CN113571409B - Preparation method of high-thermal-conductivity diamond-enhanced silicon carbide substrate - Google Patents
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- CN113571409B CN113571409B CN202110753116.2A CN202110753116A CN113571409B CN 113571409 B CN113571409 B CN 113571409B CN 202110753116 A CN202110753116 A CN 202110753116A CN 113571409 B CN113571409 B CN 113571409B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/0445—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising crystalline silicon carbide
- H01L21/0475—Changing the shape of the semiconductor body, e.g. forming recesses
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/3065—Plasma etching; Reactive-ion etching
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/308—Chemical or electrical treatment, e.g. electrolytic etching using masks
- H01L21/3083—Chemical or electrical treatment, e.g. electrolytic etching using masks characterised by their size, orientation, disposition, behaviour, shape, in horizontal or vertical plane
- H01L21/3086—Chemical or electrical treatment, e.g. electrolytic etching using masks characterised by their size, orientation, disposition, behaviour, shape, in horizontal or vertical plane characterised by the process involved to create the mask, e.g. lift-off masks, sidewalls, or to modify the mask, e.g. pre-treatment, post-treatment
Abstract
A preparation method of a high-thermal-conductivity diamond-enhanced silicon carbide (SiC) substrate belongs to the field of semiconductor material preparation. The invention realizes the imaging on the carbon polar surface of the SiC through gluing, photoetching and developing. And then electron beam evaporation or magnetron sputtering of a metal mask is used. And after removing the photoresist, performing reactive ion etching, mask removing and secondary ion etching on the SiC with the periodically arranged metal mask to obtain the micro-column array. The diamond layer was then grown by microwave plasma chemical vapour deposition technique. And after the diamond layer completely covers the micro-column and has a certain thickness, laser scanning leveling and subsequent precision polishing are adopted to obtain the high-thermal-conductivity diamond-reinforced SiC substrate. The heat conduction efficiency is improved by increasing the effective contact interface area of diamond and SiC, and meanwhile, the insufficient binding force and the local defect expansion of a single plane interface are effectively avoided. The method lays a foundation for obtaining SiC/Diamond and GaN/SiC/Diamond wafers for high power and high frequency by thinning SiC silicon polar surfaces and depositing GaN on the surfaces at high temperature in the future.
Description
Technical Field
The invention belongs to the field of semiconductor material preparation, and relates to a preparation method of a high-thermal-conductivity diamond-enhanced silicon carbide substrate.
Background
Silicon carbide (SiC) and gallium nitride (GaN) are ideal materials for radio frequency and power devices as wide band gap semiconductors, and will play an increasingly important role in developing technologies such as the future photovoltaic industry, high-speed trains, electric vehicles, 5G radio frequency, satellite communication and radar. High strength and hardness, high thermal shock resistance and corrosion resistance make SiC perform well in extreme temperature environments. Further, SiC, as a representative third generation semiconductor material, can be used as a high power, high frequency electronic device in a severe environment by utilizing its wide band gap and high dielectric breakdown electric field strength. However, for the miniaturization and high integration of modern high-power electronic and optoelectronic devices, a large amount of heat is generated during use. The reliability and lifetime of the device is directly related to the device temperature. The reliability and the service life of the device are exponentially increased when the temperature of the device is reduced. Both for SiC power devices and SiC-based GaN power devices face the risk of device performance degradation or even complete failure due to "self-heating effects" at high power outputs. Especially how to transfer heat in a small space is a new challenge for power electronic devices, and thus thermal management has become an increasingly important factor in electronic device design.
The thermal conductivity of diamond at room temperature can reach more than 2000W/(m.K) to the maximum, which is 5 times of that of copper, 6 times of that of aluminum nitride and more than 7 times of that of beryllium oxide, and the heat generated by electronic devices can be effectively transferred. And the resistivity of the diamond is as high as 1016Ω · cm is a typical insulator, and there is no concern about the possibility of occurrence of leakage current. Diamond is therefore the most desirable heat sink material. The SiC-on-Diamond and the GaN/SiC-on-Diamond wafers formed by combining SiC and Diamond can obviously improve the heat dissipation capability of the SiC bottom layer, thereby improving the output power and frequency of SiC and SiC-based GaN devices and prolonging the service life. However, there are many problems in depositing diamond on the surface of SiC or GaN, and plasma etching, interface strength, and the like need to be considered,Interface heat conduction and stress. Particularly, the problems that the stress, the SiC-diamond interface strength and the nucleation defects influence the thermal conductivity during the thinning of SiC or the high-temperature deposition of GaN on the SiC surface based on the SiC substrate deposited with the diamond thin layer are particularly prominent.
