CN111472045A - Aluminum nitride single crystal preparation method based on large-size seed crystals - Google Patents
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Abstract
The invention discloses a preparation method of an aluminum nitride single crystal based on large-size seed crystals, which comprises the steps of depositing the large-size seed crystal layer of the aluminum nitride by a magnetron sputtering method, and after AlN crystals with certain thickness grow on the sputtered AlN seed crystal layer, adjusting a temperature field to return to a normal growth state for continuous growth of AlN to obtain the large-size AlN single crystal. The seed crystal has a compact and flat surface, has no primary cracks, and is favorable for obtaining crack-free crystals by subsequent growth; the size of the seed crystal can reach more than 2 inches in the in-plane size, and different sizes can be customized according to the needs, so that the growth of AlN single crystals of 2 inches or more is met; and AlN sputtering effectively reduces the cost and improves the efficiency.
Description
Technical Field
The invention relates to the technical field of crystal growth, in particular to a method for preparing a large-size aluminum nitride (AlN) single crystal by a Physical Vapor Transport (PVT) method.
Background
Because the Water Authority on Mercury is implemented in 2020, the extensive and urgent need of replacing the traditional mercury-containing light source by the deep ultraviolet L ED is formed, the deep ultraviolet L ED can be used for medical sterilization, while the successive outbreak of new crown pneumonia epidemic situation can certainly promote the market scale to be further expanded, and the expectation on the AlN substrate for the performance of power devices and radio frequency electronic devices, and the AlN substrate becomes the hotspot of research in the semiconductor photoelectron field and is also the urgent strategic need of the state.
Currently, only the us HexaTech company has realized the largest 2-inch AlN single crystal substrate without macroscopic defects in the world in 2019 internationally, which is the highest level of AlN single crystal production, but 2-inch AlN substrate wafers have not yet been commercialized, are small in volume and high in price, and have no available AlN single crystal substrate in the domestic market due to strict ban on our country. The large-size AlN seed crystal or the replaceable seed crystal substrate is one of the key points of the technological breakthrough of the AlN single crystal substrate with the size of more than 2 inches.
The seed crystal scheme commonly used comprises two schemes: and the other is a diameter expansion technology of spontaneous nucleation, namely AlN crystals with good millimeter-grade quality are obtained in the spontaneous nucleation process, then small AlN crystals with spontaneous nucleation are taken as seed crystals, diameter expansion growth is carried out through a specially designed crucible, and large-size AlN crystals are obtained through multiple iterations. The biggest difficulty of the method is large size, theoretical calculation and practice find that in the diameter expansion technology, the inclination angle of the side wall of the seed crystal must be smaller than 22-27 degrees, the diameter expansion growth technology has low efficiency and high seed crystal cost, and the AlN crystal growth difficulty of more than 2 inches is large; and secondly, a PVT iteration technology of the SiC seed crystal is adopted, namely an AlN layer grows on the SiC substrate through heterogeneous PVT, and the AlN layer is used as the seed crystal to grow in an iteration mode for multiple times to obtain the AlN single crystal substrate with optimized quality. This method can be easily scaled up in size, but has the greatest problems of low single crystallinity, poor crystal quality, and accompanied by serious problems of cracking and low light transmittance. Obviously, the conventional technology at present has the problems of low efficiency and high cost, and is difficult to solve the problems existing in the growth of 2-inch seed crystals.
The AlN thin layer sputtering technology is widely applied to MOCVD growth of a nitride-based optoelectronic device structure. Researches show that the magnetron sputtering AlN thin film has the advantages of high density, preferred c-direction growth, any size, low cost and the like, and simultaneously has good seed crystal layer effect, the seed crystal effect of the AlN layer depends on the structure of the AlN layer more, and the orientation relation of the AlN layer and a substrate is not great. Based on the characteristics, a large-size seed crystal technology of directly sputtering an AlN layer on a metal cover of a crucible is provided, and a special PVT growth technology of two-section type positive temperature field relay is matched to obtain a large-size AlN crystal. The AlN/W sputtering or AlN/(Ta or TaC or Ta/TaC) sputtering composite seed crystal technology can reduce the difficulty of the AlN seed crystal technology, enlarge the size at will, avoid the technical difficulty of high-temperature seed crystal bonding, and has high practicability and industrialization value.
