CN112387974B - Preparation method of crucible material for growing aluminum nitride crystal by PVT method - Google Patents
Preparation method of crucible material for growing aluminum nitride crystal by PVT method Download PDFInfo
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Abstract
A preparation method of crucible material for growing aluminum nitride crystal by PVT method belongs to the technical field of crystal growth. The invention aims to solve the technical problem of short service life of the crucible material for growing the aluminum nitride crystal. The method comprises the steps of weighing tantalum carbide powder, tungsten powder and yttrium oxide powder with certain mass, adding the tantalum carbide powder, the tungsten powder and the yttrium oxide powder into a three-dimensional vibration mixer, adding the mixed powder obtained after uniform mixing into a polyvinyl chloride crucible mold, performing cold isostatic pressing, press forming, placing in a hot-pressing sintering furnace, vacuumizing, performing sintering treatment under the pressure of 20-30 MPa to obtain a sintered crucible material, performing processing forming by using a lathe or linear cutting, then placing in a vacuum sintering furnace, vacuumizing, and performing sintering treatment to obtain the crucible material for growing the aluminum nitride crystal by the PVT method. The crucible material for growth has the advantages of reducing the defect density of the crystal, eliminating the abnormal growth of TaC crystal grains at high temperature and prolonging the service life of the crucible.
Description
Technical Field
The invention belongs to the technical field of crystal growth; in particular to a preparation method of a crucible material for growing aluminum nitride crystals by a PVT method.
Background
The growth temperature required by the prior Physical Vapor Transport (PVT) aluminum nitride crystal growth technology is 1850-2200 ℃, so that a heat-resistant and chemical-resistant crucible material is required.
The materials used at present are tantalum carbide and tungsten crucible materials, but tungsten carbide can be formed in a tungsten crucible under a graphite heater and a heat-preservation environment, and the service life of the tungsten crucible can be rapidly shortened due to the fact that the tungsten carbide crucible is unstable in an AlN steam environment; the TaC crucible has cracks in the use environment with the temperature of over 2200 ℃ due to the phenomenon of the regrowth of TaC crystal grains, and the service life of the crucible is sharply reduced.
Disclosure of Invention
The invention aims to provide a preparation method of a crucible material for growing aluminum nitride crystals by a PVT method, which has long service life.
The invention is realized by the following technical scheme:
a preparation method of crucible material for growing aluminum nitride crystal by PVT method comprises the following steps:
step 1, respectively weighing tantalum carbide powder, tungsten powder and yttrium oxide powder with certain mass according to parts by weight for later use;
step 2, adding the weighed tantalum carbide powder, tungsten powder and yttrium oxide powder into a three-dimensional vibration mixer, and uniformly mixing to obtain mixed powder for later use;
step 3, adding the mixed powder obtained in the step 2 into a polyvinyl chloride crucible mold, and performing cold isostatic pressing and compression molding to obtain a molded crucible material for later use;
step 4, placing the formed crucible material obtained in the step 3 into a hot-pressing sintering furnace, vacuumizing, and sintering under the pressure of 20-30 MPa to obtain a sintered crucible material for later use;
step 5, machining and forming the sintered crucible material obtained in the step 4 by using a lathe or wire cutting to obtain a machined and formed crucible material for later use;
and 6, placing the crucible material processed and molded in the step 5 into a vacuum sintering furnace, vacuumizing, and sintering to obtain the crucible material for growing the aluminum nitride crystal by the PVT method.
The invention relates to a preparation method of a crucible material for growing aluminum nitride crystals by a PVT method, which comprises the following steps of 100 parts by weight of tantalum carbide powder, 1-5 parts by weight of tungsten powder and 0.1-0.5 part by weight of yttrium oxide powder in step 1.
The invention relates to a preparation method of crucible material for PVT method aluminum nitride crystal growth, in step 1, the grain diameter of tantalum carbide powder is 0.9-1.0 mu m, the purity is 99.999-99.9999%, the grain diameter of tungsten powder is 0.5-1.0 mu m, and the purity is 99.999-99.9999%.
The preparation method of the crucible material for PVT method aluminum nitride crystal growth, disclosed by the invention, has the advantage that the mixing time in the step 2 is 10-15 h.
According to the preparation method of the crucible material for PVT method aluminum nitride crystal growth, the average cold isostatic pressure in the step 3 is 200-300 MPa, and the pressing time is 10-20 min.
