CN113044816A - Preparation method of porous aluminum nitride raw material for aluminum nitride crystal growth - Google Patents
Preparation method of porous aluminum nitride raw material for aluminum nitride crystal growth Download PDFInfo
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Abstract
The invention relates to a preparation method of a porous aluminum nitride raw material for aluminum nitride crystal growth, belonging to the technical field of aluminum nitride crystal preparation. In order to solve the problems of complex preparation process and high cost of the existing porous aluminum nitride raw material, the invention provides a preparation method of a porous aluminum nitride raw material for aluminum nitride crystal growth, which comprises the steps of slurry preparation, ball milling treatment, freeze-drying treatment, sintering and acid pickling treatment. The preparation method of the porous aluminum nitride provided by the invention has the advantages of simple process, low equipment requirement and low cost, and is more suitable for industrial production of aluminum nitride crystals. The invention enables the aperture of the porous aluminum nitride to be relatively controllable by accurately controlling the freeze-drying temperature, the aperture of the prepared porous aluminum nitride raw material is less than 30 mu m, and the aperture is not only beneficial to gas rising, but also can filter carbon particles and improve the crystal quality. The adhesive and the dispersant added in the preparation process can be completely removed in the sintering process, so that the high purity of the aluminum nitride raw material is ensured.
Description
Technical Field
The invention belongs to the technical field of aluminum nitride crystal preparation, and particularly relates to a preparation method of a porous aluminum nitride raw material for aluminum nitride crystal growth.
Background
Aluminum nitride is a good blue light ultraviolet luminescent material, and a continuous luminescent spectrum from red light to ultraviolet can be obtained by using a special growth mode such as doping, which means that full color display from infrared to ultraviolet can be realized, so the aluminum nitride becomes one of the best energy materials for manufacturing LEDs.
At present, the most common method for growing aluminum nitride crystals is Physical Vapor Transport (PVT), in which an aluminum nitride raw material is placed in a high-temperature region to sublimate into a vapor substance, and the vapor substance is transported from the surface of the raw material to a seed crystal in a low-temperature region to crystallize and grow the aluminum nitride crystal under the driving of a temperature gradient by controlling the temperature gradient of a growth chamber. Therefore, the quality of the aluminum nitride raw material is the key to growing high quality aluminum nitride crystals. The aluminum nitride raw material purified by simple sintering has compact texture, and is not beneficial to the volatilization of aluminum nitride and the growth of crystals.
The application number 202010743904.9 discloses a preparation method of a porous high-purity aluminum nitride raw material, which comprises the steps of preparing Mg-Al alloy by taking an aluminum metal block and a magnesium metal block as raw materials, grinding the Mg-Al alloy to obtain alloy powder, and then placing the alloy powder under nitrogen pressure to perform three steps of nitriding treatment, sintering and acid washing to obtain the porous high-purity aluminum nitride raw material. The preparation method disclosed by the application has the advantages of higher requirement on nitriding treatment conditions, complex process and high cost, and is not suitable for industrial production.
Disclosure of Invention
The invention provides a preparation method of a porous aluminum nitride raw material for aluminum nitride crystal growth, aiming at solving the problems of complex preparation process and high cost of the existing porous aluminum nitride raw material.
The technical scheme of the invention is as follows:
a preparation method of a porous aluminum nitride raw material for aluminum nitride crystal growth comprises the following steps:
step one, preparing slurry:
dissolving polyvinyl alcohol in deionized water, adding a dispersing agent, and uniformly stirring to obtain slurry;
step two, ball milling treatment:
adding aluminum nitride powder into the slurry obtained in the step one, uniformly stirring, and carrying out ball milling to obtain mixed slurry;
step three, freeze-drying treatment:
injecting the mixed slurry obtained in the step two into a mold, freezing and curing at-60 ℃, demolding, and carrying out sublimation drying at-60 ℃;
step four, sintering and acid washing treatment:
and sintering and acid washing the freeze-dried material obtained in the step three to obtain the porous aluminum nitride raw material.
Further, in the first step, the concentration of the adhesive in the slurry is 1-5 wt%, and the concentration of the dispersant is 1-5 wt%.
Furthermore, the adhesive is polyvinyl alcohol, agarose and sodium alginate, and the dispersing agent is HPMA, polyacrylamide and sodium stearate.