Disclosure of Invention
The invention provides a method for preparing an aluminum nitride single crystal based on large-size seed crystals, which is characterized in that an AlN large-size seed crystal layer is deposited by adopting a magnetron sputtering method, a special PVT growth method is adopted to prepare the aluminum nitride single crystal, and after AlN crystals with certain thickness are grown on the sputtered AlN seed crystal layer, a temperature field is adjusted to return to a normal long-time growth state for continuous growth, so that the large-size AlN single crystal is obtained, the cost is effectively reduced, and the efficiency is improved.
The preparation method is different from the core of the prior art, namely sputtering the large-size seed crystal layer of AlN and a special PVT growth method matched with the seed crystal layer, and specifically comprises the following steps:
and depositing an AlN large-size seed crystal layer on the surface of the polished crucible cover (made of one or more of tungsten W, tantalum Ta, tantalum carbide TaC and other materials used for PVT growth of AlN) by adopting a magnetron sputtering method to form the AlN composite substrate. On the surface of the composite substrate, a two-section type positive temperature field successive growth technology is adopted: the position of the crucible in the thermal field is moved or the power ratio of the multi-temperature area is changed, so that the purpose of lower temperature of the surface of the sputtering seed crystal and larger temperature difference inside the crucible in the temperature rising stage is achieved. Thus, the decomposition of the sputtering seed layer can be inhibited, and the source powder can be ensured to have high enough temperature and certain sublimation. After AlN crystals with a certain thickness grow on the sputtered AlN seed crystal layer, the temperature field is adjusted to return to a normal long-time growth state (realized by moving a crucible or changing the power ratio), and the large-size AlN single crystals are continuously grown.
The technical scheme provided by the invention is as follows:
a preparation method of aluminum nitride single crystal based on large-size seed crystal comprises the following steps: firstly, performing pretreatment such as mechanical polishing, chemical cleaning and the like on a crucible cover (the diameter of the crucible cover is more than 2 inches, the crucible cover is made of one or more of materials used for PVT growth of AlN, such as tungsten W, tantalum Ta, tantalum carbide TaC and the like, and the crucible cover is used as a substrate) of a selected crucible, wherein the surface roughness Ra is required to be less than 1.6 mu m; then, carrying out magnetron sputtering on the surface of the crucible cover to form an AlN thin film, and controlling the thickness of the AlN seed crystal layer to be more than 600nm by adopting a multi-time sputtering method to form a composite substrate; and finally, placing the composite substrate on a crucible, filling a proper amount of pre-sintered AlN powder into the crucible, and placing the whole crucible into PVT equipment for subsequent successive growth. The two-stage type positive temperature field technology is adopted in the successive growth: in the heating stage and the initial stage of starting growth, the surface temperature of the composite substrate is ensured to be less than 1900 ℃ by moving the position of the crucible in a thermal field or changing the power ratio of a plurality of temperature zones, and the composite substrate is grown for 10-60min at the lower temperature; then raising the temperature (by moving the position of the crucible in the thermal field or changing the power ratio of the multiple temperature zones), so that the surface temperature of the composite substrate is more than 2100 ℃, and the temperature rise time t is less than 10 min; finally, growing the AlN single crystal for a long time at a higher temperature of more than 2100 ℃.
