Solid material surface processing method

Abstract

The invention provides a solid material surface processing method which comprises the following steps: S1, arranging a conductive film layer on the surface of a solid material to obtain a semi-finished product A; s2, a groove is formed in the surface of the semi-finished product A with the ion beam current of 0.05-0.5 [mu] A through the focused ion beam technology, and a semi-finished product B is prepared; and S3, removing the conductive film layer on the surface of the semi-finished product B. According to the processing method for the surface of the solid material, the current of the ion beam can be accurately regulated and controlled, so that grooves with different depths are accurately formed in the surface of the solid material, and the bottoms of the grooves protrude towards the notch direction of the grooves. The surface of the finished product prepared by the processing method provided by the invention is provided with nanoscale grooves with different depths, the bottoms of the grooves protrude towards the notch direction of the grooves, and the protrusions at the bottoms of the grooves enable design patterns formed by the grooves to present higher definition and contrast through enhanced optical contrast characteristics, so that the product quality is improved. Good mechanical stability and damage resistance are realized.

Description

Technical Field

[0001] This application relates to the field of etching technology, and in particular to a method for processing the surface of a solid material. Background Technology

[0002] Currently, the main surface processing methods for solid materials include reactive ion etching (RIE), inductively coupled plasma (ICP), deep trench reactive ion etching (DRIE), and focused ion beam etching (FIB). Among them, focused ion beam etching (FIB) is widely used for small-batch sample preparation due to its high processing precision and the fact that it does not require a mask. However, it has significant drawbacks: First, the ion beam spot size increases with the beam current, requiring the use of a small beam current to process fine patterns, resulting in low etching efficiency. Second, when processing non-conductive materials, surface charge accumulation can cause ion beam trajectory deviation, severely affecting the processing precision of submicron-level structures.

[0003] To address the charge accumulation problem, existing technologies generally employ electron neutralization guns (E-Gun) for charge compensation. However, this approach has inherent drawbacks: firstly, the spatiotemporal synchronization accuracy of the electron and ion beams requires extremely high precision, and deviations in electron injection can easily lead to a significant decrease in etching rate or pattern deformation; secondly, the additional electron optical system significantly increases equipment complexity and complicates electromagnetic shielding design. Furthermore, when processing wide-bandgap semiconductor materials such as diamond, the electron neutralization gun struggles to balance the conflict between charge compensation and material activity suppression. Excessive electron injection neutralizes the chemical activity of CH dangling bonds on the material surface, reducing the etching rate; while insufficient charge compensation leads to anisotropic lattice distortion, further degrading processing quality. Summary of the Invention

[0004] This invention provides a method for processing the surface of a solid material. This method allows for precise control of the ion beam current, thereby accurately constructing grooves of varying depths on the surface of the solid material, with the bottom of the grooves bulging towards the groove opening. The finished product surface obtained by the processing method of this invention has nanoscale grooves of varying depths, and the bottom of the grooves bulges towards the groove opening. This bulging at the bottom of the grooves enhances optical contrast, resulting in a design pattern with high clarity and contrast, and good mechanical stability and damage resistance.

[0005] According to one aspect of the present invention, a method for processing the surface of a solid material is provided, comprising the following steps: S1. forming a conductive film layer on the surface of the solid material to obtain a semi-finished product A; S2. forming a groove on the surface of the semi-finished product A using focused ion beam technology with an ion beam current of 0.05~0.5 μA to obtain a semi-finished product B; S3. removing the conductive film layer from the surface of the semi-finished product B.

