Disclosure of Invention
Therefore, the invention provides a crystal growth method of large-size single crystals, which is used for solving the problems that the prior art is easy to deform or even break in the pulling process due to the increase of the volume and the weight of the crystals and the influence on the integrity and the stability of the large-size single crystals under the interference of gravity.
In order to achieve the above object, the present invention provides a method for growing a large-sized single crystal, comprising:
step S1, fixing seed crystals on the liquid level of a single crystal material, and pulling the seed crystals to pull the single crystal material to grow so as to obtain the stress value of a seed crystal chuck in the initial stage of crystal growth in the pulling direction and the profile characteristics of the grown single crystal;
S2, analyzing the characteristic difference quantity of the profile width of the middle part of the grown single crystal and the profile width of the liquid surface according to the profile characteristics of the grown single crystal, and calculating a crystal growth expansion characterization coefficient by combining the stress value fluctuation of the seed chuck in the lifting direction so as to judge the crystal growth expansion type of the single crystal material;
Step S3, determining technological parameters according to the crystal growth extension type of the single crystal material, pulling the single crystal material to grow, including,
Determining the pulling speed of a seed chuck according to the crystal growth extension characterization coefficient, and judging whether the crystal growth characterization coefficient meets the morphological variation standard according to the change rate of the profile characteristics of the grown single crystal so as to carry out gradient pulling and synchronously increasing the temperature of the single crystal material, wherein the gradient pulling comprises stopping pulling, starting pulling after a preset time length, and the preset time length is determined based on the maximum width of the profile characteristics;
Or, maintaining the reference pull rate to migrate single crystal material growth.
Further, the process of analyzing the characteristic difference amount of the middle contour width and the liquid level contour width comprises,
Determining a middle contour width of a grown single crystal and a liquid level contour width;
Solving a difference value between the width of the middle contour and the width of the liquid level contour;
And determining the difference value as the characteristic difference amount.
Further, in step S2, the growth expansion characterization coefficient is calculated according to the formula (1),
In the formula (1), E represents a crystal growth expansion characterization coefficient, L represents a characteristic difference value, L 0 represents a preset standard characteristic difference value, F represents a stress fluctuation value in the lifting direction of the seed chuck, F 0 represents a stress fluctuation value in the lifting direction of the preset standard seed chuck, a represents a characteristic difference value weight coefficient, and b represents a stress fluctuation value weight coefficient.
Further, in step S2, the type of the growth extension of the single crystal material is determined according to the growth extension characterization coefficient, including,
If the growth crystal extension characterization coefficient is smaller than or equal to the reference growth crystal extension characterization coefficient, judging that the single crystal material belongs to the weak growth crystal extension class;
and if the crystal growth expansion characterization coefficient is larger than the reference crystal growth expansion characterization coefficient, judging that the single crystal material belongs to the strong crystal growth expansion category.
Further, in step S3, process parameters are determined according to the type of the crystal growth extension, including,
If the single crystal material belongs to the weak crystal extension category, determining the pulling speed of a seed chuck according to the crystal extension characterization coefficient, judging whether the single crystal material meets the morphological variation standard according to the change speed of the profile characteristics of the grown single crystal so as to carry out gradient pulling and synchronously increasing the temperature of the single crystal material;
And if the single crystal material belongs to the strong crystal growth extension category, maintaining the reference process parameters.
Further, in step S3, the pulling speed of the seed chuck is determined according to the crystal growth expansion characterization coefficient, wherein,
The determined pulling speed is positively correlated with the growth crystal extension characterization coefficient.
Further, in step S3, the process of analyzing the rate of change of the profile features of the growing single crystal includes,
Determining a middle profile width of the grown single crystal;
determining a liquid level profile width of the grown single crystal;
and determining the ratio of the profile width change value to the change time to be the change rate of the profile characteristic of the growing single crystal.
Further, the process of determining whether the morphological variation criterion is met according to the rate of change of the profile features of the grown single crystal includes,
Determining a difference between a rate of change of the profile feature within the current reference time period and a rate of change of the profile feature within the adjacent reference time period;
if the difference is larger than a preset difference threshold, judging that the shape variation standard is not met, and synchronously increasing the temperature of the monocrystalline material.
Further, a predetermined time period is calculated according to the formula (2),
In the formula (2), T represents a predetermined time period, te represents a reference predetermined time period, D represents a maximum width of the profile feature, D 0 represents a maximum width of a preset standard profile feature, and c represents a maximum width precision coefficient.
Further, the rotation of the seed chuck is maintained during the pulling process.