Disclosure of Invention
The invention aims to provide a preparation method of a high-thermal-conductivity diamond-enhanced silicon carbide substrate. The problems of plasma etching, interface strength, interface heat conduction, stress and the like are solved. Particularly solves the problem that the stress of the SiC substrate deposited with the diamond thin layer influences the thermal conductivity in the process of thinning SiC or depositing GaN on the SiC surface at high temperature, and the interface strength and nucleation defects of SiC and diamond.
The technical scheme of the invention is as follows:
a preparation method of a high-thermal-conductivity diamond-enhanced silicon carbide substrate realizes patterning on a carbon polar surface of SiC through gluing, photoetching and developing. And then electron beam evaporation or magnetron sputtering of a metal mask is used. After the photoresist is removed, the SiC with the periodically arranged metal masks is subjected to reactive ion etching, mask removal and secondary ion etching to obtain the micro-column array. The diamond layer was then grown by microwave plasma chemical vapour deposition technique. And after the diamond layer completely covers the micro-column and has a certain thickness, scanning the diamond growth surface by laser to flatten and then precisely polish, thus obtaining the high-thermal-conductivity diamond-reinforced SiC substrate. The method lays a foundation for obtaining high-power and high-frequency SiC/Diamond and GaN/SiC/Diamond wafers by thinning the SiC silicon polar surface and depositing GaN on the surface at high temperature in the future.
The preparation method of the diamond-enhanced silicon carbide substrate with high thermal conductivity is characterized by comprising the following steps:
step 1: SiC surface gluing and exposure patterning
The carbon polar surface of the SiC is coated with photoresist in a spinning mode, and ultraviolet photoetching is achieved through a mask plate. And then, developing and removing photoresist to realize periodic micropores, and exposing the periodically arranged diamond patterned surface.
Step 2: deposition of metal masks
And depositing a metal mask on the SiC with the patterned photoresist by electron beam evaporation or magnetron sputtering. And removing the residual photoresist to obtain SiC with the metal pattern mask deposited on the surface.
And step 3: reactive ion etching of SiC periodic microcolumn structures
And preparing the SiC microcolumn and performing arc etching on the edge by reactive ion etching.
And 4, step 4: growth of diamond layer
And placing the SiC with the micro-column structure in a microwave plasma chemical vapor deposition chamber, and growing a diamond layer to cover the micro-column structure.
And 5: laser scanning leveling and grinding polishing of diamond growth surface
And the YAG laser local ablation technology is adopted to realize the flattening processing of the diamond growth surface in a plane scanning mode, so that the flatness of the surface of the diamond growth layer is realized. And then further reducing the surface roughness of the diamond through grinding and precise polishing of the diamond nano particles.
Further, the deposition step of the metal mask in the step 2 is to deposit a 10-50nm metal titanium layer and then deposit a 100-150nm metal aluminum layer, wherein the substrate temperature does not exceed 100 ℃ in the coating process.
Further, the step of reactive ion etching of the SiC periodic microcolumn structure in the step 3 is to etch SiC by using a gas source CF4:O2Etching the SiC to an etching depth of 1-20 μm under the conditions of a ratio of 5:1-2:1 and a bias power of 100-. The metal mask is then removed by chemical dissolution. The SiC was then etched again through pure CF4 at bias power below 50W to achieve a radiused etch of the micropillar edges.
Further, the diamond layer growth step in the step 4 is to control the microwave power at 3-5kW and the deposition temperature at 640-780 ℃ and to nucleate at 5-8% methane ratio for 1-6h, and then to grow the diamond layer at 2-5%.
Further, the laser scanning planarization step of the diamond growth surface in the step 5 is to set the laser incidence angle at 60-80 degrees, the current at 60-70A, the pulse at 400-. Then, the diamond growth surface is polished by diamond powder with the granularity of 1 mu m, 500nm and 100nm respectively and then is placed on a precision diamond polishing disk for final planarization. The key of the implementation process of the invention is as follows:
1) the spacing of the micropillars obtained by SiC etching needs to be more than 2 μm. Experiments prove that when the spacing is smaller than 2 mu m, because the space between the microcolumns is too small, gas flow cannot effectively enter the region in the plasma chemical vapor deposition process, so that a diamond growth interface has a large number of hole defects and cannot be uniformly contacted with SiC, and the interface thermal conductivity and the mechanical stability are obviously influenced. Meanwhile, the height of the micro-pillars should not exceed 10 μm (in the case of micro-pillar spacing larger than 20 μm). Again, the excessive aspect ratio spacing is detrimental to the high quality nucleation growth of the depressed portion diamond.
