Manufacturing method of cast target from tantalum-based alloy for magnetron sputtering

FIELD: metallurgy.

SUBSTANCE: manufacturing method of cast target for magnetron sputtering from tantalum-based alloy and target obtained using the above method is proposed. Method involves obtaining of an ingot of alloy on the basis of tantalum. First, tantalum ingot of high purity degree is obtained by means of deep vacuum refining by electron-beam drip re-melting of a workpiece made by pressing of high-purity tantalum powders; besides, ingots of intermetallic compounds TaFe2 and YFe3 are obtained by melting of tantalum with iron and yttrium with iron; after that, arc vacuum remelting of high-purity tantalum ingot with ingots of intermetallic compounds TaFe2 and YFe3 is performed at their ratio, wt %: TaFe2 3.0-10.0, YFe3 0.3-3.0, Ta - the rest; ingot of tantalum-based alloy with composition of Ta + 1 wt % Fe + 0.1 wt % Y is obtained and subject to machining.

EFFECT: improving the quality of sputtered targets in order to increase the yield ratio of thin-film capacitors.

2 cl, 1 tbl, 1 ex

 

The invention relates to the field of metallurgical production of sprayed metal targets for microelectronics, and materials science, the development and manufacture of integrated circuits and thin-film capacitors on the basis of tantalum and its alloys. Currently, the main industrial technology for deposition of thin-film capacitors and many elements of the integrated circuits is magnetron sputtering targets.

The choice of tantalum as the source material is largely due to the fact that depending on the conditions obtaining tantalum films they may have a different structure and, accordingly, it becomes possible in a wide range to modify the resistivity of the film, and its temperature coefficient. In the crystal structure and electrophysical properties to massive sample closest film of tantalum with volume-centered cubic lattice having a crystalline structure and a relatively low resistivity (20-40 µohm·cm). Another modification of tantalum has a tetragonal crystalline structure and resistivity 160-200 µohm·cm and in massive samples does not occur. This metastable modification of tantalum characteristic only for thin films.

In the prior art it is known that on the basis of tantalum is possible to provide a bulk manufacturer of passive elements (resistors, capacitors, connecting wires and pads) as with lumped and distributed parameters, which in their complexity are not inferior elements made from other materials, but in fact have a much greater precision, stability and reliability. The versatility of tantalum and no need to use other materials suggests that on the basis of "tantalum technology" can be produced the vast majority of passive elements integrated circuits [S. Seki et al. "Formation of high-quality, magnetron-sputtered TA2O5films by controlling the transition region at the TA2O5/Si Interface", J. Vac. Sci. Technol., 1987, v.5(4), pp.1771-1774]. One of the major drawbacks of thin films of pure tantalum is unpredictable adhesion to various materials and poor structure of the films that have forced researchers to look for tantalum alloys with other chemical elements, such as aluminum or chromium, improve the structural and adhesive properties of tantalum while maintaining its other benefits.

An object of the invention is to increase the structural and chemical quality sputtering targets to increase the yield of thin-film capacitors by improving the reproducibility of the elemental composition of the material and reduce the possible losses, associated with evaporation of yttrium and iron in their introduction to tantalum.

DISCLOSURE of INVENTIONS

This problem is solved due to the fact that the used method for the production of molded targets for magnetron sputtering from an alloy based on tantalum, including the production of an ingot of the alloy on the basis of tantalum. In this advance will receive a tantalum ingot of high purity by deep vacuum refining electron beam drip melting of the workpiece, is made by pressing powders of high purity tantalum also receive ingots intermetallics TaFe2and YFe3by alloying tungsten with iron and yttrium iron, then carry out the vacuum arc remelting ingot of high purity tantalum with ingots of intermetallics TaFe2and YFe3when their ratio, wt.%: TaFe23,0-10,0, YFe3of 0.3 to 3.0, The rest with obtaining an ingot of the alloy on the basis of tantalum composition TA+1 wt.% Fe+0.1 wt.% Y, which is subjected to mechanical processing.

Cast target for magnetron sputtering from an alloy on the basis of tantalum, however, she received the claimed method.

The lower limit of the selected ratio is limited to low adhesion of the proposed alloy, when the content of TaFe2and YF3when alloying with high-purity tantalum was found to be less than 3.0 wt.% and 0.3 wt.%, respectively. Top predestine these compounds when alloying with tantalum constrained by the need to have a low specific resistivity of the material, as well as the inability to obtain reproducible thin-film elements.

