The method of obtaining crystalline hollow products and device for its implementation


C30B21 - Unidirectional solidification of eutectic materials

 

(57) Abstract:

The invention relates to a method of obtaining from a melt of crystalline bodies with precisely defined dimensions of the channel and can be used in various fields pretsizionnoi equipment, in particular for the manufacture of monocrystalline capillaries and waveguides. The purpose of the invention is a material savings and increased productivity. To achieve this goal by obtaining products with precisely defined dimensions directly from the melt using a molding device ensures a snug fit of the post melt for forming the rod, by creating additional pressure of the melt and the growing crystal is conducted at a temperature horizontal surface of the shaper, not lower, and the upper end is exposed above her stud is not higher than the crystallization temperature of the melt at the location of the solidification front in height between the horizontal surface of the shaper and the upper end exposed above her core. The device for implementing this method, comprising a container for the melt, a movable rod with structuralism and not wetted by the melt forvarras the Oh predetermined cross-sectional shape protrudes above the upper horizontal surface 1 4 mm, and the piston on the rod, raising the melt to create additional pressure. 2 N. p. F.-ly, 3 ill.

The invention relates to a process for the production of melt hollow shaped crystalline bodies with precisely defined dimensions of the channel and can be used in various fields of precision engineering, in particular for the manufacture of monocrystalline capillaries and waveguides.

There is a method of growing crystalline bodies from a cross-section of a given shape (including tubes), in which the crystalline body is pulled from the film of the melt located on a horizontal surface that defines the shape of the cross section of the grown crystal (I). This method has the following disadvantages. One of the conditions of cultivation is to maintain such conditions of temperature and speed of extrusion film to melt covers the entire surface and its thickness did not exceed 0.25 mm otherwise crystalline body does not repeat forms a horizontal surface on which the film of the melt. The exact observance of constant cross-sectional sizes kristallicheskogo body requires solidification front at constant height for wroclawia there are accidental changes of thermal conditions, caused by the characteristics of the temperature controllers (constant temperature is not supported at the front of crystallization in the melt, and in some parts of technological equipment, which summed up thermocouple) and controls the rate of withdrawal, changes in the voltage supply of the heaters and temperature changes and the flow speed of the coolant crystallization plants, as well as convection in the melt, leading to fluctuations in the position of the solidification front in height. In addition, crystallization of materials with impurities (e.g. metal alloys) observed periodic oscillations of the crystallization front, caused by the redistribution of impurities between the liquid and solid phases. All this leads to a varying cross-sectional sizes kristallicheskogo body in the process of growing, and sometimes, when the solidification front rises so high that the surface tension of the melt reduces the surface area - to the disruption of the cross-sectional shape (for example, there is a rounding of sharp edges when growing tubes with rectangular cross section) or to complete the swimming channel. Thus to obtain hollow bodies with tacinskaja processing. Subsequent processing, especially mechanical, cause undesirable changes in the material properties, and in some cases it is impossible, if the dimensions of the channel are small. Additionally, when processing a large amount of crystalline material goes to waste.

A device for implementing the method (I) contains the crucible with the melt and the shaper of the wetted by the molten material with an upper horizontal surface above the level of the melt in the crucible, the edges which define the size and shape of the grown crystal. The upper horizontal surface of the shaper are connected by capillaries with the melt in the crucible in which the melt is applied to it due to the surface tension forces for the formation of a film of the melt. When the crystal is grown from a film of melt formed on the upper horizontal surface of the shaper, its transverse dimensions vary due to changes in thermal conditions, since the solidification of the melt is higher than the former, and the transverse dimensions of the film of the melt in this case are determined by the balance of surface tension forces and depend on the position of the solidification front This leads to the fact that to get the crystal is trojstvo, the size of the cross-section of a film or melt would not depend on the position of the solidification front at least to some extent.