The method specifically comprises the following steps:
1) substrate (crucible cover) selection:
growing AlN single crystal by PVT method, selecting crucible cover made of W, Ta, TaC and other materials as substrate, diameter more than 50mm, thickness more than 1mm, highly polishing, surface roughness Ra less than 1.6 μm;
2) substrate pretreatment:
soaking the substrate material in dilute hydrochloric acid for 5-10min (or other methods for removing pollutants and oxide layers), cleaning with deionized water, ultrasonic cleaning in acetone and alcohol for 10-30min, and vacuum preserving before sputtering;
3) and (3) sputtering an AlN film:
by utilizing a magnetron sputtering technology, using a high-purity Al source as a target material, firstly pre-sputtering in an argon atmosphere to remove a surface oxide layer and pollutants, then sputtering in a mixed atmosphere of nitrogen and argon at the temperature of 100-;
4) crystal growth:
placing the pre-sintered AlN powder in a crucible, placing the composite substrate and the crucible in a metal PVT growth furnace, pumping and ventilating, and heating in vacuum or nitrogen atmosphere. The two-stage type positive temperature field technology is adopted in the successive growth: in the heating stage and the initial stage of starting growth, the surface temperature of the composite substrate is ensured to be less than 1900 ℃ by moving the position of the crucible in a thermal field or changing the power ratio of a plurality of temperature zones, and the composite substrate is grown for 10-60min at the lower temperature; then, the surface temperature of the composite substrate is enabled to be more than 2100 ℃ by moving the position of the crucible in the thermal field or changing the power ratio of the multiple temperature zones, and the temperature rise time t is enabled to be less than 10 min; and finally, growing the AlN single crystal for a long time at a high temperature of more than 2100 ℃ for 4-96 hours.
Through the steps, the large-size AlN crystal is prepared.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method for preparing an aluminum nitride single crystal based on large-size seed crystals. Firstly, the surface of the seed crystal is compact and flat, has no primary cracks, and is beneficial to obtaining crack-free crystals by subsequent growth; secondly, the size of the seed crystal can reach more than 2 inches in the in-plane size, and the seed crystal can be customized to be larger or different sizes according to the needs, so that the growth of AlN single crystals of 2 inches and more is met; thirdly, compared with the traditional AlN seed crystal (spontaneous nucleation or SiC heteroepitaxy), the AlN sputtering effectively reduces the cost and improves the efficiency.
Drawings
FIG. 1 is a schematic view of a furnace body for growing AlN single crystals by a PVT method in an embodiment of the present invention:
wherein, 1 is a furnace body and a nitrogen environment; 2 is an air inlet; 3 is an air outlet; 4 is a crucible; 5 is a composite substrate; 6 is a high-temperature growth chamber; 7 is high-purity AlN source powder; 8 is a supporting base, and the height is adjustable; 9, a double heater (heating body) with adjustable power.
Detailed Description
The invention will be further described by way of examples, without in any way limiting the scope of the invention, with reference to the accompanying drawings.
FIG. 1 is a schematic view of a furnace body for growing an AlN single crystal by a PVT method in an embodiment of the present invention. The crucible 4 is internally provided with a reaction zone, the double heater 9 can provide the crucible with high temperature over 2000 ℃, a high temperature zone (a high temperature growth chamber 6) has certain temperature gradient distribution and can be maintained, the requirement of crystal growth temperature field distribution is met, meanwhile, the heater can adjust the power ratio, the supporting base 8 can be lifted, and the crucible 4 can realize the switching between high temperature difference and low temperature difference. The crucible 4 and the outer heating insulation area are not completely sealed, and air flow can pass through the gap. The dry pump and the molecular pump can be vacuumized and maintain a certain vacuum degree. When nitrogen is continuously introduced during growth, the vacuum pump works to replace the gas in the furnace and ensure the pressure stability. Within the high temperature growth chamber 6, the AlN source powder sublimes and AlN deposition occurs at the top composite substrate.
Example A W plate-sputtered AlN seed layer composite substrate for PVT growth
1) Substrate pretreatment:
soaking the highly polished W plate in dilute hydrochloric acid for 5-10min, cleaning with deionized water, ultrasonic cleaning in acetone and alcohol for 10-30min, and vacuum preserving before sputtering;
2) and (3) sputtering an AlN film:
by utilizing a magnetron sputtering technology, using a high-purity Al source as a target material, firstly pre-sputtering in an argon atmosphere to remove a surface oxide layer and pollutants, then sputtering in a mixed atmosphere of nitrogen and argon at the temperature of 100-;
3) placing a crucible:
sealing a tungsten crucible filled with sintered AlN source powder by using a composite substrate, placing the crucible in a metal furnace, and sealing the furnace body;
4) pressure maintaining and temperature rising:
the environment in the furnace body is pumped to vacuum (10)-4Pa), keeping vacuum or injecting certain nitrogen for pressure maintaining, starting temperature rise, and ensuring that the position of the crucible is highest in the temperature rise process to enable the position of the composite substrate to be always lower than 1900 ℃;
5) and (3) low-temperature growth:
after the temperature rise is finished, keeping the pressure at 200-1000 Torr, moving the crucible downwards, adjusting the power ratio, and ensuring that the temperature of the composite substrate is below 1900 ℃, the temperature of the source powder is high enough, and the growth time is 10-60 min;
6) high-temperature growth:
adjusting the power ratio to ensure that the surface temperature of the composite substrate is more than 2100 ℃, and the temperature rise time t is less than 10 min; and finally, growing the AlN single crystal for a long time at a high temperature of more than 2100 ℃ for 4-96 hours.