Further, in the second step, the aluminum nitride powder is subjected to hydrolysis-resistant pretreatment, and the specific method of the hydrolysis-resistant pretreatment is to immerse the aluminum nitride powder into Al (H) with the mass concentration of 1-6%2PO4)3Soaking the solution for 1-3 h.
Further, the mass volume ratio of the aluminum nitride powder to the slurry in the second step is 5g:1 mL-10 g:1 mL.
Further, the ball milling rotation speed of the ball milling treatment in the step two is 60-100 rpm, and the ball milling time is 12-24 hours.
Further, the processing time of the sublimation drying in the third step is 24-48 hours.
Further, the sintering treatment in the fourth step is to heat up to 1450 ℃ at a heating rate of 5 ℃/min and preserve heat for 2 h.
Further, in the step four, acid washing is carried out on the sintered material for 3-8 hours by using acid liquor at the temperature of 40-50 ℃, wherein the acid liquor is HF and HNO3Mixed acid prepared according to the volume ratio of 1: 2.
The invention has the beneficial effects that:
the preparation method of the porous aluminum nitride provided by the invention has a simple process, and the prepared porous aluminum nitride raw material is easier to volatilize in the crystal growth process, so that the utilization rate of the aluminum nitride raw material is improved, and the cost of the aluminum nitride crystal growth is reduced. The preparation method has low requirement on equipment and low cost, can prepare porous aluminum nitride raw materials with various shapes to adapt to different crucibles, and is more suitable for the industrial production of aluminum nitride crystals.
According to the invention, the porous aperture of the aluminum nitride raw material is relatively controllable by accurately controlling the freeze-drying temperature, and the average aperture of the prepared porous aluminum nitride raw material is smaller than 30 μm, so that the aperture is beneficial to the rising of gas in the crystal growth process, and carbon particles can be filtered, thereby improving the crystal quality. The porous aluminum nitride prepared by the method has thinner hole walls, so that the porous aluminum nitride raw material has certain mechanical strength, and the raw material is prevented from being easily damaged in the packaging and air-extracting process. The adhesive and the dispersant added in the preparation process can be completely removed in the sintering process, so that the high purity of the aluminum nitride raw material is ensured.
Drawings
FIG. 1 is a photograph showing the appearance of an aluminum nitride crystal prepared using the porous aluminum nitride prepared in example 3 as a starting material;
fig. 2 is a photograph showing the appearance of aluminum nitride crystals prepared using the aluminum nitride prepared in comparative example 1 as a raw material.
Detailed Description
The technical solutions of the present invention are further described below with reference to the following examples, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention. The process equipment or apparatus not specifically mentioned in the following examples are conventional in the art, and if not specifically mentioned, the raw materials and the like used in the examples of the present invention are commercially available; unless otherwise specified, the technical means used in the examples of the present invention are conventional means well known to those skilled in the art.
Example 1
The embodiment provides a preparation method of a porous aluminum nitride raw material for aluminum nitride crystal growth, which comprises the following steps:
step one, preparing slurry:
dissolving polyvinyl alcohol in deionized water, adding a dispersing agent, and uniformly stirring to obtain slurry, wherein the concentration of the adhesive in the slurry is 1-5 wt%, and the concentration of the dispersing agent is 1-5 wt%. In this example, the binder was polyvinyl alcohol and the dispersant was HPMA.
Step two, ball milling treatment:
adding the aluminum nitride powder into the slurry obtained in the step one according to the mass-volume ratio of 5g:1 mL-10 g:1mL of the aluminum nitride powder to the slurry, stirring for 2 hours, and carrying out ball milling for 12-24 hours at the ball milling rotating speed of 60-100 rpm to obtain mixed slurry;
step three, freeze-drying treatment:
injecting the mixed slurry obtained in the step two into a mold, freezing and curing at-60 ℃, demolding, and carrying out sublimation drying at-60 ℃ for 24-48 h;
step four, sintering and acid washing treatment:
heating the freeze-dried material obtained in the step three to 1450 ℃ at the heating rate of 5 ℃/min, preserving the heat for 2h for sintering treatment, and then placing the sintered material in HF and HNO by using acid liquor at the temperature of 40-50 DEG C3And (3) pickling in mixed acid prepared according to the volume ratio of 1:2 for 3-8 h, washing with deionized water for 3-5 times after pickling, and drying to obtain the porous aluminum nitride raw material.