[0006] This invention effectively solves the problems of dim, blurred, or distorted patterns caused by charge accumulation or neutralization imbalance during processing by setting a conductive film layer on the surface of solid materials, thereby improving the clarity and contrast of the finished pattern. Secondly, the conductive film layer also acts as an energy buffer layer, preventing ion beam etching damage to the solid material. This improves the uniformity of ion beam etching on the solid material surface, reducing amorphization, and enhances the solid material's resistance to high-dose ion beam etching, thus further increasing the ion beam current threshold suitable for solid material surface processing. Therefore, by precisely controlling the ion beam current, grooves of different depths can be accurately constructed on the surface of the solid material. These grooves of different depths form the pattern in the processed product, preventing direct contact of the pattern with external forces and improving the scratch resistance of the finished product. In practical applications, grooves are formed by sputtering and etching a large dose of ion beam agent on the surface of a solid material. During this process, some ions can be injected into the solid material, causing the solid material lattice to expand and strain. This expansion of the solid lattice results in the bottom of the groove protruding towards the groove opening. These protrusions not only allow for more precise and flexible control of the groove depth, but also improve the optical properties of the solid material, giving the pattern formed by these grooves excellent clarity and contrast.

[0007] Preferably, the solid material includes at least one of diamond, moissanite, silicon, gallium nitride, sapphire, ruby, emerald, crystal, tourmaline, aquamarine, and morganite.

[0008] Preferably, the setting method in S1 includes at least one of magnetron sputtering and electron beam evaporation.

[0009] Preferably, the resistivity of the conductive film layer is 1×10⁻⁶. -7 ~1×10 -9 Ω·m.

[0010] Preferably, the conductive film layer includes at least one of gold, platinum, copper, chromium, and aluminum. When gold, platinum, copper, chromium, or aluminum is used as the material for the conductive film layer, the bonding strength between the conductive film layer and the solid material substrate can be further enhanced, and the impact of high-dose ion beams can be effectively resisted, optimizing the ion energy transfer efficiency. This allows the conductive film layer to maintain structural stability during processing, effectively improving the processing precision of the solid material surface. Preferably, the conductive film layer includes at least one of gold, platinum, and chromium.

[0011] Preferably, the thickness of the conductive film layer obtained by S1 is 5~500 nm.

[0012] Preferably, the thickness of the conductive film layer obtained by S1 is 10~100 nm.

[0013] Preferably, the processing time is 5 to 300 seconds. By adjusting the thickness of the conductive film layer to 5 to 500 nm and the processing time to 5 to 300 seconds, the ion beam can effectively penetrate the conductive film layer and protect the solid material substrate, thereby improving the scratch resistance of the finished product. The current intensity and processing time together determine the ion dose injected into the solid material, thereby increasing the processing rate of the solid material and adjusting the groove depth to improve the processing accuracy.

[0014] According to another aspect of the present invention, a solid material is provided, the surface of which has grooves, the bottom of which protrudes towards the opening of the groove. The finished product obtained by the processing method provided by the present invention has the following characteristics: the surface of the finished product has nanoscale grooves of varying depths, and the bottom of the grooves protrudes towards the opening of the groove. This protrusion at the bottom of the groove enhances optical contrast, resulting in higher clarity and contrast for the design pattern formed by the grooves. Furthermore, the depth of the grooves and the height of the protrusion at the bottom of the grooves are both lower than the surface of the solid material, preventing scratches on the protrusions due to external forces, thus possessing a certain degree of mechanical stability and damage resistance.

[0015] Preferably, the surface of the solid material has at least two grooves of different depths.

[0016] Preferably, the surface of the solid material has a plurality of grooves.

[0017] Preferably, the depth of the groove is 10~100 nm and the width of the groove is 20~50000 nm. Attached Figure Description

[0018] Figure 1 The grayscale image of the pattern designed in Example 1; Figure 2 The structural diagrams of the processed products provided in Comparative Example 1 (top) and Example 1 (bottom) under an optical microscope; Figure 3 This is a test diagram of the groove depth of the finished product provided in Example 1. Detailed Implementation

[0019] To enable those skilled in the art to better understand the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments.