The invention relates to a preparation method of a crucible material for growing aluminum nitride crystals by a PVT method, wherein the sintering treatment in the step 4 is step-by-step sintering treatment, the temperature is firstly increased to 1100-1200 ℃ at the heating rate of 3 ℃/min, then heated to 1800-1950 ℃ at the heating rate of 1 ℃/min, then the temperature is kept for 2-8 h, then the temperature is reduced to 1250 ℃ at the cooling rate of 0.5 ℃/min, and the temperature is reduced to room temperature at the cooling rate of 2.5 ℃/min after the temperature is kept for 2h.
According to the preparation method of the crucible material for growing the aluminum nitride crystal by the PVT method, in the step 6, the temperature is increased to 2000 ℃ at the heating rate of 1 ℃/min through sintering treatment, then the temperature is kept for 3-8 h, and then the temperature is reduced to the room temperature at the cooling rate of 0.5 ℃/min.
According to the preparation method of the crucible material for PVT method aluminum nitride crystal growth, the defect density of the prepared crucible material for PVT method aluminum nitride crystal growth is reduced, the abnormal growth phenomenon of TaC crystal grains at high temperature is eliminated, the service life of the crucible is prolonged, and the problem of thermal mismatch between the substrate and the crystal is reduced.
According to the preparation method of the crucible material for PVT method aluminum nitride crystal growth, the service life of the prepared crucible material for PVT method aluminum nitride crystal growth is prolonged to 400h, and compared with the existing material which can only be used for 100-200h, the service life is prolonged by 1-4 times.
Drawings
FIG. 1 is an SEM photograph of a crucible material for PVT method aluminum nitride crystal growth prepared by the method according to the embodiment after being used for 50 hours;
FIG. 2 is an SEM photograph of the crucible material for PVT method aluminum nitride crystal growth prepared by the method of the embodiment after 300 hours of use;
FIG. 3 is an SEM photograph of a comparative tantalum carbide crucible material after 50 hours of use;
FIG. 4 is an SEM photograph of a comparative tantalum carbide crucible material after 300 hours of use.
Detailed Description
The first embodiment is as follows:
a preparation method of crucible material for growing PVT method aluminum nitride crystal comprises the following steps:
step 1, respectively weighing tantalum carbide powder, tungsten powder and yttrium oxide powder with certain mass according to parts by weight for later use;
step 2, adding the weighed tantalum carbide powder, tungsten powder and yttrium oxide powder into a three-dimensional vibration mixer, and uniformly mixing to obtain mixed powder for later use;
step 3, adding the mixed powder obtained in the step 2 into a polyvinyl chloride crucible mold, and performing cold isostatic pressing and compression molding to obtain a molded crucible material for later use;
step 4, placing the formed crucible material obtained in the step 3 into a hot-pressing sintering furnace, vacuumizing, and sintering under the pressure of 20-30 MPa to obtain a sintered crucible material for later use;
step 5, machining and forming the sintered crucible material obtained in the step 4 by using a lathe or wire cutting to obtain a machined and formed crucible material for later use;
and 6, placing the crucible material processed and molded in the step 5 into a vacuum sintering furnace, vacuumizing, and sintering to obtain the crucible material for growing the aluminum nitride crystal by the PVT method.
In the preparation method of the crucible material for growing the aluminum nitride crystal by the PVT method according to the embodiment, in step 1, the weight parts of the tantalum carbide powder are 100 parts, the weight parts of the tungsten powder are 2 parts, and the weight parts of the yttrium oxide powder are 0.2 part.
In the method for preparing a crucible material for growing aluminum nitride crystals by a PVT method according to the present embodiment, the particle size of the tantalum carbide powder in step 1 is 0.9 μm, the purity is 99.999%, and the particle size of the tungsten powder is 0.5 μm, and the purity is 99.999%.
In the method for preparing a crucible material for growing aluminum nitride crystals by a PVT method according to this embodiment, the mixing time in step 2 is 10 hours.
In the preparation method of the crucible material for growing the aluminum nitride crystal by the PVT method, the average cold isostatic pressing pressure in the step 3 is 200MPa, and the pressing time is 10min.
In the preparation method of the crucible material for PVT method aluminum nitride crystal growth, the sintering treatment in the step 4 is step-by-step sintering treatment, the temperature is firstly increased to 1100 ℃ at the heating rate of 3 ℃/min, then heated to 1800 ℃ at the heating rate of 1 ℃/min, then kept for 4h, then reduced to 1250 ℃ at the cooling rate of 0.5 ℃/min, kept for 2h, and then reduced to room temperature at the cooling rate of 2.5 ℃/min.
In the preparation method of the crucible material for growing the aluminum nitride crystal by the PVT method in the embodiment, in the step 6, the temperature is increased to 2000 ℃ at the heating rate of 1 ℃/min by sintering treatment, then the temperature is kept for 5 hours, and then the temperature is reduced to the room temperature at the cooling rate of 0.5 ℃/min.
