Technique of furnace feed additional charging during process of silicon single crystal growing by czochralski method

FIELD: metallurgy.

SUBSTANCE: invention concerns technique of receiving single crystal field by means of method of growth from melt. Method of furnace feed additional charging at growing of silicon single crystals by means of Czochralski method includes charge feeding on the melt surface in capsule from container with charged furnace feeding, where it is provided ability of charge feeding dose on the melt surface through the bottom end, dumping of container till the melt surface in capsule, melt temperature pulldown till formation on the surface of viscous layer of melt, interfere with feeding of unfused charge into melt volume, after what container is opened and charge portion is poured onto viscous layer surface. Then melt temperature is gradually applied till total melting of charged furnace feed, after what empty (or partially discharged) container is taken out from the growth region, to its place it is dropped rod with seed single crystal, it is implemented ingot dummy bar and implemented another silicon single crystals growth process.

EFFECT: higher parameters repeatability of grown ingots, and also reducing of growing of single crystals production cycle duration and energy saving at the expense of technological cycle optimisation.

1 ex

 

The method relates to the field of microelectronics, and more particularly to technology for the production of single-crystal silicon by growing from the melt.

A large part of the monocrystalline silicon used in the manufacture of semiconductor devices and circuits, produced by Czochralski method.

The method consists in the following: the initial charge (polycrystalline silicon and / or crushed pieces of monocrystalline silicon is loaded into the crucible installation of growing single crystals, melt the mixture, put on the melt surface single-crystal seed, a thin oriented bar monocrystalline silicon, and according to the established schedule in an inert environment (the rotation of the seed with a simultaneous rise in zone temperature of crystallization) receive the ingot (the single crystal silicon has a cylindrical shape and a given length) [1]. The volume of the resulting ingot is limited to the amount loaded in the crucible charge. After separation of the grown ingot from the surface of the molten mixture, the ingot is removed from the zone of growth (usually by lifting the top part of the installation), cooled it and unloaded from the installation, and the crucible is also cooled. To ensure that the next cycle of growing a single crystal in a crucible load the next portion of the charge, and the process of cultivation on Traut. The duration of the technological cycle of cultivation (from the boot of the charge in the crucible to cool down the crucible) is approximately 12-16 hours and depends primarily on the quantity of the charge.

As the classic process of growing silicon single crystals by Choralschola does not provide for uploading of charge in the growing process, its shortcomings are obvious:

- low productivity of the process, due to the discrete regulation of growth (cool down of the crucible, the uploading of the charge and the subsequent melting of the charge take at least 4 hours)

poor reproducibility of electrophysical parameters of the ingot due to changes in the parameters of the melt and growing conditions after loading a new portion of the charge.

There is a method of loading the charge, namely, that fine mixture of open container placed on the outside of the crucible, through a special vacuumized dispenser is on the surface of the melt continuously in descending order of the volume of the melt during crystallization of the molten mixture in the seed [2].

The disadvantages of this method include the following:

- places of receipt of the charge from the dispenser decreases the surface temperature of the melt, which leads to inhomogeneity of the temperature field of the surface of the melt and, consequently, requires significant is the amount of time for recovery mode stationarity of the growth process, due to the need to adjust the heating temperature of the crucible and adjust the parameters of the extrusion ingot (speed and lifting speed);

- if you implement this method so that the necessary Gating vacuumized chamber, which increases the installation and complicates the regulation of the cultivation process.

These shortcomings deprived of the way so that the charge, in which the container with the charge made in the form of pre-vacuumized chamber located outside the unit above the crucible, and the filing of a charge on the surface of the melt is carried out by means of electromagnetic dosing [3].

The disadvantages of this method are as follows:

since the container with the mixture and heating units installation vacuumized separately, when the flow of charge through the dispenser required process pressure equalization between the container with the mixture and heat node setup, which reduces the performance of the growth process.

