Method for promoting growth of dysprosium scandate single crystal

Abstract

The invention provides a method for promoting growth of dysprosium scandate single crystals, which comprises the following steps: preparing raw materials: uniformly mixing the raw materials, and putting into a crucible; setting growth conditions: putting the crucible filled with the raw materials into a high-temperature furnace, and setting temperature gradient, pressure and growth speed; growing by a lifting method: in the growth process, slowly lifting the seed crystal from the molten raw material at a constant speed through a lifting device, and controlling the cooling rate of the crystal to promote the growth of the single crystal; real-time weighing monitoring: in the upward lifting process, carrying out real-time weighing monitoring on the growing single crystal by using a high-precision weighing device, and adjusting growth parameters to maintain the stability and uniformity of the quality of the single crystal; compared with the prior art, the method has the following beneficial effects that by controlling the growth speed and the temperature gradient, defects and internal stress caused by thermal stress in the crystal growth process can be effectively reduced, and the integrity and the mechanical strength of the crystal are improved.

Description

Technical Field

[0001] The invention belongs to the technical field of material science and crystal growth, and particularly relates to a method for promoting the growth of dysprosium scandate single crystal. Background Art

[0002] Dysprosium scandate single crystal is a crystalline material with excellent properties. Due to its high melting point, high stability and excellent electrical conductivity, it has broad application prospects in the fields of laser, electronics, energy, etc. However, the existing dysprosium scandate single crystal growth method has some problems, such as slow growth rate, high cost, and susceptibility to contamination, which limits its promotion in practical applications. Summary of the invention

[0003] In view of the shortcomings of the prior art, the object of the present invention is to provide a method for promoting the growth of dysprosium scandate single crystals to solve the problems raised in the above background technology.

[0004] The present invention is achieved through the following technical solution: A method for promoting the growth of dysprosium scandate single crystals, comprising the following steps:

[0005] Prepare raw materials: mix the raw materials evenly and put them into the crucible;

[0006] Setting growth conditions: placing the crucible with raw materials in a high-temperature furnace and setting the temperature gradient, pressure and growth rate;

[0007] Upper pull growth: During the growth process, the seed crystal is slowly pulled up from the molten raw material at a constant speed by an upper pull device, and the cooling rate of the crystal is controlled to promote the growth of the single crystal;

[0008] Real-time weighing monitoring: During the pulling process, a high-precision weighing device is used to monitor the growing single crystal in real time, and the growth parameters are adjusted to maintain the stability and uniformity of the single crystal quality;

[0009] Crystal growth optimization: Based on real-time weighing data, the growth rate and temperature gradient are dynamically adjusted to optimize the growth process of dysprosium scandate single crystals and improve the quality and size of single crystals.

[0010] As a preferred embodiment, the raw materials include: dysprosium oxide, with a mass percentage of 73%;

[0011] Scandium oxide, mass percentage is 27%.

[0012] As a preferred embodiment, the temperature gradient of the high temperature furnace is 1800°C to 2200°C.

[0013] As a preferred embodiment, the lifting speed of the lifting device is 0.5 mm / h to 2 mm / h.

[0014] As a preferred embodiment, after the crucible containing the raw materials is placed in a high-temperature furnace, an inert gas is introduced into the high-temperature furnace to prevent oxidation of the raw materials or mixing of impurities.

[0015] As a preferred embodiment, the specific steps of crystal growth optimization are:

[0016] Step 1: Real-time weighing data collection

[0017] During the process of growing dysprosium scandate single crystals by the Czochralski method, the mass change of the single crystal is monitored in real time by a high-precision weighing device. Assume that the mass of the single crystal measured at time t is m(t);

[0018] Step 2: Calculate the growth rate

[0019] Growth rate g (t) is calculated by the following formula:

[0020]

[0021] in:

[0022] Δm(t) is the change in the mass of the single crystal within the time interval Δt, Δm(t)=m(t+Δt)-m(t);