Example 2
The embodiment provides a preparation method of a porous aluminum nitride raw material for aluminum nitride crystal growth, which comprises the following steps:
step one, preparing slurry:
dissolving polyvinyl alcohol in deionized water, adding a dispersing agent, and uniformly stirring to obtain slurry, wherein the concentration of the adhesive in the slurry is 1-5 wt%, and the concentration of the dispersing agent is 1-5 wt%. In this example, the binder was polyvinyl alcohol and the dispersant was HPMA.
Step two, ball milling treatment:
immersing aluminum nitride powder into Al (H) with the mass concentration of 1-6%2PO4)3Soaking the solution for 1-3 h for hydrolysis resistance pretreatment, then adding the pretreated aluminum nitride powder into the slurry obtained in the step one according to the mass-volume ratio of 5g to 1 mL-10 g to 1mL, stirring for 2h, and carrying out ball milling at the ball milling rotation speed of 60-100 rpm for 12-24 h to obtain mixed slurry;
step three, freeze-drying treatment:
injecting the mixed slurry obtained in the step two into a mold, freezing and curing at-60 ℃, demolding, and carrying out sublimation drying at-60 ℃ for 24-48 h;
step four, sintering and acid washing treatment:
heating the freeze-dried material obtained in the step three to 1450 ℃ at the heating rate of 5 ℃/min, preserving the heat for 2h for sintering treatment, and then placing the sintered material in HF and HNO by using acid liquor at the temperature of 40-50 DEG C3And (3) pickling in mixed acid prepared according to the volume ratio of 1:2 for 3-8 h, washing with deionized water for 3-5 times after pickling, and drying to obtain the porous aluminum nitride raw material.
Example 3
The embodiment provides a preparation method of a porous aluminum nitride raw material for aluminum nitride crystal growth, which comprises the following steps:
step one, preparing slurry:
slowly adding polyvinyl alcohol into deionized water, continuously stirring until the polyvinyl alcohol is completely dissolved, then adding HPMA, and stirring for 20min to obtain slurry with the polyvinyl alcohol concentration of 1 wt% and the HPMA concentration of 1.5 wt%;
step two, ball milling treatment:
immersing aluminum nitride powder into Al (H) with mass concentration of 1%2PO4)3Soaking the solution for 3 hours for hydrolysis resistance pretreatment, then adding the pretreated aluminum nitride powder into the slurry obtained in the step one according to the mass volume ratio of 5g to 1mL of the aluminum nitride powder to the slurry, stirring for 2 hours, and carrying out ball milling for 24 hours at the ball milling rotating speed of 60rpm to obtain mixed slurry; the ball milling can lead the powder to be dispersed more uniformly and can refine the particle size.
Step three, freeze-drying treatment:
injecting the mixed slurry obtained in the step two into a mold, freezing and curing at-60 ℃, demolding, and carrying out sublimation drying at-60 ℃ for 48 hours;
step four, sintering and acid washing treatment:
heating the freeze-dried material obtained in the step three to 1450 ℃ at the heating rate of 5 ℃/min, preserving the heat for 2h, and sintering, wherein the polyvinyl alcohol and the HPMA are decomposed in the sintering process, so that the purity of the aluminum nitride raw material is ensured; then placing the sintered material in HF and HNO by acid liquor at 40 DEG C3Pickling in mixed acid prepared according to the volume ratio of 1:2 for 8 hours, washing with deionized water for 3-5 times after pickling, and drying to obtain the final productHigh-purity porous aluminum nitride raw material with average pore diameter less than 30 mu m.
In the embodiment, the freeze-drying temperature is controlled at-60 ℃, the aperture of the obtained aluminum nitride raw material is smaller than 30 mu m, the porosity is improved, and the porous material is not only beneficial to the rise of gas in the crystal growth process, but also capable of filtering some carbon particles and improving the crystal quality. Meanwhile, the porous aluminum nitride hole wall is relatively reasonable at the temperature, so that the porous aluminum nitride raw material has certain mechanical strength, the compressive strength can reach 12MPa, and the raw material is prevented from being easily damaged in the packaging and air-exhausting process.