[0020] Example 1 This embodiment provides a method for processing the surface of a solid material, including the following steps: S1. A 50 nm thick layer with a resistivity of 1.29 × 10⁻⁶ was deposited on the diamond surface by magnetron sputtering. -7A chromium film with an Ω·m thickness is used as a conductive film layer to obtain semi-finished product A; S2. Using focused ion beam technology, a groove is formed on the surface of semi-finished product A under the conditions of ion beam current of 0.3 μA and processing time of 15 seconds to obtain semi-finished product B; Specifically, ensure the surface of the diamond to be patterned is placed vertically upwards, then place it in the focused ion beam sample chamber and initiate vacuum extraction; once the vacuum conditions are met, activate SEM mode, locate the position where the pattern needs to be created, and lock the distance between the sample and the focused ion beam gun; input the grayscale image of the designed pattern ( Figure 1 The maximum ion beam dose set by the parameter machine is denoted as Vinject. Vinject = processing ion beam current × processing time. The ion beam injection dose corresponding to each pixel = gray value / 255 × Vinject. Start the etching mode. After etching is completed, turn off the vacuum pump and purge the sample with gas. S3. Remove the conductive film layer on the surface of semi-finished product B by chemical etching to obtain the finished product. Figure 2 (Below) is a structural diagram of the finished product provided in this embodiment under an optical microscope.

[0021] Example 2 This embodiment provides a method for processing the surface of a solid material, including the following steps: S1. A 50 nm thick layer with a resistivity of 1.29 × 10⁻⁶ was deposited on the diamond surface by magnetron sputtering. -7 A chromium film with an Ω·m thickness is used as a conductive film layer to obtain semi-finished product A; S2. Using focused ion beam technology, a groove is formed on the surface of semi-finished product A under the conditions of ion beam current of 0.05 μA and processing time of 15 seconds to obtain semi-finished product B; Specifically, ensure the surface of the diamond to be patterned is placed vertically upwards, then place it in the focused ion beam sample chamber and initiate vacuum extraction; once the vacuum conditions are met, activate SEM mode, locate the position where the pattern needs to be created, and lock the distance between the sample and the focused ion beam gun; input the grayscale image of the designed pattern ( Figure 1 The maximum ion beam dose set by the parameter machine is denoted as Vinject. Vinject = processing ion beam current × processing time. The ion beam injection dose corresponding to each pixel = gray value / 255 × Vinject. Start the etching mode. After etching is completed, turn off the vacuum pump and purge the sample with gas. S3. Remove the conductive film layer on the surface of semi-finished product B by chemical etching to obtain the finished product.

[0022] Example 3 This embodiment provides a method for processing the surface of a solid material, including the following steps: S1. A 50 nm thick layer with a resistivity of 1.29 × 10⁻⁶ was deposited on the diamond surface by magnetron sputtering. -7 A chromium film with an Ω·m thickness is used as a conductive film layer to obtain semi-finished product A; S2. Using focused ion beam technology, a groove is formed on the surface of semi-finished product A under the conditions of ion beam current of 0.5 μA and processing time of 15 seconds to obtain semi-finished product B; Specifically, ensure the surface of the diamond to be patterned is placed vertically upwards, then place it in the focused ion beam sample chamber and initiate vacuum extraction; once the vacuum conditions are met, activate SEM mode, locate the position where the pattern needs to be created, and lock the distance between the sample and the focused ion beam gun; input the grayscale image of the designed pattern ( Figure 1 The maximum ion beam dose set by the parameter machine is denoted as Vinject. Vinject = processing ion beam current × processing time. The ion beam injection dose corresponding to each pixel = gray value / 255 × Vinject. Start the etching mode. After etching is completed, turn off the vacuum pump and purge the sample with gas. S3. Remove the conductive film layer on the surface of semi-finished product B by chemical etching to obtain the finished product.

[0023] Example 4 This embodiment refers to Embodiment 1 for processing the diamond surface. The difference between this embodiment and Embodiment 1 is that in S1, a thickness of 50 nm and a resistivity of 2.44 × 10⁻⁶ are deposited on the diamond surface by magnetron sputtering. -8 A gold film with a density of Ω·m is used as the conductive film layer to obtain semi-finished product A. Except for the differences mentioned above, the materials, formulation ratios, and preparation operations used in this embodiment are strictly consistent with those in Example 1.

