CN115855844B - A photoelectric testing method for identifying electronic-grade diamonds - Google Patents
A photoelectric testing method for identifying electronic-grade diamondsInfo
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Abstract
本发明涉及金刚石鉴定技术领域，具体涉及一种鉴定电子级金刚石的光电测试方法。本发明提供了一种利用光电测试来鉴定电子级金刚石的无损手段，在被测金刚石顶部和底部溅射电极制成器件，根据金刚石在不同入射光波长下的光电流信号计算出其随波长变化的外量子效率，再利用随波长变化的外量子效率光谱获取金刚石的光谱响应峰半高宽，最后将光谱响应峰半高宽小于15nm的金刚石判定为电子级金刚石。采用本发明的光电测试方法可以准确的鉴别电子级金刚石单晶质量是否达标，与ICP和SIMS检测方法相比具有无损耗、低成本、更全面反映金刚石质量等级的优点，为电子级金刚石质量鉴定领域提供了一种新型可靠的验证手段。
The present invention relates to the field of diamond identification technology, and specifically to a photoelectric testing method for identifying electronic-grade diamonds. The present invention provides a non-destructive means for identifying electronic-grade diamonds using photoelectric testing. Electrodes are sputtered on the top and bottom of the diamond to be tested to form a device. The external quantum efficiency of the diamond that varies with wavelength is calculated based on the photocurrent signal of the diamond under different incident light wavelengths. The wavelength-varying external quantum efficiency spectrum is then used to obtain the half-maximum width of the diamond's spectral response peak. Finally, diamonds with a half-maximum width of the spectral response peak less than 15nm are determined to be electronic-grade diamonds. The photoelectric testing method of the present invention can accurately identify whether the quality of electronic-grade diamond single crystals meets the standards. Compared with ICP and SIMS detection methods, it has the advantages of no loss, low cost, and more comprehensive reflection of the diamond quality grade, providing a new and reliable verification method for the field of electronic-grade diamond quality identification.
Description
Technical Field
The invention relates to the technical field of diamond identification, in particular to a photoelectric test method for identifying electronic grade diamond.
Background
Diamond, which is an ultra-wide band-gap semiconductor, has excellent characteristics of high carrier mobility and saturation velocity, large breakdown electric field, high thermal conductivity, high chemical inertness, thermal stability and the like, and thus makes it an ideal material for manufacturing power electronic devices. Currently, methods for artificially synthesizing diamond include two major types, namely a high-temperature high-pressure method and a chemical vapor deposition method. The quality of the diamond obtained varies depending on the particular growth method and parameters. However, only high purity, high quality electronic grade diamond meets the application requirements of power electronics, which requires characterization and identification of the quality of the diamond produced. In particular, it can be classified into characterization of the crystal structure and characterization of the elemental composition. The characterization method of the element component of the diamond comprises Inductively Coupled Plasma (ICP) and Secondary Ion Mass Spectrometry (SIMS), and the impurity element and content in the diamond can be quantitatively analyzed by the characterization means, so that the accuracy can reach ppb level. However, the above characterization means can reflect only the characteristics of diamond in a certain aspect, and ICP and SIMS also have the disadvantages of being costly and damaging to the sample. Therefore, there is an urgent need to develop a new detection method that is not damaged and can comprehensively reflect the quality of diamond.
The presence of various defects in diamond determines the quality of diamond, such as impurity defects (point defects), line defects and surface defects, which increase the scattering of carriers to affect carrier mobility, and the level of defects formed by these defects also produce recombination or trapping effects on carriers to affect carrier lifetime. And carrier mobility and carrier lifetime together determine the photoelectric response characteristics of the material. Based on this, the present invention proposes a new method for identifying electronic grade diamond material using a photoelectric test.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a photoelectric testing method for identifying electronic grade diamond, which is used for calculating the half-width of a curve response peak of external quantum efficiency along with spectral change and deducing the trap state density of diamond by using the half-width of the response peak so as to judge whether a tested sample is the electronic grade diamond.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the invention provides a photoelectric testing method for identifying electronic grade diamond, which comprises the following steps:
s1, respectively sputtering a layer of metal on the top and the bottom of a diamond monocrystal to form a diamond device as an anode and a cathode, wherein the top metal is a semitransparent electrode, and connecting the anode and the cathode into a circuit;
S2, irradiating the top of the diamond device by using a light source with the wavelength of 160-280 nm of incident light under a vacuum condition, outputting photocurrent signals with different wavelengths by using a source meter, calculating external quantum efficiency changing along with the wavelength, acquiring the half-width of a spectral response peak of the diamond by using an external quantum efficiency spectrum changing along with the wavelength, and finally judging the diamond with the half-width of the spectral response peak being less than 15nm as the electronic grade diamond.
