A method of obtaining a crystalline product from the melt

 

(57) Abstract:

The invention relates to techniques for growing shaped crystals of refractory oxides for components and products. The technical result - expanding range of products and increasing the yield by improving quality. The method includes the persecution of the crystal, its razresevanje gradual extrusion of the melt through the shaper in the form of a continuous sequence of crystal elements with different profile from the system moving and stationary formers. During pulling of the crystal element with the micro-relief on the side provide a condition n/V>1/L, where n is the rotational speed of the crystal, V is the velocity of the drawing, L is the height of the meniscus of the melt between the working surface of the shaper and the crystallization front. The transition to the element with the micro-relief on the side surface is carried out at a = re+ 0.5 beor a = Re- Rfwhere a is the distance between the axis of rotation of the crystal and the axis of the shaper, re- inner diameter of the tubular element, bethe wall thickness of the tubular element, Reis the radius of the rod element, Rfis the radius of formaleto spiral shape is carried out at a > re+ beor a > Re. 3 C.p. f-crystals, 10 ill.

The invention relates to techniques for growing shaped crystals from the melt and can be used to obtain crystals of refractory oxides used in the form of ready-made components and products in various devices.

A method of obtaining single-crystal products from the melt [U.S. patent N 3915662, class B 01 j 17/20, date of publication, October 28, 1975] , which includes the change of the cross-section of the crystal in the form of a pipe, which is used as seed.

The disadvantage of this method is the limitation of the application. It allows you to change the cross-section pipes. In addition, the use of diluted previously grown pipes leads to a low yield, since the contact tube seed butt shaper contact area is large, which often leads to a block structure, germinating in the growing crystal, or to thermal shock and, consequently, to the appearance of internal stresses that lead to cracking of the pipe or stackable layer (bottom). In addition, any asymmetry in thermal field can also trigger the occurrence of b is s output.

The closest technical solution is the way to obtain crystalline products with variable cross-sectional shape of the melt [U.S. patent N 3868228, B 01 j 17/18, published on 25 February 1975] - the prototype, including the persecution of the crystal, its razresevanje, pulling from the melt through the shaper and changing the shape of the growing crystal.

The disadvantage of the prototype is the inability to obtain a desired range of cultivated products, because this method is only a transition from an element with one constant cross-section to the element with another constant cross-section.

The technical result of the invention consists in the expansion of the product range grown products and in increasing the yield by improving the crystalline quality of the products.

The technical result is achieved in that in the method of obtaining crystalline products from the melt, including the persecution of the crystal, its razresevanje, pulling through the shaper and changing the shape of the growing crystal, the crystal is pulled in stages in the form of a continuous sequence of crystal elements with different profile from sistemului surface provide a condition n/V>1/L, where n is the rotational speed of the crystal, rpm, V - speed extrusion, mm/min, L is the height of the meniscus of the melt between the working surfaces of the shaper and the crystallization front, mm; at the stage of pulling the crystal element with a spiral relief at the stage of the pulling element crystal spiral shape provide a condition n/V1/L; at the stage of pulling the crystal element with continuously variable profile of the lateral surface provide a condition n/V>1/L, with a relative horizontal displacement of the axis of rotation of the crystal and the axis of the shaper for a given program; during pulling of the crystal element with a constant along the growth axis cross-section provide the condition n = 0, and the transition from one element to another exercise horizontal offset of the formers relative to each other and/or relative to the axis of rotation of the crystal and/or changing the position of the level of the melt relative to the working surface of the shaper.

The transition to the element with the micro-relief on the side surface is carried out at a relative horizontal displacement of the axis of rotation of the crystal and the axis of the shaper on the value a=re+0.5 be, where a is the distance between the axis of rotation of the second radius tubular element, mm, or a=Re-Rfwhere Reis the radius of the rod, mm, Rf- radius shaper, mm Transition to an element with a spiral relief is carried out at a relative horizontal displacement of the axis of rotation of the crystal and the axis of the shaper by the amount abeor aReand go to item spiral shape is carried out at a relative horizontal displacement of the axis of rotation of the crystal and the axis of the shaper on the value a>re+beor a>Re.

The present invention makes it possible to grow a wide range of crystal products: a variety of complex shape, consisting of variable elements with constant cross-section, of the elements with micro-relief on the side surface elements with screw relief having a different step of the spiral elements and form elements with continuously variable profile of the lateral surface.