In the method for preparing a crucible material for growing aluminum nitride crystals by a PVT method according to the present embodiment, SEM pictures of the prepared crucible material for growing aluminum nitride crystals by the PVT method are shown in FIGS. 1 and 2, FIG. 1 is a SEM picture of the crucible material for growing aluminum nitride crystals by the PVT method after being used at 2100 ℃ for 50 hours, FIG. 2 is a SEM picture of the crucible material for growing aluminum nitride crystals by the PVT method after being used at 2100 ℃ for 300 hours, FIGS. 3 and 4 are SEM pictures of a pure tantalum carbide crucible material of a comparative example, FIG. 3 is a SEM picture of the tantalum carbide crucible material after being used at 2100 ℃ for 50 hours, FIG. 4 is a SEM picture of the tantalum carbide crucible material after being used at 2100 ℃ for 300 hours, and it can be seen from the SEM pictures that grains of the pure TaC material are obviously increased after being used at 2100 ℃ for a period, and the grains are secondarily grown, which can cause cracking of the crucible after being heated for a long time; as can be seen from FIGS. 1 and 2, the crystal grain size of the crucible material for growing aluminum nitride crystals by the PVT method has little change and almost no change after being used at 2100 ℃ for a period of time.
In the preparation method of the crucible material for growing the PVT method aluminum nitride crystal, the service life of the crucible material for growing the PVT method aluminum nitride crystal is 400h.
The second embodiment is as follows:
a preparation method of crucible material for growing aluminum nitride crystal by PVT method comprises the following steps:
step 1, respectively weighing tantalum carbide powder, tungsten powder and yttrium oxide powder with certain mass according to parts by weight for later use;
step 2, adding the weighed tantalum carbide powder, tungsten powder and yttrium oxide powder into a three-dimensional vibration mixer, and uniformly mixing to obtain mixed powder for later use;
step 3, adding the mixed powder obtained in the step 2 into a polyvinyl chloride crucible mold, and performing cold isostatic pressing and compression molding to obtain a molded crucible material for later use;
step 4, placing the formed crucible material obtained in the step 3 into a hot-pressing sintering furnace, vacuumizing, and sintering under the pressure of 25MPa to obtain a sintered crucible material for later use;
step 5, machining and forming the sintered crucible material obtained in the step 4 by using a lathe or wire cutting to obtain a machined and formed crucible material for later use;
and 6, placing the crucible material processed and formed in the step 5 into a vacuum sintering furnace, vacuumizing, and sintering to obtain the crucible material for growing the aluminum nitride crystal by the PVT method.
In the preparation method of the crucible material for growing the aluminum nitride crystal by the PVT method according to the embodiment, in step 1, the weight part of the tantalum carbide powder is 100 parts, the weight part of the tungsten powder is 1 part, and the weight part of the yttrium oxide powder is 0.5 part.
In the preparation method of the crucible material for growing the aluminum nitride crystal by the PVT method, the particle size of the tantalum carbide powder in the step 1 is 1.0 μm, the purity is 99.999%, and the particle size of the tungsten powder is 0.5 μm, and the purity is 99.999%.
In the method for preparing a crucible material for growing aluminum nitride crystals by a PVT method according to this embodiment, the mixing time in step 2 is 12 hours.
In the preparation method of the crucible material for growing the aluminum nitride crystal by the PVT method in the embodiment, the average cold isostatic pressing pressure in the step 3 is 300MPa, and the pressing time is 10min.
In the preparation method of the crucible material for PVT method aluminum nitride crystal growth, the sintering treatment in the step 4 is a step-by-step sintering treatment, the temperature is firstly increased to 1200 ℃ at the heating rate of 3 ℃/min, then heated to 1950 ℃ at the heating rate of 1 ℃/min, then kept for 2h, then reduced to 1250 ℃ at the cooling rate of 0.5 ℃/min, kept for 2h, and then reduced to room temperature at the cooling rate of 2.5 ℃/min.
In the preparation method of the crucible material for growing the aluminum nitride crystal by the PVT method in the embodiment, in the step 6, the temperature is increased to 2000 ℃ at the heating rate of 1 ℃/min by sintering treatment, then the temperature is kept for 3 hours, and then the temperature is reduced to the room temperature at the cooling rate of 0.5 ℃/min.
In the preparation method of the crucible material for growing the PVT method aluminum nitride crystal, the service life of the crucible material for growing the PVT method aluminum nitride crystal is 390h.
