CN113308742A - Application of aluminum nitride single crystal material in piezoelectric material - Google Patents

Application of aluminum nitride single crystal material in piezoelectric material Download PDF

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CN113308742A
CN113308742A CN202110655187.9A CN202110655187A CN113308742A CN 113308742 A CN113308742 A CN 113308742A CN 202110655187 A CN202110655187 A CN 202110655187A CN 113308742 A CN113308742 A CN 113308742A
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single crystal
aluminum nitride
nitride single
crystal material
lithium aluminate
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陈晨龙
李俊谕
王俪霖
蔡文汉
孙姝婧
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Fujian Institute of Research on the Structure of Matter of CAS
Mindu Innovation Laboratory
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    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C30B29/403—AIII-nitrides
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/18—Epitaxial-layer growth characterised by the substrate

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Abstract

The application discloses an application of an aluminum nitride single crystal material in a piezoelectric material, wherein the aluminum nitride single crystal material is an aluminum nitride single crystal and/or an aluminum nitride single crystal film formed by communicating a nano hole with a nano wall. The aluminum nitride single crystal material has the characteristics of bulk crystal non-crystal boundary connection and nano material non-stress, only holes on the surface of the aluminum nitride single crystal material have no dislocation, and the aluminum nitride single crystal material has excellent piezoelectric performance and can be used as a high-quality piezoelectric material of an aluminum nitride-based device.

