CN115928201A - Method for realizing temperature distribution required by growth of aluminum nitride single crystal - Google Patents
Method for realizing temperature distribution required by growth of aluminum nitride single crystal Download PDFInfo
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- CN115928201A CN115928201A CN202310225035.4A CN202310225035A CN115928201A CN 115928201 A CN115928201 A CN 115928201A CN 202310225035 A CN202310225035 A CN 202310225035A CN 115928201 A CN115928201 A CN 115928201A
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Abstract
The invention discloses a method for realizing temperature distribution required by growth of an aluminum nitride single crystal. Under the condition that a double-heater thermal field is not arranged in an adopted high-temperature furnace, a circular heater is vertically arranged in the high-temperature furnace, a tungsten crucible and a circular tungsten sleeve are coaxially arranged, and the bottoms of the circular tungsten sleeve and the tungsten crucible are on the same horizontal plane with the middle part of the circular heater in the vertical direction; the circular tungsten sleeve is divided into a thin-walled region and a thick-walled region. The tungsten sleeve with a specific shape is nested on the outer side of the tungsten crucible, the characteristics of high thermal conductivity and high specific heat capacity of metal tungsten are utilized to realize accurate reconstruction of a high-realization temperature distribution mode, and finally the requirement of aluminum nitride single crystal growth on temperature distribution is met. The invention effectively avoids the problems of large design difficulty of a high-temperature furnace temperature distribution mode, obvious improvement of the complexity of a single crystal growth process, obvious improvement of equipment cost and maintenance cost and the like introduced by the conventional method.
Description
Technical Field
The invention relates to optimization of temperature distribution of a high-temperature furnace, in particular to a method for realizing temperature distribution required by growth of aluminum nitride single crystals, which is a reconstruction method for realizing a temperature distribution mode of the high-temperature furnace for growth of the aluminum nitride single crystals.
Background
When growing an aluminum nitride single crystal using a high temperature furnace, a raw material is placed in a region below the growth crucible, and an aluminum nitride crystal growth region is in an upper region. In order to inhibit the polycrystalline deposition behavior of the raw material for aluminum nitride growth on the seed crystal at the temperature rising stage, particularly at the temperature of 1700-2100 ℃, the temperature distribution mode of the position of the growth crucible in the high-temperature furnace is required to meet the requirements of upper heat and lower heat, and the requirement of lower heat and upper cool is met at the constant-temperature growth stage of the crystal. However, in the case of a high-temperature furnace having only one heater, since the internal structure thereof directly determines the temperature distribution pattern in the high-temperature furnace, the reconstruction of the temperature distribution pattern cannot be realized at any stage.
In order to realize reconstruction of a temperature distribution mode in a high-temperature furnace and meet the requirement of different temperature distribution modes of aluminum nitride single crystal growth in a temperature rise stage and a constant temperature stage, a double-heater structure which is distributed up and down is generally required, and the power of an upper heater and a lower heater is adjusted to ensure that an aluminum nitride crystal growth region positioned above a crucible has higher temperature relative to a raw material volatilization region positioned below the crucible in the temperature rise stage; in the constant temperature stage of crystal growth, the power of the upper heater is reduced to obtain a temperature distribution mode of lower heat and upper cool. However, the use of dual heaters results in: (1) The design difficulty of the temperature distribution mode of the high-temperature furnace is high, and the complexity of the single crystal growth process is obviously improved; and (2) equipment cost and maintenance cost are obviously improved.