2) In the process of SiC patterned etching, CF is used for SiC by a gas source4:O2Etching the SiC to an etching depth of 1-20 μm under the conditions of a ratio of 5:1-2:1 and a bias power of 100-. To ensure faster etch rates and pattern integrity. And then cleaning and removing the metal mask by adopting a chemical dissolution method. The SiC was then passed through pure CF again4The SiC is etched at a bias power below 50W. And (3) by eliminating oxidation and bias ion bombardment, utilizing the existing edge effect to realize the arc etching of the edge of the micro-column.
3) Placing SiC with a micro-column structure in a microwave plasma chemical vapor deposition chamber, controlling the microwave power at 3-5kW and the deposition temperature at 640-780 ℃ and controlling the methane proportion at 5-8% for nucleation for 1-6h, and then growing a diamond layer at 2-5%.
4) The flattening of the diamond surface not only can meet the practical application requirements of the SiC substrate, but also can provide a flat surface foundation for future GaN deposition and circuit preparation. Namely, after the diamond deposition layer completely covers the microcolumn and has a certain thickness, laser scanning is adopted to flatten the diamond growth surface and then precision polishing is carried out. The YAG laser local ablation technology is adopted to realize the flattening processing of the diamond growth surface in a plane scanning mode, so that the diamond flattening process can be greatly accelerated, and cracks possibly caused by directly mechanically polishing the very rough surface of the diamond in a growth state can be effectively avoided. If a high-power right-angle scanning is adopted, the possibility of cracking caused by instantaneous heat concentration can be caused, and the surface flattening effect can be influenced by severe ablation. Therefore, the laser incidence angle is required to be 60-80 deg., the current is 60-70A, the pulse is 400-. Then, diamond growth surfaces are polished by diamond powder with the granularity of 1 mu m, 500nm and 100nm respectively and then are placed on a precise diamond polishing disk for final planarization.
Compared with the prior art, the invention has the beneficial effects that:
1) for a solid-solid interface of two crystalline materials, it is desirable to maintain high crystallinity at the interface. In general, structural defects generated by the non-compact grain arrangement characteristic of the grain boundary of the diamond growth surface on the surface of the non-diamond solid can seriously reduce the heat conduction performance of the interface. The SiC surface deposited diamond with the periodic micro-column structure can not only improve the contact area of SiC and the surface deposited diamond, but also weaken the influence of the single plane interface diamond nucleation surface high-density crystal structure defects, thereby more effectively utilizing the ultrahigh heat conduction characteristic of the diamond to further improve the heat diffusion capability of the SiC device. In addition, the periodic microstructure surface can also improve nucleation and growth efficiency during diamond deposition. Namely, a local gas flow field can be formed between the microcolumns in the diamond growth process, so that CH is ensuredxThe groups can stay longer at the interface, improving nucleation growth between microstructures. Meanwhile, the growth mode of the diamond film can be homogenized to a certain degree, the formation of the crystal boundary hole defects of the nucleation surface is improved, and the results of stress nonuniformity and overlarge stress in a single direction which may exist in the disordered nucleation growth of a single plane interface are avoided.
2) The SiC surface growth diamond with the periodic micro-column structure can improve the combination of SiC and diamond and improve the interface cracking easily caused by insufficient binding force of a single plane interface. The periodic micro-column structure can block the crack expansion of a local interface and improve the possibility of cracking caused by stress to a certain extent. More importantly, the structure can avoid cracking failure possibly caused by stress in the process of thinning the subsequent SiC layer and epitaxially growing GaN on the surface of SiC at the temperature of 1000 ℃. Therefore, the processing stability of the wide bandgap semiconductor material is effectively improved, and the preparation and packaging of related electronic devices in the future and the operation stability of the final devices under the conditions of high power and high heat flux density are ensured.
Drawings
FIG. 1 is a method of making a high thermal conductivity diamond enhanced silicon carbide (SiC) substrate of the present invention.
