RU2580127C1 - Method of connection and fixation of monocrystals (versions), device for method implementation and stack obtained using them - Google Patents

Abstract

FIELD: technological processes.

SUBSTANCE: invention relates to mechanical methods of processing monocrystalline ingots. Method of connecting and fixing mono crystals involves the positioning of several mono crystals, their orientation in a certain way and fixation of mono crystals with each other by means of adhesive, whereupon pre-selection of the necessary number of monocrystalline ingots is carried out, and then carry out orientation of the ends of the selected ingots with required tolerance and removal of base pre-cut with the length of 18-20 mm, whereupon glue mono crystal ingots using device to connect and fix mono crystals as follows: apply adhesive material onto previously degreased end of the mono crystal ingot, mount ingot with preliminary base cut on the base plane 1 of the device while pressing the ingot with clean end against the fixed stop 4 and ingot generant to the surface of the side guard 2, mount next ingot with preliminary base cut on the base plane 1 of the device firmly against the end of the previous ingot, and rotating the knob 7 of the pressing screw 6, press ingots against each other by means of movable stop 5, repeat these operations until the stack of required length is obtained, maintain stack in the device until complete curing of the adhesive material using two-component, colorless epoxy rubber adhesive, and then carry out calibration of the stack to the desired diameter and detach the main base cut, control orientation of the base cut and perpendicularity of ends to the generate. Alternatively, the method of connection and fixation of monocrystals can be implemented without removal of preliminary base cut using device for applying general auxiliary line.

EFFECT: simplified connection and fixation of monocrystals, reduced time costs, higher accuracy of alignment of crystallographic axes of monocrystal ingots.

8 cl, 4 dwg, 1 tbl

Description

FIELD OF THE INVENTION

The invention relates to mechanical methods for processing single-crystal ingots, and also to a device intended for implementing this method, and can be used in the manufacture of stacks of single crystals, in particular sapphire single crystals.

State of the art

A known method of joining parts of refractory oxides, including aluminum oxide (RF patent for the invention No. 2477342, class IPC C30B33 / 06, C30B29 / 16, C30B29 / 22, C30B29 / 28, C30B29 / 18, publ. 03/10/2013 ), including polishing the joined surfaces, their combination and heating. At least one of the polished surfaces to be bonded is coated with a layer of solid solution forming material with at least one of the materials of the parts to be joined. The melting temperature of the solid solution is lower than the melting temperature of each of the materials of the parts to be joined. After that, the combined parts are annealed at a temperature above the temperature of formation of a solid solution. The known method, thus, solves the problem of “blurring” the optical boundary between firmly connected (practically in a monolithic) components of refractory oxides (crystals or ceramics).

The disadvantage of this method is the high energy consumption due to the presence of annealing of the connected parts, also this method does not provide the ability to combine the optical axes of the parts with high accuracy (for example, up to 0.1 degrees).

A known method and device for measuring, orienting and fixing at least one single crystal (RF patent for the invention No. 2365905, class IPC G01N23 / 20, publ. 08/27/2009). In the method, several single crystals are positioned separately one above the other to form a stack, measured, oriented and fixed in a certain way, and then single crystals stacked in stacks are simultaneously rigidly connected to the carrier oriented in the main direction. Moreover, single crystals located one above the other in a stack can be bonded to each other with an adhesive.

A device for measuring, orienting and fixing at least one single crystal contains a rotary table with a receiving device for at least one crystal mount, which has an alignment and fixing unit for orienting the crystal lattice of the single crystal and for oriented fixing of the single crystal, a height-movable x-ray source and detector, with the help of which the determination of the normal angles of the planes of the crystal lattice of a single crystal. The fastening of the crystal in the device consists of an external frame with an internal frame for a single crystal reinforced with a gimbal and second mounting means for adjusting and fixing the single crystal clamped in the internal frame. The device may also be provided with horizontal guides and a linear guide.

The disadvantage of this method and device are:

- high complexity in the design and manufacture of the device, a large number of small and precision parts;

- the need for periodic adjustment of the device, respectively, the need for the availability of reference samples and the creation of conditions for their storage;

- significant time for measuring and fixing a single crystal in accordance with the claimed method, due to the need to use a diffractometer to measure the deviation and adjust the deviation from the desired orientation before fixing each single crystal;

- the need to use protective equipment and compliance with special working conditions, since goniometric (X-ray) devices are used in the process of orienting and fixing single crystals.