Disclosure of Invention
The invention provides a method for realizing temperature distribution required by growth of aluminum nitride single crystal, in order to obtain a temperature distribution mode which meets the requirements of hot-up and cold-down in a temperature rising stage and hot-up and cold-down in a constant temperature stage in a high-temperature furnace working by using a heater. According to the method, by utilizing the characteristics of high heat conductivity and high specific heat capacity of metal tungsten, a circular tungsten sleeve with thick wall at the lower part and thin wall at the upper part is nested at the outer side of a tungsten crucible for growth. By utilizing the characteristic of high specific heat capacity of metal tungsten, the temperature of a raw material volatilization region corresponding to the thick-wall part of the tungsten sleeve is always lower than that of an aluminum nitride crystal growth region corresponding to the thin-wall part in the temperature rising stage; by utilizing the characteristic of high thermal conductivity of metal tungsten, the temperature of a raw material volatilization area corresponding to a thick-wall area of the tungsten sleeve is higher than that of an aluminum nitride crystal growth area corresponding to a thin-wall area at a constant temperature stage, so that the reconstruction of a temperature distribution mode in the high-temperature furnace is realized.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a method for realizing the temperature distribution required by the growth of aluminum nitride single crystal is that under the condition that a double-heater thermal field is not arranged in a high-temperature furnace, a circular heater is vertically arranged in the high-temperature furnace, a tungsten crucible is coaxially arranged in the circular heater, a circular tungsten sleeve is coaxially arranged outside the tungsten crucible, and the bottoms of the circular tungsten sleeve and the tungsten crucible are on the same horizontal plane with the middle part of the circular heater in the vertical direction; the circular tungsten sleeve is divided into two regions, wherein the upper half part is a thin-wall region, and the lower half part is a thick-wall region; executing an automatic temperature rise program of the high-temperature furnace, wherein the circular heater works for 0h-3h and is in a temperature rise stage; when the output power of the circular heater is linearly increased from 0kW to 30kW in the temperature rising stage, the temperature of the upper part of the tungsten crucible close to the thin-wall area of the circular tungsten sleeve is as follows: increasing the temperature from 898-902 ℃ with the temperature rise of 1h to 2245-2250 ℃ with the temperature rise of 3 h; the temperature of the lower half part of the tungsten crucible close to the thick-wall area of the circular tungsten sleeve is as follows: increasing the temperature from 890-894 ℃ with the temperature rising for 1h to 2235-2240 ℃ with the temperature rising for 3 h; when the circular heater works for 3 hours with the output power of 30kW as a constant temperature stage, after the constant temperature stage is carried out for 2 hours, the temperature of the upper part of the tungsten crucible close to the thin-wall area of the circular tungsten sleeve is 2280-2285 ℃; the temperature of the lower part of the tungsten crucible close to the thick-wall area of the circular tungsten sleeve is 2300-2305 ℃; finally realizing the temperature distribution type of the tungsten crucible to be 'upper hot lower cold' at the temperature rising stage required by the growth of the aluminum nitride single crystal; the temperature distribution of the tungsten crucible is realized in a constant temperature stage required by the growth of the aluminum nitride single crystal, namely the temperature distribution is 'hot and cool down'.
The invention provides a method for realizing temperature distribution required by growth of an aluminum nitride single crystal, wherein a thin-wall region positioned above a circular tungsten sleeve provides required temperature difference for growth of the aluminum nitride single crystal on one hand, and on the other hand, the corresponding thin-wall region above a growing tungsten crucible has higher instantaneous temperature than a thick-wall region in a temperature rise stage, and a temperature distribution state of being hot and cold is realized after a growth system is stable. Moreover, the thick-wall area below the circular tungsten sleeve also plays a role in uniform temperature distribution, so that the temperature difference below the tungsten crucible can be effectively reduced, the growth raw materials of the aluminum nitride can be maintained to be uniformly volatilized in the crystal growth process, and the reconstruction of the temperature distribution mode in the temperature rise stage and the constant temperature stage of the aluminum nitride crystal is finally realized.
The beneficial effects produced by the invention are as follows: compared with the traditional mode of realizing the temperature distribution of heating up and cooling down in the heating-up stage and heating up and cooling down in the constant-temperature stage by using double heaters, the method not only can effectively avoid the problems of large design difficulty of the temperature distribution mode of the high-temperature furnace, obvious improvement of the complexity of the single crystal growth process, obvious improvement of equipment cost and maintenance cost and the like introduced by the conventional method, but also can enable the volatilization of the raw materials to be more uniform and stable in the constant-temperature stage due to smaller temperature difference and more uniform temperature distribution in the area below the tungsten crucible.