Example two TaC/Ta plate-sputtered AlN seed layer composite substrate for PVT growth
1) Carbonizing a Ta plate:
cleaning the Ta plate, and carbonizing the Ta plate at a high temperature of more than 2000 ℃ in a graphite furnace to form a compact TaC layer on the surface of the Ta plate;
2) substrate pretreatment:
soaking the TaC/Ta plate in dilute hydrochloric acid for 5-10min, cleaning with deionized water, sequentially performing ultrasonic cleaning in acetone and alcohol for 10-30min, and preserving in vacuum before sputtering;
3) and (3) sputtering an AlN film:
by utilizing a magnetron sputtering technology, using a high-purity Al source as a target material, firstly pre-sputtering in an argon atmosphere to remove a surface oxide layer and pollutants, then sputtering in a mixed atmosphere of nitrogen and argon at the temperature of 100-;
4) placing a crucible:
sealing a tungsten crucible filled with sintered AlN source powder by using a composite substrate, placing the crucible in a metal furnace, and sealing the furnace body;
5) pressure maintaining and temperature rising:
the environment in the furnace body is pumped to vacuum (10)-4Pa), keeping vacuum or injecting certain nitrogen for pressure maintaining, starting temperature rise, and ensuring that the position of the crucible is highest in the temperature rise process to enable the position of the composite substrate to be always lower than 1900 ℃;
6) and (3) low-temperature growth:
after the temperature rise is finished, keeping the pressure at 200-1000 Torr, moving the crucible downwards, adjusting the power ratio, and ensuring that the temperature of the composite substrate is below 1900 ℃, the temperature of the source powder is high enough, and the growth time is 10-60 min;
7) high-temperature growth:
adjusting the power ratio to ensure that the surface temperature of the composite substrate is more than 2100 ℃, and the temperature rise time t is less than 10 min; and finally, growing the AlN single crystal for a long time at a high temperature of more than 2100 ℃ for 4-96 hours.
It is noted that the disclosed embodiments are intended to aid in further understanding of the invention, but those skilled in the art will appreciate that: various substitutions and modifications are possible without departing from the spirit and scope of the invention and appended claims. Therefore, the invention should not be limited to the embodiments disclosed, but the scope of the invention is defined by the appended claims.
Claims (7)
1. A method for preparing aluminum nitride single crystals based on large-size seed crystals comprises the steps of depositing aluminum nitride large-size seed crystal layers by a magnetron sputtering method, growing AlN crystals with a certain thickness on the sputtered AlN seed crystal layers, adjusting a temperature field to return to a normal growth state for continuous growth of AlN, and obtaining large-size AlN single crystals; the method comprises the following steps:
firstly, selecting a crucible with the diameter of the crucible cover larger than 2 inches, and pretreating the crucible cover to ensure that the surface roughness Ra of the crucible cover is smaller than 1.6 mu m; the crucible cover is used as a substrate; the crucible cover as a substrate is made of a material for growing an AlN single crystal by the PVT method;
then, magnetron sputtering an AlN thin film on the surface of the crucible cover by adopting a magnetron sputtering method, and controlling the thickness of the AlN seed crystal layer to be more than 600nm by adopting a multi-time sputtering method to form a composite substrate;
finally, the composite substrate is placed on a crucible, pre-sintered AlN powder is filled in the crucible, and the whole crucible is placed in PVT equipment for subsequent successive crystal growth;
the two-stage type positive temperature field technology is adopted in the successive growth of the crystal: in the temperature rising stage and the initial stage of starting growth, the surface temperature of the composite substrate is less than 1900 ℃, and the composite substrate grows for 10-60min at the lower temperature; then raising the temperature to make the surface temperature of the composite substrate be greater than 2100 ℃, and the temperature rise time t is less than 10 min; long-term growth at higher temperatures >2100 ℃;
through the steps, the large-size AlN single crystal is prepared.
