CN110015648B - High-purity aluminum nitride powder and aluminum nitride powder purification method - Google Patents
High-purity aluminum nitride powder and aluminum nitride powder purification method Download PDFInfo
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Abstract
The invention relates to high-purity aluminum nitride powder and a method for purifying the aluminum nitride powder. Carrying out high-temperature gas washing treatment on a synthesis cavity in which the mixed powder of the Al powder and the AlN powder is positioned by using reducing gas, and removing oxygen in the synthesis cavity; removing hydroxide in the mixed powder impurities at a first purification temperature in a vacuum state, removing carbon in the mixed powder impurities at a second purification temperature, and removing alumina in the mixed powder impurities by using the Al steam at a third purification temperature. The purification method is simple, the decomposition of AlN powder in the purification process is effectively inhibited and the loss of raw materials is reduced by reasonably designing the impurity removal sequence and corresponding purification steps and adding Al powder, and the carbon content of the aluminum nitride powder obtained by the method is 42PPM, the oxygen content is 220PPM and the purity is high by testing through a high-frequency combustion infrared absorption method and an inert gas pulse infrared thermal conductivity method.
Description
Technical Field
The invention relates to aluminum nitride preparation, in particular to high-purity aluminum nitride powder and a method for purifying the aluminum nitride powder.
Background
The semiconductor material and the synthesis technology are the cornerstones of the development of modern information technology, the first and second semiconductor materials represented by silicon (Si) and gallium arsenide (GaAs) in the 20 th century promote the rapid development of electronic and photoelectric technologies, and the third generation semiconductor material represented by aluminum nitride (AlN), silicon carbide (SiC) and gallium nitride (GaN) makes up the intrinsic performance deficiencies of the first and second semiconductor materials with higher requirements on the material performance, and greatly promotes the development of the semiconductor industry.
AlN has a direct forbidden band width of 6.2eV and a large spectral band width, and the luminescent waveband of the AlN can be as deep as 200nm, so that the AlN is an important blue light and purple light luminescent material; the melting point is high, and the theoretical calculation value is 2800 ℃; in addition, the material has good chemical stability, high breakdown field strength of 11.7MV/cm, low dielectric constant and excellent heat conduction performance, can be widely applied to electronic materials of high-temperature, high-voltage and high-frequency high-power electrical appliances, and the performance comparison of the first-generation and second-generation semiconductor materials is shown in Table 1.
Table 1: comparison of semiconductor Material Properties
More importantly, compared with Si, sapphire and SiC, AlN is an ideal substrate for growing III-group nitride epitaxial layers and device structures, and has the advantages that: the crystal lattice mismatch with GaN is only 2.4 percent, and the thermal mismatch is almost 0; the crystal structure is the same, and no layer fault layer appears; chemically stable and less contaminating the substrate without the presence of other elements. Table 2 shows the matching of a portion of the semiconductor to GaN.
Table 2: lattice and thermal matching of semiconductor and GaN
| As a GaN substrate | Si | Al2O3 | SiC | AlN |
| Lattice mismatch ratio | 17％ | 13.8％ | 3.4％ | 2.4％ |
| Heat loss ratio | 56％ | 33.9％ | 25％ | 0 |
At present, two methods for synthesizing aluminum nitride are mainly used, one method is gas phase physical transport (PVT), the other method is Hydride Vapor Phase Epitaxy (HVPE), and according to different synthesis principles, the HVPE method has low synthesis temperature but slow growth speed and is suitable for film growth; the PVT method has the disadvantage of high synthesis temperature, but high synthesis speed, so the method is suitable for crystal growth. The PVT method for crystal growth is a process of crystal growth in a low-temperature region through sublimation and decomposition of AlN powder in a high-temperature region, in order to solve the problems that carbon and oxygen impurity elements brought by powder in the growth process affect the performance of crystals, such as ultraviolet transmittance, heat conductivity, high pressure resistance and the like, and even aggregation of a large amount of impurity elements can cause crystal cracking and the like, the impurity removal treatment of raw material powder is needed, the existing powder impurity removal treatment method is to put the powder into a high-temperature-resistant crucible, then remove impurity substances in the powder through high-temperature calcination treatment, form irregular cylindrical powder after impurity removal and ceramic or even crystallize the powder, and cylindric structure is unfavorable for the inside impurity of block to get rid of, and the high rigidity of porcelainization brings huge difficulty in the broken grinding process in later stage, causes powder transition loss, adopts mechanical breakage, causes the secondary pollution of raw materials again very easily. The above problems are urgently needed to be solved.