Drawings
FIG. 1 is a schematic cross-sectional view showing the relative positions of the structures for realizing the temperature distribution required for growing an aluminum nitride single crystal according to the present invention;
FIG. 2 is a schematic diagram of the three-dimensional structure of the circular heater of FIG. 1;
FIG. 3 is a schematic three-dimensional structure of the circular tungsten sleeve of FIG. 1;
FIG. 4 is a schematic diagram showing the temperature distribution in the upper and lower regions of a tungsten crucible heated by a heater 1h in example 1 of the present invention;
FIG. 5 is a schematic diagram showing the temperature distribution in the upper and lower regions of a tungsten crucible heated by a heater 3h in example 1 of the present invention;
FIG. 6 is a schematic diagram showing the temperature distribution in the upper and lower regions of a tungsten crucible heated by a heater 5h in example 1 of the present invention;
FIG. 7 is a schematic temperature distribution of the heater ramp 1h in the upper and lower regions of a tungsten crucible of example 2 of the present invention;
FIG. 8 is a schematic temperature profile of the zone above and below the tungsten crucible for a heater ramp of 3h in example 2 of the present invention;
FIG. 9 is a schematic diagram showing the temperature distribution in the upper and lower regions of a tungsten crucible heated by a heater 5h in example 2 of the present invention;
FIG. 10 is a schematic diagram showing the temperature distribution in the upper and lower regions of a tungsten crucible heated by a heater 1h in example 3 of this invention;
FIG. 11 is a schematic diagram showing the temperature distribution in the upper and lower regions of a tungsten crucible heated by a heater 3h in example 3 of this invention;
FIG. 12 is a schematic diagram showing the temperature distribution in the upper and lower regions of a tungsten crucible heated by a heater 5h in example 3 of the present invention.
Description of the preferred embodiment
The invention is further illustrated by the following examples in conjunction with the drawings:
as shown in fig. 1 to fig. 3, in the method, under the condition that a double-heater thermal field is not arranged in a high-temperature furnace, a circular heater 3 is vertically arranged in the high-temperature furnace, a tungsten crucible 1 is coaxially arranged in the circular heater 3, a circular tungsten sleeve 2 is coaxially arranged outside the tungsten crucible 1, and the bottoms of the circular tungsten sleeve 2 and the tungsten crucible 1 and the middle part of the circular heater 3 in the vertical direction are on the same horizontal plane; the circular tungsten sleeve 2 is divided into two regions, wherein the upper half part is a thin-wall region 2-1, and the lower half part is a thick-wall region 2-2; executing an automatic temperature rise program of the high-temperature furnace, wherein the circular heater 3 works for 0h-3h and is in a temperature rise stage; when the output power of the circular heater 3 is linearly increased from 0kW to 30kW in the temperature rise stage, the temperature of the upper part of the tungsten crucible 1 near the thin-walled region 2-1 of the circular tungsten sleeve is: increasing the temperature from 898-902 ℃ with the temperature rise of 1h to 2245-2250 ℃ with the temperature rise of 3 h; the temperature of the lower half part of the tungsten crucible 1 close to the thick-wall area 2-2 of the circular tungsten sleeve is as follows: increasing the temperature from 890-894 ℃ with the temperature rising for 1h to 2235-2240 ℃ with the temperature rising for 3 h; when the circular heater 3 works for 3 hours with the output power of 30kW, the constant temperature stage is realized, and after the constant temperature stage is carried out for 2 hours, the temperature of the upper part of the tungsten crucible 1 close to the thin-wall area 2-1 of the circular tungsten sleeve is 2280-2285 ℃; the temperature of the lower part of the tungsten crucible 1 close to the thick-wall area 2-2 of the circular tungsten sleeve is 2300-2305 ℃; finally, the temperature distribution type of the tungsten crucible 1 is 'upper heat and lower cool' at the temperature rising stage required by the growth of the aluminum nitride single crystal; the temperature distribution of the tungsten crucible 1 is realized in the constant temperature stage required for the growth of the aluminum nitride single crystal, and the temperature distribution is in the type of "hot-down and cold-up".
