CN111948235A - Method for measuring semipolar plane III group nitride film defect density and application thereof - Google Patents
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Abstract
The invention discloses a method for measuring the defect density of a semipolar plane III-group nitride film and application thereof. The method comprises the following steps: measuring the semipolar plane III-nitride film growing on the heterogeneous substrate by adopting an X-ray diffractometer, thereby obtaining the maximum value of the semiwidth of the rocking curve in the plane of the film, the semiwidth of the rocking curve of the crystal face (10-10), the crystal face (20-20) and the crystal face (30-30) of the film and the peak position value; calculating to obtain the full width at half maximum of the a-type dislocation and the stacking fault distance L of the semipolar surfaceLcLWidening the half-height width; calculating to obtain the half-width broadening of c-type dislocation; and obtaining the dislocation densities of a type and c type according to the corrected dislocation density calculation formula to obtain the defect density of the semipolar surface of the thin film. The method provided by the invention can conveniently and quickly obtain the dislocation density of the semipolar plane III-nitride film, is beneficial to performing rapid feedback regulation and control on the semipolar plane III-nitride film growth technology, and has the advantages of low cost, no damage and the like.
Description
Technical Field
The invention particularly relates to a method for measuring the defect density of a semipolar plane III-group nitride film and application thereof, belonging to the technical field of semiconductors.
Background
In 2014, Nobel prize was won based on group III nitride development technology, which is the most successful manifestation of heteroepitaxial growth technology. On one hand, high-quality GaN single crystals are obtained on the sapphire with larger lattice mismatch; on the other hand, the field of p-GaN and blue light InGaN emitters is created. However, most of the efforts made in the development of group III nitrides have focused on c-plane polar GaN crystals, and spontaneous polarization electric fields exist in the c direction, which causes a quantum stark effect (QCSE) to significantly reduce quantum efficiency in the field of light emitting devices such as LEDs. Until now, no effective method for confining and eliminating spontaneous polarization electric fields has been found on c-plane ill-nitride light emitting devices. The semipolar plane can weaken spontaneous polarization effect in a space structure, eliminate the influence of the semipolar plane on a light-emitting device, and related results are published on nature in 2000. However, in contrast to c-plane materials, there is a higher density of stacking faults in the semipolar plane than in c-plane materials, in addition to a higher density of dislocations. Therefore, rapid development of semipolar plane group III nitrides is led in terms of scientific problems to be solved urgently in terms of crystal quality, size, thickness, and the like.
In the development process of the growth regulation and control technology of the semipolar surface III group nitride film, only expensive transmission electron microscope technology can be adopted in the aspect of analyzing the defects of the semipolar surface III group nitride film, and the defects of the technology are long period, regional microcosmic and high price, and the technology cannot meet the requirements of feeding back quality information in time and regulating and controlling the growth technology.
However, because of the influence of complicated dislocation types and distribution and the structural irrelevance of the semipolar plane, no effective, convenient and quick dislocation density measuring and calculating method has been proposed so far, the growth quality feedback can not be carried out quickly, the growth process can not be improved, and the development of the semipolar plane group III nitride film technology is severely restricted.