[0023] ρ is the density of dysprosium scandate single crystal;

[0024] A is the cross-sectional area of ​​the single crystal;

[0025] Step 3: Set a target growth rate

[0026] Set the target growth rate v g,target To ensure the quality and uniformity of the single crystal. Usually, the target growth rate is determined by experimental data and empirical values;

[0027] Step 4: Adjust growth parameters

[0028] According to the real-time weighing data and the target growth rate, the growth rate and temperature gradient are dynamically adjusted. The adjustment formula is as follows;

[0029] Growth rate adjustment formula:

[0030] v new =v current +k v ·(v g,target -v g (t))

[0031] Real-time monitoring of single crystal quality changes through high-precision weighing devices

[0032] in:

[0033] v newAdjusted lifting speed

[0034] v current Current lifting speed

[0035] k v is the adjustment factor,

[0036] Temperature gradient adjustment formula:

[0037] G new =G current +k G ·(v g,target -v g (t))

[0038] in:

[0039] G new The temperature gradient after adjustment

[0040] G current is the current temperature gradient

[0041] k G It is an adjustment factor, usually determined by experiment.

[0042] Step 5: Feedback Control

[0043] The above adjustment steps are automated through a computer system, which analyzes the weighing data in real time and provides feedback to adjust the growth parameters to ensure stability and optimization during the growth process.

[0044] After adopting the above technical solution, the beneficial effects of the present invention are:

[0045] 1. Precisely control the quality and size of single crystals:

[0046] Through real-time weighing monitoring, the growth process of the single crystal can be accurately grasped, and the growth parameters can be dynamically adjusted according to the weighing data. This real-time feedback and adjustment mechanism can effectively avoid defects and unevenness within the crystal and improve the quality and size consistency of the single crystal.

[0047] 2. Improve production efficiency and yield rate:

[0048] Since real-time monitoring and dynamic adjustment can quickly respond to and correct abnormal situations in the growth process, it reduces human intervention and trial and error costs, improves production efficiency and yield, and reduces production costs.

[0049] 3. Optimize crystal growth conditions:

[0050] The present invention sets appropriate temperature gradient and lifting speed, and optimizes and adjusts them in combination with real-time data, so that the crystal can grow under optimal conditions, thereby obtaining a higher quality single crystal. This is particularly important for high-demand materials such as dysprosium scandate single crystals.

[0051] 4. Reduce crystal defects and internal stress:

[0052] By controlling the growth rate and the temperature gradient, the present invention can effectively reduce defects and internal stress caused by thermal stress during the crystal growth process, and improve the integrity and mechanical strength of the crystal. DETAILED DESCRIPTION

[0053] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0054] The present invention provides a technical solution: a method for promoting the growth of dysprosium scandate single crystal, comprising the following steps:

[0055] Prepare raw materials: mix the raw materials evenly and put them into the crucible;

[0056] Setting growth conditions: placing the crucible with raw materials in a high-temperature furnace and setting the temperature gradient, pressure and growth rate;

[0057] Upper pull growth: During the growth process, the seed crystal is slowly pulled up from the molten raw material at a constant speed by an upper pull device, and the cooling rate of the crystal is controlled to promote the growth of the single crystal;

[0058] Real-time weighing monitoring: During the pulling process, a high-precision weighing device is used to monitor the growing single crystal in real time, and the growth parameters are adjusted to maintain the stability and uniformity of the single crystal quality;

[0059] Crystal growth optimization: Based on real-time weighing data, the growth rate and temperature gradient are dynamically adjusted to optimize the growth process of dysprosium scandate single crystals and improve the quality and size of single crystals.

[0060] As a preferred embodiment, the raw materials include: dysprosium oxide, with a mass percentage of 73%;

[0061] Scandium oxide, mass percentage is 27%.

[0062] As a preferred embodiment, the temperature gradient of the high temperature furnace is 1800°C to 2200°C.