In the method, the preferred range of the thickness of the thin-wall area 2-1 above the circular tungsten sleeve is 0.5-1mm, and the preferred range of the thickness of the thick-wall area 2-2 below the circular tungsten sleeve is 1.5-10mm; the height of the adopted round heater 3 is 25cm, and the diameter is 16cm; the heights of the circular tungsten sleeve 2 and the tungsten crucible 1 are equal and are both 4-10cm; the height of the thick-wall area 2-2 in the circular tungsten sleeve 2 is 3-9cm; the outer diameter of the circular tungsten sleeve 2 is 6-14cm; the outer diameter of the tungsten crucible 1 is 5-13cm.
Examples
In the first step, a circular heater 3 having a height of 25cm and a diameter of 16cm was placed in a high temperature furnace.
Secondly, coaxially placing the circular tungsten sleeve 2 and the tungsten crucible 1 in the circular heater 3, wherein the bottoms of the tungsten crucible 1 and the circular tungsten sleeve 2 and the middle part of the circular heater 3 in the vertical direction are positioned on the same horizontal plane; the outer diameter of the adopted tungsten crucible 1 is 5cm; the outer diameter of the adopted circular tungsten sleeve 2 is 8 cm, the thickness of a thin-wall area 2-1 of the circular tungsten sleeve 2 is 1mm, the thickness of a thick-wall area 2-2 is 5mm, the height of the thick-wall area 2-2 is 3cm, and the heights of the circular tungsten sleeve 2 and the tungsten crucible 1 are equal and are both 6cm.
And thirdly, after the assembly is finished, executing an automatic temperature rise program of the high-temperature furnace, and linearly raising the power of the circular heater 3 from 0kW to 30kW within 3 h. As shown in FIG. 4, at 1h during the temperature increase, the temperature of the raw material volatilization region below the tungsten crucible 1 corresponding to the thick-walled region 2-2 of the circular tungsten sleeve 2 was 894 ℃, and the temperature of the aluminum nitride crystal growth region above the tungsten crucible 1 corresponding to the thin-walled region 2-1 of the tungsten sleeve was 900 ℃. At the time of the temperature rise to the 3h, as shown in fig. 5, the thick-walled region 2-2 and the thin-walled region 2-1 of the circular tungsten sleeve 2 had temperatures of 2235 ℃ and 2249 ℃, respectively. The temperature of the thick-walled region 2-2 is always lower than that of the thin-walled region 2-1 in the temperature rise stage, and the temperature distribution mode is upper heat and lower cold. At the 5 th hour of heating, as shown in FIG. 6, the temperatures of the thick-walled region 2-2 and the thin-walled region 2-1 were 2300 ℃ and 2284 ℃, respectively. It is shown that the temperature of the thick-walled region 2-2 is higher than that of the thin-walled region 2-1 at the constant temperature stage. The temperature distribution purposes of 'upper heat and lower cool' in the temperature rise stage and 'lower heat and upper cool' in the constant temperature stage required by the growth of the aluminum nitride single crystal are realized.
Examples
In the first step, a circular heater 3 having a height of 25cm and a diameter of 16cm was placed in a high temperature furnace.
Secondly, coaxially placing the circular tungsten sleeve 2 and the tungsten crucible 1 in the circular heater 3, wherein the bottoms of the tungsten crucible 1 and the circular tungsten sleeve 2 and the middle part of the circular heater 3 in the vertical direction are positioned on the same horizontal plane; the outer diameter of the adopted tungsten crucible 1 is 5cm; the outer diameter of the adopted circular tungsten sleeve 2 is 8 cm, the thickness of a thin-wall area 2-1 of the circular tungsten sleeve 2 is 1mm, the thickness of a thick-wall area 2-2 is 10mm, the height of the thick-wall area 2-2 is 3cm, and the heights of the circular tungsten sleeve 2 and the tungsten crucible 1 are both 6cm.
