming texture, but has fine
• Advantages of a preferential orientation can be optimally combined with fine, globulitic grains (homogeneous sputtering removal).
• fine, globulitic grains homogeneous sputtering removal.
• sputtering targets according to the invention reduced by sputtering of material, especially in flat targets resulting distortion or even completely avoided. It is believed that such a default by
• a recrystallized structure entails the risk of undesired grain coarsening, which may also be inhomogeneous in a sputtering target according to the invention, in which, in addition to the matrix, mixed-crystal particles having an average molybdenum content of greater than or equal to 15 at% are present , this will
• Grain growth / grain coarsening in a particularly efficient manner.
• an optimized fine-grained structure can be achieved, which leads to a particularly homogeneous sputtering removal.
• the mean grain size of the matrix is less than or equal to 100 ⁇ m, preferably less than or equal to 60 ⁇ m.
• the average grain size can easily be determined by a line-cut method on a light-microscopic photograph of a metallographic
• Magnification image section 040 x 780 pm in each case five lines are placed in the image at equidistant intervals from edge to edge and measured the grain size in both directions (forming and normal direction) and taken the average value.
• the particles at least partially have a recrystallized structure.
• the Umformtextur the particles is also retained, as well as their elongated shape, but the grain structure in the interior of the particles in this case is at least partially fine and globulitic. This can be the
• both the matrix and the particles are at least partially
• a sputtering target according to the invention is preferably the
• Oxygen content 0.5 at% this corresponds to a value of 800 wt ppm. Too high an oxygen content can lead to the formation of unwanted oxides, which in turn can negatively affect the sputtering behavior. For example, oxides can cause the occurrence of local smudges (arcs).
• Sputtering target is kept low and thus a formation of unwanted oxides is largely prevented.
• the oxygen can not be further degraded during consolidation and some oxide is left in the structure of the sputtering target.
• oxides can also weaken the interfaces between the particles present in the microstructure and the matrix and thus reduce the formability, it is also particularly advantageous if these interfaces between matrix and particles are substantially free of oxides. In such a structure, however, oxides may be present in the interior of the particles. Oxides present inside the particles do not lead to a reduction of the formability, so they are no obstacle to the production of large-area targets or long tube targets.
• the relative density of a sputtering target according to the invention is preferably greater than or equal to 98.5% of the theoretical density.
• pores may also be present in the structure of the sputtering target, but the porosity is preferably less than 5%.
• a high relative density combined with a low oxygen content ensures a particularly Are-free sputtering.
• the composition of the sputtering target consists of 5 to 15 at% of at least one metal from the group (tantalum, niobium), moiety Mo and typical impurities. Under typical
• Contaminants are both impurities that are usually already found in the raw materials or are due to the manufacturing process.
• the sputtering target in this case thus consists of a binary alloy Mo-Nb or Mo-Ta. Compared to alloys with additional constituents or elements, such alloys have a cost advantage. Furthermore, the solid solution hardening that occurs is usually lower and thus the formability is better.
• the metal from the group (tantalum, niobium) in a sputtering target according to the invention is niobium.
• Mo-Nb alloys have a particularly favorable corrosion and etching behavior and are also more cost-effective than Mo-Ta alloys.
• a sputtering target according to the invention is designed as a tube target. With a tube target larger surfaces can be coated and the material utilization of the sputtering target in the sputtering process is higher.
• a sputtering target according to the invention can be produced in a particularly simple and process-constant manner if the method comprises the following steps:
• the powder mixture is filled into a jug (typically made of steel) and sealed.
• a jug typically made of steel
• Consolidation via HIP typically occurs at Temperatures of between 1000 and 1600 ° C and pressures of between 80 MPa and 200 MPa.
• the at least one heat treatment step as part of the inventive process is carried out at a suitable combination of pressure and temperature so that the inventive structure is formed, ie at least containing a matrix having an average molybdenum content of greater than or equal 92 at% and particles embedded in the matrix one
• one or more forming steps may additionally be carried out.