A method of obtaining hollow crystalline bodies with a cross-section of a given shape, in which the crystalline body is grown from a film of the melt located on a horizontal surface with the configuration of the outer edges that define the external shape and size of the crystal, and the non-wetted area of the melt is exposed above the horizontal surface of the material that defines the shape and dimensions of the channel (2). The plot is not wetted by the molten material prevents the swimming channel at small sizes. Otherwise, this method has the same drawbacks as described above, i.e. due to changes in thermal conditions in the process of growing the resulting crystalline body is characterized by the deviation of the sizes of the channel from the horizontal plane with simultaneous rotation of the crop body or crucible to provide thermal symmetry. The position of the solidification front may vary from the surface of the melt in the crucible to a top position, when there is separation of the melt from the grown crystal, as is camping in height. This leads to the fact that due to changes in thermal conditions varies the position of the solidification front height and the grown crystal is characterized by the deviation of cross-sectional sizes from the set. Thus obtained crystal needs further processing. These drawbacks could be eliminated, if the melt is pushed to the non-wetted stem at some length, then changing the position of the solidification front would not violate the dimensions of the channel and would allow us to obtain crystals with a high purity surface inside the channel.

It is known (device) 3 for the implementation of the proposed method with a container for the melt and the shaper in the form located in the center of the rod, is not wetted by the melt, the movable rod with structuralism for crystal pulling. This device is developed for the formation of a melt column due to surface tension forces and thus does not provide the continuity of the transverse dimensions by changing the position of the solidification front height violation thermal conditions, and obtain crystalline products with precisely defined dimensions of the channel and high quality on top of the W pressure in the melt at the crystallization front for a snug fit to melt resistant Central core. In this case, the cross-sectional sizes of the obtained crystal would not depend on the position of the solidification front within certain limits.

Thus, the technical shortcomings of these methods and devices lead to the need for further processing of the grown crystalline products with the aim of bringing them up to exactly defined sizes and specific surface, i.e. to the material losses and additional costs of time and money, reduces productivity in General.

The aim of the invention is a material savings and increased productivity.

With this purpose it is proposed to form a column of melt, closely adjacent to the Central is not wetted by the melt of the core shaper, a speaker on the upper horizontal surface of the molding device, also not wetted by the melt below the melt level in the crucible, i.e., on a column of melt from the bottom to act more pressure, and the growing crystal is carried out at a temperature horizontal surface below, and the top end of the speaker terminal is not higher than the crystallization temperature of the melt, TKR, when the solidification front rasego rod. To suppress capillary effects in the gap shaper, you must create pressure, provide post melt height h1determined from the following expression:

h1= 2 cos / gt, where is the surface tension of the melt;

- contact angle of wetting of the molten material shaper;

the density of the melt;

g - acceleration of gravity;

t - thickness cracks.

For a snug fit post melt to the terminal creates additional pressure provided by the column of melt height h within: h1< h < ho+ h1where ho- the height of the Central rod above the horizontal surface of the shaper.

The lower limit of the height of the column of melt h1defines the passage of the melt through a slit in the former, when h < h1the melt does not pass in the slot and does not form around the Central core of the amount subject to crystallization. The upper limit of the height of the column of melt ho+ h1determines the optimum pressure of the melt at the highest permissible position of the solidification front, when h > ho+ h1surface tension forces are not able to keep the melt in the form of vertical stab melt height h, providing the necessary pressure is created by dip molding device below the level of the melt in the crucible.

The known device to implement the method (2) contains the crucible with the melt and the shaper of the wetted by the molten material with an upper horizontal surface above the level of the melt in the crucible, the edges which define the size and shape of the grown crystal. On a horizontal surface shaper area not wetted by the melt, the speaker above the horizontal surface of the material. The upper horizontal surface is connected with the melt in the crucible by means of the channels through which the melt is applied to it due to capillary effects. When growing crystals using such a device, the plot is not wetted by the molten material prevents the decrease in the size of the channel is less than the specified dimensions when changing temperature conditions, it is not possible deviation in size in the direction of their increase, i.e., the size of the receipt of the crystal depends on the position of the solidification front height, and the grown crystal products require additional processing.

Closest to the present invention is a method (3) gleysteen surface tension around not wetted by the molten core the speaker above the melt level in the crucible, create a temperature gradient along the height of the column of melt-grown crystal from the top of the cold side of the pillar melt at a given speed by increasing the body simultaneously at all points.