And thirdly, after the assembly is finished, executing an automatic temperature rise program of the high-temperature furnace, and linearly raising the power of the circular heater 3 from 0kW to 30kW at 3 h. As shown in FIG. 7, in the 1 st h during the temperature rise, the temperature of the raw material volatilization region below the tungsten crucible corresponding to the thick-walled region 2-2 of the circular tungsten sleeve 2 was 890 deg.C, and the temperature of the aluminum nitride crystal growth region above the tungsten crucible 1 corresponding to the thin-walled region 2-1 of the tungsten sleeve 2 was 898 deg.C. At the time of raising the temperature to the 3 rd h, as shown in FIG. 8, the temperatures of the thick-walled region 2-2 and the thin-walled region 2-1 were 2240 ℃ and 2250 ℃, respectively. It is explained that the temperature of the thick-walled region 2-2 is always lower than that of the thin-walled region 2-1 in the temperature rise stage, and the temperature distribution mode is upper heat and lower cold. When the temperature of 5h is raised, as shown in fig. 9, the temperatures of the thick-walled region 2-2 and the thin-walled region 2-1 are 2305 ℃ and 2285 ℃, respectively. It is shown that the temperature of the thick-walled region 2-2 is higher than that of the thin-walled region 2-1 at the constant temperature stage. The temperature distribution of 'upper heat and lower cool' in the temperature rising stage and 'lower heat and upper cool' in the constant temperature stage required by the growth of the aluminum nitride single crystal is realized.
Examples
In the first step, a circular heater 3 having a height of 25cm and a diameter of 16cm was placed in a high temperature furnace.
Secondly, coaxially placing the circular tungsten sleeve 2 and the tungsten crucible 1 in the circular heater 3, wherein the bottoms of the tungsten crucible 1 and the circular tungsten sleeve 2 and the middle part of the circular heater 3 in the vertical direction are positioned on the same horizontal plane; the outer diameter of the adopted tungsten crucible 1 is 5cm; the outer diameter of the adopted circular tungsten sleeve 2 is 8 cm, the thickness of a thin-wall region 2-1 of the circular tungsten sleeve 2 is 0.5 mm, the thickness of a thick-wall region 2-2 is 5mm, the height of the thick-wall region 2-2 is 3cm, and the heights of the circular tungsten sleeve 2 and the tungsten crucible 1 are equal and are both 6cm.
And thirdly, after the assembly is finished, executing an automatic temperature rise program of the high-temperature furnace, and linearly raising the power of the circular heater 3 from 0kW to 30kW at 3 h. As shown in FIG. 7, in the 1 st h during the temperature rise, the temperature of the raw material volatilization region below the tungsten crucible 1 corresponding to the thick-walled region 2-2 of the circular tungsten sleeve 2 was 894 ℃, and the temperature of the aluminum nitride crystal growth region above the tungsten crucible 1 corresponding to the thin-walled region 2-1 of the circular tungsten sleeve 2 was 902 ℃. When the temperature is raised to the 3 rd h, as shown in FIG. 8, the temperatures of the thick-walled region 2-2 and the thin-walled region 2-1 are 2240 ℃ and 2245 ℃ respectively. The temperature of the thick-walled region 2-2 is always lower than that of the thin-walled region 2-1 in the temperature rise stage, and the temperature distribution mode is upper heat and lower cold. When the temperature of 5h is raised, as shown in fig. 9, the temperatures of the thick-walled region 2-2 and the thin-walled region 2-1 are 2300 ℃ and 2280 ℃, respectively. It is shown that the temperature of the thick-walled region 2-2 is higher than that of the thin-walled region 2-1 at the constant temperature stage. The temperature distribution purposes of 'upper heat and lower cool' in the temperature rise stage and 'lower heat and upper cool' in the constant temperature stage required by the growth of the aluminum nitride single crystal are realized.