Growing produce in a single cycle, step by step, without removing the crystal from the working surface of the shaper. This method of cultivation significantly reduces or even eliminates the danger of a block structure or internal stresses in the crystal at the moment go to the Oia does not distort the shape of the side surface, since there is no need for a complicated process of combining already grown crystal element with a shaper, having other forms of the crystal surface.

The growing crystal element with the micro-relief on the side of the implement, subject to the condition n/V>1/L and moving the axis of rotation of the crystal and the axis of the shaper on the value a=re+0.5 befor a tubular element or a= Re- Rffor a truss element. In this case, the working surface of the shaper is a form element that is part of the cross-sectional area of the crystal. The melt is concluded between the shaper and some local area of the crystal surface. During the rotation and pulling of the crystal, each segment forming surface sequentially introduced into the melt in and out of the melt. Passing through the melt, the surface of the previously crystallized first layer is fused by a certain amount, and then build a new layer. As along the perimeter surface of the shaper is implemented boundary condition the gearing for edge during the entire drawing process, the capacity of the surface pulling kristanix.com melt at the end of the shaper.

In order to proceed to the pulling of the crystal element with a spiral relief, it is necessary to shift the axis of rotation of the crystal and the axis of the shaper by the amount abefor a tubular element or aRefor a truss element and go to the condition n/V1/L. In this case, each revolution of the rotating crystal crystallized part does not coincide with the liquid meniscus on the surface of the shaper to the magnitude of the abeor aRethat forms a spiral relief. For the formation of spiral crystal set value a>re+beor a>Re. Under the condition that n/V1/L is necessary in order layer mass of crystals this way at the next turn of the crystal is not in contact with the meniscus, that is not podplavleniya, and thus does not distort the shape of the screw relief or spiral. Required step screw relief or spiral is obtained by matching the speed of extrusion and the speed (h=V/n).

The crystal element with continuously variable profile of the lateral surface obtained when the condition n/V>1/L, introducing the relative horizontal movement of the axis of rotation of the crystal and the axis of the former, representing the form element for a given program surface with the same shaper. Horizontal movement according to a given program simultaneously with the rotation and pulling of the crystal defines the desired shape of the side surface of the crystal, which can take any shape rotation.

For pulling the crystal element with a constant along the growth axis cross-section fulfill the condition n=0. The former, used in this case has a working surface corresponding to the cross section of the desired item.

The horizontal offset of the formers with different shape and dimensions of the work surface relative to each other until the moment of contact between the meniscus of the melt at these formers or change the level of the melt relative to the working surfaces of the shaper leads to the change of the area of the meniscus of the melt in contact with the already raised element of the crystal. In this issue changing the cross-section of the crystal element with the micro-relief on the side surface, with a spiral relief, spiral shape and constant along the growth axis cross-section remains unchanged until the next shift of formers or changing the position of the melt level.

Expenences shaper, so without further perestanavlivaya, dramatically increases the structural perfection (quality) of the finished product and thereby increases the yield.

Thus, the proposed method allows to obtain a wide range of crystal products for a variety of complex shapes and thus significantly increase the yield by improving the quality of products.

In Fig. 1 presents a diagram of one device to implement the method of obtaining crystalline products from the melt, which is a contiguous sequence of elements with different profile when receiving the rod of radius RE1, bent in the form of a spiral (element I); Fig. 2 - the same, top view; Fig. 3 is a diagram of the device when receiving the screw relief on the core element of radius RE1(item III), or to obtain a rod with a microrelief on the lateral surface of radius RE2=RE1+a2(IV) (top view), and Fig.4 is a diagram of the device when receiving pipes with micro-relief on the side surface of the inner radius rE1and wall thickness bE1=2RF1(item VI) of Fig. 5 is a top view of Fig. 6 is a diagram of the device at the time of receipt of TRU is 7-cross section of the crystal in the form of a tube with the tab; in Fig. 8 is a diagram of the device when receiving the pipe inner radius rE2(item IX) of Fig. 9 - diagram of the device when receiving the rod of radius RE3 effects= rf+bf(element X); Fig. 10 is a view grown products of the ten elements.