Example 4
The embodiment provides a preparation method of a porous aluminum nitride raw material for aluminum nitride crystal growth, which comprises the following steps:
step one, preparing slurry:
slowly adding polyvinyl alcohol into deionized water, continuously stirring until the polyvinyl alcohol is completely dissolved, then adding HPMA, and stirring for 20min to obtain slurry with the polyvinyl alcohol concentration of 2 wt% and the HPMA concentration of 2.5 wt%;
step two, ball milling treatment:
immersing the aluminum nitride powder body into Al (H) with the mass concentration of 2%2PO4)3Soaking the solution for 3 hours for hydrolysis resistance pretreatment, then adding the pretreated aluminum nitride powder into the slurry obtained in the step one according to the mass volume ratio of 6g to 1mL of the aluminum nitride powder to the slurry, stirring for 2 hours, and carrying out ball milling for 20 hours at the ball milling rotating speed of 70rpm to obtain mixed slurry;
step three, freeze-drying treatment:
injecting the mixed slurry obtained in the step two into a mold, freezing and curing at-60 ℃, demolding, and sublimation drying at-60 ℃ for 32 hours;
step four, sintering and acid washing treatment:
heating the freeze-dried material obtained in the step three to 1450 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 2h for sintering treatment, and then placing the sintered material in HF and HNO by using acid liquor at the temperature of 45 DEG C3Pickling in mixed acid prepared according to the volume ratio of 1:2 for 5 hours, washing with deionized water for 3-5 times after pickling, and drying to obtain the product with the average pore diameter less than 30 mum is high-purity porous aluminum nitride raw material.
Example 5
The embodiment provides a preparation method of a porous aluminum nitride raw material for aluminum nitride crystal growth, which comprises the following steps:
step one, preparing slurry:
slowly adding polyvinyl alcohol into deionized water, continuously stirring until the polyvinyl alcohol is completely dissolved, then adding HPMA, and stirring for 20min to obtain slurry with the polyvinyl alcohol concentration of 3 wt% and the HPMA concentration of 3.5 wt%;
step two, ball milling treatment:
immersing aluminum nitride powder into Al (H) with mass concentration of 3%2PO4)3Soaking the solution for 2 hours for hydrolysis resistance pretreatment, then adding the pretreated aluminum nitride powder into the slurry obtained in the step one according to the mass volume ratio of 7g to 1mL of the aluminum nitride powder to the slurry, stirring for 2 hours, and carrying out ball milling for 18 hours at the ball milling rotating speed of 80rpm to obtain mixed slurry;
step three, freeze-drying treatment:
injecting the mixed slurry obtained in the step two into a mold, freezing and curing at-60 ℃, demolding, and sublimation drying at-60 ℃ for 32 hours;
step four, sintering and acid washing treatment:
heating the freeze-dried material obtained in the step three to 1450 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 2h for sintering treatment, and then placing the sintered material in HF and HNO by using acid liquor at the temperature of 45 DEG C3And (3) pickling in mixed acid prepared according to the volume ratio of 1:2 for 5 hours, washing with deionized water for 3-5 times, and drying to obtain the high-purity porous aluminum nitride raw material with the average pore diameter less than 30 mu m.
Example 6
The embodiment provides a preparation method of a porous aluminum nitride raw material for aluminum nitride crystal growth, which comprises the following steps:
step one, preparing slurry:
slowly adding polyvinyl alcohol into deionized water, continuously stirring until the polyvinyl alcohol is completely dissolved, then adding HPMA (hydroxyethyl methacrylate) and stirring for 20min to obtain slurry with the polyvinyl alcohol concentration of 5 wt% and the HPMA concentration of 5 wt%;
step two, ball milling treatment:
immersing aluminum nitride powder into Al (H) with mass concentration of 6%2PO4)3Soaking the solution for 3 hours for hydrolysis resistance pretreatment, then adding the pretreated aluminum nitride powder into the slurry obtained in the step one according to the mass volume ratio of 10g to 1mL of the aluminum nitride powder to the slurry, stirring for 2 hours, and carrying out ball milling for 12 hours at the ball milling rotation speed of 100rpm to obtain mixed slurry;
step three, freeze-drying treatment:
injecting the mixed slurry obtained in the step two into a mold, freezing and curing at-60 ℃, demolding, and carrying out sublimation drying at-60 ℃ for 24 hours;
step four, sintering and acid washing treatment:
heating the freeze-dried material obtained in the step three to 1450 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 2h for sintering treatment, and then placing the sintered material in HF and HNO by using acid liquor at the temperature of 50 DEG C3And (3) pickling in mixed acid prepared according to the volume ratio of 1:2 for 3 hours, washing with deionized water for 3-5 times, and drying to obtain the high-purity porous aluminum nitride raw material with the average pore diameter less than 30 mu m.