The above examples illustrate the type of temperature profile of the tungsten crucible during the warm-up phase as "hot-up and cool-down"; the temperature distribution type of the tungsten crucible in the constant temperature stage is "hot and cold at the bottom". Finally, the requirements of the aluminum nitride single crystal growth on the temperature distribution of 'heating up and cooling down' in the temperature rise stage and 'heating up and cooling down' in the constant temperature stage are met.
According to the invention, the circular tungsten sleeve with a specific shape is nested on the outer side of the tungsten crucible for growth, and the characteristics of high thermal conductivity and high specific heat capacity of metal tungsten are utilized to realize accurate reconstruction of a temperature distribution mode.
Claims (7)
1. A method for realizing temperature distribution required by growth of aluminum nitride single crystal is characterized in that under the condition that a double-heater thermal field is not arranged in an adopted high-temperature furnace, a circular heater is vertically arranged in the high-temperature furnace, a tungsten crucible is coaxially arranged in the circular heater, a circular tungsten sleeve is coaxially arranged outside the tungsten crucible, and the bottoms of the circular tungsten sleeve and the tungsten crucible are on the same horizontal plane with the middle part of the circular heater in the vertical direction; the circular tungsten sleeve is divided into two regions, wherein the upper half part is a thin-wall region, and the lower half part is a thick-wall region;
executing an automatic temperature rise program of the high-temperature furnace, wherein the circular heater works for 0-3 h as a temperature rise stage; when the output power of the circular heater is linearly increased from 0kW to 30kW in the temperature rising stage, the temperature of the upper part of the tungsten crucible close to the thin-wall area of the circular tungsten sleeve is as follows: increasing the temperature from 898-902 ℃ with the temperature rise of 1h to 2245-2250 ℃ with the temperature rise of 3 h; the temperature of the lower half part of the tungsten crucible close to the thick-wall area of the circular tungsten sleeve is as follows: increasing the temperature from 890-894 ℃ with the temperature rising for 1h to 2235-2240 ℃ with the temperature rising for 3 h;
when the circular heater works for 3 hours with the output power of 30kW, the circular heater is in a constant temperature stage, and after the circular heater enters the constant temperature stage for 2 hours, the temperature of the upper part of the tungsten crucible close to the thin-wall area of the circular tungsten sleeve is 2280-2285 ℃; the temperature of the lower part of the tungsten crucible close to the thick-wall area of the circular tungsten sleeve is 2300-2305 ℃;
finally realizing the temperature distribution type of the tungsten crucible to be 'upper hot lower cold' at the temperature rising stage required by the growth of the aluminum nitride single crystal; the temperature distribution of the tungsten crucible is realized in a constant temperature stage required by the growth of the aluminum nitride single crystal, namely the temperature distribution is 'hot and cool down'.
2. The method for realizing the temperature distribution required by the growth of the aluminum nitride single crystal as claimed in claim 1, wherein the thickness of the thin-walled region above the circular tungsten sleeve is preferably in the range of 0.5-1mm, and the thickness of the thick-walled region below the circular tungsten sleeve is preferably in the range of 1.5-10mm.
3. A method for realizing a temperature profile required for the growth of an aluminum nitride single crystal according to claim 2, wherein a circular heater having a height of 25cm and a diameter of 16cm is used.
4. The method as set forth in claim 3, wherein the height of the circular tungsten sleeve is equal to that of the tungsten crucible and is 4-10cm.
5. The method of claim 4, wherein the height of the thick-wall region in the circular tungsten sleeve is 3-9cm.
6. The method of claim 5, wherein the circular tungsten sleeve has an outer diameter of 6-14cm.
7. A method for realizing a temperature profile required for the growth of an aluminum nitride single crystal according to claim 6, wherein the tungsten crucible has an outer diameter of 5 to 13cm.
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| CN114752999A (en) * | 2022-03-30 | 2022-07-15 | 深圳大学 | Equipment and method for preparing crystal |
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| CN106149057A (en) * | 2015-03-10 | 2016-11-23 | 深圳大学 | The controlled aluminum nitride crystal growth device in temperature field and technique |
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