Compared with the prior art, the method has the advantages that the seed crystal is fixed on the liquid level of the single crystal material, the seed crystal is pulled to pull the single crystal material to grow, the stress value of the seed crystal chuck in the pulling direction at the initial stage of crystal growth and the profile characteristic of the grown single crystal are obtained, the characteristic difference quantity of the profile width of the middle part and the profile width of the liquid level is analyzed according to the profile characteristic of the grown single crystal, the crystal growth expansion characterization coefficient is calculated by combining the stress value fluctuation of the seed crystal chuck in the pulling direction, the crystal growth expansion type of the single crystal material is judged, the technological parameters are determined, the single crystal material is pulled to grow, the pulling speed of the seed crystal chuck is determined according to the crystal growth characterization coefficient, and whether the shape variation standard is met or not is judged according to the change rate of the profile characteristic of the grown single crystal, so that gradient pulling is carried out and the temperature of the single crystal material is synchronously adjusted.
In particular, the invention calculates the extension characterization coefficient of the crystal growth, which is calculated by the characteristic difference of the width of the middle contour and the width of the liquid surface contour and the fluctuation of the stress value in the lifting direction of the seed chuck, in the practical situation, the extension of the single crystal material can affect the lifting process, if the uniformity of the single crystal material is poor, the multi-directional stress can be generated on the seed chuck, and the stress value in the lifting direction can be affected under the decomposition of the stress, therefore, the phenomenon is represented by the fluctuation of the stress value in the lifting direction of the seed chuck, and the influence of the extension of the single crystal material on the lifting process can be amplified by the poor uniformity, if the extension is weak, the width of the middle contour can be reduced, therefore, the extension strength is represented by the width of the middle contour, the smaller the characteristic difference is, the stronger the extension is, and the breakage and the deformation easily appear when the extension uniformity is poor, therefore, the invention calculates the extension characterization coefficient of the crystal growth of the crystal material, the extension uniformity of the single crystal material is represented, the data support is provided for the subsequent division of the extension category of the crystal growth, and the initial technological parameters of the crystal growth of the large-size crystal is adaptively determined, and the integrity and stability of the large-size crystal growth are improved.
Particularly, the invention divides the crystal growth and extends the classification, in the actual situation, the single crystal growth has definite reference technological parameter, and the large-size single crystal and ordinary single crystal need to pull the speed and self-extension degree to be different, especially when the crystal growth and extends the classification to be weak and extends the classification, the large-size single crystal is expanded the homogeneity is bad, the improper pulling speed and temperature can aggravate the above-mentioned phenomenon at this moment, if keep maintaining the reference technological parameter and carrying on and lifting, the single crystal is easy to break, reduce and pull the speed and carry on the heating up to process the single crystal material of single crystal growth can make the single crystal growth flow go on continuously, therefore, the invention confirms the large-size single crystal growth initial technological parameter according to the characteristic coefficient of crystal growth and extends, improve the integrality and stability of the large-size single crystal growth.
In particular, in the process of operating the single crystal growth, the technological parameters are adjusted by calculating the change rate of the profile characteristics of the grown single crystal, in the actual situation, the morphological change of the grown single crystal is generally uniform in the process of pulling, and the morphological change of the single crystal material is uneven and quick before fracture or abnormal deformation, so that whether the profile characteristics of the grown single crystal meet the morphological change standard is determined according to the change rate of the profile characteristics of the grown single crystal, the single crystal is pulled in a gradient manner, the temperature of the single crystal material is adjusted, and the integrity and stability of the single crystal growth are improved.
Detailed Description
In order that the objects and advantages of the invention will become more apparent, the invention will be further described with reference to the following examples; it should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are merely for explaining the technical principles of the present invention, and are not intended to limit the scope of the present invention.
It should be noted that, in the description of the present invention, terms such as "upper," "lower," "middle," and the like indicate directions or positional relationships based on the directions or positional relationships shown in the drawings, which are merely for convenience of description, and do not indicate or imply that the apparatus or elements must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention.
Referring to fig. 1 to 4, fig. 1 is a schematic diagram illustrating steps of a large-size single crystal growth method according to an embodiment of the invention, fig. 2 is a logic block diagram illustrating a determination of dividing a crystal growth type of a single crystal material according to an embodiment of the invention, fig. 3 is a logic block diagram illustrating a pulling speed of a seed chuck according to a crystal growth characterization coefficient, and fig. 4 is a schematic diagram illustrating a large-size single crystal growth method according to an embodiment of the invention, wherein the method comprises:
Step S1, fixing a seed crystal 3 on the liquid level of a single crystal material, and pulling the seed crystal 3 to pull the single crystal material to grow, so as to obtain a stress value of a seed chuck in the initial stage of crystal growth in the pulling direction and profile characteristics of the grown single crystal;
S2, analyzing the characteristic difference quantity of the profile width of the middle part of the grown single crystal and the profile width of the liquid surface according to the profile characteristics of the grown single crystal, and calculating a crystal growth expansion characterization coefficient by combining the stress value fluctuation of the seed chuck in the lifting direction so as to judge the crystal growth expansion type of the single crystal material;
Step S3, determining technological parameters according to the crystal growth extension type of the single crystal material, pulling the single crystal material to grow, including,
Determining the pulling speed of a seed chuck according to the crystal growth extension characterization coefficient, and judging whether the crystal growth characterization coefficient meets the morphological variation standard according to the change rate of the profile characteristics of the grown single crystal so as to carry out gradient pulling and synchronously increasing the temperature of the single crystal material, wherein the gradient pulling comprises stopping pulling, starting pulling after a preset time length, and the preset time length is determined based on the maximum width of the profile characteristics;
Or, maintaining the reference pull rate to migrate single crystal material growth.