[0063] As a preferred embodiment, the lifting speed of the lifting device is 0.5 mm / h to 2 mm / h.

[0064] As a preferred embodiment, after the crucible containing the raw materials is placed in a high-temperature furnace, an inert gas is introduced into the high-temperature furnace to prevent oxidation of the raw materials or mixing of impurities.

[0065] The specific steps for crystal growth optimization are:

[0066] Step 1: Real-time weighing data collection

[0067] During the process of growing dysprosium scandate single crystals by the Czochralski method, the mass change of the single crystal is monitored in real time by a high-precision weighing device. Assume that the mass of the single crystal measured at time t is m(t);

[0068] Step 2: Calculate the growth rate

[0069] Growth rate g (t) is calculated by the following formula:

[0070]

[0071] in:

[0072] Δm(t) is the change in the mass of the single crystal within the time interval Δt, Δm(t)=m(t+Δt)-m(t);

[0073] ρ is the density of dysprosium scandate single crystal;

[0074] A is the cross-sectional area of ​​the single crystal;

[0075] Step 3: Set a target growth rate

[0076] Set the target growth rate v g,target To ensure the quality and uniformity of the single crystal. Usually, the target growth rate is determined by experimental data and empirical values;

[0077] Step 4: Adjust growth parameters

[0078] According to the real-time weighing data and the target growth rate, the growth rate and temperature gradient are dynamically adjusted. The adjustment formula is as follows;

[0079] Growth rate adjustment formula:

[0080] v new =v current +k v ·(v g,target -v g (t))

[0081] Real-time monitoring of single crystal quality changes through high-precision weighing devices

[0082] in:

[0083] v new Adjusted lifting speed

[0084] v current Current lifting speed

[0085] k v is the adjustment factor,

[0086] Temperature gradient adjustment formula:

[0087] G new =G current +k G ·(v g,target -v g (t))

[0088] in:

[0089] G new The temperature gradient after adjustment

[0090] G current is the current temperature gradient

[0091] k G It is an adjustment factor, usually determined by experiment.

[0092] As an embodiment of the present invention:

[0093] Prepare raw materials:

[0094] Mix 547.55 g of dysprosium oxide and 202.45 g of scandium oxide evenly and put them into a crucible.

[0095] Set the growth conditions:

[0096] The crucible containing the raw materials is placed in a high-temperature furnace with a set temperature range of 1800°C to 2200°C under the protection of inert gas to avoid oxidation of the raw materials or mixing of impurities.

[0097] Upper pull growth method:

[0098] During the growth process, the seed crystal is slowly lifted up from the molten raw material at a speed of 0.5 mm / h to 2 mm / h by an upward pulling device, and the cooling rate of the crystal is controlled to promote the growth of the single crystal.

[0099] Real-time weighing monitoring:

[0100] During the pulling process, a high-precision weighing device (with an accuracy of 0.01 grams) is used to monitor the weight of the growing single crystal in real time. Assuming that the mass of the single crystal measured at time t is m(t), the growth rate is calculated by the following formula:

[0101]

[0102] Crystal Growth Optimization:

[0103] Set the target growth rate v g,target The growth rate and temperature gradient are adjusted dynamically through real-time weighing data: 1. Growth rate adjustment:

[0104] v new =v current +k v ·(v g,target -v g (t))

[0105] Among them, the adjustment coefficient k v =0.1.

[0106] 2. Temperature gradient adjustment:

[0107] G new =G current +k G ·(v g,target -v g (t))

[0108] Among them, the adjustment coefficient k G =0.05.