Disclosure of invention

The basis of the invention is the task of developing a simple and reliable method of connection and fixation of single crystals, allowing the use in the manufacture of ingots of single crystals of various lengths.

The technical result of the invention is to simplify the process of connecting and fixing single crystals, reducing time costs, improving the accuracy of combining the crystallographic axes of single crystal ingots.

The specified technical result is achieved in that the method of connecting and fixing single crystals includes positioning several single crystals, orienting them in a certain way and fixing the single crystals with each other with an adhesive, and according to the invention, the required number of single crystal ingots is preliminarily selected; then, the ends of the selected ingots are oriented with the necessary tolerance and the preliminary base cut is removed with a length of 18-20 mm; then the single crystal ingots are glued together using the device for connecting and fixing the single crystals as follows: apply adhesive material to the previously defatted end face of the single crystal ingot; the ingot is set with a preliminary base cut on the plane of the base wall of the device, while pressing the ingot with its clean end against the fixed stop and forming the ingot against the surface of the side wall; set the next ingot with a preliminary base cut on the plane of the base wall of the device close to the end face of the previous ingot and, rotating the handle of the clamping screw, the ingots are pressed together using a movable stop; repeat these operations until a stack of the required length is obtained; maintain the stack in the device until the adhesive material has completely hardened, moreover, a two-component colorless epoxy rubber adhesive is used as the adhesive material; then the stack is calibrated to the required diameter and the main base cut is removed; then control the orientation of the base slice and the perpendicularity of the ends to the generatrix.

The specified technical result is also achieved by the fact that the method of connecting and fixing single crystals includes positioning several single crystals, orienting them in a certain way and fixing the single crystals with each other with an adhesive, and according to the invention, the required number of single crystal ingots is preliminarily selected; then the ends of the selected ingots are made with the necessary orientation tolerance; after which a common auxiliary line is applied to the selected ingots using a device that is a rectangular parallelepiped having a "V" -shaped cut, as follows: using a goniometric device, a base cut line is applied to one of the ends of each selected ingot; then, one by one, the ingots of the single crystal are placed on the “V” -shaped cut of the device and each ingot is turned so that the applied line of the base cut is parallel to the surface of the table; then, using a ruler, a common auxiliary line is applied to the forming of all installed ingots; then the single crystal ingots are glued together using the device for connecting and fixing the single crystals as follows: apply adhesive material to the previously defatted end face of the single crystal ingot; set the ingot on the plane of the base of the device, while pressing the ingot with a clean end to the fixed stop and forming the ingot to the surface of the side fence; set the next ingot on the plane of the base of the device close to the end face of the previous ingot, while aligning the auxiliary lines of the single crystal ingots to obtain a common auxiliary line, and, rotating the handle of the clamping screw, the ingots are pressed together using a movable stop; repeat these operations until a stack of the required length is obtained; maintain the stack in the device until the adhesive material has completely hardened, moreover, a two-component colorless epoxy rubber adhesive is used as the adhesive material; then the stack is calibrated to the required diameter and the main base cut is removed; then control the orientation of the base slice and the perpendicularity of the ends to the generatrix.

The orientation of the ends of the selected ingots can be carried out with a tightening of 2 times from the established requirements.

It is possible to withstand the stack in the device until the expiration of the "survivability" of the adhesive material, then stand upright until the adhesive material is completely hardened.

The achievement of the technical result is also ensured by the use of a device for connecting and fixing single crystals containing a base wall and located to it at right angles: the side wall and end walls, on the inner surface of one of the end walls at its center there is a fixed stop, on the opposite end wall - movable emphasis, moved with a clamping screw with a handle; moreover, both stops have a spherical surface with a diameter of 20-30 mm

As the material of the device, metal and / or synthetic thermoplastic polymer can be used.

A stack made using the claimed method and device contains several single crystals oriented in a certain way and fixed with each other by an adhesive.

The analysis of the prior art showed that the claimed combination of essential features set forth in the claims is unknown. This allows us to conclude that the claimed technical solution meets the condition of patentability “novelty”.