Specifically, the method for obtaining the seed crystal 3 is not limited, and only needs to meet the requirement of single crystal growth, for example, natural formation and artificial cultivation can be performed, and a person skilled in the art can select based on specific requirements, which is not described again.
Specifically, the tool for pulling the seed crystal 3 and the specific implementation method are not limited, and only the seed crystal 3 can be driven to move up and down, including a motor, an electromagnetic clutch, a curling wheel and the like, which are the prior art and are not described again.
Specifically, the material of the seed chuck is not limited, and the seed 3 is only required to be clamped, which is not described again.
Specifically, the method for acquiring the profile features of the single crystal is not limited, and only needs to meet the calculation requirement, preferably, the single crystal profile features can be acquired by a high-definition camera and a profile scanner, and a person skilled in the art can select tools according to the requirement, which is not repeated.
Specifically, as shown in fig. 4, the pulling end 2 and the liquid surface contact end 1 have characteristic differences during single crystal growth;
Specifically, in step S1, the process of analyzing the characteristic difference amount of the middle profile width and the liquid surface profile width includes,
Determining a middle contour width of a grown single crystal and a liquid level contour width;
Solving a difference value between the width of the middle contour and the width of the liquid level contour;
And determining the difference value as the characteristic difference amount.
In particular, the middle profile is determined based on the profile of the pull-up end and the profile of the liquid level contact end, wherein,
Determining the central line of the profile of the opposite lifting end and the profile of the liquid level contact end;
Determining the point of contact of the midline with the edge profile of the growing single crystal;
The midline segment between the contact points is defined as the mid-profile.
Specifically, in the step S2, the growth expansion characterization coefficient is calculated according to the formula (1),
In the formula (1), E represents a crystal growth expansion characterization coefficient, L represents a characteristic difference value, L 0 represents a preset standard characteristic difference value, F represents a stress fluctuation value in the lifting direction of the seed chuck, F 0 represents a stress fluctuation value in the lifting direction of the preset standard seed chuck, a represents a characteristic difference value weight coefficient, and b represents a stress fluctuation value weight coefficient.
The standard characteristic difference value is obtained by pre-calculation, wherein the characteristic difference value in the process of no abnormal crystal growth of different single crystals can be recorded in advance, the average standard characteristic difference value delta D is solved, D 0 = gx delta D is set, g is taken as a characteristic difference precision coefficient, and g is more than 1.02 and less than 1.12.
The stress value of the standard to-be-pulled direction of the seed chuck is obtained by pre-calculating, wherein stress fluctuation values of the seed chuck in the pulling direction in a plurality of pulling processes can be recorded in advance, the average standard stress fluctuation value delta M is solved, M 0 = hx delta M is set, h is the precision coefficient of the stress fluctuation value, and h is more than 1.15 and less than 1.4.
The stress fluctuation value is the variance of the stress value of the seed chuck in the pulling direction at different moments in the initial stage of crystal growth.
Specifically, the initial stage of crystal growth is 5% -10% of the length of the preset large-size single crystal growth.
In this embodiment, a is 0.39 and b is 0.61.
According to the invention, the crystal growth expansion characterization coefficient is calculated and obtained by calculating the characteristic difference of the middle contour width and the liquid level contour width and the stress value fluctuation of the crystal seed chuck in the lifting direction, in the practical situation, the ductility of the single crystal material can influence the lifting process, if the uniformity of the single crystal material is poor, the stress value of the crystal seed chuck in the lifting direction can be influenced under the decomposition of force, therefore, the phenomenon is characterized by the fluctuation of the stress value of the crystal seed chuck in the lifting direction, the influence of the ductility of the single crystal material on the lifting process is amplified, and when the expansion uniformity is poor, the breakage and the deformation are easy to occur.
Specifically, the method comprises dividing the class of the growth extension of the single crystal material in the step S2 according to the characterization coefficient of the growth extension, including,
If the growth crystal extension characterization coefficient is smaller than or equal to the reference growth crystal extension characterization coefficient, judging that the single crystal material belongs to the weak growth crystal extension class;
and if the crystal growth expansion characterization coefficient is larger than the reference crystal growth expansion characterization coefficient, judging that the single crystal material belongs to the strong crystal growth expansion category.