Disclosure of Invention
In order to solve the above-mentioned problems, an object of the present invention is to provide a high-purity aluminum nitride powder and a method for purifying an aluminum nitride powder.
According to one aspect of the present invention, there is provided a method for purifying aluminum nitride powder, comprising the steps of:
carrying out high-temperature gas washing treatment on a synthesis cavity in which the mixed powder of the Al powder and the AlN powder is positioned by using reducing gas, and removing oxygen in the synthesis cavity;
purifying the mixed powder by aluminum nitride powder under vacuum state, wherein,
removing hydroxide in the mixed powder impurities at a first purification temperature,
removing carbon in the mixed powder impurities at a second purification temperature,
and introducing high-purity nitrogen at a third purification temperature, forming Al steam from the Al powder in the mixed powder, removing alumina in impurities in the mixed powder by using the Al steam, cooling, and crushing and grinding under the protection of high-purity inert gas to obtain the high-purity aluminum nitride powder.
Further, the molar ratio of the Al powder to the AlN powder is 0.1-0.5: 1. A small amount of high-purity Al powder is added into the AlN powder, so that the transitional decomposition of the AlN powder in high-temperature purification can be effectively reduced, and the decomposition rate of impurity substances in the AlN powder is improved. The proportion of the Al powder and the AlN powder is proved by a large number of experiments that the effect of the Al powder is best when the molar ratio of the Al powder to the AlN powder is 0.1-0.5: 1.
And the mixed powder is subjected to cold press molding under the protection of high-purity inert gas and then is placed in the synthesis cavity. The mixed powder is cold-pressed and molded into a cylinder shape through a die, so that the powder can be uniformly calcined at high temperature, manual crushing and grinding are facilitated, and secondary pollution caused by mechanical crushing and grinding is reduced.
And the reducing gas is filled into the synthesis cavity when the synthesis cavity is in a vacuum state.
The vacuum degree in the vacuum state is less than 1 multiplied by 10-4Pa。
The reducing gas is a mixed gas of hydrogen and nitrogen, wherein the hydrogen accounts for 0.5-5% of the total volume.
The temperature of the high-temperature air washing treatment is 200-400 ℃.
The first purification temperature is 800-1000 ℃, the second purification temperature is 1700-1800 ℃, and the third purification temperature is 1900-2200 ℃.
In the third purification stage, charging high purity nitrogen gas, reducing pressure to 1000 deg.C at a temperature lowering speed of less than 10 deg.C/min, and vacuumizing to 1 × 10-4Pa below, until the temperature is reduced to roomAnd (4) warming.
According to another aspect of the invention, high-purity aluminum nitride powder is provided, and is prepared according to the aluminum nitride powder purification method.
Compared with the prior art, the invention has the following beneficial effects:
the high-purity aluminum nitride powder and the corresponding aluminum nitride powder purification method are simple in purification method, the decomposition of AlN powder in the purification process is effectively inhibited and the loss of raw materials is reduced through the reasonable design of the impurity removal sequence and the corresponding purification steps and the addition of Al powder, and the high-purity aluminum nitride powder obtained by the method is tested to have the carbon content of 42PPM, the oxygen content of 220PPM and high purity through a high-frequency combustion infrared absorption method and an inert gas pulse infrared thermal conductivity method.
Detailed Description
In order to better understand the technical scheme of the invention, the invention is further explained by combining the specific embodiments in the specification.