The IMPLEMENTATION of the INVENTION

The method is as follows. The original billet, made by pressing powders of high purity tantalum, placed in the melting chamber of the electron beam furnace, producing the pumping chamber to create a vacuum and then gradually melt the workpiece, bringing under electron beam generated axial gun. The rate of electron-beam melting is 0.5-0.6 kg/min Then along the obtained ingot of high purity tantalum every 100 mm using a thin tantalum wire attach a thin bars intermetallics F2and YFe3and it is produced in electric arc remelting installation with intense electromagnetic stirring of the melt. The rotation of the melt contributes to the averaging of the chemical composition of iron and yttrium, eliminating temperature gradients and obtaining fine-grained cast structure due to the destruction of the crystallites.

An example implementation of the method.

The implementation of the method implemented in the manufacture of cast targets based alloy of tantalum. As the source material for the production of ingots of high purity tantalum used billet, produced by compacting and sintering powders of high purity tantalum. Vacuum the shop were performed on electron-beam installation in vertical crystallizers, resulting received polycrystalline ingots of high purity tantalum. Intermetallic compounds TaFe2and YFe3designed for doped tantalum high purity iron and yttrium, was obtained by means of high-frequency levitation in an atmosphere of pure helium. The obtained ingots complex intermetallic (F2+YF3) fastened tantalum wire of 2 mm diameter consumable ingot electrode of tantalum high purity with a diameter of 80 mm, Melting in an electric arc furnace were carried out in a helium atmosphere using electromagnetic stirring of the melt for averaging of the chemical composition. As a result, after removal of the seed and its parts received ingots with a diameter of 200 mm and a height of 140-200 mm From ingots produced magnetron target diameter 187 mm and a thickness of 3 mm, which was sprayed by magnetron sputtering to obtain a thin-film capacitors.

Comparative results on the reproducibility of the elemental composition of the alloys of tantalum with additions of iron and yttrium are shown in Table 1. You can see that this method allows to obtain a material with more reproducible elemental composition than by the traditional method, consisting in the direct fusion of all three components.

Table 1.
Comparative results on the reproducibility of the elemental composition of the alloys of tantalum with additions of iron and yttrium
The composition of the charge*The composition of the alloy** (wt. %)Frenzy, %
ExpectedReceived
The traditional wayThe proposed methodThe traditional wayThe proposed method
245 g YFe3
4240 g TaFe2
The rest of The
Ta+0,01%Y+
+1%Fe
Ta+0,03%Y+
+0,75%Fe
Ta+0,01%Y+
+1%Fe
Fe - 2,86
Y - 33,3
Fe - 2,0
Y - 9,1
2450 g YFe3
2800 g of TaFe2
The rest of The
Ta+0,1%Y+
+1%Fe
Ta+0,45%Y+
+0,6%Fe
Ta+0,105%Y+
+1%Fe
Fe - 3,33
Y - 2,22
Fe - 2,0
Y - 9,52
2450 g YFe3 Ta+0,01%Y+Ta+0,027%Y+Ta+0,105%Y+Fe - 3,12Fe - 2
6800 g TaFe2+2%Fe+1,28%Fe+2%FeY - 37,04Y - 9,52
The rest of The
245 g YFe3Ta+0,01%Y+Ta+0,0035%Y+Ta+0,01%Y+Fe - 2,58Fe - 1,95
8640 g TaFe2+2%Fe+1,55%Fe+2,5%FeY - to 28.57Y - 10
The rest of The
*Charge calculated on the weight of the ingot 83400, the Adjustment of the content That was conducted by varying the length of consumable parts electrode.
**According to the results of neutron activation analysis, the average of the three heats.

Thus, the use of the proposed method of producing sputtering targets of high-purity tantalum doped with iron and yttrium, can significantly improve the quality of sputtered thin films. The use of alloy Ta+1%Fe+0,1%Y (wt.%), obtained in this method, lets you increase the percentage of output capacitors by 10%.

1. Method of manufacturing molded targets for magnetron sputtering from an alloy based on tantalum, including the production of an ingot of the alloy on the basis of tantalum, wherein the pre-receive an ingot of high purity tantalum by deep vacuum refining drip electron beam remelting billet, made by pressing powders of high purity tantalum also receive ingots intermetallics TaFe2and YF3by alloying tungsten with iron and yttrium iron, then carry out the vacuum arc remelting ingot of high purity tantalum with ingots of intermetallics F2and YF3when their ratio, wt.%: F23,0-10,0, YFe3of 0.3 to 3.0, The rest with obtaining an ingot of the alloy on the basis of tantalum composition TA+1 wt.% Fe+0.1 wt.% Y, which is subjected to mechanical processing.

2. Cast target communicated to the throne sputtering from an alloy based on tantalum, characterized in that it is obtained by the method according to claim 1.



 

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