Single-crystal – oriented-crystal – and epitaxy growth processes; – Processes of growth from liquid or supercritical state – Having moving solid-liquid-solid region
Reexamination Certificate
2002-02-20
2003-12-16
Hiteshew, Felisa (Department: 1765)
Single-crystal, oriented-crystal, and epitaxy growth processes;
Processes of growth from liquid or supercritical state
Having moving solid-liquid-solid region
C117S040000, C117S049000, C117S051000
Reexamination Certificate
active
06663711
ABSTRACT:
This application is a national phase of PCT/FR00/02667 which was filed on Sep. 27, 2000, and was not published in English.
1. Technical Field
The present invention concerns the growth., in solution in a floating zone, of crystals of a compound or alloy. It concerns in particular the growth of crystals of silicon carbide.
2. State of the Prior Art
Silicon carbide is a material that is being used more and more in the semiconductors field. It can be produced in the form of layers or in a bulk by growth in the vapour phase according to what is termed the Lely method. This method produces good quality crystals but has the disadvantage of, using very high temperatures (greater than 2000° C.).
Another process has been proposed that allows lower temperatures to be used. This process is described in the article “Growth of Silicon Carbide from Liquid Silicon by a Travelling Heater Method” by K. GILLESSEN and W. von MUNCH, which was published in the Journal of Crystal Growth, 19 (1973), pages 263-268. The authors propose creating, via induction heating, a liquid solvent zone, as it happens silicon, between two bars of polycrystalline silicon carbide placed in a vertical alignment. The production of a floating zone of silicon by induction is a technique fully mastered by those skilled in the art. The growth conditions are such that the process is used in a sealed quartz ampoule. In fact, a temperature of 1800° C. is necessary at the top of the liquid zone and iodine is added to offset the consequent significant evaporation of silicon. The transfer reaction that takes place between the iodine and the silicon in the gas phase means that a sealed system must be used.
A slow upwards movement of the ampoule causes an asymmetric distribution in the temperature within the liquid zone, which sets off the transfer of silicon carbide from the lower bar towards the upper bar where a solid crystal is obtained.
This process has a certain number of disadvantages, which can be summarised as follows: the constraints linked to the growth in an ampoule, the problems caused by the addition of iodine and those due to the relatively high temperature.
The ampoule has to be prepared beforehand. All of the components have to be integrated into the ampoule, with the difficulty of correctly aligning the two bars, and achieving the de-gassing and the sealing. The size of the ampoule has to be taken into account: for a given diameter of induction coil, the dimension of the crystals that are obtained is inevitably smaller than the dimensions one would expect without an ampoule. Moreover, an optimal charge—wall distance for the ampoule must be found and maintained. It is also necessary to work with very pure components in order to avoid impurities being deposited on the walls of the ampoule. The presence of an ampoule implies more complicated thermal phenomena and therefore more difficult temperature control.
The addition of iodine also causes problems. In order to avoid condensation of the iodine on the walls of the ampoule, it must be maintained at sufficiently high temperature (temperature at the coldest point: 700° C.). The use of second heating system, in addition to the induction coil, therefore makes the assembly more complex. In addition, the possible insertion of iodine into the crystals obtained may have a harmful effect in subsequent applications of the crystals.
Furthermore, 3C polytype SiC crystals are more easily obtained at lower temperatures because they are more stable. This is an important limitation in the process.
DESCRIPTION OF THE INVENTION
According to the present invention, it is proposed to achieve the growth of the material that one wants to obtain at a sufficiently low temperature so that the phenomenon of evaporation becomes negligible. In the case where silicon carbide crystals are produced, adding iodine and using an ampoule become unnecessary.
The object of the invention is therefore a process for the production of a crystal of a material with non-congruent melting and which is made from at least one first element and a second element, with the process comprising the following stages:
Placing, in a vertical alignment, and maintaining under a neutral atmosphere :or under vacuum, a bar of the first element gripped between a lower bar and an upper bar made out of said material.
Transforming the bar of the first element into a floating zone by heating to a temperature that avoids the evaporation of the first element, the heating being obtained by heating means that provides a temperature gradient in the floating zone so that one of the faces of either the lower or upper bars that are in contact with the bar of the first element appears as a cold face.
Contra-rotating the; lower and upper bars around the alignment axis and moving the whole bar assembly along the alignment axis in relation to the heating means in order to move the cold face further away and thus produce said crystal on the cold face by growth in solution.
The bars that are put in place may be maintained under an argon blanket.
The heating may be obtained via induction produced, for example, by a flat coil that encircles the bar of the first element. It may also be obtained by means of a mirror oven.
The growth of said crystal may be achieved from a seed deposited on the lower face of the upper bar or on the upper face of the lower bar.
The process may be advantageously used to obtain a crystal of silicon carbide, the bar of the first element being silicon, with the upper and lower bars being made out of polycrystalline silicon carbide obtained, for example, by powder sintering or by sublimation. In particular, it allows crystals of 3C polytype silicon carbide to be obtained. It may also be used for obtaining silicon nitride or a Si—Ge alloy.
The invention also concerns a device for the production of crystals of: a material with non-congruent melting and made from at least one first element and a second element, with the device comprising:
an enclosure that can be put under vacuum or under a neutral blanket.
means for maintaining, in the enclosure and in a vertical alignment, an assembly comprising a bar of the first element gripped between a lower bar and an upper bar made out of said material, with said means also allowing the lower and upper bars to be contra-rotated around the alignment axis.
heating means that makes it possible to transform the bar of the first element into a floating zone by heating while providing a temperature gradient in the floating zone so that one of the faces of either the upper or lower bars that is in contact with the bar of the first element appears as a cold face.
means for achieving a relative displacement, along the alignment axis, of the bar assembly in relation to the heating means, in order to move the cold face away.
The neutral atmosphere in the enclosure may be obtained via an argon blanket.
The heating means may be induction heating means. They may, for example, comprise a flat coil encircling said bar of the first element. They may also comprise a mirror oven.
REFERENCES:
patent: 1196625 (1965-07-01), None
patent: 58060699 (1983-04-01), None
Gillesen, et al., “Growth of Silicon Carbide from Liquid Silicon by a Travelling Heater Method”, vol 19, 1973, 6 pages.
Norlund, et al., “Crystal Growth of Incongruently Melting Compounds”, vol. 62, No. 2, 1983, 9 pages.
Wollweber, et al., “SixGe1-xsingle crystals grown by the RF-heated float zone technique”, vol. 163, No. 3, 6 pages.
Honda, et al., “Growth and Characterization of Bulk Si-Ge Single Crystals”, vol. 35, No. 12A, 6 pages.
Barz, et al., “Germanium-rich SiGe bulk single crystals grown by the vertical Bridgman method and by zone melting”, vol. 16, No. 5, 4 pages.
Chevrier Véronique
Duffar Thierry
Santailler Jean-Louis
Wollweber Jürgen
Commissarat a l′Energie Atomique
Hiteshew Felisa
Krebs Robert E.
Thelen Reid & Priest LLP
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