The working principle of the testing method is that the high-quality electronic grade diamond has shorter service life because of fewer defect states and most carriers cannot be trapped by traps, so that the light response is obviously reduced in a short-wave area, and the spectrum has extremely narrow half-width. Meanwhile, since light of 200nm or less is strongly absorbed by air, the photoelectric test is performed under vacuum. When light enters from the top of the crystal, photo-generated electrons and holes in the crystal drift through the single crystal under an external electric field and are collected by electrodes at two ends to output photocurrent, external quantum efficiency can be calculated according to the photocurrent, so that the half-width of a spectral response peak is obtained, the narrower half-width of the response peak shows that the smaller the trap state density of the diamond is, the higher the quality of the diamond is reflected, and when the half-width of the spectral response peak is smaller than 15nm, the diamond can meet the requirements of the electronic grade diamond.
Preferably, in the step S1, a layer of Pt is sputtered on top of the diamond monocrystal as a semitransparent anode, a layer of Pt is sputtered on bottom of the diamond monocrystal as a cathode, a glass substrate with Au metal is deposited under the cathode through silver-bonded joint, and the diamond device is composed of a Pt layer, a diamond layer, a Pt layer and a glass substrate with Au metal deposited in sequence from top to bottom.
Preferably, in the step S1, the thickness of Pt sputtered on top of the diamond layer single crystal is 15-20 nm.
Preferably, in the step S2, the light source is obtained by a continuous ultraviolet light source and a spectrometer, and the wavelength of the incident light is changed from 280nm to 160nm.
Preferably, in the step S2, the external quantum efficiency is represented by the formulaCalculated, where I ph is the photocurrent, P is the incident light power, e is the fundamental charge, h is the planck constant, c is the speed of light, and λ is the wavelength of monochromatic light.
Preferably, in the step S2, when the spectral response peak half width of the measured diamond is less than 10nm, the measured diamond is identified as high quality electronic grade diamond.
Preferably, after the step S2 is completed, the diamond device is immersed in aqua regia to wash off the electrode.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a photoelectric test method for identifying electronic grade diamond, which comprises the steps of sputtering metal on the top and the bottom of a diamond monocrystal to form a diamond device as an anode and a cathode, wherein the top metal is a semitransparent electrode, and the diamond device is connected into a circuit, then irradiating the top of the diamond device by a light source with the incident light wavelength of 160-280 nm under the vacuum condition, calculating the external quantum efficiency of the diamond along with the change of wavelength according to the photocurrent signals of the diamond under different incident light wavelengths, obtaining the half-width of a spectral response peak of the diamond by utilizing the spectrum of the external quantum efficiency along with the change of wavelength, and displaying the smaller trap state density of the diamond by the narrower half-width of the response peak, so that the diamond has higher quality, and the requirements of the electronic grade diamond can be met when the half-width of the spectral response peak is smaller than 15 nm. Compared with the traditional testing methods of XRD, ICP and SIMS, the method has the advantages that the quality of the diamond is integrally reflected in the aspect of photoelectric effect by analyzing the carrier mobility and the carrier service life, the electrode can be washed away, the diamond is not damaged, and compared with the double-crystal swing test and the SIMS, the testing result of the method is more obvious and is easy to distinguish, and the electronic grade diamond can be better identified.