Description

Application of aluminum nitride single crystal material in piezoelectric material
Technical Field
The application relates to application of an aluminum nitride single crystal material in a piezoelectric material, wherein the aluminum nitride single crystal material is an aluminum nitride single crystal and/or an aluminum nitride single crystal film formed by communicating nano holes and nano walls.
Background
Aluminum nitride (AlN), which is one of the representative third-generation semiconductor materials, is receiving attention for its excellent properties as the material technology advances and develops. The aluminum nitride crystal material has the following advantages: 1) the forbidden band width is 6.2eV, and the material has direct band gap and is an important blue light and ultraviolet luminescent material; 2) the material has high thermal conductivity, high melting point, high resistivity, strong breakdown field and small dielectric coefficient, and is an excellent electronic material for high-temperature, high-frequency and high-power devices; 3) the aluminum nitride oriented along the c axis has very good piezoelectricity and high-speed propagation performance of surface acoustic wave, and is an excellent piezoelectric material for surface acoustic wave devices. The aluminum nitride has a low thermal expansion coefficient of about 4.35ppm/K, a high thermal conductivity of 320W/(m.K), and the thermal conductivity of the piezoelectric ceramic is generally 1.5-3.5W/(m.K), and has high thermal stability. In addition, the aluminum nitride crystal has a melting point of 2100 ℃, and can still maintain the piezoelectric effect under the condition of 1150 ℃, so the aluminum nitride is a high-temperature piezoelectric material with great prospect.
However, the difficulty of growing aluminum nitride single crystal material is high, so that not only the experimental process is complicated, but also the cost is high, thereby greatly limiting the development of aluminum nitride material. Up to now, nearly 50 years of effort has been made in all countries around the world for growing large-size aluminum nitride single crystal materials, wherein physical vapor deposition (PVT) is generally accepted as the only method for growing bulk aluminum nitride single crystal, but there are also problems of narrow growth window, high growth temperature, low crystal quality and the like.
Therefore, there is a need to provide a simpler method for preparing large-size aluminum nitride single crystal material to provide high-quality large-size piezoelectric material for aluminum nitride-based devices.
Disclosure of Invention
According to one aspect of the application, the application of the aluminum nitride single crystal material in the piezoelectric material is provided, the aluminum nitride single crystal material has the characteristics of bulk crystal non-grain boundary connection and nano material non-stress, only holes on the surface of the aluminum nitride single crystal material have no dislocation, the aluminum nitride single crystal material has excellent piezoelectric performance, and the aluminum nitride single crystal material is a high-quality piezoelectric material for an aluminum nitride-based device. The aluminum nitride single crystal material in the application has uniformly distributed nano holes and nano walls in the interior and on the surface, and has the characteristics of ordered crystal lattices of bulk crystals and disordered channels of nano materials.
The invention prepares porous aluminum nitride based on the crystal reconstruction principle, and obtains the high-quality aluminum nitride single crystal material with low stress and no cracking by regulating and controlling test parameters. The material has high-temperature piezoelectric property as other common aluminum nitride materials, and has nano holes inside, so that the material can play a role in stress release and dislocation digestion when being used as an aluminum nitride-based device substrate to grow other materials. In addition, the material has low synthesis cost, easy operation and easy repetition, can be prepared in large size, and provides high-quality large-size polar (0001) C surface and nonpolar components for aluminum nitride-based devices
Figure BDA0003113448610000025
M face and
Figure BDA0003113448610000026
the porous aluminum nitride single crystal substrate and template on the A surface solve the problem of high difficulty in aluminum nitride growth.
According to a first aspect of the application, an application of an aluminum nitride single crystal material in a piezoelectric material is provided, wherein the aluminum nitride single crystal material is an aluminum nitride single crystal and/or an aluminum nitride single crystal thin film formed by communicating nanopores and nanowalls.
Optionally, the size of the aluminum nitride single crystal is 0.1-25 cm;
the thickness of the aluminum nitride single crystal film is 10 nm-600 mu m.
Optionally, the size of the aluminum nitride single crystal thin film is 0.1-25 cm.
Optionally, the surface and the interior of the aluminum nitride single crystal material both contain pores with the pore diameter of 10-2000 nm;
the holes in the aluminum nitride single crystal material are three-dimensional communicating holes.
Optionally, the pores in the aluminum nitride single crystal material are in a creep shape.
Optionally, the surface of the aluminum nitride single crystal thin film is the (0001) plane of the aluminum nitride single crystal,
Figure BDA0003113448610000021
Figure BDA0003113448610000022
At least one side of;
the surface of the aluminum nitride single crystal is the (0001) plane of the aluminum nitride single crystal,
Figure BDA0003113448610000023
Flour,
Figure BDA0003113448610000024
At least one of the faces.