[0024] Example 5 This embodiment refers to Embodiment 1 for processing the diamond surface. The difference between this embodiment and Embodiment 1 is that in S1, a thickness of 50 nm and a resistivity of 1.06 × 10⁻⁶ are deposited on the diamond surface by magnetron sputtering. -7 A platinum film with a density of Ω·m is used as the conductive film layer to obtain semi-finished product A. Except for the differences mentioned above, the materials, formulation ratios, and preparation operations used in this embodiment are strictly consistent with those in Example 1.

[0025] Example 6 This embodiment refers to Embodiment 1 for processing the diamond surface. The difference between this embodiment and Embodiment 1 is that in S1, a thickness of 50 nm and a resistivity of 1.68 × 10⁻⁶ are deposited on the diamond surface by magnetron sputtering. -8 A copper film with a density of Ω·m is used as the conductive film layer to obtain semi-finished product A. Except for the differences mentioned above, the materials, formulation ratios, and preparation operations used in this embodiment are strictly consistent with those in Example 1.

[0026] Example 7 This embodiment refers to Embodiment 1 for processing the diamond surface. The difference between this embodiment and Embodiment 1 is that in S1, a thickness of 50 nm and a resistivity of 2.82 × 10⁻⁶ are deposited on the diamond surface by magnetron sputtering. -8 An aluminum film with a density of Ω·m is used as the conductive film layer to obtain semi-finished product A. Except for the differences mentioned above, the materials, formulation ratios, and preparation operations used in this embodiment are strictly consistent with those in Example 1.

[0027] Example 8 This embodiment processes the diamond surface according to Example 1. The difference between this embodiment and Example 1 is that the thickness of the conductive film layer obtained in S1 is 5 nm, and the processing time using focused ion beam technology in S2 is 5 seconds. Apart from the above differences, the materials, formulation ratios, and preparation operations used in this embodiment are strictly consistent with those in Example 1.

[0028] Example 9 This embodiment processes the diamond surface according to Example 1. The difference between this embodiment and Example 1 is that the thickness of the conductive film layer obtained in S1 is 500 nm, and the processing time in S2 is 300 seconds. Apart from the above differences, the materials, formulation ratios, and preparation operations used in this embodiment are strictly consistent with those in Example 1.

[0029] Example 10 This embodiment processes the diamond surface according to Example 1. The difference between this embodiment and Example 1 is that the thickness of the conductive film layer obtained in S1 is 3 nm, and the processing time in S2 is 3 seconds. Apart from the above differences, the materials, formulation ratios, and preparation operations used in this embodiment are strictly consistent with those in Example 1.

[0030] Example 11 This embodiment processes the diamond surface according to Example 1. The difference between this embodiment and Example 1 is that the thickness of the conductive film layer obtained in S1 is 550 nm, and the processing time in S2 is 350 seconds. Apart from the above differences, the materials, formulation ratios, and preparation operations used in this embodiment are strictly consistent with those in Example 1.

[0031] Comparative Example 1 This comparative example provides a method for processing the surface of a solid material, the specific steps of which are as follows: S1. Clean the surface of the diamond with water; S2. Apply photoresist to the diamond surface and bake at 90°C for 300 seconds; S3. Design patterns are directly written onto the photoresist surface using ultraviolet laser, followed by exposure; S4. Use a developer to remove the photoresist that has been exposed on the diamond surface; S5. Dry etching of the diamond surface is performed using a reactive plasma etching system; S6. Remove the remaining photoresist from the diamond surface using chemical agents to obtain the finished product. Among these steps... Figure 2 (Above) is a structural diagram of the processed product provided in this comparative example under an optical microscope.

[0032] Comparative Example 2 This comparative example processes the diamond surface according to Example 1. The difference between this comparative example and Example 1 is that step S1 is omitted. That is, no conductive film layer is applied to the diamond surface in this comparative example; instead, focused ion beam technology is used directly to form grooves on the diamond surface under conditions of an ion beam current of 0.3 μA and a processing time of 15 seconds. Apart from the above differences, the materials, formulation ratios, and preparation operations used in this comparative example are strictly consistent with those in Example 1.