Example 7
The embodiment provides a preparation method of a porous aluminum nitride raw material for aluminum nitride crystal growth, which comprises the following steps:
step one, preparing slurry:
slowly adding agarose into deionized water, continuously stirring until the agarose is completely dissolved, then adding polyacrylamide, and stirring for 20min to obtain a slurry with the agarose concentration of 1 wt% and the polyacrylamide concentration of 1.5 wt%;
step two, ball milling treatment:
immersing aluminum nitride powder into Al (H) with mass concentration of 1%2PO4)3Soaking the solution for 3 hours for hydrolysis resistance pretreatment, then adding the pretreated aluminum nitride powder into the slurry obtained in the step one according to the mass volume ratio of 5g to 1mL of the aluminum nitride powder to the slurry, stirring for 2 hours, and carrying out ball milling for 24 hours at the ball milling rotating speed of 60rpm to obtain mixed slurry; the ball milling can lead the powder to be dispersed more uniformly and can refine the particle size.
Step three, freeze-drying treatment:
injecting the mixed slurry obtained in the step two into a mold, freezing and curing at-60 ℃, demolding, and carrying out sublimation drying at-60 ℃ for 48 hours;
step four, sintering and acid washing treatment:
heating the freeze-dried material obtained in the step three to 1450 ℃ at the heating rate of 5 ℃/min, preserving the heat for 2h, and sintering, wherein agarose and polyacrylamide are decomposed in the sintering process, so that the purity of the aluminum nitride raw material is ensured; then placing the sintered material in HF and HNO by acid liquor at 40 DEG C3And (3) pickling the mixture acid prepared according to the volume ratio of 1:2 for 8 hours, washing the mixture acid for 3-5 times by using deionized water, and drying the washed mixture to obtain the high-purity porous aluminum nitride raw material with the average pore diameter less than 30 mu m.
Example 8
The embodiment provides a preparation method of a porous aluminum nitride raw material for aluminum nitride crystal growth, which comprises the following steps:
step one, preparing slurry:
slowly adding sodium alginate into deionized water, continuously stirring until the sodium alginate is completely dissolved, then adding sodium stearate, and stirring for 20min to obtain a slurry with the sodium alginate concentration of 1 wt% and the sodium stearate concentration of 1.5 wt%;
step two, ball milling treatment:
immersing aluminum nitride powder into Al (H) with mass concentration of 1%2PO4)3Soaking the solution for 3 hours for hydrolysis resistance pretreatment, then adding the pretreated aluminum nitride powder into the slurry obtained in the step one according to the mass volume ratio of 5g to 1mL of the aluminum nitride powder to the slurry, stirring for 2 hours, and carrying out ball milling for 24 hours at the ball milling rotating speed of 60rpm to obtain mixed slurry; the ball milling can lead the powder to be dispersed more uniformly and can refine the particle size.
Step three, freeze-drying treatment:
injecting the mixed slurry obtained in the step two into a mold, freezing and curing at-60 ℃, demolding, and carrying out sublimation drying at-60 ℃ for 48 hours;
step four, sintering and acid washing treatment:
heating the freeze-dried material obtained in the third step to 1450 ℃ at the heating rate of 5 ℃/min, preserving the heat for 2h, and sintering, wherein the sodium alginate and the sodium stearate are decomposed in the sintering process, so that the purity of the aluminum nitride raw material is ensured; then placing the sintered material in HF and HNO by acid liquor at 40 DEG C3And (3) pickling the mixture acid prepared according to the volume ratio of 1:2 for 8 hours, washing the mixture acid for 3-5 times by using deionized water, and drying the washed mixture to obtain the high-purity porous aluminum nitride raw material with the average pore diameter less than 30 mu m.
Comparative example 1
The comparative example provides a method for preparing a porous aluminum nitride raw material, comprising the following steps:
step one, preparing slurry:
comparative example
Slowly adding polyvinyl alcohol into deionized water, continuously stirring until the polyvinyl alcohol is completely dissolved, then adding HPMA, and stirring for 20min to obtain slurry with the polyvinyl alcohol concentration of 1 wt% and the HPMA concentration of 1.5 wt%;
step two, ball milling treatment:
immersing aluminum nitride powder into Al (H) with mass concentration of 1%2PO4)3Soaking the solution for 3 hours for hydrolysis resistance pretreatment, then adding the pretreated aluminum nitride powder into the slurry obtained in the step one according to the mass volume ratio of 5g to 1mL of the aluminum nitride powder to the slurry, stirring for 2 hours, and carrying out ball milling for 24 hours at the ball milling rotating speed of 60rpm to obtain mixed slurry;
step three, freeze-drying treatment:
injecting the mixed slurry obtained in the step two into a mold, freezing and curing at-10 ℃, demolding, and sublimation drying at-10 ℃ for 48 hours;
step four, sintering and acid washing treatment:
heating the freeze-dried material obtained in the step three to 1450 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 2h for sintering treatment, and then placing the sintered material in HF and HNO by using acid liquor at the temperature of 40 DEG C3And (3) pickling in mixed acid prepared according to the volume ratio of 1:2 for 8 hours, washing with deionized water for 3-5 times, and drying to obtain the porous aluminum nitride raw material with the average pore diameter of 66 mu m.