Optionally, the preparation method of the aluminum nitride single crystal material comprises the following steps:
and (2) dissociating the lithium aluminate single crystal material at the temperature of more than 500 ℃, volatilizing Li and O, carrying out contact reaction on aluminum decomposed from the surface of the lithium aluminate single crystal material and feed gas containing ammonia gas to carry out lattice reconstruction to form an aluminum nitride single crystal material, and completely converting the lithium aluminate single crystal material from the outside to the inside along with the reaction to obtain the aluminum nitride single crystal material.
Specifically, Li and O volatilized from the surface of the lithium aluminate single crystal material are volatilized in the form of ions.
Alternatively, the above surface decomposition means that more aluminum is exposed as lithium and oxygen volatilize.
Optionally, the method comprises: the lithium aluminate single crystal material is dissociated at high temperature, Li and O volatilize, Al decomposed on the surface of the lithium aluminate single crystal material is in contact reaction with feed gas containing ammonia gas, lattice reconstruction is carried out to form aluminum nitride, and the lithium aluminate crystal is completely converted from the surface to the inside along with the reaction process to obtain the aluminum nitride single crystal material.
Optionally, the size of the lithium aluminate single crystal material is 0.1-25 cm.
Optionally, the reaction pressure is 20 torr to 500 torr; the reaction temperature is 500-1300 ℃.
Preferably, the reaction pressure is 100-200 torr; the reaction temperature is 800-1300 ℃.
Optionally, the reaction time is 10min to 100 h.
Optionally, the feed gas containing ammonia further comprises nitrogen and hydrogen;
the flow rate of ammonia gas is recorded as a, and a is more than or equal to 0.05SLM and less than or equal to 4 SLM;
the flow rate of the nitrogen is recorded as b, and b is more than or equal to 0SLM and less than or equal to 5 SLM;
the flow rate of the hydrogen is recorded as c, and c is more than or equal to 0SLM and less than or equal to 5 SLM.
Optionally, the lithium aluminate single crystal material is contacted with a feed gas containing ammonia gas on at least one of the (100), (010), and (001) planes of the lithium aluminate single crystal material.
Optionally, the piezoelectric constant of the aluminum nitride single crystal material is 5-100 Pc/N.
In one embodiment, when the aluminum nitride single crystal material is an aluminum nitride single crystal thin film, the time for the contact reaction of the lithium aluminate single crystal material and the feed gas containing ammonia gas is 30min to 20 h. The length of the reaction time is positively correlated with the thickness of the novel aluminum nitride single crystal film, and the longer the contact reaction time is, the larger the thickness of the obtained novel aluminum nitride single crystal film is.
Preferably, when the aluminum nitride single crystal material is an aluminum nitride single crystal thin film, the lower limit of the time range of the contact reaction of the lithium aluminate single crystal material and the feed gas containing ammonia gas is selected from 10min, 20min, 30min, 1h, 2h, 3h, 4h or 5h, and the upper limit is selected from 20h, 18h, 15h or 10 h.
When the prepared aluminum nitride single crystal material is aluminum nitride single crystal, the contact reaction time is required to ensure that the lithium aluminate single crystal material is completely converted into the novel aluminum nitride single crystal material.
In one embodiment, when the aluminum nitride single crystal material is an aluminum nitride single crystal, the time for the contact reaction of the lithium aluminate single crystal material and the feed gas containing ammonia gas is 10 to 100 hours.
One skilled in the art can determine the appropriate contact reaction time based on the actual requirements and the size of the lithium aluminate single crystal material employed.
Preferably, when the aluminum nitride single crystal material is aluminum nitride single crystal, the lower limit of the time range of the contact reaction of the lithium aluminate single crystal material and the feed gas containing ammonia gas is selected from 24h, 36h or 48h, and the upper limit is selected from 100h, 96h, 84h, 72h or 60 h.
By adopting the method provided by the application, the crystal size of the obtained novel aluminum nitride single crystal is equal to that of the adopted lithium aluminate single crystal material. The skilled person can select the lithium aluminate single crystal material with proper size according to the actual requirement to obtain the required novel aluminum nitride single crystal.
Optionally, the lithium aluminate single crystal material is contacted with a feed gas containing ammonia gas on at least one of the (100), (010), and (001) planes of the lithium aluminate single crystal.
Optionally, the preparation method of the aluminum nitride single crystal material comprises the following steps:
(1) according to the experimental requirements, the parts of devices required by the experiment, such as a vacuum gauge, a pressure gauge, a ceramic tube with proper size and the like, are self-assembled.
(2) A piece of 1cm × 1cm (100) surface of a lithium aluminate single crystal substrate was placed in an ethanol solution, ultrasonic cleaning was performed for 15 minutes, and then cleaning was performed with deionized water and purging was performed with a nitrogen gun.
(3) Then putting the lithium aluminate single crystal substrate into a ceramic boat, putting the ceramic boat in a furnace body constant temperature area, closing a furnace cover, vacuumizing, filling a proper amount of nitrogen after vacuumizing to the limit, vacuumizing again until the pressure in the furnace body is 4.0 multiplied by 10-3Torr。