[0033] Comparative Example 3 This comparative example processes the surface of a diamond according to Example 1. The difference between this comparative example and Example 1 is that in step S2, focused ion beam technology is used to form grooves on the surface of the semi-finished product A under conditions of an ion beam current of 0.03 μA and a processing time of 15 seconds. Apart from the above differences, the materials, formulation ratios, and preparation operations used in this comparative example are strictly consistent with those in Example 1.

[0034] Comparative Example 4 This comparative example processes the surface of a diamond according to Example 1. The difference between this comparative example and Example 1 is that in step S2, focused ion beam technology is used to form grooves on the surface of the semi-finished product A under conditions of an ion beam current of 0.6 μA and a processing time of 15 seconds. Apart from the above differences, the materials, formulation ratios, and preparation operations used in this comparative example are strictly consistent with those in Example 1.

[0035] Test case 1. Test subjects: The finished products obtained in Examples 1 to 11 and Comparative Examples 1 to 4 were used as test subjects.

[0036] 2. Test items: (1) Groove depth and groove width: The groove depth and groove width on the surface of the test object were measured using a white light interferometer. Before measurement, the instrument was calibrated using a step height standard template. After cleaning the sample, it was fixed on the sample stage, and the measurement was performed using vertical scanning interferometry (PSI) mode. After obtaining the three-dimensional topographic data of the surface through the instrument software, at least five profile lines perpendicular to the groove were randomly selected, and the depth and width data of each profile line were extracted. The corresponding arithmetic mean was calculated as the groove depth and groove width.

[0037] (2) Scratch resistance: Under the conditions of reciprocating motion with a load of 1 kgf and a frequency of 30 times / minute, the pattern on the surface of the test object was subjected to friction test using a corundum friction head, with a single stroke of 250,000 nm. The performance rating was divided according to the number of friction cycles experienced before the pattern on the surface of the test object showed obvious damage: 1~39 cycles, rated as "weak"; 40~69 cycles, rated as "average"; 70~100 cycles, rated as "strong".

[0038] (3) Contrast Ratio: The contrast ratio was measured using a colorimeter under D65 standard light source and 10° observation angle conditions. The CIE L values ​​(brightness) of the pattern area and background area of ​​the test object were measured separately, and the absolute difference ΔL was calculated. The contrast ratio rating criteria are as follows: when ΔL*≥30, the rating is "strong"; when 15≤ΔL*<30, the rating is "medium"; when ΔL*<15, the rating is "weak".

[0039] 3. Test Results: Table 1. Relevant performance tests of the test objects

[0040] The relevant performance test results of the processed products provided in Examples 1 to 11 were compared with the relevant performance test results of the processed products provided in Comparative Examples 1 to 4. As shown in Table 1, it can be found that the processed products provided in Comparative Examples 1 to 4 cannot simultaneously have good scratch resistance and contrast, while the processed products provided in Examples 1 to 11 can achieve a "normal" or "strong" rating in scratch resistance and a "strong" rating in contrast.

[0041] In Comparative Example 1, the finished product was obtained by plasma etching. Test results showed that although the groove depth formed by the finished product in Comparative Example 1 was greater than that in Example 1, the contrast of the finished product in Comparative Example 1 was significantly worse than that in Example 1. Figure 2 (Above) it can be seen that the patterns on finished products produced by plasma etching have very low contrast and almost no brightness under an optical microscope, and there is a severe color difference between the edges and the center of the pattern; while from Figure 2(Below) It can be seen that the concave structure made by the processed product provided in Example 1 has high contrast, and the black and white are clearly distinguishable under the microscope, and the colors are highly consistent.

[0042] Compared to Example 1, the finished product provided in Comparative Example 2 did not have a conductive film layer during processing. Test results showed that the scratch resistance of the finished product in Comparative Example 2 was significantly worse than that in Example 1. This is because, in Comparative Example 2, no conductive film layer was used as a buffer during processing. The kinetic energy of the ion beam directly acted on the solid material, causing severe lattice damage and amorphization. This resulted in a microscopically fragile layer forming at the bottom and sidewalls of the groove. This fragile layer peeled off or cracked when scratched by external force, leading to a significant decrease in scratch resistance.