Disclosure of Invention
The invention mainly aims to provide a method for rapidly, cheaply and nondestructively measuring the defect density of a semipolar plane III-nitride film and application thereof, thereby overcoming the defects in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a method for measuring the defect density of a semipolar plane III-nitride film, which comprises the following steps:
measuring the semipolar plane III nitride film growing on the heterogeneous substrate by adopting an X-ray diffractometer, thereby obtaining the maximum value of the semipolar plane in-plane rocking curve semiheight width of the semipolar plane III nitride film, and the values of the semipolar plane rocking curve semiheight width and peak position of the (10-10), (20-20) and (30-30) crystal planes of the polar plane III nitride film;
the half-width broadening of a-type dislocation in the III-nitride film is obtained by calculation according to formula 1),
in formula 1), beta(h0-h0)Is the rocking curve full width at half maximum of the (10-10), (20-20) and (30-30) crystal planes, theta(h0-h0)Testing Bragg diffraction angle values of the (10-10) crystal plane, (20-20) crystal plane and (30-30) crystal plane, wherein lambda is the wavelength of X-rays, the stacking fault interval of the semipolar plane III-nitride film, and betatiltThe broadening value corresponding to the a-type dislocation;
calculating the stacking fault distance L of the semipolar plane III-group nitride film by the formula 2)LCLFor the widening of the half-height width,
in the formula 2), λ is the wavelength of X-ray, LLCLIs the stacking fault spacing, theta, of a semipolar plane III-nitride film(hkil)Bragg angle for semi-polar plane (hkil);
calculating and obtaining the half-height-width broadening alpha of c-type dislocation in the semipolar plane III-nitride film by the formula 3)c，
In formula 3), beta(hkil)Is maximum value of half-width of surface of semipolar plane III nitride filmChi is the included angle between the semipolar plane III-group nitride film and the c (0001) plane;
calculating and obtaining the density of a-type dislocation and the density of c-type dislocation in the semipolar plane III-nitride film by the formula 4),
in formula 4), D is the dislocation density; beta is beta obtained by formula 1) or formula 3)tiltAnd alphac(ii) a b is the Berkeley vector corresponding to the corresponding dislocation type, and has the size of lattice constant a or lattice constant c (the a-type dislocation in the present invention means that the Berkeley vector of the dislocation is 1/3<11-20>(ii) a The c-type dislocation in the present invention means a dislocation having a Berkeley vector of<0001>)；
The sum of the a-type dislocation density and the c-type dislocation density is the defect density of the semipolar plane III-nitride film.
Further, the semipolar plane III-nitride film is grown on the heterojunction substrate.
Further, the heterojunction substrate comprises a sapphire substrate.
Further, the semipolar plane group III nitride film includes an AlN film.
Further, the semipolar plane of the semipolar plane group III nitride thin film includes a (11-22) plane.
Further, the method for measuring the defect density of the semipolar plane III-nitride thin film specifically comprises the following steps: and measuring and obtaining the rocking curve in the (11-22) plane of the semipolar plane III nitride film by adopting an X-ray diffractometer, wherein the maximum value of the half-height width of the rocking curve in the (11-22) plane of the semipolar plane III nitride film is the half-height width value of the X-ray incident ray along the [1-100] direction.
Further, the method for measuring the defect density of the semipolar plane III-nitride thin film specifically comprises the following steps: construction of sin (. theta.) by equation 1)(h0-h0)) Lambda and beta(h0-h0)×sin(θ(h0-h0)) A linear curve of/λ (h ═ 1, 2, 3), so as to obtain a half-width broadening of a-type dislocations,wherein the half-width broadening of the a-type dislocation is the slope of a linear curve, namely betatiltThe difference value of the intersection point of the (30-30) point in the linear curve in the direction of the longitudinal axis and the linear curve corresponding to the abscissa is the interval L of the stacking faultLCLThe density of the stacking faults is the reciprocal of the spacing of the stacking faults (according to the widening effect of the stacking faults and the extinction rule of the crystal faces, the difference value of the intersection point of an image point corresponding to a (30-30) crystal face in the linear curve in the direction of the longitudinal axis and the linear curve of the corresponding abscissa can be obtained, namely the spacing of the stacking faults is the spacing of the stacking faults, and the reciprocal of the spacing of the stacking faults is the density of the stacking faults).
Further, the a-type dislocations include pure a-type dislocations and dislocation components in the a-type direction.
Further, the c-type dislocations include pure c-type dislocations and dislocation components in the c-type direction.
The embodiment of the invention also provides a method for measuring the defect density of the semipolar plane III-nitride film and application of the semipolar plane III-nitride film in a preparation method.
