Tungsten-titanic target formagnetron sputtering and method of its receiving

FIELD: metallurgy.

SUBSTANCE: it is implemented deep vacuum refinement by multiple remelting of tungsten and titanium with receiving of polycrystalline ingots of titanium and tungsten monocrystal. Then from the polycrystalline ingot of titanium it is manufactured disk, in which in diffusing area per two concentric circles alternate there are bored holes and by press fit there are fixed in it cast cylindrical inserts from tungsten monocrystal, preliminarily subject to grinding and cutting per exact lengths. Target, recived by mentioned method, consists of cast disk made of high-clean titanium and cast cylindrical inserts made of high-clean monocrystalline tungsten, located in diffusing area of disk by two concentric circles alternate. Additionally area ratio on surface of target, taken up by tungsten and titanium, provides receiving of films at magnetron sputtering composition 35-40 wt % of titanium, tungsten is the rest.

EFFECT: improving and reliability growth of applied films of barrier plate tungsten - titanic alloy.

3 cl, 4 dwg, 1 ex

 

The invention relates to the production of atomized metal targets for microelectronics. In the production technology of silicon very large scale integrated circuits (VLSI), alloys 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. Such targets are produced by mixing the original powders of tungsten and titanium, followed by heating and pressing.

Closest to the claimed object is U.S. patent No. 5896553 from 20.04.1999 (prototype), which describes a single-phase tungsten-titanium sputtered target and method of manufacture, which consists in mixing powders of tungsten and titanium and pressing at a temperature, pressure and time sufficient to achieve a mutual solid solution of tungsten and titanium with the formation of the beta phase. The disadvantages of the prototype include the following:

- The product obtained from the complex operations including extrusion and annealing the mixture of powder materials, which may result in saving or making uncontrolled impurities, including carbon, oxygen and nitrogen, i.e. the impurity composition of the target defined by the manufacturing method.

- Don is but the achievement of the minimum porosity of the target material. Produced according to the description of the target has a specific density, comprising 90-95% of theoretical, as a result, when the operation is observed instability of the dispersion, swelling of the target due to outgassing from the volume and the formation of columnar microstructure in sputtered tungsten-titanium films.

- Getting-phase targets the beta-phase is difficult to achieve. In the manufacture of sprayed tungsten-titanium target, due to the passing of mutual diffusion processes, the balance in real time not is never, therefore, tungsten and titanium are unevenly spaced, the microstructure of multiphase and it has a negative impact on the quality of the deposited barrier layers.

- The use of high pressure (up to 40 kpsi) in combination with high temperatures (up to 1650°C) in inert gas or vacuum within 3-6 hours leads to extraordinary hardware and process more complicated and expensive the whole process of production targets.

Technical problem - improving the quality and reliability of barrier layers of a tungsten-titanium alloy through the use of targets for magnetron sputtering, obtained by vacuum metallurgy. In this case, the dispersion is subjected alloy target with a specific density of 100%, do not have the disadvantages of metal-ceramic Mish is yum. Process variants can be the use of a target made of cast blocks of high-purity tungsten and titanium, or simultaneous sputtering (co-sputtering) two cast targets of tungsten and titanium of high purity. The latter case is the interesting possibility of obtaining a tungsten-titanium films of any composition by choosing the rate and deposition time for each metal. This method used by the authors for testing regimes for the films with optimal electrophysical parameters. The desire to maximize the purity of the starting materials of the targets has led to the design of a composite target. Used the results obtained by the authors in a co-sputtering two cast targets. Composite tungsten-titanium target is a flat base made of high-purity titanium with cylindrical inserts of single-crystal tungsten of high purity. For the manufacture of titanium ingots used dual electron-beam remelting in a high vacuum, the single crystals of tungsten were obtained by electron-beam zone melting in a high vacuum refining for several liquid passes molten zone. On the titanium disc made of polycrystalline ingot, in the spray zone (zone erosion) in two concentric okrujno the holes in staggered drilled holes, which zapressovyvat tungsten cylindrical insert brushed in diameter and cut to length in the sheet.

Figure 1 presents a General view of a composite target for implementing the inventive method: 1 - titanium disk, 2 - insertion of a single crystal in the amount of 56 pieces. Tungsten inserts the specified diameter and number were placed so that the sprayed surface of the target in the area of the erosion area ratio plots of tungsten and titanium corresponded to the desired value in the tungsten-titanium films.