[0043] Compared to Example 1, the difference between the processed products provided in Comparative Examples 3 and 4 lies in the magnitude of the ion beam current during processing. Test results show that the scratch resistance of the processed products provided in Comparative Examples 3 and 4 is significantly worse than that of Example 1. This is because the ion beam current used in Comparative Example 3 during processing is too small, resulting in insufficient etching energy. Consequently, the groove depth formed on the solid material surface is too shallow, and the shallow pattern is more easily worn away by external scratching, resulting in weak scratch resistance. Conversely, the ion beam current used in Comparative Example 4 during processing is too large. The conductive film layer cannot effectively buffer the ion beam, and the instantaneous energy input of the ion beam exceeds the ideal etching threshold of the solid material, causing excessive etching damage and surface amorphization. Cracks appear in the grooves on the solid material surface, and these cracks further expand under external scratching, resulting in weak scratch resistance.

[0044] The finished products provided in Examples 1 and 4-7 were compared. The difference between these finished products lies in the material of the conductive film layer. The test results show that as the resistivity of the material used in the conductive film layer increases, the groove depth of the finished product decreases. This indicates that using gold, platinum, copper, chromium, or aluminum as the material for the conductive film layer can further enhance the bonding strength between the conductive film layer and the solid material substrate, effectively withstand the impact of high-dose ion beams, optimize ion energy transfer efficiency, and enable the conductive film layer to maintain structural stability during processing, effectively improving the processing precision of solid material surfaces.

[0045] The processed products provided in Examples 1 and 8-11 were compared. The differences between these processed products lie in the thickness of the conductive film and the processing time. The test results show that as the thickness of the conductive film and the processing time increase, the test results of the processed products exhibit the following trend: the groove depth of the processed products decreases, and the scratch resistance increases. This indicates that when the thickness of the conductive film is controlled at 5-500 nm and the processing time at 5-300 seconds, the ion beam can effectively penetrate the conductive film and protect the solid material substrate, thereby improving the scratch resistance of the processed product. The current intensity and processing time together determine the ion dose injected into the solid material, increasing the processing rate of the solid material, and controlling the groove depth, thereby improving the processing accuracy. In the above examples, the processed products provided in Examples 1 and 9 have the best overall performance, possessing a moderate groove depth and achieving a "strong" rating in scratch resistance and contrast.

[0046] The above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention, but such modifications or substitutions are all within the scope of protection of the present invention.

Claims

1. A method of machining a surface of a solid material, characterized in that, The method comprises the following steps: S1. setting a conductive film layer on the surface of a solid material to obtain a semi-finished product A; S2. forming a groove on the surface of the semi-finished product A by using a focused ion beam technology with an ion beam current of 0.05-0.5 μA to obtain a semi-finished product B; S3. removing the conductive film layer on the surface of the semi-finished product B.

2. The method of claim 1, wherein The resistivity of the conductive film layer is 1 x 10 -7 ~1 x 10 -9 Ω-m.

3. The method of claim 1 wherein the step of processing further comprises the step of: The conductive film layer comprises at least one of gold, platinum, copper, chromium and aluminum.

4. The method of claim 3, wherein the step of processing is performed by a computer. The conductive film layer comprises at least one of gold, platinum and chromium.

5. The method of claim 1 wherein the step of processing further comprises the step of: 5.

1. applying a coating to the surface of the substrate. The thickness of the conductive film layer obtained by the S1 is 5-500 nm. ​ 6. The processing method as described in claim 1, characterized in that, The processing time is 5-300 seconds.

7. A solid state material, characterized in that, The surface of the solid material has a groove, and the bottom of the groove is convex towards the direction of the groove opening.

8. The solid state material of claim 7, wherein, The surface of the solid material has at least one or more grooves with different depths.

9. The solid state material of claim 7, wherein, The surface of the solid material has a plurality of grooves.

10. The solid state material of claim 7, wherein, The depth of the groove is 10-100 nm, and the width of the groove is 20-50000 nm.

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