A method of obtaining a crystalline product is implemented on a single device, including made with the possibility of rotation and vertical movement of the crucible 1 melt 2 (indicated by the position of the melt level), which features a shaper 3 with the capillary channel 4, the working surface 5 which is a circle of radius RF1. On the stand 6 is set formers 7 and 8 with the capillary channels 9 and 10 respectively, is inserted coaxially into one another with capillary gap 11. The working surface 12 of the shaper 7 is a ring of inner radius rfand a thickness of bfand the working surface 13 of the shaper 8 is a circle of radius RF2with the length of the shaper 8 is less than the length of the shaper 7. Structurally 14 with the seed crystal 15 is mounted so that its axis of rotation offset from the axis of rotation of the crucible 1 by the value of ROCDwhere ROCD- the claim of the melt 16 height L, located between the growing crystal 17 and the working surface of one or more of the formers.

The method is as follows.

At the initial moment of the crucible 1 is turned so that the distance from the axis of rotation of structurally 14 to the axis of the shaper 3 was equal to a1where RF1<a<2Rand the vertical movement of the crucible establish working surface 5, 12, 13, formers 3, 7, 8 in the same horizontal plane. Loaded into the crucible 1 of the original material so that when it is melt in the melt were shipped formers 3 and 7. The seed 17 is mounted above the shaper 3. Upon reaching the melting temperature of the crystal 17 tatrallyay and raskrashivaut by pulling it from the meniscus of the melt 16 formed between the growing crystal 17 and the working surface 5 of the shaper 3. Then structurally 14 start to rotate around its axis of rotation. With respect to the ratio n/V 1/L grown crystal element in the form of curved spiral rod of radius RE1= RF1(item I). The radius of the spiral - a1step h=V/n. Then stop the rotation and grow straight rod of radius RE1(e is avnue a2RE1begin to rotate structurally 14, keeping the ratio n/V1/L. In this case, the surface of the crystal element 17 is formed a spiral relief depth a2and step h=V/n (item III). Increasing the rotational speed of structurally 14 to n>V/L, raise the rod with a microrelief on the lateral surface of radius RE2=RF1+a2(item IV). Then move the shaper 3 by rotating the crucible 1 (clockwise) for a given program so that the change of distance from the axis of rotation of structurally shaper 14 to 3 corresponded to the growth of the crystal element in the form of a hollow cone with a wall thickness bE1= 2RF1(item V). After the offset of the shaper 3 the value of a3>RF1relative to the axis of rotation of structurally stop rotating the crucible 1. In this case, there will be a growing element of the crystal in the form of a pipe with a microrelief on the side surface of the inner radius rE1= a3-RF1and wall thickness 2RF1(item VI). To build on the grown crystal element 17 in the form of a hollow hemisphere (item VII), turn the crucible 1 counterclockwise for a given program. Items V, VI, VII grown under the condition of n/V&g what ovately 3 and 7. After that, the crucible 1 is stopped to stop the rotation of structurally 14. The melt from the crucible 1 by the capillary gap 18 and the capillary channel 9 rises and spreads along the working surface 12 of the shaper 7, and is razresevanje and stationary growth item VII of the crystal 17 in the form of a tube of inner radius rE2= rfwall thickness bE2= bfwith the tab on the outer side of the tube, the configuration of which is defined by the end surface of the shaper 3. Then put the crucible 1 to break the meniscus of the melt 16, located between the working surface 5 of the shaper 3 and the growing crystal 17, and grow item IX in the form of a tube of inner radius rE2with wall thickness equal to bE2. Rotating the crucible 1 clockwise, divert shaper 3 from shaper 7 so that between them was a capillary gap, and then raise it so that the shaper 8 is also immersed in the melt. In this case, the melt will rise by capillary gap 11 and the capillary channel 10 on the working surface of the shaper 8. From this position produce growth element X of the crystal 17 in the form of a rod of radius RE3 effects=rf+bthe, sledovatelno passing from one to another: and curved in the form of a spiral rod with a radius of 2 mm (inner diameter of the helix 32 mm, 50 mm) (item I), a straight rod with a radius of 2 mm (item II), the core radius of 3 mm with thread (thread depth 2 mm, 2 mm) (item III), a rod with a microrelief on the side surface with a radius of 3 mm (item IV), hollow cone angle at the vertex of 30 degrees, wall thickness of 4 mm and a maximum internal radius of 18 mm (item V), pipe with microrelief on the side surface of the inner radius of 18 mm and a wall thickness of 4 mm (item VI), the inner hemisphere with a radius of 18 mm and a wall thickness of 4 mm (item VII), the pipe inner radius of 4 mm and a wall thickness of 1 mm with a ledge on the outer side wall (item VIII), the same pipe without hanging (item IX), the core radius of 6 mm (item X). The product was grown in the machine with induction heating in an argon atmosphere. The working surface of the shaper installed in the crucible, was represented by a circle with a radius of 2 mm Working surface of the formers installed on the cradle coaxially one in the other, represented respectively a circle with a radius of 2 mm and the ring inner radius of 4 mm and an outer radius of 6 mm. Capillary gap between what alas 0.20-0.25 mm