Specifically, the reference long crystal expansion characterization coefficient E0 is selected within the interval [0.9,1.1 ].
The invention divides the crystal growth extension category, in the actual situation, the single crystal growth has definite reference process parameters, and the pulling speed and the extension degree required by the large-size single crystal and the common single crystal are possibly different, especially when the crystal growth extension category is the weak crystal growth extension category, the large-size single crystal is poor in crystal growth extension uniformity and easy to generate abnormality, at the moment, the phenomenon is aggravated by unsuitable pulling speed and temperature, if the reference process parameters are continuously maintained for pulling, the single crystal growth is easy to break, the pulling speed is reduced, and the heating and heating treatment is carried out on the single crystal growth material, so that the single crystal growth process can be continuously carried out.
In particular, the process parameters are determined according to the crystal growth extension category, including,
If the single crystal material belongs to the weak crystal extension category, reducing the pulling speed;
And if the single crystal material belongs to the strong crystal growth extension category, maintaining the reference process parameters.
Specifically, the pulling speed of the seed chuck is positively correlated with the growth characteristic coefficient.
Comparing the crystal growth expansion characterization coefficient E with a first crystal growth expansion characterization coefficient comparison threshold E1 and a second crystal growth expansion characterization coefficient comparison threshold E2,
If E2 < E0, determining the first pull-up speed V1, setting v1=ve×0.8;
if E1 is less than or equal to E2, determining the second pulling speed V2, and setting v2=Vex0.65;
If E < E1, determining the third pull-up speed V3, setting v3=ve×0.5;
wherein e1= 0.75E0, e2=0.95e0, ve represents the reference pull speed, 100mm/h < Ve < 200mm/h.
Specifically, in the step S3, the process of analyzing the change rate of the profile characteristic of the grown single crystal includes,
Determining a middle profile width of the grown single crystal;
determining a liquid level profile width of the grown single crystal;
and determining the ratio of the profile width change value to the change time to be the change rate of the profile characteristic of the growing single crystal.
Specifically, the method for obtaining the middle part and the liquid level contour width is not limited, and the method can be obtained by high-speed photography, and only the middle part and the liquid level contour width need to be clearly displayed and calculated, and the detailed description is omitted.
Specifically, the process of determining whether the morphological variation criterion is met according to the rate of change of the profile features of the grown single crystal includes,
Determining a difference between a rate of change of the profile feature within the current reference time period and a rate of change of the profile feature within the adjacent reference time period;
if the difference is larger than a preset difference threshold, judging that the shape variation standard is not met, and synchronously increasing the temperature of the monocrystalline material.
Specifically, the difference threshold does not exceed 0.2 times the rate of change of the profile feature within the contiguous reference time period.
Specifically, the temperature of the single crystal material is increased at a rate of 3% of the original temperature per minute for 5 minutes or until the variation condition of the single crystal growth meets the morphological variation standard.
Specifically, the change rate of the profile characteristics of the grown single crystal is not more than 1% of the original rate, and the variation condition of the single crystal is considered to meet the morphological variation standard.
Specifically, a predetermined time period is calculated according to the formula (2),
In the formula (2), T represents a predetermined time period, te represents a reference predetermined time period, D represents a maximum width of the profile feature, D 0 represents a maximum width of a preset standard profile feature, and b represents a maximum width precision coefficient.
Specifically, the maximum width of the preset standard profile feature is determined based on the liquid level width, and does not exceed 85% of the liquid level width.
In this example, b is 1.25.
In particular, the maximum width D of the profile features is compared with the maximum width D 0 of the preset standard profile features,
If D 0<D≤1.5D0 is reached, the reference preset time Te is selected within 2.2min and 3.5 min;
if D > 1.5D 0, the reference predetermined length Te is selected within (3.5 min,5 min).
Specifically, the technological parameters are adjusted by calculating the change rate of the profile features of the grown single crystal in the operation process of the single crystal growth, if the change rate of the profile features of the grown single crystal does not meet the morphological variation standard, the single crystal growth is subjected to gradient pulling, the temperature of the single crystal material is increased, and the integrity and stability of the single crystal growth are improved.
Specifically, the rotation of the seed chuck is maintained during the pulling process, and the rotation rate is not limited, so long as the single crystal is ensured to be continuously attracted by the seed crystal 3 and not to be separated.
Thus far, the technical solution of the present invention has been described in connection with the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of protection of the present invention is not limited to these specific embodiments. Equivalent modifications and substitutions for related technical features may be made by those skilled in the art without departing from the principles of the present invention, and such modifications and substitutions will be within the scope of the present invention.