The third concrete implementation mode:
a preparation method of crucible material for growing aluminum nitride crystal by PVT method comprises the following steps:
step 1, respectively weighing tantalum carbide powder, tungsten powder and yttrium oxide powder with certain mass according to parts by weight for later use;
step 2, adding the weighed tantalum carbide powder, tungsten powder and yttrium oxide powder into a three-dimensional vibration mixer, and uniformly mixing to obtain mixed powder for later use;
step 3, adding the mixed powder obtained in the step 2 into a polyvinyl chloride crucible mold, and performing cold isostatic pressing and compression molding to obtain a molded crucible material for later use;
step 4, placing the formed crucible material obtained in the step 3 into a hot-pressing sintering furnace, vacuumizing, and sintering under the pressure of 30MPa to obtain a sintered crucible material for later use;
step 5, machining and forming the sintered crucible material obtained in the step 4 by using a lathe or wire cutting to obtain a machined and formed crucible material for later use;
and 6, placing the crucible material processed and molded in the step 5 into a vacuum sintering furnace, vacuumizing, and sintering to obtain the crucible material for growing the aluminum nitride crystal by the PVT method.
In the preparation method of the crucible material for growing the aluminum nitride crystal by the PVT method according to the embodiment, in step 1, the weight parts of the tantalum carbide powder are 100 parts, the weight parts of the tungsten powder are 5 parts, and the weight parts of the yttrium oxide powder are 0.5 part.
In the method for preparing a crucible material for growing aluminum nitride crystals by a PVT method according to the present embodiment, the particle size of the tantalum carbide powder in step 1 is 1.0 μm, the purity is 99.9999%, and the particle size of the tungsten powder is 1.0 μm, and the purity is 99.9999%.
In the method for preparing the crucible material for growing the aluminum nitride crystal by the PVT method according to the embodiment, the mixing time in the step 2 is 15 hours.
In the preparation method of the crucible material for growing the aluminum nitride crystal by the PVT method, the average cold isostatic pressing pressure in the step 3 is 200MPa, and the pressing time is 20min.
In the preparation method of the crucible material for PVT method aluminum nitride crystal growth, the sintering treatment in the step 4 is a step-by-step sintering treatment, the temperature is firstly increased to 1100 ℃ at the heating rate of 3 ℃/min, then heated to 1900 ℃ at the heating rate of 1 ℃/min, then kept for 8h, then reduced to 1250 ℃ at the cooling rate of 0.5 ℃/min, kept for 2h, and then reduced to room temperature at the cooling rate of 2.5 ℃/min.
In the preparation method of the crucible material for growing the aluminum nitride crystal by the PVT method in the embodiment, in the step 6, the temperature is increased to 2000 ℃ at the heating rate of 1 ℃/min by sintering treatment, then the temperature is kept for 8 hours, and then the temperature is reduced to the room temperature at the cooling rate of 0.5 ℃/min.
In the preparation method of the crucible material for growing the PVT method aluminum nitride crystal, the service life of the crucible material for growing the PVT method aluminum nitride crystal is 400h.
The fourth concrete implementation mode is as follows:
a preparation method of crucible material for growing aluminum nitride crystal by PVT method comprises the following steps:
step 1, respectively weighing tantalum carbide powder, tungsten powder and yttrium oxide powder with certain mass according to parts by weight for later use;
step 2, adding the weighed tantalum carbide powder, tungsten powder and yttrium oxide powder into a three-dimensional vibration mixer, and uniformly mixing to obtain mixed powder for later use;
step 3, adding the mixed powder obtained in the step 2 into a polyvinyl chloride crucible mold, and performing cold isostatic pressing and compression molding to obtain a molded crucible material for later use;
step 4, placing the formed crucible material obtained in the step 3 into a hot-pressing sintering furnace, vacuumizing, and sintering under the pressure of 20MPa to obtain a sintered crucible material for later use;
step 5, machining and forming the sintered crucible material obtained in the step 4 by using a lathe or wire cutting to obtain a machined and formed crucible material for later use;
and 6, placing the crucible material processed and molded in the step 5 into a vacuum sintering furnace, vacuumizing, and sintering to obtain the crucible material for growing the aluminum nitride crystal by the PVT method.
In the preparation method of the crucible material for growing the aluminum nitride crystal by the PVT method according to the embodiment, in step 1, the weight part of the tantalum carbide powder is 100 parts, the weight part of the tungsten powder is 1 part, and the weight part of the yttrium oxide powder is 0.1 part.
In the method for preparing a crucible material for growing aluminum nitride crystals by a PVT method according to the present embodiment, the particle size of the tantalum carbide powder in step 1 is 0.9 μm, the purity is 99.999%, and the particle size of the tungsten powder is 0.5 μm, and the purity is 99.999%.