Grown crystalline body pull, pre-creating the temperature gradient at the height of the formed pole melt, with the upper cold side, at a given speed by increasing the body simultaneously at all points in the horizontal plane with a constant replenishment of the post melt through a slit in the shaper. Due to the tight fit of the melt to the Central rod size and shape of the cross section of the channel in the obtained crystalline body and the surface quality it does not depend on the position of the solidification front in height between the horizontal surface of the shaper and the upper end of the rod and are determined only by the size, shape cross-section and the surface of the shaping core. The position of the solidification front, which is determined by the altitude at which the temperature is equal to the crystallization temperature Tkrdepends on temperature the forming rod (the first is always higher than the second due to the temperature gradient along the height of the column of melt). Increasing temperature leads to the rise of the crystallization front, lowering its lowering. The lowering of the crystallization front below the horizontal surface forming with decreasing temperature below Tkrleads to the coupling of the crystal with the shaper and its mechanical destruction, and the rise of the solidification front above the upper end of the rod when the temperature rise it above Tkrto reduce the size of the channel. The position of the solidification front is within the specified limits when the temperature changes, for example on T, on the horizontal surface of the shaper from Tkrto Tkr+ T, where T=ho(dT/dX), and dT/dX is the temperature gradient at the height of the column of melt. Under these conditions, random changes of thermal conditions in the growing process does not affect the size and quality of the surface in the crystal body.

In Fig. 1 depicts a diagram of an apparatus for growing crystals, the cross-section of Fig. 2 - scheme of the device for growing hollow crystalline bodies, elevation, and Fig. 3 - wiring diagram parts shaper for receiving the hollow crystals with channels of any given shape.

The device (the Oka 3, graphite glass 4, the shaper with 5 speakers above him the Central rod 6, thermocouple 7, structurally 8 on the movable rod 9 and the furnace 10. The shaper consists of two parts (Fig.3) connected to each other by means of the screws 11, and screwed into the bottom of the glass 4. Replacement parts shaper allows you to rebuild a device for growing crystalline bodies with different cross-section. The shaper is made from is not wetted by the molten material, for example graphite, alloys based on copper. To obtain crystals in the form of tubes and capillaries in the upper part of the shaper 5 has a round hole, sudsee external crystal size of the product, and the lower rod 6 with a diameter specifies the size of the channel (Fig. 3). To obtain waveguides hole and rod have a corresponding rectangular shape, i.e., the rod may have any cross-sectional shape that defines the shape of the cross section of the channel. In the assembled shaper rod 6 acts on the upper horizontal surface by the value of ho= 1-4 mm Lower height of the protrusion does not provide retention of the solidification front between the horizontal top of the market (3aboutC). At the height of the protrusion is more than 4 mm decrease in the size of the crystal in the process of cooling above the solidification front leads to jamming on the forming rod, deformation and mechanical failure of the product.

The proposed device operates as follows.

Melt 12 by movement of the piston 1 to the container 2 through the rod 3 is lifted up until between the walls of the container 2 and Cup 4 will not have a column of height h (Fig.2), providing additional pressure of the melt. The height of the melt is determined by the amount of movement of the lower stem. At the same time the melt fills the shaper 5 and around the Central rod 6 is formed, the volume of melt crystallization. Using the rod 9 is lowered strukturdaten 8 13 seed, the seed crystal melts, is its adhesion to the melt. After that by means of the rod 9 starts pulling the crystal at a given speed. The temperature in the crystallization zone is controlled by thermocouple 7. Changes in temperature, measured by thermocouple, not exceeding 3aboutWith relatively temperature growth leads to change the position of the solidification front is not more than 0.5 mm, that is, within the ledge cent the AE is determined only by the size and shape of cross-section of the Central rod. The temperature variation value 3aboutWith usually observed in the changes of the voltage of the heater turning on and off other consumers) and when the temperature and the flow speed of the coolant (water).

Crystalline body obtained by using the proposed method and the device has a channel shape and dimensions exactly match the shape and size of the forming section of a rod, slightly reduced when cooled to room temperature by an amount determined by the difference of coefficient of thermal expansion of as-grown material and the material of the shaper. Therefore, the shape, dimensions and surface finish of the inner channel defined by the shape, dimensions and surface finishes of the Central rod shaper. Replacing the former, it is possible to obtain crystalline solids with different shape and cross-sectional sizes.