The porous aluminum nitride raw materials prepared in example 3 and comparative example 1 were used as raw materials, and aluminum nitride crystals were prepared by a conventional PVT method. FIG. 1 is a photograph showing the appearance of an aluminum nitride crystal prepared using the porous aluminum nitride prepared in example 3 as a starting material; fig. 2 is a photograph showing the appearance of aluminum nitride crystals prepared using the aluminum nitride prepared in comparative example 1 as a raw material. It can be seen from an inspection that the crystal surface in fig. 2 produced distinct channels, primarily due to the ingress of carbon particles during crystal growth. The surface of the crystal in fig. 1 has no obvious pore channel, because the average pore diameter of the porous aluminum nitride raw material prepared in example 3 is less than 30 μm, the porous aluminum nitride raw material can filter carbon particles, and the carbon particles are prevented from entering the crystal, so that the growth quality of the aluminum nitride crystal is further improved.
Claims (9)
1. A preparation method of a porous aluminum nitride raw material for aluminum nitride crystal growth is characterized by comprising the following steps:
step one, preparing slurry:
dissolving the adhesive in deionized water, adding a dispersant and uniformly stirring to obtain slurry;
step two, ball milling treatment:
adding aluminum nitride powder into the slurry obtained in the step one, uniformly stirring, and carrying out ball milling to obtain mixed slurry;
step three, freeze-drying treatment:
injecting the mixed slurry obtained in the step two into a mold, freezing and curing at-60 ℃, demolding, and carrying out sublimation drying at-60 ℃;
step four, sintering and acid washing treatment:
and sintering and acid washing the freeze-dried material obtained in the step three to obtain the porous aluminum nitride raw material.
2. The method for preparing a porous aluminum nitride raw material for aluminum nitride crystal growth according to claim 1, wherein the concentration of the binder in the slurry in the step one is 1 to 5 wt%, and the concentration of the dispersant is 1 to 5 wt%.
3. The method for preparing a porous aluminum nitride raw material for aluminum nitride crystal growth according to claim 1 or 2, wherein the binder is polyvinyl alcohol, agarose, or sodium alginate, and the dispersant is HPMA, polyallylamine, or sodium stearate.
4. The method for preparing a porous aluminum nitride raw material for aluminum nitride crystal growth according to claim 3, wherein the aluminum nitride powder in the second step is an aluminum nitride powder subjected to hydrolysis-resistant pretreatment by immersing the aluminum nitride powder in Al (H) with a mass concentration of 1-6%2PO4)3Soaking the solution for 1-3 h.
5. The method for preparing the porous aluminum nitride raw material for aluminum nitride crystal growth according to claim 4, wherein the mass-to-volume ratio of the aluminum nitride powder to the slurry in the second step is 5g:1 mL-10 g:1 mL.
6. The method for preparing the porous aluminum nitride raw material for aluminum nitride crystal growth according to claim 5, wherein the ball milling rotation speed of the ball milling treatment in the second step is 60-100 rpm, and the ball milling time is 12-24 h.
7. The method for preparing a porous aluminum nitride raw material for aluminum nitride crystal growth according to claim 6, wherein the sublimation drying treatment time of the third step is 24-48 hours.
8. The method for preparing a porous aluminum nitride raw material for aluminum nitride crystal growth according to claim 7, wherein the sintering treatment of the fourth step is carried out by raising the temperature to 1450 ℃ at a rate of 5 ℃/min for 2 hours.
9. The method for preparing a porous aluminum nitride raw material for aluminum nitride crystal growth according to claim 8, wherein the acid washing in the fourth step is performed by acid washing the sintered material with an acid solution at 40-50 ℃ for 3-8 h, wherein the acid solution is HF and HFHNO3Mixed acid prepared according to the volume ratio of 1: 2.
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