Example one
The aluminum nitride powder purification process of the embodiment is as follows:
s1, mixing high-purity Al powder (99.99%) and AlN powder uniformly according to a molar ratio of 0.1-0.5:1, then, cold-pressing and molding the mixed powder by adopting a tungsten mold (or aluminum) in an inert glove box according to the designed size proportion (the inner diameter of the crucible is phi 60mm and the height of the crucible is 60mm) of a high-temperature calcination crucible, filling the powder with better fluidity into a tungsten metal mold cavity, and performing cold-pressing cylindrical design on the powder under the molding pressure of 0.5-4MPa so as to ensure that the subsequent powder is uniformly calcined at high temperature, thereby being beneficial to manual crushing and grinding and reducing secondary pollution caused by mechanical crushing and grinding. The external diameter of the formed cylinder is less than 60mm, the internal diameter is more than 20mm, the ratio of the internal diameter to the external diameter is more than 1/3, and the height is 50-60mm (according to the size of the calcining crucible).
S2, placing the formed powder into a tungsten crucible, covering the tungsten crucible with a crucible cover, and filling high-purity nitrogen into the tungsten crucible at the moment. Then the crucible is put into a high temperature furnace and vacuumized to 1 x 10-4Less than Pa, then filling mixed gas of hydrogen and nitrogen, wherein the hydrogen accounts for 0.5-5% of the total volume, and the temperature is raised to 200-40%Keeping the gas in a circulating state at 0 ℃ for 1-2 hours, discharging oxygen in the synthesis cavity in the form of water vapor at the high temperature of 200-400 ℃ by filling mixed reducing gas of hydrogen and nitrogen, and performing high-temperature gas washing treatment on the cavity of the synthesis equipment, wherein the reaction process at the moment is as follows:
H2(g)+O2(g)＝H2O(g)
s3, vacuumizing to 1 × 10-4When the temperature is reduced to room temperature, the ultrahigh vacuum state is maintained, the temperature is increased to 800-1000 ℃, the heat preservation is carried out for 6-10 hours, as the AlN powder is in contact with the air and is easy to rapidly generate a hydroxide film (the main component is AlOOH), a corresponding process flow needs to be formulated according to the reaction of the AlOOH at high temperature, and the reaction process at the moment is as follows:
2AlOOH(s)＝Al2O3(s)+H2O(g)
s4, keeping the high vacuum state, raising the temperature to 1700-1800 ℃, and preserving the heat for 6-10 hours, wherein the reaction process at the moment is as follows:
Al2O3(s)+3C(s)＝2Al(g)+3CO(g)
Al2O3(s)+3C(s)＝Al2(g)+3CO(g)
Al2O3(s)+C(s)＝Al2O(g)+2CO(g)
Al2O3(s)+C(s)＝2AlO(g)+CO(g)
s5, raising the temperature to 1900-2200 ℃, introducing high-purity nitrogen, keeping the pressure at 80-120KPa, preserving the heat for 6-10 hours, inhibiting the decomposition of AlN at the moment under high pressure, reducing the loss of powder materials, and simultaneously reacting Al steam formed by metal Al at high temperature with alumina, wherein the reaction process at the moment is as follows:
Al2O3(s)+4Al(g)＝3Al2O(g)
s6, after the reaction is finished, reducing the temperature to 1000 ℃ at a cooling rate of less than 10 ℃/min, and then vacuumizing to 1 × 10- 4And Pa below, cooling to room temperature, filling high-purity nitrogen of 1atm, taking out the crucible, putting the crucible into an inert glove box, crushing and grinding, and detecting after the treatment is finished.
Example two
The aluminum nitride powder purification process of the embodiment is as follows:
s1, mixing high-purity Al powder (99.99%) and AlN powder uniformly according to a molar ratio of 0.1:1, then, cold-pressing and molding the mixed powder by adopting a tungsten mold (or aluminum) in an inert glove box according to the designed size proportion (the inner diameter of the crucible is phi 60mm and the height of the crucible is 60mm) of a high-temperature calcination crucible, filling the powder with better fluidity into a tungsten metal mold cavity, and performing cold-pressing cylindrical design on the powder under the molding pressure of 0.5-4MPa so as to ensure that the subsequent powder is uniformly calcined at high temperature, thereby being beneficial to manual crushing and grinding and reducing secondary pollution caused by mechanical crushing and grinding. The external diameter of the formed cylinder is less than 60mm, the internal diameter is more than 20mm, the ratio of the internal diameter to the external diameter is more than 1/3, and the height is 50-60mm (according to the size of the calcining crucible).