P R I m e R 1. Using the proposed method and device were obtained monocrystalline capillaries with an inner diameter of 1.0 mm and a surface inside the channel of 0.10, an external diameter of 3 mm alloy Cu-Al-Ni containing, wt.%: Al 14,2; Ni 3: Cu Stalino using stem 3 to the formation of a melt column h = 7 mm between the walls of the container 2 and 4 cups of graphite while filling shaper of graphite with the speakers on it for 2 mm of the Central rod with a diameter of 1.02 mm and surface finishes 0,10, the diameter of the forming rod 1,02 mm was selected on the basis of established experimentally, the shrinkage values kristallicheskogo material in relation to the graphite snap-in 1.5% after cooling to room temperature. Then the seed fell to the ground with a pole melt around a forming rod and melting. After coupling of the volume of the melt to be crystallized, with seed in structurale 8 started pulling of the crystal by means of a rolling rod 9 with a speed of 3-4 mm/min. and the Temperature measured by thermocouple was 10522aboutC. At the end of the process of growing the crystal was detached from the melt by reducing the pressure of the melt when the piston is moved down and enable quick movement of the seed.

The study obtained crystalline product showed that the crystals tubular shape with a diameter of 1.00 mm and purity of the surface closest to 0,10, does not require further processing.

P R I m m e R 2. Using the proposed method and devices were also obtained waveguides made of copper with a cross-section of the channel 3.6 x 1.8 mm, the surface in the channel of 0.10 and a wall thickness of 1.0 mm, the Central rod of graphite based on experimenta mm and purity of the surface treatment of 0.10. To obtain these products melt copper movement of the piston 1 to the container 2 made of graphite up with rod 3 has risen to the formation of a melt column height h = 13 mm between the walls of the container 2 and 4 cups of graphite while filling shaper of graphite with protruding above him on the 3 mm Central core and the formation of a melt column. In contact with the column of melt through the rod 9 contained the seed enshrined in structurale 8, the seed was melt occurred adhesion to the volume of the melt to be crystallized. The pulling of the crystal was performed at a speed of 3-4 mm/min when the temperature measured by thermocouple 7, equal 10782aboutC. temperature Fluctuations on the 2aboutWith not led to a change in the size of the channel cross section in the grown crystal body. At the end of the process of growing the crystal was detached from the melt by reducing the pressure of the melt when the piston is moved down and enable quick movement of the stem with seed. The resulting waveguides have cross-section dimensions of the channel 3,h,80 mm and surface purity in it, close to 0,10, and did not require further processing.

Examples confirmed that comprises the different sizes of channel round and rectangular cross-section and a high frequency surface, determined by the size, shape cross-section and surface of the Central rod shaper. The cross-section of the channel may be not only circular or rectangular, but can have any other desired shape depending on the shape of the cross-sectional shaping of the rod. Similarly, the external shape of the crystal body, too, can be any, depending on the shape of the hole in the top of the shaper. Such crystalline solids do not require further machining in order to bring the size and cleanliness of the surface to the required in the manufacture of products. Thereby eliminating the loss of a crystalline material, associated with the processing, and saves processing time, i.e. significantly increases productivity. In addition, in many cases, mechanical treatment would lead to a deterioration of the material properties, and it is impossible in the case of small dimensions of the channel cross section of products and great length.

THE METHOD OF OBTAINING CRYSTALLINE HOLLOW PRODUCTS AND DEVICE FOR ITS IMPLEMENTATION.

1. The method of obtaining crystalline hollow products, including the formation of a melt column around not wetted by the melt, formao is arnosti, characterized in that, to improve performance on the post of the melt from the bottom to the effect of additional pressure.

2. Apparatus for producing crystalline hollow articles comprising a container for molten installed over the stem with structuralism and not wetted by melt molding the rod, characterized in that, to improve performance, the device is provided with a piston mounted on a rod in the bottom of the container, and shaper, located coaxially with the molding core and less than core height.

 

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