Method for obtaining composite target for sputtering from tungsten-titanium-silicon alloy

FIELD: metallurgy.

SUBSTANCE: manufacturing method of composite target for obtaining films by magnetron sputtering and target obtained using the above method is proposed. Method involves manufacture of disc from polycrystalline titanium ingot obtained by multiple vacuum titanium re-melting, drilling of holes in staggered order in sputtered zone of titanium disc along two concentric circles and fixture of cylindrical inserts in them. Cylindrical inserts are made by cutting of ingots of monocrystalline tungsten and monocrystalline silicon, which have been obtained by multiple vacuum remelting of tungsten and silicon. Inserts attachment is performed by press fitting to drilled holes at the ratio of surface areas occupied with tungsten and silicon inserts on surface of target in titanium disc providing the production of films consisting of the following, wt %: silicon 0.1-1.3, titanium 11-33, and tungsten is the rest.

EFFECT: increasing thermal stability of metal coating and reproducibility of its formation process.

2 cl, 1 tbl, 1 ex


The invention relates to the production of atomized metal targets for microelectronics. In the production technology of very large scale integrated circuits (VLSI) silicon thin film of an alloy of tungsten and titanium are used as diffusion barrier layers between the silicon substrate and the metallization of aluminum alloys. Tungsten-titanium thin film barriers are made by spraying a tungsten-titanium target.

The prior art method of manufacturing a tungsten-titanium target for sputtering [RF Patent №2352684, 03.08.07], which includes multiple vacuum remelting of tungsten and titanium with obtaining a polycrystalline ingot of titanium and a single crystal, manufacture of polycrystalline ingot of the titanium disk, in which, in the spray zone, in two concentric circles in a checkerboard pattern drill holes and press fit attached to them cast cylindrical insert from a single crystal, previously subjected to grinding and cutting to length. This method of reception of targets have been severely tested in production and is well proven. However, the use of composite targets double quasiplane helped to identify a number of deficiencies in the tungsten-titanium film, which is directly the consequence of the physical nature of this difficult material - first of all, the relatively high level of mechanical stresses in the films, low resistance metallization and the lack of reproducibility of the technological process of forming metallization.

The objective of the invention is improving the heat resistance of the metallization and the reproducibility of the technological process of its formation.


This is achieved in that in the method of manufacturing a composite target to obtain films by magnetron sputtering, comprising manufacturing a disk from an ingot of polycrystalline titanium, received multiple vacuum remelting of titanium, drilling holes in a checkerboard pattern in the spray zone of the titanium disk in two concentric circles and mount them in a cylindrical inserts, with a sharp tungsten ingots of monocrystalline and multicrystalline and monocrystalline silicon, received multiple vacuum remelting of tungsten and silicon, is made cylindrical insert and mount inserts provide press fit into the holes when the ratio of the areas occupied by the inserts of tungsten and silicon on the surface of the target in the titanium disk, providing films of the composition, wt.%: silicon 0,1-1,3, titanium 11-33, tungsten - rest. A composite target to obtain films magnetron spraying is by getting the specified method.


The method is as follows. Is the vacuum remelting components such as titanium, silicon and tungsten. Titanium melt in electron-beam installation in a horizontal mould with getting a flat polycrystalline ingot in the form of a "pancake", which is subjected to machining to obtain a disk. In the titanium disk drill holes of a certain diameter to accommodate single-crystal inserts of tungsten and silicon. The original tungsten is subjected to electron-beam zone melting with obtaining single crystals of tungsten. Cylindrical rods of silicon and tungsten grinding on gauge length, resulting in a gain of cylindrical inserts that are pressed into holes in the titanium disk. Inserts of tungsten and silicon in the titanium disk is placed uniformly over the area of the spray. The ratio between the number of single-crystal inserts of tungsten and silicon drive titanium depends on the given contents of titanium, tungsten and silicon in the sputtered film. In exceptional cases, to maintain specified ratios in the sprayed film in the holes pressed inserts made of polycrystalline titanium, which allows to compensate for the lack of content in the film.

Films with silicon content less than 0.1 m is S.% though have satisfactory electrical performance, however, are characterized by relatively high levels of mechanical stress and a low resistance metallization. The silicon content higher than 1.3 wt.% leads to increased resistivity of the films.