S2, placing the formed powder into a tungsten crucible, covering the tungsten crucible with a crucible cover, and filling high-purity nitrogen into the tungsten crucible at the moment. Then the crucible is put into a high temperature furnace and vacuumized to 1 x 10-4And (2) below Pa, then filling a mixed gas of hydrogen and nitrogen, wherein the hydrogen accounts for 0.5 percent of the total volume, raising the temperature to 400 ℃, keeping the gas in a circulating state, keeping the gas for 1-2 hours, discharging oxygen in the synthesis cavity in a form of water vapor at the high temperature of 400 ℃ by filling a mixed reducing gas of hydrogen and nitrogen, and performing high-temperature gas washing treatment on the cavity of the synthesis equipment, wherein the reaction process at the moment is as follows:
H2(g)+O2(g)＝H2O(g)
s3, vacuumizing to 1 × 10-4When the temperature is reduced to room temperature, the ultrahigh vacuum state is maintained, the temperature is increased to 800 ℃, the temperature is maintained for 10 hours, as AlN powder is in contact with air, a hydroxide film (the main component is AlOOH) is easily and rapidly generated, a corresponding process flow needs to be formulated according to the reaction of the AlOOH at high temperature, and the reaction process at the moment is as follows:
2AlOOH(s)＝Al2O3(s)+H2O(g)
s4, keeping the high vacuum state, raising the temperature to 1700 ℃, and preserving the heat for 10 hours, wherein the reaction process is as follows:
Al2O3(s)+3C(s)＝2Al(g)+3CO(g)
Al2O3(s)+3C(s)＝Al2(g)+3CO(g)
Al2O3(s)+C(s)＝Al2O(g)+2CO(g)
Al2O3(s)+C(s)＝2AlO(g)+CO(g)
s5, raising the temperature to 1900 ℃, introducing high-purity nitrogen, keeping the pressure at 80-120KPa, keeping the temperature for 10 hours, inhibiting the decomposition of AlN under high pressure, reducing the loss of powder, and simultaneously reacting Al steam formed by metal Al at high temperature with alumina, wherein the reaction process at the moment is as follows:
Al2O3(s)+4Al(g)＝3Al2O(g)
s6, after the reaction is finished, reducing the temperature to 1000 ℃ at a cooling rate of less than 10 ℃/min, and then vacuumizing to 1 × 10- 4And Pa below, cooling to room temperature, filling high-purity nitrogen of 1atm, taking out the crucible, putting the crucible into an inert glove box, crushing and grinding, and detecting after the treatment is finished.
EXAMPLE III
The aluminum nitride powder purification process of the embodiment is as follows:
s1, mixing high-purity Al powder (99.99%) and AlN powder uniformly according to a molar ratio of 0.5:1, then, cold-pressing and molding the mixed powder by adopting a tungsten mold (or aluminum) in an inert glove box according to the designed size proportion (the inner diameter of the crucible is phi 60mm and the height of the crucible is 60mm) of a high-temperature calcination crucible, filling the powder with better fluidity into a tungsten metal mold cavity, and performing cold-pressing cylindrical design on the powder under the molding pressure of 0.5-4MPa so as to ensure that the subsequent powder is uniformly calcined at high temperature, thereby being beneficial to manual crushing and grinding and reducing secondary pollution caused by mechanical crushing and grinding. The external diameter of the formed cylinder is less than 60mm, the internal diameter is more than 20mm, the ratio of the internal diameter to the external diameter is more than 1/3, and the height is 50-60mm (according to the size of the calcining crucible).