Drawings
FIG. 1 shows the results of the bicrystal rocking test for diamonds A, B and C;
FIG. 2 shows SIMS test results for diamonds A, B and C;
FIG. 3 is a photo-electrical test structure of a diamond device;
FIG. 4 is a graph showing the results of photoelectric testing of diamonds A, B and C;
FIG. 5 is a photograph showing the results of a photo-electric test of two diamond pieces grown (CVD) using the same conditions;
FIG. 6 is a diagram of the exciton emission mechanism study under photoexcitation of diamond A, wherein (a) the main physical processes that occur in diamond A under photoexcitation, (b) the PL spectra of diamond A under 193nm pulse excitation;
FIG. 7 is a photoexcitation-induced carrier mechanism study of diamond A, in which (a) the photoexcitation excess carrier generation rate G in diamond A, (b) the spatial distribution of steady-state carriers, (c) experimental EQE and simplified calculation EQE for diamond A labeled with three selected wavelengths;
FIG. 8 is a schematic diagram of the principal physical processes that may occur for (a) diamond B and C under photoexcitation, (B) PL spectra for diamond A, B and C under 193nm pulse excitation, and (C) voltage signal for diamond A, B, C under 93nm pulse excitation;
fig. 9 is a photoexcitation lower carrier mechanism study of diamond C, in which (a) photoexcitation excess carrier generation rate G in diamond C, (b) spatial distribution of steady state carriers, (C) experimental EQE and simplified calculation of EQE for diamond C labeled with three selected wavelengths.
Detailed Description
The following describes the invention in more detail. The description of these embodiments is provided to assist understanding of the present invention, but is not intended to limit the present invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
The experimental methods in the following examples, unless otherwise specified, were conventional, and the experimental materials used in the following examples, unless otherwise specified, were commercially available from conventional sources.
Example 1 establishment of electronic grade diamond photoelectric identification method and feasibility mechanism study
This example, in which three different diamond single crystals were used for comparative experiments to further verify the effectiveness of the present invention, was designated as diamond a, B and C, respectively, with a thickness of 680 μm and a thickness of 780 μm for diamond C. Diamonds A and C were grown by Chemical Vapor Deposition (CVD) and diamond B was grown by high temperature and high pressure methods, preparation methods were described in the literature (doi. Org/10.1016/B978-0-444-63303-3.00017-1).
1. Testing diamond by conventional method
Three diamonds were first characterized using conventional methods, including the bicrystal rocking test and the SIMS test. The full width at half maximum of the rocking curves for diamond a, B and C (004) planes are 28.9arcsec, 34.9arcsec and 39.3arcsec (fig. 1), respectively, which reflect the lower dislocation density of diamond a. The analysis of SIMS test results is shown in FIG. 2, and the contents of the respective elements and chemical bonds are substantially the same. The above results do not clearly distinguish the quality of the three diamonds.
2. Preparation of diamond device
First, a thin layer of Pt (17 nm) is sputtered on top of single crystals of diamond A, B and C as a semitransparent anode, a layer of Pt is sputtered on the bottom of the single crystals as a cathode, a glass substrate with Au metal is evaporated under the cathode through silver-bonded joint, and diamond devices A, B and C are prepared, wherein the diamond devices are composed of the Pt layer, the diamond layer, the Pt layer and the glass substrate with Au metal in sequence from top to bottom (see figure 3). And connecting the anode and the cathode with the probe, accessing the probe into a circuit, and reading out an electrical output signal through a source meter. When light is incident from the top of the crystal, photo-generated electrons and holes in the crystal drift through the single crystal under the action of an applied electric field and are collected by the two end electrodes to output photocurrents.
3. Photoelectric testing of diamond
Since light below 200nm is strongly absorbed by air, the photoelectric test is performed under vacuum. And placing the diamond devices A, B and C in a vacuum cavity for testing, vertically incidence from the top of the diamond device by using monochromatic light within the range of 160-280 nm, wherein the monochromatic light is obtained by a deuterium lamp and a monochromatic spectrometer, the wavelength of the incident light is changed from 280nm to 160nm, and corresponding photocurrent signals are read out by a source meter. From the formulaThe External Quantum Efficiency (EQE) as a function of wavelength can be calculated, where I ph is the photocurrent, P is the incident optical power, e is the fundamental charge, h is the planck constant, c is the speed of light, and λ is the wavelength of monochromatic light. After the test is finished, the diamond device is soaked in aqua regia to wash away the metal electrode, so that the sample is not damaged.
The EQE spectra with wavelength change are shown in FIG. 4, and the half-widths of the spectral response peaks of the diamonds A, B and C are 8nm,31nm and 52nm, respectively, which indicates that the diamond A has the highest quality because the trap state density is the smallest, and when the half-width of the spectral response peak of the measured diamond is less than 10nm, it is identified that the diamond is high quality electronic grade diamond, so that the diamond A is high quality electronic grade diamond, and the quality of the diamonds B and C are sequentially reduced.
