High-purity sputtering molybdenum target and method of its production

FIELD: metallurgy.

SUBSTANCE: invention relates to non-ferrous metallurgy, namely to production of sputtering molybdenum targets and can be used in microelectronics to apply coatings by thin-film metallisation. The method involves a consistent deep vacuum refining by electron-beam remelting of a high-purity metal-ceramic bar obtaining monocrystalline or polycrystalline molybdenum. Whereupon a semi-finished target shaped as a monocrystalline or polycrystalline ingot is formed from the obtained product using electron-beam remelting in the horizontal or vertical mold. The ingot produced is then machined.

EFFECT: improved quality and reliability of the barrier and conducting films when sputtering cast high-purity molybdenum targets.

3 cl, 1 dwg, 1 ex

 

The invention relates to the production of atomized metal targets for microelectronics. Molybdenum is of considerable interest due to its unique capabilities as a material of the low resistance contact with silicon (10-5-10-4Ohmcm) and conductive systems. Molybdenum has a relatively low electrical resistance and is closest to the silicon the value of the coefficient of thermal expansion. However, the use of molybdenum is complicated by the difficulties of obtaining films with the physical properties of bulk samples. Currently, the main industrial technology for deposition of thin films in the industry is magnetron sputtering targets. For the manufacture of targets using the methods of powder metallurgy.

Closest to the claimed object is U.S. patent No. 20060042728 from 02.03.2006, in which the method for obtaining sputtering targets made of molybdenum, which consists in using the methods of powder metallurgy: pressing and sintering powder of high purity molybdenum at a temperature, pressure and time sufficient to form a target with a fine-grained microstructure. When implementing this method arise principal obstacles that make it difficult to obtain quality targets.

Even when using the vacuum process is in and high temperatures cannot remove a thin impurity shell, which covered each Poroshenko molybdenum high purity. Subsequently, these impurities are redistributed between the borders and the volume of the grains in the sintered target. Magnetron sputtering of such targets is accompanied by significant structural and chemical heterogeneity of thin films.

- Receiving material with high density, close to theoretical density, even at the extreme values of all process parameters of the methods of powder metallurgy is unreal. Due to the high content of gaseous impurities in grain boundaries and microdefects heating of the sintered target of 250-300C. during the spraying process is accompanied by excessive discharge gas, a violation of the geometry of the target and the instability of the electrical properties of evaporated thin films.

When the sputtering of metal targets plasma stream fine ionized particles is accompanied by a large flow of neutral particles of the applied substances deposited on the surface of the sprayed film and dramatically reduce the quality of the films due to the formation "of pinholes and other defects.

- Synthesis of metal targets using powder technology under extreme pressure, vacuum and aging is characterized by significant hardware and technological SL is gnosti in the manufacturing process targets and so far only implemented in Japan.

Technical problem - improving the quality sputtering targets of Mo.

This is achieved by the production method applied to the sputtered target of high purity includes deep vacuum refining electron-beam zone melting the sintered billet of high purity with obtaining monocrystalline molybdenum, to form the electron-beam remelting in a horizontal mould procurement target in the form of a polycrystalline ingot and mechanical processing of the workpiece. This is achieved by the production method applied to the sputtered target of high purity includes serial deep vacuum refining electron beam drip melting the sintered billet of high purity with obtaining polycrystalline molybdenum, to form the electron-beam remelting in a vertical mould procurement target in the form of a polycrystalline ingot and mechanical processing of the workpiece. This is achieved by a sputtered target of molybdenum high purity obtained by the method according to claim 1 or 2.

The proposed method of obtaining cast molybdenum targets of high purity allows you to get massive alloy target having a much higher purity and density compared with metal-ceramic or latimeriidae. The formation of polycrystalline ingots of various shapes (round, rectangular) produced by electron-beam melting of high-purity single-crystal molybdenum, obtained by electron-beam zone melting of metal workpieces. Polycrystalline ingots for billets targets smelted in a horizontal mold (round, rectangular) geometry corresponding to the geometry of the finished target and allowing for minimal finish machining to obtain the target with the specified dimensions (see drawing).

An example implementation of the method.

The implementation of the method implemented in the manufacture of cast targets of polycrystalline ingots of high purity molybdenum. As the source material for the production of ingots of molybdenum used sintered billet of high purity. Refining produced by electron-beam zone melting in a high vacuum on the installation-701. Then, the produced electron-beam remelting monocrystalline molybdenum on the installation EMO-250 horizontal crystallizers different geometry for polycrystalline ingots having a geometry similar to the geometry of the finished target. Mechanical handling and waste during finishing of workpieces sputtering targets were minimum is passed. Physico-chemical and metallographic analysis of molybdenum ingots were performed on samples cut from each ingot in transverse and longitudinal sections. The carbon content in the samples was determined by coulometric method, oxygen - neutron activation method, a metal impurity - mass spectrometry. Bullion molybdenum contains: carbon 110-4%, sodium 510-3%of potassium 510-3%tungsten 110-2%, other impurities - <110-4%. In the macrostructure of the ingots cast molybdenum mainly present grain length 40-60 mm and an average diameter of 0.2 to 3.0 mm Made 6 sputtering targets of molybdenum are two types of round and rectangular (oval). Conducted a detailed study of processes of magnetron sputtering targets made of molybdenum, and thin films and devices obtained by the sputtering targets of high-purity molybdenum. In the sputtering targets formed the zone of erosion (sputtering), the dimensions of which exceed the scope of the deposition in the magnetron unit, which ensured the reproducibility of the thickness of the applied layer on the substrate with an accuracy of 2%. The use of targets of either type were stopped after reaching a certain depth (~10 mm) throughout the area of erosion. It is established that the yield targets of the proposed method is 100%and the replacement of the project on thin films of molybdenum were minimal and were not associated with quality sputtering targets.

So, getting cast sputtering targets of high purity molybdenum massive sizes showed them a significant advantage in obtaining integrated circuits compared to the preparation of thin films by magnetron sputtering target of sintered molybdenum.

1. Method for the production of sputtered target of molybdenum high purity, comprising the sequential deep vacuum refining electron-beam zone melting the sintered billet of high purity with obtaining monocrystalline molybdenum, to form the electron-beam remelting in a horizontal mould procurement target in the form of a polycrystalline ingot and mechanical processing of the workpiece.

2. Method for the production of sputtered target of molybdenum high purity, comprising the sequential deep vacuum refining electron beam drip melting the sintered billet of high purity with obtaining polycrystalline molybdenum, to form the electron-beam remelting in a vertical mould procurement target in the form of a polycrystalline ingot and mechanical processing of the workpiece.

3. A sputtered target of molybdenum high purity obtained by the method according to claim 1 or 2.



 

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5 cl, 4 dwg, 3 tbl

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