S2, placing the formed powder into a tungsten crucible, covering the tungsten crucible with a crucible cover, and filling high-purity nitrogen into the tungsten crucible at the moment. Then the crucible is put into a high temperature furnace and vacuumized to 1 x 10-4Less than Pa, filling mixed gas of hydrogen and nitrogen, wherein the hydrogen accounts for 5% of the total volume, and raising the temperature toKeeping the gas in a circulating state at 300 ℃, keeping the gas for 1-2 hours, discharging oxygen in a synthesis cavity in a form of water vapor at the high temperature of 300 ℃ by filling mixed reducing gas of hydrogen and nitrogen, and performing high-temperature gas washing treatment on the cavity of the synthesis equipment, wherein the reaction process at the moment is as follows:
H2(g)+O2(g)＝H2O(g)
s3, vacuumizing to 1 × 10-4When the temperature is reduced to room temperature, the ultrahigh vacuum state is maintained, the temperature is increased to 900 ℃, the heat preservation is carried out for 8 hours, as the AlN powder is in contact with the air, a hydroxide film (the main component is AlOOH) is easily and rapidly generated, a corresponding process flow needs to be formulated according to the reaction of the AlOOH at high temperature, and the reaction process at the moment is as follows:
2AlOOH(s)＝Al2O3(s)+H2O(g)
s4, keeping the high vacuum state, raising the temperature to 1800 ℃, and keeping the temperature for 6 hours, wherein the reaction process at the moment is as follows:
Al2O3(s)+3C(s)＝2Al(g)+3CO(g)
Al2O3(s)+3C(s)＝Al2(g)+3CO(g)
Al2O3(s)+C(s)＝Al2O(g)+2CO(g)
Al2O3(s)+C(s)＝2AlO(g)+CO(g)
s5, raising the temperature to 2200 ℃, introducing high-purity nitrogen, keeping the pressure at 80-90KPa, keeping the temperature for 6 hours, inhibiting the decomposition of AlN under high pressure, reducing the loss of powder, forming Al steam by metal Al at high temperature to react with alumina, and the reaction process at the moment is as follows:
Al2O3(s)+4Al(g)＝3Al2O(g)
s6, after the reaction is finished, reducing the temperature to 1000 ℃ at a cooling rate of less than 10 ℃/min, and then vacuumizing to 1 × 10- 4And Pa below, cooling to room temperature, filling high-purity nitrogen of 1atm, taking out the crucible, putting the crucible into an inert glove box, crushing and grinding, and detecting after the treatment is finished.
Example four
The aluminum nitride powder purification process of the embodiment is as follows:
s1, mixing high-purity Al powder (99.99%) and AlN powder uniformly according to a molar ratio of 0.1-0.5:1, then, cold-pressing and molding the mixed powder by adopting a tungsten mold (or aluminum) in an inert glove box according to the designed size proportion (the inner diameter of the crucible is phi 60mm and the height of the crucible is 60mm) of a high-temperature calcination crucible, filling the powder with better fluidity into a tungsten metal mold cavity, and performing cold-pressing cylindrical design on the powder under the molding pressure of 0.5-4MPa so as to ensure that the subsequent powder is uniformly calcined at high temperature, thereby being beneficial to manual crushing and grinding and reducing secondary pollution caused by mechanical crushing and grinding. The external diameter of the formed cylinder is less than 60mm, the internal diameter is more than 20mm, the ratio of the internal diameter to the external diameter is more than 1/3, and the height is 55mm (according to the size of the calcining crucible).