Detailed Description
Detailed description of the invention
The carbon polar surface of the SiC is coated with photoresist in a spinning mode, and ultraviolet photoetching is achieved through a mask plate. Then, periodic micropores with a diameter of 2 μm and an interval of 4 μm were formed by developing to remove photoresist, and the periodically arranged diamond patterned surface was exposed. And depositing a Ti metal mask for 50nm and then depositing Al metal for 150nm on the SiC with the patterned photoresist by electron beam evaporation. And removing the residual photoresist to obtain SiC with the metal pattern mask deposited on the surface. To SiC by gas source CF4:O2And etching the SiC to the etching depth of 2 mu m under the conditions that the proportion is 5:1 and the bias power is 300W. The metal mask is then removed by chemical dissolution. The SiC was then passed through pure CF again4And etching the SiC under the condition of bias power of 20W to realize circular arc etching of the edge of the microcolumn. The patterned SiC wafer was then placed in a microwave plasma chamber with a microwave power of 3kW and a deposition temperature of 640 ℃ for 6h nucleation with a methane ratio of 5% followed by growth of a diamond layer at 2%. And after the diamond growth is finished, carrying out laser scanning and flattening on the growth surface of the diamond, wherein the laser incidence angle is 70 degrees, the current is 60 degrees A, the pulse is 400 microseconds, the frequency is 200Hz, and the scanning speed is 200 mm/min. And then polishing the diamond growth surface by gradually adopting diamond powder with the granularity of 1 mu m, 500nm and 100nm respectively, and placing the polished diamond powder on a precise diamond polishing disk for final planarization.
Detailed description of the invention
The carbon polar surface of the SiC is coated with photoresist in a spinning mode, and ultraviolet photoetching is achieved through a mask plate. Then, periodic micropores with a diameter of 2 μm and an interval of 2 μm were formed by removing photoresist by development to expose the periodically arranged diamond patterned surface. And depositing a Ti metal mask for 30nm and then depositing Al metal for 120nm on the SiC with the patterned photoresist by electron beam evaporation. And removing the residual photoresist to obtain SiC with the metal pattern mask deposited on the surface. To SiC by gas source CF4:O2And etching the SiC to the etching depth of 1 mu m under the conditions that the proportion is 4:1 and the bias power is 200W. The metal mask is then removed by chemical dissolution. The SiC was then passed through pure CF again4And etching the SiC under the condition that the bias power is 10W to realize the circular arc etching of the edge of the micro-column. The patterned SiC wafer was then placed in a microwave plasma chamber with microwave power controlled at 4kW and deposition temperature at 680 ℃ for 4h nucleation with methane ratio controlled at 6% followed by growth of a diamond layer at 3%. And after the diamond growth is finished, carrying out laser scanning and flattening on the growth surface of the diamond, wherein the incidence angle of laser is 75 degrees, the current is 60A, the pulse is 400 mus, the frequency is 200Hz, and the scanning speed is 300 mm/min. And then polishing the diamond growth surface by gradually adopting diamond powder with the granularity of 1 mu m, 500nm and 100nm respectively, and placing the polished diamond powder on a precise diamond polishing disk for final planarization.
Detailed description of the invention
The carbon polar surface of the SiC is coated with photoresist in a spinning mode, and ultraviolet photoetching is achieved through a mask plate. Then, periodic micropores with a diameter of 5 μm and an interval of 8 μm were formed by developing to remove photoresist, and the periodically arranged diamond patterned surface was exposed. And depositing a Ti metal mask 40nm and then depositing Al metal 150nm on the SiC with the patterned photoresist by electron beam evaporation. And removing the residual photoresist to obtain SiC with the metal pattern mask deposited on the surface. To SiC by gas source CF4:O2And etching the SiC to the etching depth of 3 mu m under the conditions that the proportion is 2:1 and the bias power is 100W. The metal mask is then removed by chemical dissolution. The SiC was then passed through pure CF again4Etching SiC under the condition of bias power of 10W to realize the arc of the edge of the micro-columnAnd (5) forming and etching. The patterned SiC wafer was then placed in a microwave plasma chamber with a microwave power of 5kW and a deposition temperature of 740 ℃ for nucleation for 1h at a methane ratio of 8%, followed by growth of a diamond layer at 4%. And after the diamond growth is finished, carrying out laser scanning and flattening on the diamond growth surface, wherein the laser incidence angle is 75 degrees, the current is 65 degrees A, the pulse is 400 microseconds, the frequency is 250Hz, and the scanning speed is 400 mm/min. And then polishing the diamond growth surface by gradually adopting diamond powder with the granularity of 1 mu m, 500nm and 100nm respectively, and placing the polished diamond powder on a precise diamond polishing disk for final planarization.