A comparative analysis showed that in the prior art no solutions have been identified that have features that match the distinctive features of the claimed invention, and the popularity of the influence of these signs on the technical result is not confirmed. Thus, the claimed technical solution satisfies the condition of patentability "inventive step".

Brief Description of the Drawings

In FIG. 1 shows a structural diagram of a device for connecting and fixing two single crystals.

In FIG. 2 shows a structural diagram of a device for connecting and fixing more than two single crystals.

In FIG. 3 shows a device for applying a common auxiliary line to single crystal ingots.

In FIG. 4 shows a photo of a stack of sapphire single crystals obtained by the claimed method.

The implementation of the invention

A device for connecting and fixing single crystals includes: a base 1 and located at a right angle to it: a side fence 2 and end walls 3. On the inner surface of one of the end walls 3 (usually left), a fixed stop 4 is located at its center, on the opposite end wall 3 - movable stop 5, moved by a clamping screw 6 with a handle 7. The movable stop 5 also has the ability to freely rotate on the axis of the clamping screw 6. Therefore, in the last stage of pressing the ingot, the movable stop 5 does not rotate together but with a clamping screw 6, which eliminates the ingot turning together with the clamping screw 6 until it is fixed in the stack.

Side railing 2 provides the necessary structural rigidity and emphasis for ingots. To facilitate the design of the fence 2 can be made perforated or in the form of a strip connecting the end walls 3 at the height of the stops.

Both stops have a spherical surface with a diameter of 20 to 30 mm; this size was determined empirically based on the necessary accuracy of the geometric parameters of the stack being manufactured. The choice of the shape of the stops is due to the fact that the spherical shape of the stops makes it possible to expose the joined ingots so that their end surfaces are aligned, which ensures the necessary accuracy of combining single crystals with a fairly simple device design, which also does not require precision manufacturing precision.

The structural elements of the device can be made of metal and / or a polymeric material, for example fluoroplastic. In particular, the prototype device for connecting and fixing single crystals was made of metal, and to protect the single crystal ingots, stops 4 and 5 were covered with caps made of a synthetic thermoplastic polymer - fluoroplastic.

The method of connecting and fixing single crystals includes the following steps.

1. Selection of the required number of single crystal ingots. The number of ingots is determined based on the length of the available single crystal ingots and the required length of the stack to be made.

2. Production of ends of selected ingots with the necessary tolerance for orientation, for example, it is possible to tighten 2 times from the established requirements to obtain a guaranteed result. For example: for a given orientation requirement ± 6 min from the nominal - the misorientation tolerance for the ends of the single crystal ingot should be no more than ± 3 min from the nominal.

3. Removing the preliminary base cut. The length of the base cut depends on the diameter of the single crystal ingot, for example, for a diameter of 51 mm, the cut length should be in the range of 18-20 mm. This length value is determined empirically based on the necessary accuracy of the geometric parameters of the stack. An increase in the length of the preliminary base cut is impractical due to unjustified losses of the single crystal.

4. Bonding ingots of single crystals using a device for connecting and fixing single crystals is as follows:

- apply adhesive material to the previously defatted end face of the single crystal ingot;

- set the ingot with a preliminary base cut on the plane of the base 1 of the device, while pressing the ingot with a clean end to the fixed stop 4 and the side surface (forming) of the ingot to the surface of the side fence 2;

- set the next ingot with a preliminary base cut on the plane of the base 1 of the device close to the end face of the previous ingot and, rotating the handle 7 of the clamping screw 6, the ingots are pressed against each other using a movable stop 5;

- repeat the indicated operations until a stack of the required length is obtained;

- maintain the stack in the device until the adhesive material has completely hardened (from 9 to 24 hours, depending on the brand of adhesive material). If necessary, the stack can be removed from the device after 1 ÷ 6 hours, after the “survivability” period has elapsed, depending on the type of adhesive material and held upright until the adhesive material has completely hardened and only after that proceed with further processing of the stack.

As an adhesive material, a two-component colorless epoxy rubber adhesive is used, which has high adhesion, strength of the adhesive joint, resistance to vibration and shock loads, resistance to water, dilute acids and alkalis, as well as solvents. Epoxy rubber glue does not give subsequent shrinkage during curing in the layer of almost any thickness, retains its properties at temperatures from -50 to + 120 degrees Celsius. The lack of color in the adhesive material allows visual inspection of defects of both individual ingots in the stack and the manufactured stack.

