Raw material pretreatment method for high-quality aluminum nitride crystal growth
A technology of crystal growth and aluminum nitride, applied in the directions of crystal growth, single crystal growth, single crystal growth, etc., can solve the problem of low purity of AlN powder raw materials, and achieve the effect of improving gas phase transport capacity and reducing impurity content
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Embodiment 1
[0032] (1) First clean the firing crucible (boron nitride crucible, tungsten crucible or tantalum carbide crucible) and growth crucible (tungsten crucible or tantalum carbide crucible) to remove surface pollutants. It can be cleaned first with a heated acetone solution, followed by an ethanol solution.
[0033] (2) Put AlN powder raw materials with an average particle size of 2 μm in a sintered crucible, place the sintered crucible in an AlN crystal growth device, and seal the device. AlN crystal growth equipment is existing conventional equipment, such as figure 1 As shown, it includes intermediate frequency induction coil 4 , graphite insulation material 2 and infrared thermometer 1 , AlN powder raw material 6 is placed in sintering crucible 5 , and AlN crystal 3 is grown by intermediate frequency induction coil 4 heating.
[0034] (3) Use a vacuum system to evacuate the growth equipment, and the vacuum degree is not greater than 10 -3 Pa, then pass high-purity nitrogen (p...
Embodiment 2
[0041] The difference between this embodiment and embodiment 1 lies in steps (3), (4) and (6):
[0042] (3) In a nitrogen atmosphere of 0.6mbar, first raise the temperature to 1200°C at 8°C / min, hold for 2 hours, then raise the temperature to 1700°C at 5°C / min, hold for 6 hours, then slowly cool down to room temperature, and the cooling rate is about 100°C / h to obtain a white sintered body of AlN raw material;
[0043] (4) Place the sintered AlN raw material sintered body in a pulverizer to pulverize to obtain AlN powder particles with a particle size of about 0.5 mm;
[0044] (6) In a nitrogen atmosphere of 1.5mbar, firstly raise the temperature to 1800°C at 9°C / min, then raise the temperature to 2100°C at 5°C / min, keep it warm for 15h, and then slowly cool down to room temperature, and the cooling rate is 40°C / h The temperature was lowered to 1600°C, and then cooled to room temperature at 50°C / h to obtain a light yellow AlN high-purity polycrystalline raw material sintered ...
Embodiment 3
[0046] The difference between this embodiment and embodiment 1 lies in steps (2), (3), (4) and (6):
[0047] (2) placing the AlN powder raw material with an average particle size of 5 μm in a boron nitride crucible;
[0048] (3) In a nitrogen atmosphere of 0.7 mbar, first raise the temperature to 1200°C at 9°C / min, keep it for 1.5h, then raise the temperature to 1600°C at 3°C / min, keep it for 7h, then slowly cool down to room temperature, and the cooling rate is about at 50°C / h to obtain a white sintered body of AlN raw material;
[0049] (4) Put the sintered AlN raw material sintered body in a pulverizer to pulverize to obtain AlN powder particles with a particle size of about 0.8 mm;
[0050] (6) Under a nitrogen atmosphere of 1.2mbar, firstly raise the temperature to 1800°C at 8°C / min, then raise the temperature to 2050°C at 3.5°C / min, keep it warm for 20h, and then slowly cool down to room temperature, and the cooling rate is 50°C / h The temperature was lowered to 1800°C,...
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