Compared with the prior art, the invention has the advantages that:
(1) the method for measuring the defect density of the semipolar plane III-nitride film provided by the embodiment of the invention can conveniently and quickly obtain the dislocation density of the semipolar plane III-nitride film, so that the rapid feedback regulation and control of the semipolar plane III-nitride film growth technology can be carried out;
(2) the method for measuring the defect density of the semipolar plane III-nitride thin film provided by the embodiment of the invention has the advantages of low cost, no damage and the like, and is suitable for large-scale commercial use.
Drawings
FIG. 1 is a schematic structural view of a semipolar plane III-nitride film;
FIG. 2 is a graph showing an in-plane rocking curve of AlN thin films (11-22) according to an exemplary embodiment of the present invention;
FIG. 3 shows in-plane AlN thin films (11-22) according to an exemplary embodiment of the present invention
And beta(h0-h0)×sin(θ(h0-h0)) Linear plot of/λ (h ═ 1, 2, 3);
FIGS. 4a and 4b are electron micrographs of an AlN thin film according to an exemplary embodiment of the present invention.
Detailed Description
In view of the deficiencies in the prior art, the inventors of the present invention have made extensive studies and extensive practices to provide technical solutions of the present invention. The technical solution, its implementation and principles, etc. will be further explained as follows.
The embodiment of the invention provides a calculation method of dislocation density in semipolar plane III nitride, in particular to a semipolar plane III nitride film obtained by a heteroepitaxy technology, which can realize rapid, cheap and lossless obtaining of defect density in the semipolar plane III nitride film and a defect density measurement method for filling the field.
According to the calculation method for the dislocation density in the semipolar plane III group nitride, provided by the embodiment of the invention, necessary mass distribution information data (including semipolar semiheight width, (10-10) (20-20) (30-30) crystal face half-peak width and peak position numerical values) are obtained by adopting a high-resolution X-ray diffraction mode, and then the accurate dislocation density in a thin film is obtained by a calculation method between test data and dislocation density.
Example 1
A method of measuring defect density of a semipolar plane III-nitride thin film, which may include the processes of:
1) obtaining a semipolar plane III nitride film on an m-plane sapphire substrate by a hydride vapor phase epitaxy growth technology (HVPE or other growth technologies capable of obtaining semipolar plane III nitride films), or growing the semipolar plane III nitride film on an r-plane or other crystal planes capable of being used for growing the semipolar plane III nitride film, of course, the heterojunction substrate is not limited to a sapphire substrate, and other heterojunction substrates capable of obtaining the semipolar plane III nitride films can be realized; as follows, an example of (11-22) semipolar plane AlN thin films grown on m-plane sapphire substrates is described, the structure of the AlN thin films being as shown in FIG. 1;
2) testing the AlN thin film by adopting a high-resolution X-ray diffractometer (HRXRD) (a parallel light device adopts Ge (220) for 4 times of diffraction; the biaxial crystal mode is slit opening; the biaxial crystal mode is Si (111) analysis crystal), and the maximum value of the full width at half maximum of the rocking curve in the semipolar plane of the AlN thin film (11-22) (biaxial crystal mode) is obtained by measurement, and the maximum value of the full width at half maximum of the rocking curve in the semipolar plane of the AlN thin film (10-10), the crystal plane (20-20) and the crystal plane (30-30) (biaxial crystal mode) are obtained by measurement, wherein, as shown in figure 2, the X-ray incident line in the semipolar plane of the AlN thin film (11-22) is the maximum value of the full width at half maximum of the rocking curve along the direction of [1-100 ];