The closest in technical essence and the achieved result is a way so that the burden on the patent [4].

In a specified way so that the mixture is used a cylindrical container filled with the mixture in the form of fractions of a given size, the specified container (after lifting the grown ingot in the area of the extraction of the installation) is dipped into the crucible to contact the lower torus is as filled with the mixture of the container with the surface of the melt. As melting of the charge in the lower part of the container due to the pressure of the mass of unmelted batch in the container is provided by the displacement of the molten part of the charge and admission to the melting zone of a new portion of the charge until the complete emptying of the container.

The disadvantages of this method are as follows:

the method requires the use of a mixture of a certain faction, which leads to additional time and financial costs of redistribution preparation charge, and the performance of the process;

the method does not provide the uniformity of penetration of the charge in the container, which can lead to uneven income of unmelted portions of the mixture in the melt, and this in turn can lead to splashing of the melt or to the disappearance of individual unmelted pieces of the mixture into the bottom of the crucible, which can lead to damage and / or destruction of the crucible, which reduces the reproducibility of the process.

The objective of the invention is to improve the performance and reproducibility of the process of growing silicon single crystals.

This is due to the fact that in the method of loading the charge, including the filing of a charge on the surface of the melt in the crucible from the container loaded with the charge, which provides the opportunity for dosed supply of the charge on the surface of the melt through the bottom of the t is reetz, the container is lowered to the surface of the melt in the crucible, then the temperature of the melt is reduced to the formation on the surface of the melt viscous layer, preventing from entering unmelted charge in the volume of the melt, after which the container is open and pour out a portion of the charge on the surface of the viscous layer. The melt temperature is then gradually increased until complete melting of charge, then an empty (or partially emptied containers are removed from the growth zone, in its place put the stem by the seed single crystal, carry out a seed crystal ingot and the regular process of growing the silicon single crystal.

In known science and technology solutions to similar problems not detected the use of the formation of a viscous layer that holds the loaded charge on the surface of the melt to its penetration and prevents the ingress of particles of unmelted charge on the bottom of the crucible, so all of the claimed differences of the present invention meet the criterion of "Inventive step".

Specific example

Source sorted the charge (polycrystalline silicon and the crushed pieces monocrystalline silicon of arbitrary size with a resistivity of 10÷15 Ohm·cm) in an amount of 35-45 kg load through the open door in the air lock chamber in a quartz crucible, the location is contained within the graphite heater of thermal unit of the growing crystals. The prepared seed representing oriented in a predetermined crystallographic plane of the bar monocrystalline silicon layer from one end (in our example, the crystallographic orientation of the seed - [100]) is secured on the attachment point on the lower end of the steel cable, the upper end of which is secured to the winch drum of the upper rod installation, close the door airlock, then install vacuum to a pressure of <5·10-2ATM. When the preset pressure in thermal unit serves ultrapure argon, and reduce the pressure in thermal node to a value of ˜10-2ATM, on schedule serves on the graphite heater DC voltage, bringing the temperature of the charge in the crucible to T≥1420°and melt the charge.

After melting of the charge include the rotation of the quartz crucible and the horizontal rotation of the winch, a seed crystal using the winch lowered into the crucible until it touches the thinned end of the seed crystal with the melt surface and by an insignificant decrease in the surface temperature of the melt to provide the beginning of the process of solidification of the melt on a seed. Further, according to the established schedule (rotation of the seed with a simultaneous rise in zone temperature of crystallization) first form "vechny taper of the wedge (i.e. gradually increasing di is m kristallisoituu on the seed mass of the melt prior to the specified diameter (150 mm ± 0.5 mm) as-grown ingot), then the process continue growing at a stable process parameters up until the crucible begins to decrease the surface area of the melt (i.e. until the remainder of the melt in the crucible begins to concentrate within the spherical bottom of the crucible), and then start to build a "reverse taper of the wedge (i.e. gradually reduce the diameter of the zone of crystallization by increasing the speed of the hoist rope until complete separation of the ingot from the melt surface).