An EXAMPLE of carrying out the INVENTION

A method of obtaining a composite of the target was carried out when applying the tungsten-silicon-titanium films with a given ratio of components. Thus the main task was to establish the optimal modes of atomization and the ratio of the elements in the diffusion contact barrier layers, which are characterized by the lowest mutual solubility on the border with aluminum metallization, high temperature resistance layer in combination with a low specific resistivity, good adhesion and optimum mechanical properties of the barrier layer. The basis of the target, which is a flat disc with a diameter of 190 mm, made of flat polycrystalline ingot of high purity titanium melted under vacuum in glucomannan water-cooled copper mold in electron-beam installation with an axial electron gun. The single crystals of tungsten with a diameter of 11.5 mm arbitrary crystallographic orientation were grown in vacuum apparatus for electron-beam zone melting with special annular electron gun with samisen the m ring cathode. Crystals of high-purity silicon received induction method with pulling from the melt. Before spark cutting single crystals of tungsten and silicon at length obtaining inserts have them grinding to a diameter of 11 mm, the Obtained insertion of single crystals of tungsten and silicon were pressed into holes in the titanium disk, and the number of inserts were selected according to a given ratio of the three components in the finish of the film. The deposition of the films was carried out on the installation magnetron sputtering with a magnetron source with a water-cooled electromagnet and a composite target with a diameter of 190 mm, the Tests were carried out on the alloys of titanium-tungsten and with varying silicon content, depending on the specified content of the three components in the film. Spraying conducted in argon under the following conditions: working pressure argon 5*10-1PA, the discharge current from 1.5 to 2.0 a, the voltage at the anode from 390 to 410, the current of the electromagnet 260 And magnetic induction 0,12 T.

Figure conductive elements of the alloy film on a silicon substrate with an oxidized surface, and the contact Windows were obtained when applying the film through precision free the mask of the molybdenum foil having a thickness of 50 μm, the obtained double-sided etching through the combined figure photoresistive film. Used the same standard photolithography process. For the first method of forming a pattern of the silicon wafer was heated in the process of applying the film to 140±10°C, and the second to 220-250°C. the Control of the elemental composition of the films was carried out on the electron microprobe analyzer, equipped with x-ray console. The thickness of the alloy films at the level of 0.15 μm was provided by analysis of the composition with an accuracy of ±1.5 percent.

Test samples with the contact barrier layers of the developed alloy was annealed in argon at a temperature of 550-575°C for 45 minutes Repeated cycles of annealing was performed on the pilot plant pulsed lamp annealing at the temperature limit of 600°C in argon. Analysis of samples from the results of repeated multiple annealing and source (after isothermal annealing of the samples was conducted in an optical microscope, and the condition of the contact layer after removing the metal film by etching. Similar conditions were made and tested samples with the contact-barrier layer of a binary alloy of titanium-tungsten. On the number of test samples had a p-n junction located at a depth of 0.35 μm, the reverse current IRwhich indirectly allows to judge about the safety barrier properties of the analyzed layer. Several test structures were performed prior to application of the platinum layer with a thickness of 0.1 μm and a subsequent heat treatment p and 400°C for 10 min in argon for forming studied under the contact-barrier layer a layer of platinum silicide. The results are shown in Table 1.

Table 1,
The test results of alloy silicon-titanium-tungsten.
№ p/pThe composition of the alloy, wt.%The number of cycles, it can withstand without changing more than 10%Changing the p-n junction, %
Contact to n-SiContact to the p-Si
1Silicon 0.1; titanium 11; tungsten 88,990-110>100<10
2Silicon 0,4; titanium 27; tungsten 72,690-110>100<10
3*Silicon 1,0; titanium 30; tungsten 69,0>120>120<10
4*Silicon 1,3; titanium 33; tungsten 65,7>120>1205Silicon 0,07; titanium 17; tungsten 82,9330-4040-5040-45
6Silicon 1,4; titanium 30; tungsten 68,640-5050-5535-40
7Titanium 11; tungsten 8930-4035-4595
8Titan 30; tungsten 7025-3530-40>100
*structures with silicide sublayer of silicon with a thickness of 0.1 μm

From Table 1 it is evident that the best results were obtained for the ternary alloy of the proposed structure. High thermal stability characterized by a contact barrier layers with a sub-layer of platinum silicide. Thin films of ternary alloy of the optimal composition located on the p-n regions of silicon test structures have a significantly higher thermal stability and less impact on the p-n junction located under the contact window, than any of the binary alloys on the basis of the system is neither titanium-tungsten. Reproducibility process of forming a contact barrier layers was estimated by the change in the reverse current of the p-n junction. The reproducibility of the results for ternary alloys was the best.

Thus, a composite target and method of reception ensure the application of the contact barrier metallization layer of silicon integrated circuits, characterized by high thermal stability and a unique technological reproducibility of the process of its formation, which generally contributes to improving the quality of integrated circuits.

1. Method of manufacturing a composite target to obtain films by magnetron sputtering, comprising manufacturing a disk from an ingot of polycrystalline titanium, received multiple vacuum remelting of titanium, drilling holes in a checkerboard pattern in the spray zone of the titanium disk in two concentric circles and mount them in a cylindrical inserts, characterized in that the cutting of ingots of monocrystalline tungsten and monocrystalline silicon, received multiple vacuum remelting of tungsten and silicon, is made cylindrical insert and mount inserts provide press fit into the holes when the ratio of the areas occupied by the inserts of tungsten and silicon on the surface m is Sheni in the titanium disk, providing film composition, wt.%: silicon 0,1-1,3, titanium 11-33, tungsten - rest.

2. A composite target to obtain films by magnetron sputtering, characterized in that it is obtained by the method according to claim 1.


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