4. Photoelectric test method verification of diamond
To evaluate the accuracy of this method, to avoid accidental factors, two diamonds grown using the same Conditions (CVD) were subjected to the above-described opto-electronic test. It was found that the EQE spectra of both diamonds showed a narrow peak near the absorption edge, centered at about 228nm, and the full width at half maximum of the EQE was only about 8nm (fig. 5). The consistency of the test results for two identical diamonds demonstrates the reliability of the test method.
5. Mechanism interpretation of optoelectronic test methods
For the proposed optoelectric test method, a mechanism explanation is given that, first of all, for high quality electron-grade diamond, most carriers will not be trapped by traps and have a shorter lifetime due to fewer defect states. In the low absorption coefficient region, carriers can be excited inside the whole crystal so as to be collected by the electrode under the action of an electric field. As the wavelength decreases, the absorption coefficient gradually increases resulting in a significant increase in the optical response. After reaching the response peak, as the photoexcitation wavelength continues to decrease, the photo-generated carriers are generated more and more to concentrate on the surface of the crystal, and at this time, the photo-generated carriers are annihilated mainly through the radiation recombination process and cannot be transmitted to the back of the crystal to be collected by the electrode. This results in a significant drop in the light response in the short-wave region, i.e. in a spectrum with an extremely narrow half-width. Whereas for non-electron-grade diamond, more trap energy states allow carriers to be trapped by the traps with longer lifetimes. Even under excitation with shorter wavelength light, carriers are generated close to the surface but can diffuse into the crystal interior due to small radiative recombination. Meanwhile, carriers with longer service life can be collected by the back electrode under the action of an electric field, so that the light response is not reduced, and the spectrum has larger half-width.
Specifically, taking diamond a and diamond C as examples, respectively, the derivation process is given:
For diamond a, the physical processes that mainly occur in the optoelectronics test include absorption of photons (energy greater than bandgap) to excite electrons from the valence band to the conduction band or higher (relaxation to the bottom of the conduction band by phonon emission etc.) thus creating free mobile electrons in the conduction band and leaving free mobile holes in the valence band that can induce photoconductive signals under the influence of an electric field (process 1) while radiative recombination can also be created via localized energy states in the forbidden band (process 2) (fig. 6 a). Fig. 6b shows the luminescence spectrum of diamond a under 193nm pulsed light excitation, where super-strong exciton-assisted free exciton emission is observed. Spectral lines with a certain width contain the participating processes of different phonons. This result demonstrates that exciton emission is the dominant recombination process under photoexcitation.
The steady-state distribution of carriers in the crystal under photoexcitation directly affects the photoconductive output, which is determined by the photoexcitation process, diffusion process and recombination process. As the photon energy increases, the more concentrated the excess electron-hole pairs generated by photoexcitation are near the surface. As shown in fig. 7a, the spatial distribution of the photoexcited excess carrier generation rate G in the sample decays exponentially, according to the beer-lambert law, i.e., G- αe -αx (thickness d of diamond a is 680 μm), where α is the absorption coefficient of the material for light with wavelength λ and e is a natural constant. The three characteristic wavelengths selected were 228nm,225nm and 210nm, respectively, and the corresponding EQEs are shown in FIG. 7 c. Light at 228nm decays slowly with depth, can penetrate the crystal, and generate photo-generated carriers inside the crystal. And as the wavelength decreases, the generation of photoexcited carriers is more concentrated at the surface. In particular 210nm, cannot penetrate the crystal due to strong absorption by the surface. It is apparent that the generation of photogenerated carriers has an uneven distribution inside the crystal, so that they are to be diffused into the inside of the crystal. In addition, all radiative and non-radiative recombination transitions result in annihilation of the carriers, thereby reducing carrier concentration. Taking the effect of surface recombination as an example, the steady-state distribution of photogenerated carriers can be expressed as:
Where J is a constant related to the incident light flux and reflectance, D e is an electron diffusion coefficient related to mobility, s is a surface recombination velocity proportional to the excess carrier concentration of the surface, α is the absorption coefficient of the material for light of wavelength λ, D is 680 μm, 0< x < D. The spatial distribution of carriers within the crystal under excitation at different wavelengths can thus be obtained (fig. 7 b). As the wavelength decreases, the carrier concentration within the crystal gradually decreases, and the maximum value of the entire concentration moves toward the surface. In addition, strong absorption near the surface results in stronger radiative recombination and thus a significant increase in surface recombination velocity. The results may qualitatively explain the narrow band output based on the diamond a device. Specifically, on this basis, it is assumed that diamond a is perfectly crystalline, i.e., the effect of all defect levels is ignored. And the surface recombination velocity is considered to be so great that sd/D e > >1. Under the condition αd > >1, photoconduction can be expressed as:
Where A is the area of illumination, J is a constant related to the incident luminous flux and reflectance, μ n and μ p are electron and hole mobilities, τ n and τ p are electron and hole lifetimes, respectively, L D is the bipolar diffusion length, depending on μ nτn and μ pτp, α is the absorption coefficient of the material for light of wavelength λ, d is 680 μm, and s is the surface recombination velocity. From this equation, it can be seen that the change in ΔG with excitation wavelength is largely dependent on This factor, where both L D,De and d can be considered constants. Obviously, both the absorption coefficient and the surface recombination velocity increase with decreasing wavelength, resulting in a significant decrease in photoconductivity. The variation of the experimental EQE with wavelength, and the calculation of the simplified EQE from the above formula, is shown in fig. 7c, where the response peak half-width at half-maximum of diamond a under perfect crystal assumption is smaller than that of the experiment. The simplified calculation is for illustrating the trend of change, and the absolute value thereof is not significant.
For diamond C, the physical processes that occur primarily under photoexcitation of the crystal add to the donor-acceptor pair radiative recombination transition process (3), and the defect level pair carrier trapping process (1') (fig. 8 a), in addition to processes (1) and (2) previously described. Process (3) is as in process (2) where radiative recombination results in annihilation of carriers. While process (1') increases the lifetime of the carriers and thus increases the photoconductive signal, i.e. contributes to the output of the electrical signal. The radiative recombination process was measured by photoluminescence spectra, and the measurement results are shown in fig. 8B, in which exciton emission intensities (FEs emission) of diamond B and C are sequentially reduced as compared to diamond a. In addition, diamond B also had defect luminescence (defect emission) in the visible range, demonstrating the presence of process (3). Carrier lifetime is measured by the transient excitation voltage response of the device under an electric field, as shown in fig. 8c, with diamond a having the shortest carrier lifetime as expected, confirming the rapid annihilation process of carriers by radiative recombination. The longest service life of the diamond C is tens times that of the diamond A, and the fact that the larger trap state density in the diamond C causes obvious carrier trapping effect in the crystal is proved.
Fig. 9a shows the spatial distribution of photoexcitation excess carrier generation rate G in diamond C (diamond C thickness 780 μm), typical photoexcitation wavelengths are 220nm and 205nm, and the corresponding EQEs are shown in fig. 9C. Clearly, the distribution of excess carrier generation rates under excitation at these two wavelengths is similar, which is caused by the similar absorption coefficients. Based on PL spectrum and transient excitation voltage response of diamond C, it can be seen that photogenerated carriers contribute more to process (1') than process (2). Thus, a simplified case can be considered, i.e. neglecting the surface recombination of diamond, where equation (1) can be simplified toThe steady-state distribution of the photo-generated carriers thus obtained is shown in fig. 9 b. The carrier distribution under 205nm light excitation is similar to that under 220nm light excitation, but the overall carrier concentration is slightly greater for the former than for the latter, consistent with the results shown by EQE. The photoconductive formula (2) of the device is simplified to be under the premise of neglecting the surface recombination effect The EQE calculated based on this formula is shown in fig. 9c, showing a trend consistent with the experimentally measured E QE.
In summary, the above deductions prove that the photoelectric test result of diamond is an effective method for detecting the quality of diamond. The method provided by the invention proves that the narrower the half-width of the spectral response presented by the diamond with higher quality is, and a novel and reliable verification means is provided for the field of diamond quality identification.
The embodiments of the present invention have been described in detail above, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, and yet fall within the scope of the invention.
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| 金刚石光电导器件的仿真与实验研究;张玉玺;中国优秀硕士学位论文全文数据库信息科技辑;20210515(第05期);I135-57 * |
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