(4) And introducing raw material gas taking ammonia gas as main mixed gas to control the pressure in the furnace to the growth pressure. Heating to the growth temperature at the heating rate of 5 ℃/min, and keeping the temperature for 1-25 h. So that the lithium aluminate is fully mixed with the raw material gas, and a layer of white aluminum nitride single crystal grows on the substrate. And after the reaction is fully completed, introducing argon gas of 0.3slm, cooling to room temperature at the cooling rate of 5 ℃/min, and taking out the sample.
The application relates to a method for preparing aluminum nitride single crystal based on a vapor phase growth principle. The prepared aluminum nitride single crystal is a bulk crystal formed by communicating nano holes and nano walls, has the characteristics of no grain boundary connection and no stress of nano materials of the bulk crystal, has no dislocation in holes on the surface of a substrate, and is a high-quality homogeneous substrate of an aluminum nitride-based device.
In the present application, SLM is an abbreviation of Standard Litre Per Minute, and indicates a flow rate of 1L/min in a Standard state.
In the present application, the size of the single crystal refers to the distance between two points adjacent to each other on the plane having the largest area on one crystal.
The size of the single crystal thin film refers to the distance between two points adjacent to the farthest point on the surface with the largest area.
Benefits of the present application include, but are not limited to:
the application discloses application of an aluminum nitride single crystal material in a piezoelectric material, wherein the piezoelectric material is the aluminum nitride single crystal material with a special structure. The material can simplify the manufacturing process, reduce the difficulty of synthesizing the aluminum nitride crystal, and the prepared high-quality aluminum nitride can further reduce the dielectric constant, improve the dielectric property of the material, effectively improve the high-speed performance of a large-scale integrated circuit and improve the signal transmission rate. Therefore, the method has better application prospect in the fields of electronic packaging materials, electronic device substrate materials and the like.
Drawings
FIG. 1 is a scanning electron micrograph of a sample No. 1 polar (0002) C-face porous aluminum nitride single crystal thin film.
FIG. 2 is a scanning electron micrograph of a sample No. 1 polar (0002) C-face porous aluminum nitride single crystal thin film.
FIG. 3 shows the X-ray diffraction results of the polar (0002) C-plane porous aluminum nitride single-crystal thin film of sample No. 1.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
In the examples, lithium aluminate single crystal wafers were prepared according to the methods in the literature.
In the embodiment, the appearance of the sample is analyzed by using an SU-8010 scanning electron microscope.
In the examples, X-ray diffraction analysis of the samples was carried out using Miniflex 600, Cu K.alpha.Rigaku Corporation (Cu-K.alpha.1 radiation; operated at 40kV and 45 mA;
Figure BDA0003113448610000051
) A high resolution X-ray diffraction analyzer.
Example 1 preparation of sample # 1
Placing 5cm (100) surface lithium aluminate single crystal wafer in a ceramic boat, placing in a furnace body constant temperature region, closing a furnace cover, vacuumizing, introducing appropriate amount of nitrogen when the vacuum is exhausted to the limit, and vacuumizing again until the pressure in the furnace body is 4.0 × 10-3Torr, then introducing a raw material gas containing ammonia (the raw material gas consists of ammonia and nitrogen gas: ammonia 2SLM, nitrogen gas 0.5SLM) and heating the system to 1000 ℃, introducing a trace amount of H2(0.1slm) keeping the system pressure at 100 torr, after reacting for 1h, closing hydrogen, and cooling to room temperature to obtain a novel aluminum nitride single crystal film sample, wherein the thickness of the film is 150nm and is marked as sample No. 1.
Morphology characterization of sample # 1
The appearance of the sample No. 1 is characterized by adopting a scanning electron microscope, and the result shows that the surface of the sample No. 1 is provided with holes with uniformly distributed trepanning structures. The SEM spectrums are shown in figures 1 and 2.
Structural characterization of sample # 1
The sample No. 1 was structurally characterized by X-ray diffraction. Taking sample No. 1 as a typical representative, the XRD pattern is shown in FIG. 3, and only AlN (0002) and LiAlO are contained in sample No. 12(100) Of the signal of (1).
Examples 2 to 3
Preparation of the piezoelectric material: compared to example 1, the only difference is as shown in table 1:
TABLE 1 differences between the preparation methods of examples 2 to 3 and example 1
Raw materials/conditions/parameters Example 1(1#) Example 2(2#) Example 3(3#)
Flow rate of ammonia gas 2slm 0.05slm 4slm
Size of substrate 5cm 0.1cm 10cm
Constant temperature 1000℃ 500℃ 1300℃
Constant temperature time 1h 10min 18h
Constant temperature pressure 100Torr 20Torr 400Torr
Example 4 measurement of piezoelectric Properties
And (3) determining a sample: 1#
The determination method comprises the following steps: the samples were subjected to D33 testing by a piezo-responsive microscope (Dimension ICON).
Test results and analysis: the piezoelectric response test was performed on sample # 1. In the voltage range from-10V to +10V, the scanning area is 2 um' 2um, an experimental spectrogram shows that a butterfly curve with obvious 180-degree phase reversal and amplitude reversal exists, and the D33 value is calculated to be about 20pm/V, so that excellent piezoelectric performance is shown.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.