[0109] Specific Examples

[0110] Assume that the parameters measured during the experiment are as follows:

[0111] Current lifting speed v current =1.4mm / h

[0112] Current temperature gradient G current =10℃ / cm

[0113] Measured growth rate v g (t)=1.3mm / h

[0114] By adjusting:

[0115] Lifting speed adjustment:

[0116] 2. Temperature gradient adjustment:

[0117] v new =1.4mm / h+0.1×(1.5mm / h-1.3mm / h)=1.42mm / h

[0118] G new =10℃ / cm+0.05×(1.5mm / h-1.3mm / h)=10.01℃ / cm

[0119] Through the above adjustment steps, the stability and optimized quality of the dysprosium scandate single crystal growth are guaranteed.

[0120] After the growth is completed, the temperature and pressure in the furnace chamber are lowered through the control system, and then the furnace chamber is opened to take out the grown dysprosium scandate monomer.

[0121] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for promoting the growth of dysprosium scandate single crystals, characterized in that: The following steps are involved: Prepare raw materials: mix the raw materials evenly and put them into the crucible; Setting growth conditions: placing the crucible with raw materials in a high-temperature furnace and setting the temperature gradient, pressure and growth rate; Upper pull growth: During the growth process, the seed crystal is slowly pulled up from the molten raw material at a constant speed by an upper pull device, and the cooling rate of the crystal is controlled to promote the growth of the single crystal; Real-time weighing monitoring: During the pulling process, a high-precision weighing device is used to monitor the growing single crystal in real time, and the growth parameters are adjusted to maintain the stability and uniformity of the single crystal quality; Crystal growth optimization: Based on real-time weighing data, the growth rate and temperature gradient are dynamically adjusted to optimize the growth process of dysprosium scandate single crystals and improve the quality and size of single crystals.

2. A method for promoting the growth of a dysprosium scandate single crystal according to claim 1, characterized in that: Ingredients include: Dysprosium oxide, 73% by mass; Scandium oxide, mass percentage is 27%.

3. A method for promoting the growth of a dysprosium scandate single crystal according to claim 2, characterized in that: The temperature gradient of the high temperature furnace is from 1800°C to 2200°C.

4. A method for promoting the growth of a dysprosium scandate single crystal according to claim 3, characterized in that: The lifting speed of the lifting device is 0.5 mm / h to 2 mm / h.

5. A method for promoting the growth of a dysprosium scandate single crystal according to claim 4, characterized in that: After placing the crucible containing the raw materials in a high-temperature furnace, an inert gas is introduced into the high-temperature furnace to prevent oxidation of the raw materials or mixing of impurities.

6. A method for promoting the growth of a dysprosium scandate single crystal according to claim 1, characterized in that: The specific steps for crystal growth optimization are: Step 1: Real-time weighing data collection During the process of growing dysprosium scandate single crystals by the Czochralski method, the mass change of the single crystal is monitored in real time by a high-precision weighing device. Assume that the mass of the single crystal measured at time t is m(t); Step 2: Calculate the growth rate Growth rate g (t) is calculated by the following formula: in: Δm(t) is the change in the mass of the single crystal within the time interval Δt, Δm(t)=m(t+Δt)-m(t); ρ is the density of dysprosium scandate single crystal; A is the cross-sectional area of ​​the single crystal; Step 3: Set a target growth rate Set the target growth rate v g，target To ensure the quality and uniformity of the single crystal. Usually, the target growth rate is determined by experimental data and empirical values; Step 4: Adjust growth parameters According to the real-time weighing data and the target growth rate, the growth rate and temperature gradient are dynamically adjusted. The adjustment formula is as follows; Growth rate adjustment formula: v new =v current +k v ·(v g，target -v g (t)) Real-time monitoring of single crystal quality changes through high-precision weighing devices in: v new Adjusted lifting speed v current Current lifting speed k v is the adjustment factor, Temperature gradient adjustment formula: G new =G current +k G ·(v g，target -v g (t)) in: G new The temperature gradient after adjustment G current is the current temperature gradient k G It is an adjustment factor, usually determined by experiment. Step 5: Feedback Control The above adjustment steps are automated through a computer system, which analyzes the weighing data in real time and provides feedback to adjust the growth parameters to ensure stability and optimization during the growth process.

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