An EXAMPLE IMPLEMENTATION of the METHOD

Implementation options for a tungsten-titanium films with a given ratio of components co-sputtering two targets was performed to determine the optimal modes of atomization and the optimum ratio of the elements in the diffusion barrier layer, when there is the least mutual solubility on the border with aluminum metallization, is a high resistance layer in combination with a low specific resistivity, good adhesion and optimum mechanical properties of the barrier layer. Target, which is a flat disk with a diameter of 78 mm, made of polycrystalline ingots of high-purity titanium and tungsten. The deposition of the films was carried out on the installation magnetron raspy is possible with separate magnetrons. The experiments showed that the rate of deposition of both metals to be linearly dependent on the discharge power. In experiments determined the capacity of spraying each of the two targets required to obtain a tungsten-titanium film with a specified ratio of tungsten/titanium. To assess the quality of deposited films on the value of the surface resistance and the thickness of the films measured resistivity. Figure 2 presents the dependence of the electrical resistivity of the films on the ratio of titanium and tungsten (figure 2, point a, 1, 2, 3, 4, 5, 6, In). When applied to the same or similar conditions, the tungsten-titanium layer by sputtering metal-ceramic target, obtained by powder metallurgy using a high-purity source powders and with the exception of depositing contaminants on the stages of manufacture of the target, the specific resistivity was 130 µohm. cm (figure 2, point C). In films of the same composition produced by co-sputtering two cast targets of high-purity tungsten and titanium, the specific resistivity was 62 µohm. cm (figure 2, point (E), i.e. two times lower.

It should be noted structural features of the films obtained by spray powder and cast targets. Powder targets can be sprayed only at a low power (<1 kW) following the journey of the gas release and swelling in the warm-up target up to 300°C. in the sputtering process. Figure 3 presents a schematic cross-section system with barrier tungsten-titanium layer. At low speeds there is formed a columnar structure. Pores decorate the borders of the columns (crystallites), consisting of a dense core (matrix W(110) with micro inclusions of titanium), surrounded by a less dense, porous material. This structure dramatically reduces the barrier properties of the film after annealing the tungsten diffuses into the aluminum with the formation of WAl12and aluminum - tungsten-titanium film with the formation of TiAl3. The cast of the target was sprayed at high speeds (power >3 kW), while the gas release and swelling does not occur, and the microstructure of the films is characterized by a high dispersion with a grain size of 10-20 nm.

Based on the results obtained by co-sputtering two targets, proposed a composite target (figure 4), subjected to the tests to study the reproducibility of the composition and properties of tungsten-titanium films. 4 shows a composite target and new target b target produced by 20%. The sputtering was performed in an industrial setting "Oratorio-5" in argon. The rate of deposition of films of 1.8±0.1 nm. with-1. Film besieged on a silicon wafer, pre-heated to 250°C. the film Thickness of 0.18±0.02 mm, the specific resistivity is less than 5 Ω/□. Controlled composition, the article is alternia features, the reproducibility of the depth of the layer, electrophysical parameters. Spectral analysis showed that the composition of the films done by sputtering a composite target at various stages of its operation (in particular, in the initial period and after 145 cycles spraying when there is erosion of the spray zone) corresponds to a content of titanium 35 to 40 at.%, the rest of the tungsten. Deviation from this ratio during the operation of the target does not exceed 2-3%. The specific resistivity of the films was at 60-70 µohm. cm (figure 2, point E). So, the proposed target is designed so that it sprayed surface has a ratio of areas occupied by titanium and tungsten, providing a tungsten-titanium films of the desired ratio, namely 35 to 40 at.% titanium, the remainder tungsten.

1. Method for the production of tungsten-titanium target for sputtering, comprising deep vacuum refining multiple remelting of tungsten and titanium with obtaining polycrystalline titanium ingot of single crystal tungsten, production of polycrystalline ingot of the titanium disk, in which the sprayed area on two concentric circles in a checkerboard pattern drill holes and press fit attached to them cast cylindrical insertion of single crystals in which iframe, pre subjected to grinding and cutting to length.

2. Tungsten-titanium target for sputtering, characterized in that it is obtained by the method according to claim 1 and consists of a molded disc of high-purity titanium and cast cylindrical inserts of high-purity single-crystal tungsten, located in the spray zone of the disk by two concentric circles in a checkerboard pattern.

3. The target according to claim 2, characterized in that the ratio of the areas on the target surface occupied by tungsten and titanium, provides the film with magnetron sputtering composition of 35 to 40 at.% titanium, the remainder tungsten.



 

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