In the preparation method of the crucible material for growing the aluminum nitride crystal by the PVT method according to the embodiment, the mixing time in the step 2 is 10 hours.
In the preparation method of the crucible material for growing the aluminum nitride crystal by the PVT method, the average cold isostatic pressing pressure in the step 3 is 200MPa, and the pressing time is 10min.
In the preparation method of the crucible material for PVT method aluminum nitride crystal growth, the sintering treatment in the step 4 is a step-by-step sintering treatment, the temperature is firstly increased to 1100 ℃ at the heating rate of 3 ℃/min, then heated to 1950 ℃ at the heating rate of 1 ℃/min, then kept for 2h, then reduced to 1250 ℃ at the cooling rate of 0.5 ℃/min, kept for 2h, and then reduced to room temperature at the cooling rate of 2.5 ℃/min.
In the preparation method of the crucible material for growing the aluminum nitride crystal by the PVT method in the embodiment, in the step 6, the temperature is increased to 2000 ℃ at the heating rate of 1 ℃/min by sintering treatment, then the temperature is kept for 3 hours, and then the temperature is reduced to the room temperature at the cooling rate of 0.5 ℃/min.
In the preparation method of the crucible material for growing the PVT method aluminum nitride crystal, the service life of the crucible material for growing the PVT method aluminum nitride crystal is 400h.
According to the preparation method of the crucible material for PVT method aluminum nitride crystal growth, the defect density of the prepared crucible material for PVT method aluminum nitride crystal growth is reduced, the phenomenon of abnormal growth of TaC crystal grains at high temperature is eliminated, the service life of the crucible is prolonged, and the problem of thermal mismatch between the substrate and the crystal is reduced.
Claims (4)
1. A preparation method of crucible material for PVT method aluminum nitride crystal growth is characterized in that: the method comprises the following steps:
step 1, respectively weighing tantalum carbide powder, tungsten powder and yttrium oxide powder with certain mass according to parts by weight for later use;
step 2, adding the weighed tantalum carbide powder, tungsten powder and yttrium oxide powder into a three-dimensional vibration mixer, and uniformly mixing to obtain mixed powder for later use;
step 3, adding the mixed powder obtained in the step 2 into a polyvinyl chloride crucible mold, and performing cold isostatic pressing and compression molding to obtain a molded crucible material for later use;
step 4, placing the formed crucible material obtained in the step 3 into a hot-pressing sintering furnace, vacuumizing, and sintering under the pressure of 20-30 MPa to obtain a sintered crucible material for later use;
step 5, machining and forming the sintered crucible material obtained in the step 4 by using a lathe or wire cutting to obtain a machined and formed crucible material for later use;
step 6, placing the crucible material processed and molded in the step 5 into a vacuum sintering furnace, vacuumizing, and sintering to obtain the crucible material for growing the aluminum nitride crystal by the PVT method;
wherein the weight portion of the tantalum carbide powder in the step 1 is 100, the weight portion of the tungsten powder is 1-5, and the weight portion of the yttrium oxide powder is 0.1-0.5;
the sintering treatment in the step 4 is step-by-step sintering treatment, namely, firstly, the temperature is increased to 1100-1200 ℃ at the heating rate of 3 ℃/min, then the temperature is heated to 1800-1950 ℃ at the heating rate of 1 ℃/min, then the temperature is kept for 2-8 h, then the temperature is reduced to 1250 ℃ at the cooling rate of 0.5 ℃/min, and the temperature is reduced to room temperature at the cooling rate of 2.5 ℃/min after the temperature is kept for 2 h;
in the step 6, the temperature is increased to 2000 ℃ by sintering treatment at the temperature increasing rate of 1 ℃/min, then the temperature is kept for 3-8 h, and then the temperature is reduced to the room temperature at the temperature reducing rate of 0.5 ℃/min.
2. The method for preparing a crucible material for growing aluminum nitride crystals by the PVT method according to claim 1, wherein the crucible material comprises: the particle size of the tantalum carbide powder in the step 1 is 0.9-1.0 μm, the purity is 99.999-99.9999%, the particle size of the tungsten powder is 0.5-1.0 μm, and the purity is 99.999-99.9999%.
3. The method for preparing a crucible material for growing aluminum nitride crystals by the PVT method according to claim 1, wherein the crucible material comprises: the mixing time in the step 2 is 10 to 15 hours.
4. The method for preparing a crucible material for growing aluminum nitride crystals by the PVT method according to claim 1, wherein the crucible material comprises: in the step 3, the average pressure of the cold isostatic pressing is 200-300 MPa, and the pressing time is 10-20 min.
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