2. A large-size seed crystal-based aluminum nitride single crystal preparation method as claimed in claim 1, wherein the crucible cover as the substrate is made of one or more of tungsten W, tantalum Ta and tantalum carbide TaC; the diameter of the crucible cover is more than 50mm, and the thickness of the crucible cover is more than 1 mm.
3. A large-sized seed crystal-based aluminum nitride single crystal production method as set forth in claim 1, wherein the crucible cover is subjected to pretreatment including mechanical polishing and chemical cleaning pretreatment, to remove contaminants and an oxide layer, to cleaning, and to vacuum preservation before sputtering.
4. A method for preparing a large-sized seed crystal-based aluminum nitride single crystal as claimed in claim 3, wherein the substrate material is immersed in dilute hydrochloric acid for 5-10min to remove contaminants and an oxide layer, then washed with deionized water, and then ultrasonically cleaned in acetone and alcohol for 10-30 min.
5. The method for preparing the aluminum nitride single crystal based on the large-size seed crystal as claimed in claim 1, wherein the method for magnetron sputtering the AlN thin film comprises the following specific steps:
a magnetron sputtering technology is utilized, and a high-purity Al source is used as a target material;
firstly, pre-sputtering in an argon atmosphere to remove a surface oxide layer and pollutants;
then sputtering in the mixed atmosphere of nitrogen and argon at the temperature of 100-300 ℃;
after the sputtering is finished, cooling in an argon environment to obtain a c-surface AlN thin film with the thickness of 200-300nm at one time;
and (4) carrying out multiple times of sputtering to generate an AlN seed crystal layer with the thickness of more than 600nm so as to obtain the composite substrate.
6. A method for preparing a large-size seed crystal-based aluminum nitride single crystal as claimed in claim 1, wherein the subsequent successive growth of the crystal is carried out by loading pre-sintered AlN powder into a crucible, placing the composite substrate and the crucible in a metal PVT growth furnace, evacuating and ventilating, and heating in vacuum or nitrogen atmosphere.
7. A method for preparing an aluminum nitride single crystal based on a large-size seed crystal as claimed in claim 1, wherein a two-stage type normal temperature field technology is adopted in the successive growth, and specifically:
in the heating stage and the initial stage of starting growth, the surface temperature of the composite substrate is enabled to be less than 1900 ℃ by moving the position of the crucible in a thermal field or changing the power ratio of a multi-temperature zone, and the growth time is 10-60min at the lower temperature;
then, the surface temperature of the composite substrate is enabled to be more than 2100 ℃ by moving the position of the crucible in the thermal field or changing the power ratio of the multiple temperature zones, and the temperature rise time t is enabled to be less than 10 min;
and finally growing the AlN single crystal for a long time at a high temperature of more than 2100 ℃ for 4 to 96 hours.
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| CN113122928A (en) * | 2021-04-19 | 2021-07-16 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Seed crystal treatment method for reducing oxygen impurities and defects in aluminum nitride single crystal |
| CN115418713A (en) * | 2022-06-22 | 2022-12-02 | 山东大学 | Growth method for reducing growth stress of AlN crystal |
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| CN113122928A (en) * | 2021-04-19 | 2021-07-16 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Seed crystal treatment method for reducing oxygen impurities and defects in aluminum nitride single crystal |
| CN115418713A (en) * | 2022-06-22 | 2022-12-02 | 山东大学 | Growth method for reducing growth stress of AlN crystal |
| CN115418713B (en) * | 2022-06-22 | 2024-01-26 | 山东大学 | Growth method for reducing AlN crystal growth stress |
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