5. Calibrate the stack to the required diameter.

6. Removing the main base cut. Control the orientation of the base slice and the perpendicularity of the ends to the generatrix.

Alternatively, the method of connecting and fixing single crystals can be carried out without removing the preliminary base slice using a device for applying a common auxiliary line (see Fig. 3). The specified device 8 is a rectangular parallelepiped having a "V" -shaped notch. A variant of the method of connection and fixation of single crystals includes the following steps.

1. Selection of the required number of single crystal ingots.

2. Making ends of selected ingots with the necessary orientation tolerance.

3. Drawing a common auxiliary line using the device 8 is as follows:

using a goniometric device, a base cut line is applied to one of the ends of each selected ingot;

- alternately set the single crystal ingots on the “V” -shaped cutout of the device 8 and rotate each ingot so that the applied line of the base cut was parallel to the surface of the table 9 (it is possible to use a ruler 10);

- using a ruler, a common auxiliary line is applied to the generatrix of all installed ingots.

4. Bonding of single-crystal ingots using a device for connecting and fixing single crystals is carried out similarly to the first variant of the method, only with the alternate installation of the ingots, the auxiliary lines of each single crystal are combined to obtain a common auxiliary line.

5. Calibrate the stack to the required diameter.

6. Removing the main base cut. Control the orientation of the base slice and the perpendicularity of the ends to the generatrix.

It is possible to use ingots of a single crystal of rectangular cross section, and fixture 8 is not used, but in order for the ingots to be uniformly stacked, the orientation of the sides of the ingot must be indicated. Then, when gluing, the ingots are set in such a way (using the designation of the orientation of the sides) so that the sides of the ingots of the same orientation are located on each side of the resulting stack.

Implementation examples

The following are specific examples of the implementation of the claimed method.

Five pairs of single crystal synthetic sapphire ingots having a length of up to 50 mm each were selected. The ends of the selected ingots with different tolerances for orientation were made. The misorientation of each ingot was measured, then the preliminary basic slice was removed, the length of which ranged from 18 to 20 mm. After that, the misorientation of the preliminary base slice of each ingot was measured (see table).

Then, the single crystal ingots were glued using a device for connecting and fixing single crystals in accordance with the claimed method. After keeping the stack in the device until the adhesive material has completely hardened and calibrating the stack to the required diameter, the main base cut was removed. Then, the orientation of the base slice and the perpendicularity of the ends to the generatrix were monitored, the magnitude of the non-perpendicularity is also shown in the table.

Then each stack was cut into plates on a wire cutting machine, cutting was carried out in standard modes for plates with a diameter of 51 mm, the misorientation of the resulting plates is shown in the table.

In each case from the given Examples (see the table), it can be noted that even if the end face of the ingots to their generatrix is not perpendicular to 9 minutes (the first pair of ingots), but when the ends are misoriented up to 3 minutes, however, plates with a disorientation of no more 6 minutes

Table

No. pair The value of the misorientation of the ends of the ingots, min Disorientation of the preliminary base cut, min The magnitude of the non-perpendicularity of the ends of the ingots to the generatrix before cutting, min. The amount of disorientation on the plates after cutting, min. one 2 3 3 ÷ 9 4 ÷ 6 3 5 3 ÷ 9 3 ÷ 5 2 1,5 one 1 ÷ 2 1 ÷ 2 2 2 1 ÷ 2 1 ÷ 3 3 0.5 four 1 ÷ 7 3 ÷ 5 1,5 2 1 ÷ 7 3 ÷ 5 four 2 one 1 ÷ 2 1 ÷ 2 2 3 1 ÷ 2 0 ÷ 1 5 one one 1 ÷ 2 0 ÷ 1 0.5 one 1 ÷ 2 1 ÷ 2

Using a variant of the method, without removing the preliminary base slice, using a device for applying a common auxiliary line showed similar results.

Thus, the proposed technical solution allows a simple and reliable way to connect and fix the ingots of single crystals. Using the claimed method and device allows to obtain the necessary accuracy of geometric parameters, reduce time costs while maintaining high accuracy of combining the crystallographic axes of single crystal ingots in the stack.