The result is a first ingot of monocrystalline silicon cylindrical shape of a given diameter (150 mm ± 5 mm) resistivity 10 Ohm·see (with the variation of resistivity along the length of the ingot is not more than 15% and the variation of the resistivity along the radius of the ingot is not more than 5%) with a cone-shaped upper and lower parts. The weight of the obtained ingot is ˜27 kg Duration of the technological cycle of growing the first ingot was ˜7 hours.

After separation of the grown ingot from the surface of the molten mixture, the ingot is removed from the zone of growth by raising into the lock chamber, overlapping the gate valve separating thermal unit from the airlock, open the door airlock, cooled ingot and upon reaching the temperature of the ingot - 40-50°To unload it in the installation (removed from the cable together with the seed through the door in the air lock chamber. At the end of the rope is fixed to the container loaded (25-35 kg) mixture, introducing the container is loaded into the lock chamber, the lock chamber is closed and vacuum up to a pressure of <5·10-2bar.

Upon reaching a specified pressure in the lock chamber serves ultrapure argon, bring the pressure in the airlock to the value of ˜10-2ATM and open the gate valve separating the lock chamber from the heat of the node.

The rotation of the crucible is stopped, the temperature of the surface of the melt in the crucible is reduced to the formation of a viscous surface "crust" (shall be checked visually through the viewing window in the upper part of thermal unit), the container with the mixture is lowered to contact the side surface of the container with the tabs on the ring quartz nozzle located on the top side of thermal unit, and the latch hinged to the bottom of the container is unlocked and when further lowering the container into the crucible, the bottom of the container is disclosed, and the mixture is poured on a viscous melt surface in the crucible.

After the complete liberation of the container the latter is displayed in the lock chamber, the gate valve is closed and begin a gradual ascent temperature of the melt in the crucible to a full penetration weld is loaded on its sticky surface charge.

After complete melting of the charge include the rotation of the crucible, disassemble the container t is osika, fixed on the rope seed and the process of growing ingot I repeat, resulting in a gain of the second ingot with the same settings as the first ingot. After unloading the second ingot installation completely cooled, remove the quartz crucible with crucible residue (˜10-15 kg), extract crucible residue, which after cleaning, etching and grinding are used as charge material for the next process.

The duration of the technological cycle of growing the second ingot was ˜6 hours.

Thus, in the cultivation with the uploading of charge for one full growing cycle (from the initial load of the charge in the crucible removal of the crucible from the installation) received two ingot of silicon, while the number of consumables used in the process was the same as in the standard process of growing a single ingot, and the power consumption was less than 30% by eliminating the need for melting a full download of the charge in the crucible during the second growth process.

This method is compared with the prototype provides a higher reproducibility of the parameters of the grown ingots, as well as a reduction in the duration of the production cycle single crystal growth and power savings due to optimization of the technological cycle.

And the sources of information

1. Atari. Basics of VLSI technology". - Publishing house "Radio I Svyaz', Moscow, 1985, str-213.

2. U.S. patent No. 5876496, IPC: SW 15/02, March 02, 1999

3. U.S. patent No. 6896732, IPC: SW 15/02, dated may 24, 2005

4. U.S. patent No. 6805746, IPC: SW 15/02, on October 19, 2004 - the prototype.

The method of loading mixture for growing silicon single crystals by the Czochralski method, comprising the additional feed mixture from the container into the crucible during the melting of the charge in the crucible, and the container with the charge is placed above the charge initially loaded into the crucible, characterized in that the mixture from the container serves on the surface of the melt mixture in the crucible was cooled to education viscous surface layer, preventing the flow of charged metal in the volume of the melt, after which the temperature of the crucible was raised to full melting of charge.



 

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EFFECT: the invention ensures growing of polycrystallic layers from a melt of silicon.

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