Claims (5)
1. A preparation method of a high-thermal-conductivity diamond-enhanced silicon carbide substrate is characterized in that patterning is realized by gluing, photoetching and developing on a carbon polar surface of SiC, so that the carbon polar surface of the SiC is provided with patterned photoresist; then adopting electron beam evaporation or magnetron sputtering metal mask; after removing the photoresist, carrying out reactive ion etching, mask removing and secondary ion etching on the SiC with the periodically arranged metal mask to obtain a SiC micro-column array; then growing a diamond layer by a microwave plasma chemical vapor deposition technology; after the diamond layer completely covers the microcolumn and has a certain thickness, the diamond growth surface is scanned by laser to be flattened and then precisely polished, so that the high-thermal-conductivity diamond-reinforced SiC substrate is obtained, and a foundation is laid for obtaining high-power and high-frequency SiC/diamond and GaN/SiC/diamond wafers by thinning the SiC silicon polar surface and depositing GaN on the surface at high temperature in the future;
the reactive ion etching step of the SiC periodic microcolumn structure comprises the following steps: to SiC by gas source CF4:O2Etching SiC under the conditions that the proportion is 5:1-2:1 and the bias power is 100-; the metal mask is then removed by chemical dissolution, and the SiC is then passed through pure CF again4And etching the SiC under the condition that the bias power is lower than 50W to realize the circular arc etching of the edge of the micro-column.
2. The method for preparing a diamond-enhanced silicon carbide substrate with high thermal conductivity according to claim 1, characterized by comprising the steps of:
step 1: SiC surface gluing and exposure patterning
Spin-coating photoresist on the carbon polar surface of the SiC, and realizing ultraviolet lithography based on a mask plate; then, developing and removing photoresist to realize periodic micropores, and exposing the periodically arranged diamond patterned surface;
step 2: deposition of metal masks
Depositing a metal mask on the SiC with the patterned photoresist through electron beam evaporation or magnetron sputtering; removing the residual photoresist to obtain SiC with the metal pattern mask deposited on the surface;
and step 3: reactive ion etching of SiC periodic microcolumn structures
Preparing the SiC microcolumn and etching the edges in an arc shape by reactive ion etching;
and 4, step 4: growth of diamond layer
Placing SiC with the micro-column structure in a microwave plasma chemical vapor deposition chamber, and growing a diamond layer to cover the micro-column structure;
and 5: laser scanning leveling and grinding polishing of diamond growth surface
The YAG laser local ablation technology is adopted to realize the flattening processing of the diamond growth surface in a plane scanning mode, so that the flatness of the surface of the diamond growth surface is realized; and then further reducing the surface roughness of the diamond through grinding and precise polishing of the diamond nano particles.
3. The method as claimed in claim 2, wherein the step of depositing the metal mask comprises depositing a 10-50nm titanium layer and then depositing a 100-150nm aluminum layer, wherein the substrate temperature does not exceed 100 ℃ during the coating process.
4. The method for preparing a diamond enhanced silicon carbide substrate with high thermal conductivity according to claim 2, wherein the step 4 of growing the diamond layer comprises the following steps: controlling the microwave power at 3-5kW and the deposition temperature at 640-780 ℃, controlling the methane proportion at 5-8% for nucleation for 1-6h, and then growing the diamond layer at 2-5% according to the methane proportion.
5. The method as claimed in claim 2, wherein the step of laser scanning and planarization of the diamond growth surface in step 5 comprises a laser incident angle of 60-80 °, a current of 60-70A, a pulse of 400-; and then polishing the diamond growth surface by gradually adopting diamond powder with the granularity of 1 mu m, 500nm and 100nm respectively, and placing the polished diamond powder on a precise diamond polishing disk for final planarization.
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| CN115125511B (en) * | 2022-06-06 | 2023-06-02 | 北京科技大学 | Preparation method of curved-surface diamond tritium-titanium target with micro-channel structure |
| CN115365505A (en) * | 2022-08-12 | 2022-11-22 | 广东工业大学 | Metal-based diamond product and preparation method thereof |
| CN115369386B (en) * | 2022-08-15 | 2023-07-25 | 北京科技大学 | Method for depositing diamond on microstructure substrate |
| CN116666199B (en) * | 2023-08-02 | 2023-10-03 | 中国科学院微电子研究所 | SiC/diamond composite substrate manufacturing method based on temporary carrier |
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| US7501330B2 (en) * | 2002-12-05 | 2009-03-10 | Intel Corporation | Methods of forming a high conductivity diamond film and structures formed thereby |
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