Claims (10)

1. The application of the aluminum nitride single crystal material in the piezoelectric material is characterized in that the aluminum nitride single crystal material is an aluminum nitride single crystal and/or an aluminum nitride single crystal film formed by communicating nano holes and nano walls.
2. The use according to claim 1, wherein the size of the aluminum nitride single crystal is 0.1 to 25 cm.
3. The use according to claim 1, wherein the surface and the interior of the aluminum nitride single crystal material both contain pores with a pore diameter of 10 to 2000 nm;
the holes in the aluminum nitride single crystal material are three-dimensional communicating holes.
4. The use according to claim 1, wherein the pores in the aluminum nitride single crystal material are vermicular.
5. The use according to claim 1, wherein the thickness of the aluminum nitride single crystal thin film is 10nm to 600 μm.
6. The use according to claim 1, wherein the surface of the aluminum nitride single crystal thin film is a (0001) plane of the aluminum nitride single crystal,
Figure FDA0003113448600000011
At least one of the faces;
the surface of the aluminum nitride single crystal is the (0001) plane of the aluminum nitride single crystal,
Figure FDA0003113448600000012
Flour,
Figure FDA0003113448600000013
At least one of the faces.
7. The application of claim 1, wherein the preparation method of the aluminum nitride single crystal material comprises the following steps:
and (2) dissociating the lithium aluminate single crystal material at the temperature of more than 500 ℃, volatilizing Li and O, carrying out contact reaction on aluminum decomposed from the surface of the lithium aluminate single crystal material and feed gas containing ammonia gas to carry out lattice reconstruction to form an aluminum nitride single crystal material, and completely converting the lithium aluminate single crystal material from the outside to the inside along with the reaction to obtain the aluminum nitride single crystal material.
8. The use of claim 7, wherein the reaction pressure is from 20 torr to 500 torr; the reaction temperature is 500-1300 ℃.
9. Use according to claim 7, wherein the reaction time is between 10min and 100 h.
10. The use of claim 7, wherein the feed gas containing ammonia further comprises nitrogen and hydrogen;
the flow rate of ammonia gas is recorded as a, and a is more than or equal to 0.05SLM and less than or equal to 4 SLM;
the flow rate of the nitrogen is recorded as b, and b is more than or equal to 0SLM and less than or equal to 5 SLM;
the flow of the hydrogen is recorded as c, and c is more than or equal to 0SLM and less than or equal to 5 SLM;
preferably, the lithium aluminate single crystal material is contacted with the raw material gas containing ammonia gas by at least one surface of (100), (010), (001) surfaces of the lithium aluminate single crystal material;
preferably, the piezoelectric constant of the aluminum nitride single crystal material is 5-100 Pc/N.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN111809239A (en) * 2019-04-10 2020-10-23 中国科学院福建物质结构研究所 Porous metal nitride single crystal material and preparation method and application thereof

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
CN101235540A (en) * 2007-11-09 2008-08-06 中国科学院上海光学精密机械研究所 Method for preparing aluminum nitride thin film on lithium aluminate wafer surface under low temperature
CN106062238A (en) * 2014-03-03 2016-10-26 株式会社村田制作所 Aluminum nitride piezoelectric thin film, method for manufacturing aluminum nitride piezoelectric thin film, piezoelectric material, and piezoelectric component
CN111809239A (en) * 2019-04-10 2020-10-23 中国科学院福建物质结构研究所 Porous metal nitride single crystal material and preparation method and application thereof
CN110219050A (en) * 2019-07-10 2019-09-10 河北工业大学 A kind of preparation method of aluminum nitride single crystal film

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Application publication date: 20210827