S2, placing the formed powder into a tungsten crucible, covering the tungsten crucible with a crucible cover, and filling high-purity nitrogen into the tungsten crucible at the moment. Then the crucible is put into a high temperature furnace and vacuumized to 1 x 10-4And (2) below Pa, then filling a mixed gas of hydrogen and nitrogen, wherein the hydrogen accounts for 3% of the total volume, the temperature is raised to 250 ℃, the gas is kept in a circulating state and is kept for 2 hours, removing oxygen in the synthesis cavity in a form of water vapor at the high temperature of 250 ℃ by filling a mixed reducing gas of hydrogen and nitrogen, and performing high-temperature gas washing treatment on the cavity of the synthesis equipment, wherein the reaction process at the moment is as follows:
H2(g)+O2(g)＝H2O(g)
s3, vacuumizing to 1 × 10-4When the temperature is reduced to room temperature, the ultrahigh vacuum state is maintained, the temperature is increased to 800 ℃, the temperature is maintained for 10 hours, as AlN powder is in contact with air, a hydroxide film (the main component is AlOOH) is easily and rapidly generated, a corresponding process flow needs to be formulated according to the reaction of the AlOOH at high temperature, and the reaction process at the moment is as follows:
2AlOOH(s)＝Al2O3(s)+H2O(g)
s4, keeping the high vacuum state, raising the temperature to 1700-1800 ℃, and preserving the heat for 6-10 hours, wherein the reaction process at the moment is as follows:
Al2O3(s)+3C(s)＝2Al(g)+3CO(g)
Al2O3(s)+3C(s)＝Al2(g)+3CO(g)
Al2O3(s)+C(s)＝Al2O(g)+2CO(g)
Al2O3(s)+C(s)＝2AlO(g)+CO(g)
s5, raising the temperature to 2000-2200 ℃, introducing high-purity nitrogen at the pressure of 110-120KPa, and preserving the heat for 7 hours, wherein the decomposition of AlN is inhibited at high pressure, the loss of powder is reduced, and meanwhile, Al steam formed by metal Al at high temperature reacts with alumina, and the reaction process at the moment is as follows:
Al2O3(s)+4Al(g)＝3Al2O(g)
s6, after the reaction is finished, reducing the temperature to 1000 ℃ at a cooling rate of less than 10 ℃/min, and then vacuumizing to 1 × 10- 4And Pa below, cooling to room temperature, filling high-purity nitrogen of 1atm, taking out the crucible, putting the crucible into an inert glove box, crushing and grinding, and detecting after the treatment is finished.
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.
Claims (8)
1. The method for purifying the aluminum nitride powder is characterized by comprising the following steps of:
carrying out cold pressing molding on the mixed powder of the Al powder and the AlN powder into a cylindrical shape under the protection of high-purity inert gas, then placing the cylindrical shape in a synthesis cavity, and carrying out high-temperature gas washing treatment on the synthesis cavity in which the mixed powder of the Al powder and the AlN powder is located by utilizing reducing gas for removing oxygen in the synthesis cavity;
purifying the mixed powder by aluminum nitride powder under vacuum state, wherein,
removing hydroxide in the mixed powder impurities at a first purification temperature,
removing carbon in the mixed powder impurities at a second purification temperature,
filling high-purity nitrogen at a third purification temperature, wherein the pressure is 80-120KPa, Al powder in the mixed powder forms Al steam, removing alumina in impurities of the mixed powder by using the Al steam, cooling, and manually crushing and grinding under the protection of high-purity inert gas to obtain high-purity aluminum nitride powder;
wherein the first purification temperature is 800-1000 ℃, the second purification temperature is 1700-1800 ℃, and the third purification temperature is 1900-2200 ℃.
2. The method of purifying an aluminum nitride powder according to claim 1, wherein the molar ratio of the Al powder to the AlN powder is 0.1 to 0.5: 1.
3. The method for purifying aluminum nitride powder according to claim 1, wherein the reducing gas is filled into the synthesis chamber in a state where the synthesis chamber is in a vacuum state.
4. The method of purifying an aluminum nitride powder according to any one of claims 1 to 3, wherein the degree of vacuum in a vacuum state is less than 1X 10-4Pa。
5. The method for purifying aluminum nitride powder as claimed in claim 1, wherein the reducing gas is a mixture of hydrogen and nitrogen, wherein the hydrogen is 0.5-5% of the total volume.
6. The method for purifying aluminum nitride powder as claimed in claim 1, wherein the temperature of the high-temperature gas washing treatment is 200-400 ℃.
7. The method of purifying aluminum nitride powder as claimed in claim 1, wherein the third purification stage is performed at a temperature of less than 10 ℃/miThe temperature reduction speed of n is reduced to 1000 ℃, and then the vacuum pumping is carried out until the temperature is 1 multiplied by 10-4Pa below until the temperature is reduced to room temperature.
8. A high-purity aluminum nitride powder, characterized by being produced by the method for purifying an aluminum nitride powder according to any one of claims 1 to 7.
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| CN108863366A (en) * | 2018-07-11 | 2018-11-23 | 无锡市惠诚石墨烯技术应用有限公司 | A method of high thermal conductivity aluminium nitride powder is prepared based on graphene |
| CN109183143A (en) * | 2018-10-15 | 2019-01-11 | 北京大学 | A method of AlN single crystal purity is improved using reducing gas |
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