3) the half height width and peak position value of the rocking curve of the crystal face (10-10), the crystal face (20-20) and the crystal face (30-30) of the AlN thin film are plotted and analyzed according to the formula 1),
in formula 1), beta(h0-h0)Is the rocking curve full width at half maximum of the (10-10), (20-20) and (30-30) crystal planes, theta(h0-h0)Testing Bragg diffraction angle values of the (10-10) crystal face, (20-20) crystal face and (30-30) crystal face, wherein lambda is the wavelength of X-rays, and L isLCLIs the stacking fault spacing, beta, of a semipolar plane III-nitride filmtiltThe broadening value corresponding to the a-type dislocation, wherein the a-type dislocation comprises a pure a-type dislocation and a dislocation component in the a-type direction;
the half-width curve (i.e., the aforementioned linear curve) of (h0-h0) obtained by equation 1) having a slope of β is shown in FIG. 3tiltThereby obtaining half-width broadening data of a-type dislocation; extinction according to the stacking fault extinction law (g · R ═ n (n ═ 0, ± 1, ± 2.), g being diffraction facets (h0-h0), R being stacking fault vectors, 1/6<20-23>、1/3<10-10>) (ii) a The broadening of the rocking curve of the (30-30) crystal face is not influenced by the stacking fault, and the difference value of the intersection point of the image point corresponding to the (30-30) crystal face in the direction of the longitudinal axis and the corresponding abscissa on the half-height width curve is the spacing L of the stacking faultLCLThe density of the stacking faults is the reciprocal of the spacing of the stacking faults;
4) according to (11-22) halfC-type dislocation analysis is carried out on the maximum value of the polar in-plane rocking curve: c-type dislocation comprises pure c-type dislocation and dislocation component in c-type direction, (11-22) maximum value of semipolar in-plane rocking curve is affected by both dislocation and dislocation, and the spacing L of dislocation is calculated according to formula 2)LCLFor the half-width widening, the half-width broadening alpha of the c-type dislocation is calculated according to the formula 3)c，
In the formula 2), λ is the wavelength of X-ray, LLCLIs the stacking fault spacing, theta, of a semipolar plane III-nitride film(hkil)Is the Bragg angle of (11-22) semipolar plane;
in formula 3), beta(hkil)Is the maximum value of the half width in the (11-22) semipolar plane, and χ is the included angle between the (11-22) semipolar plane and the c (0001) plane;
calculating and obtaining the density of a-type dislocation and the density of c-type dislocation in the semipolar plane III-nitride film by the formula 4),
in formula 4), D is the dislocation density; beta is beta calculated by formula 1) or formula 3)tiltAnd alphac(ii) a b is a Berkos vector corresponding to the corresponding dislocation type, and the size of the vector is a lattice constant a or a lattice constant c;
the sum of the a-type dislocation density and the c-type dislocation density is the defect density of the semipolar plane III-nitride film.
In this embodiment, the density of a-type dislocation is 9.0X 10 according to XRD test9cm-2C type dislocation density of 8.4 × 109cm-2The total bit error density is 1.74 multiplied by 1010cm-2Performing on the AlN thin filmThe dislocation density was analyzed by transmission electron microscope, and as a result, as shown in FIGS. 4a and 4b, the total dislocation density was 1.3X 10 as analyzed from FIGS. 4a and 4b10cm-2The dislocation density is the same, and the value is lower than the actual value because TEM is the dislocation density of the microscopic region.