At the stage of growth of the element I of the rate of extrusion was 1.5 mm/min, speed of structurally was about 0.33/min rotation Axis of structurally was shifted relative to the axis of the first shaper 18 mm At the stage of growth of the element II the rate of extrusion was 1.5 mm/min, the speed is 0 rpm At the stage of growing element III the rate of extrusion was 1 mm/min, speed - 0.5 rpm, and the axis of the shaper was shifted by 1 mm with respect to an axis of rotation of structurally. At the stage of growing element IV the rate of extrusion was 1 mm/min, a rotational speed of 10 rpm, and the axis of the shaper was offset from the axis of rotation of structurally by 1 mm At the stage of growth of the element V is the speed of extrusion was 0.8 mm/min, a rotational speed of 10 rpm, and the axis of the shaper programmatically shifted relative to the axis of rotation of structurally to the value of this offset is equal to 20 mm At the stage of growth of the element VI of the offset of the first shaper was discontinued, and the speed of extrusion and the speed of structurally were the same, as for growing element V rearing item VII speed watagame moved in the opposite direction to align it with the axis of rotation of structurally. At the stage of growth item VIII the rate of extrusion was 1.2 mm/min, structurally does not rotate and the axis of the first shaper was shifted relative to the axis of the second shaper 8 mm so that between the walls of the first and second shaper formed capillary gap width of 1 mm At the stage of growth of item IX the speed of extrusion and the speed of structurally, mutual horizontal location of the crucible and the formers were saved, and the crucible is lowered down to 5 mm so as to break the meniscus of the melt in the capillary gap between the formers. At the stage of growth of the element X the speed of the crystal pulling was 1 mm/min, structurally not rotated, the crucible was deployed to 180 degrees and up to 15 mm was Thus obtained the required crystal containing ten different elements of desired shape and the desired quality.

1. A method of obtaining a crystalline product from the melt, including the persecution of the crystal, its razresevanje, pulling from the melt through the shaper and changing the shape of the growing crystal, wherein the crystal is pulled in stages in the form of nepreryvnorazlitoj, moreover, during pulling of the crystal element with the micro-relief on the side provide a condition

n/V > 1/L,

where n is the frequency of crystal rotation, Rev/min;

V - speed extrusion, mm/min;

L is the height of the meniscus of the melt between the working surfaces of the shaper and the crystallization front, mm,

during pulling of the crystal element with a spiral relief at the stage of the pulling element crystal spiral shape provide a condition n/V 1/L, during the pulling of the crystal element with continuously variable profile of the lateral surface provide a condition n/V > 1/L, with a relative horizontal displacement of the axis of rotation of the growing crystal and the axis of the shaper for a given program, during the pulling of the crystal element with a constant along the growth axis cross-section provide the condition n = 0, and the transition from one element to another exercise horizontal offset of the formers relative to each other and/or relative to the axis of rotation of the crystal and/or changing the position of the level of the melt relative to the working surface of the shaper.

2. The method according to p. 1, characterized in that the transition to the element with the microrelief on pocomoonshine on the value of

a = re+ 0.5 be,

where a is the distance between the axis of rotation of the crystal and the axis of the shaper, mm;

bethe wall thickness of the tubular element, mm;

re- the inner radius of the tubular element, mm,

or

a = Re- Rf,

where Reis the radius of the rod, mm;

Rf- radius shaper, mm

3. The method according to p. 1, characterized in that the transition to an element with a spiral relief is carried out at a relative horizontal displacement of the axis of rotation of the crystal and the axis of the shaper on the value of a beor a Re.

4. The method according to p. 1, wherein the transition element spiral shape is carried out at a relative horizontal displacement of the axis of rotation of the crystal and the axis of the shaper on the value a > re+ beor a > Re.

 

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