• Such a forming step can be performed either between (ii) consolidation and (iii) heat treatment, after (iii) the
• the preferred degree of deformation is 45 to 90%.
• the degree of deformation is defined as follows:
• the forming temperature is preferably at least temporarily 900 ° C to 1500 ° C. Under temporary is understood that, for example, the first forming steps are carried out at this temperature. Thereafter, the forming temperature can also be below 900 ° C. The transformation can be carried out both in one step and in several steps.
• the at least one heat treatment step preferably takes place in one
• the process stability can already be reduced by the very rapid interdiffusion.
• the molybdenum content in the particles can increase too rapidly, and thus to lead to excessive solid solution hardening.
• a temperature range of between 1450 ° C and 1750 ° C in which a particularly high efficiency and particularly advantageous structural formation can be achieved.
• the at least one heat treatment step lasts between 1 and 10 hours. In this time window, a particularly optimal combination of economy and process stability is given.
• the application of said temperature ranges and periods optimally ensures that at least one of the following effects is achieved:
• Niobium and molybdenum, with an average molybdenum content of greater than or equal to 15 at%.
• the at least one heat treatment step takes place in a reducing atmosphere, for example in hydrogen or forming gas.
• a reducing atmosphere for example in hydrogen or forming gas.
• Oxygen levels are further lowered.
• Figure 1 shows an etched (Murakami) longitudinal section of a
• inventive sputtering targets Forming and normal direction span the image plane and are marked with arrows.
• the hipped plates were set at 1250 ° C on a hot rolling stand with a total degree of deformation of 84% to a length of 2.5 m and a width of rolled about 1 m.
• the rolled sheets were then annealed in an oven at 1550 ° C for 3 hours in a hydrogen atmosphere.
• Table 1 shows the mean molybdenum contents of the particles and the matrix (determined as the average of five measurements each).
• the line-cut method with five lines each of 780 pm was used at equidistant intervals in the forming and normal directions.
• the grain size was calculated from the mean of the two directions and from the average of the four images (one per
• Sputtering Target (plate) was 52 pm.
• Particles determined. For this purpose, all particles in the forming direction have an expansion of greater than or equal to 10 pm in forming and Normal direction measured and formed the ratio of the two lengths. The particles were in the middle) in the forming direction 144 pm and in the normal direction 22 pm giving an average aspect ratio of 6.4. The distance between the Nb-rich particles in the normal direction (perpendicular to the forming direction) was also determined by means of line-cut methods. For this purpose, five lines of 780 pm in length were laid over the image at equidistant intervals and the mean distance between the particles (particle edge to particle edge in the normal direction) was determined to be 81 ⁇ m.
• Targets were determined by sputtering experiments at Ar (argon) pressures in the range of 2.5 x 10 3 to 1 x 10 2 mbar and a power of 400 and 800 watts, respectively.
• the substrate material used was soda-lime glass.
• the sputtering targets could be sputtered without the occurrence of are processes.
• Powder mixture was known in tubular steel cans, and
• HIP hot isostatically pressed
• a longitudinal sample (forming direction / direction of advance and normal direction / radial direction clamping the image plane) was removed and ground, polished and etched by means of conventional metallographic methods.
• the sample was measured by means of EDX in the scanning electron microscope.
• Table 2 shows the mean molybdenum contents of the particles and the matrix (determined as the average of five measurements each).
• the grain size of the matrix was determined by line-cutting techniques. In each case five lines of 780pm each were used at equidistant intervals in the forming and normal directions. The grain size was formed from the average of the two directions and the two samples and was 59 pm.
• Normal direction measured and formed the ratio of the two lengths.
• the particles were on average 101 ⁇ in the forming direction and 20 ⁇ in the normal direction giving an average aspect ratio of 5.
• the distance between the Nb-rich particles in the normal direction was also determined by means of line-cut methods. For this purpose, five lines each 780 ⁇ length were placed over the image with equidistant intervals and the average distance between the particles (particle edge to particle edge) determined with 97 ⁇ .

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