The method for measuring the defect density of the semipolar plane III-nitride film provided by the embodiment of the invention can conveniently and quickly obtain the dislocation density of the semipolar plane III-nitride film, so that the rapid feedback regulation and control of the semipolar plane III-nitride film growth technology can be carried out;
the method for measuring the defect density of the semipolar plane III-nitride film provided by the embodiment of the invention has the advantages of low cost and no damage, and can be suitable for large-scale commercial use.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, which are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and therefore, the protection scope of the present invention is not limited thereby. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. A method of measuring defect density of a semipolar plane group III nitride thin film, comprising:
measuring the semipolar plane III nitride film growing on the heterogeneous substrate by adopting an X-ray diffractometer, thereby obtaining the maximum value of the semipolar plane in-plane rocking curve semiheight width of the semipolar plane III nitride film, and the values of the semipolar plane rocking curve semiheight width and peak position of the (10-10), (20-20) and (30-30) crystal planes of the semipolar plane III nitride film;
calculating and obtaining the half-width broadening of a-type dislocation in the semipolar plane III-nitride film by the formula 1),
in formula 1), beta(h0-h0)Is the rocking curve full width at half maximum of the (10-10), (20-20) and (30-30) crystal planes, theta(h0-h0)Testing Bragg diffraction angle values of the (10-10) crystal face, (20-20) crystal face and (30-30) crystal face, wherein lambda is the wavelength of X-rays, and L isLCLIs the stacking fault spacing, beta, of a semipolar plane III-nitride filmtiltThe broadening value corresponding to the a-type dislocation;
calculating the stacking fault distance L of the semipolar plane III-group nitride film by the formula 2)LCLFor the widening of the half-height width,
in the formula 2), λ is the wavelength of X-ray, LLCLIs the stacking fault spacing, theta, of a semipolar plane III-nitride film(hkil)Bragg angle for semi-polar plane (hkil);
calculating and obtaining the half-height width broadening ac of c-type dislocation in the semipolar plane III-nitride film by an expression 3),
in formula 3), beta(hkil)The maximum value of the surface half-height width of the semipolar plane III group nitride film, and chi is the included angle between the semipolar plane III group nitride film and the c (0001) plane;
calculating and obtaining the density of a-type dislocation and the density of c-type dislocation in the semipolar plane III-nitride film by the formula 4),
in formula 4), D is a dislocation density, and β is β obtained from formula 1) and formula 3)tiltAnd alphac(ii) a b is a Berkos vector corresponding to the corresponding dislocation type, and the size of the vector is a lattice constant a or a lattice constant c;
the sum of the a-type dislocation density and the c-type dislocation density is the defect density of the semipolar plane III-nitride film.
2. The method of claim 1, wherein: the semipolar plane III-nitride film is grown on a foreign substrate.
3. The method of measuring defect density of semipolar plane group III nitride thin film according to claim 1 or 2, wherein: the heterojunction substrate comprises a sapphire substrate.
4. The method of measuring defect density of semipolar plane ill-nitride thin films according to claim 1, wherein: the semipolar plane group III nitride film includes an AlN film.
5. The method of measuring defect density of semipolar plane ill-nitride thin films according to claim 1, wherein: the semipolar plane of the semipolar plane group III nitride thin film includes (11-22) planes.
6. The method of claim 5, further comprising: and measuring and obtaining the rocking curve in the (11-22) plane of the semipolar plane III nitride film by adopting an X-ray diffractometer, wherein the maximum value of the half-height width of the rocking curve in the (11-22) plane of the semipolar plane III nitride film is the half-height width value of the X-ray incident ray along the [1-100] direction.
7. The method of claim 1, further comprising: construction of sin (. theta.) by equation 1)(h0-h0)) Lambda and
thereby obtaining a full width at half maximum spread of a-dislocations, wherein the full width at half maximum spread of a-dislocations is a linear curveIs the slope of (i) is betatiltThe difference value of the intersection point of the (30-30) point in the linear curve in the direction of the longitudinal axis and the linear curve corresponding to the abscissa is the interval L of the stacking faultLCLThe density of the stacking faults is the inverse of the stacking fault spacing.
8. The method of measuring defect density of semipolar plane ill-nitride thin films according to claim 1, wherein: the a-type dislocations include pure a-type dislocations and a dislocation component in the a-type direction.
9. The method of measuring defect density of semipolar plane ill-nitride thin films according to claim 1, wherein: the c-type dislocations include pure c-type dislocations and a dislocation component in the c-type direction.
10. Use of the method of any one of claims 1-9 in a method of making a semipolar plane ill-nitride thin film.
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