Industrial applicability

The method of connecting and fixing single crystals, in which a device for implementing the method is used, is indeed a simple and reliable method of manufacturing stacks with the necessary accuracy of geometric parameters, which allows using single crystals in the manufacture of ingots. As a result of the implementation of the claimed method, a simplification of the process of connection and fixation of single crystals, reduction of time costs, as well as increased reliability of the connection is provided.

The claimed invention can be used in the manufacture of stacks of various single crystals, in particular sapphire single crystals.

Claims (8)

1. The method of connecting and fixing single crystals, including positioning several single crystals, orienting them in a certain way and fixing the single crystals with each other with an adhesive, characterized in that they first pre-select the required number of single crystals of the single crystal, then produce the ends of the selected ingots with the necessary orientation tolerance and removal of the preliminary base cut, after which the ingots of single crystals are glued using a device for connecting and fixing a single crystal fishing as follows: apply the adhesive material to the previously defatted end face of the single crystal ingot, set the ingot with a preliminary base cut to the plane of the base of the device, while pressing the ingot with its clean end to the fixed stop and forming the ingot to the surface of the side fence, set the next ingot with a preliminary base cut to the plane of the base of the device close to the end face of the previous ingot and, turning the handle of the clamping screw, the ingots are pressed against each other by means of a movable stop repeat the above operations until the stack of the required length is obtained, hold the stack in the device until the adhesive material has completely hardened, moreover, two-component colorless epoxy rubber glue is used as the adhesive material, then the stack is calibrated to the required diameter and the main base cut is removed, after which control is carried out orientation of the base slice and perpendicularity of the ends to the generatrix. 2. A method of connecting and fixing single crystals, including positioning several single crystals, orienting them in a certain way and fixing the single crystals with each other with an adhesive, characterized in that they first pre-select the required number of single crystals of the single crystal, then produce the ends of the selected ingots with the necessary orientation tolerance, after which a common auxiliary line is applied to the selected ingots using a device that is a rectangular parallel a lepiped having a “V” -shaped cut, as follows: using a goniometric device, a base slice line is applied to one of the ends of each selected ingot, then single-crystal ingots are alternately placed on the “V” -shaped fixture and each ingot is rotated so that the deposited the base cut line was parallel to the surface of the table, after which, using a ruler, a common auxiliary line is applied to the forming of all installed ingots, then the single crystals are glued together using the device for joining and fixing single crystals as follows: apply the adhesive material to the previously defatted end face of the single crystal ingot, install the ingot on the plane of the base of the device, while pressing the ingot with its clean end to the stationary stop and forming the ingot on the surface of the side fence, install the next ingot on the plane of the base of the device close to the end face of the previous ingot, while combining the auxiliary lines of the single crystal ingots to obtain a common auxiliary line, and, rotating the clamping screw handle, the ingots are pressed against each other using a movable stop, repeat the indicated operations until a stack of the necessary length is obtained, hold the stack in the device until the adhesive material has completely hardened, moreover, two-component colorless epoxy rubber adhesive is used as the adhesive material, then the stack is calibrated to the required diameter and the removal of the main base cut, after which control the orientation of the base cut and the perpendicularity of the ends to the generatrix. 3. The method according to p. 1 or 2, characterized in that the manufacture of the ends of the selected ingots is carried out with a tightening of 2 times from the established requirements for orientation. 4. The method according to p. 1 or 2, characterized in that the stack is kept in the device until the expiration of the "survivability" of the adhesive material, then stand upright until the adhesive material is completely hardened. 5. A device for connecting and fixing single crystals, comprising a base and a side fence and end walls located at right angles to it, a fixed stop is located on the inner surface of one of the end walls at its center, and a movable stop moved by a pressure clamp on the opposite end wall screws with a handle, and the movable stop also has the function of free rotation on the axis of the clamping screw, and both stops have a spherical surface with a diameter of 20-30 mm 6. The device according to p. 5, characterized in that the side fence is perforated or in the form of a strip connecting the end walls at the height of the stops. 7. The device according to p. 5, characterized in that the material of the device uses metal and / or synthetic thermoplastic polymer. 8. A stack containing several single crystals oriented in a certain way and fixed to each other by an adhesive, characterized in that for the manufacture of the stack the method according to paragraphs is used. 1-4, as well as the device according to paragraphs. 5-7.

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