WO2022000120A1 - 一种石墨岛滑块阵列的制备方法 - Google Patents
一种石墨岛滑块阵列的制备方法 Download PDFInfo
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- WO2022000120A1 WO2022000120A1 PCT/CN2020/098477 CN2020098477W WO2022000120A1 WO 2022000120 A1 WO2022000120 A1 WO 2022000120A1 CN 2020098477 W CN2020098477 W CN 2020098477W WO 2022000120 A1 WO2022000120 A1 WO 2022000120A1
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- Prior art keywords
- graphite
- photoresist
- island
- preparation
- grain
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 73
- 239000010439 graphite Substances 0.000 title claims abstract description 73
- 238000004519 manufacturing process Methods 0.000 title abstract description 4
- 238000003491 array Methods 0.000 title description 5
- 238000005530 etching Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 17
- 229920002120 photoresistant polymer Polymers 0.000 claims description 40
- 238000002360 preparation method Methods 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001514 detection method Methods 0.000 claims description 8
- 238000000059 patterning Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 238000001020 plasma etching Methods 0.000 claims description 6
- 229910052681 coesite Inorganic materials 0.000 claims description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 229910052682 stishovite Inorganic materials 0.000 claims description 5
- 229910052905 tridymite Inorganic materials 0.000 claims description 5
- 238000004528 spin coating Methods 0.000 claims description 4
- 238000000333 X-ray scattering Methods 0.000 claims description 3
- 238000005229 chemical vapour deposition Methods 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 3
- 238000001887 electron backscatter diffraction Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 abstract description 13
- 238000007689 inspection Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- 238000012545 processing Methods 0.000 description 6
- 238000009659 non-destructive testing Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012937 correction Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00198—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems comprising elements which are movable in relation to each other, e.g. comprising slidable or rotatable elements
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
- B81B5/00—Devices comprising elements which are movable in relation to each other, e.g. comprising slidable or rotatable elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00206—Processes for functionalising a surface, e.g. provide the surface with specific mechanical, chemical or biological properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
Definitions
- the invention relates to the field of ultra-slippery solid structures, in particular to a method for preparing a graphite island slider array in batches.
- Structural super-slip is one of the ideal solutions to solve the problem of friction and wear.
- Structural super-slip refers to the friction between two van der Waals solid surfaces (such as graphene, molybdenum disulfide and other two-dimensional material surfaces) that are atomically smooth and incommensurate contact. , The phenomenon of wear is almost zero. In 2004, the research group of Dutch scientist J.
- the slider may contain several horizontal grain boundaries penetrating the slider. These horizontal grain boundaries are easy-slip surfaces in the slider, and when the slider is pushed, the slider can slide away from any of these horizontal grain boundaries, so the location of its slip surface is unknown.
- mass-producing a large number of graphite island sliders their respective sliding surface positions and heights are not consistent, so that the slider quality cannot be uniformly controlled.
- the purpose of the present invention is to provide a method based on adding a grain structure detection step in the process of preparing the graphite island slider array, and by controlling the subsequent etching steps, so that there is only one and only one inside the slider. crystallographic interface, and when these sliders are sheared, they will slide away from the only crystallographic interface.
- the technical solution provided by the present invention is: a preparation method of a graphite island slider array, comprising the following steps:
- Step 1 at least cover photoresist on the highly oriented pyrolytic graphite
- Step 2 patterning the photoresist, retaining a plurality of photoresist islands
- Step 3 etching the highly oriented pyrolytic graphite, removing part of the highly oriented pyrolytic graphite that is not protected by the photoresist, to form a plurality of island structures;
- Step 4 removing the residual photoresist to obtain the graphite island slider array
- step 1 the three-dimensional grain structure near the surface of the highly oriented pyrolytic graphite is detected, and the grain information of the polycrystalline structure near the graphite surface is obtained;
- step 3 based on the detected grain information of the polycrystalline structure, the etching time is controlled so that the etched graphite island slider only includes one layer of horizontal grain boundaries.
- the photoresist is preferably covered by spin coating.
- the average diameter of the photoresist islands formed in the second step is preferably 1 ⁇ m ⁇ 30 ⁇ m, and the average interval between the photoresist islands is preferably 1 ⁇ m ⁇ 100 ⁇ m.
- the etching in step 3 is reactive ion etching.
- detection is electron backscatter diffraction, X-ray scattering or elliptically polarized light detection.
- grain information is grain thickness.
- the etching time is controlled so that the etching depth is just greater than the thickness of one crystal grain in the outermost layer of graphite, and less than the height from the outermost layer to the bottom of the second crystal grain.
- each graphite island slider (7) has a connection layer (9) on the top of the graphite island.
- connection layer (9) on the top of the graphite island is formed by depositing the connection layer (8) on the highly oriented pyrolytic graphite by a plasma chemical vapor deposition method.
- connection layer (8) is preferably SiO2, and the thickness is preferably 50 nm ⁇ 500 nm.
- the existing preparation method of the graphite island slider array does not have the detection of the grain structure before processing, so the etching depth cannot be strictly controlled according to the detection information, so the processed graphite island slider array contains a large number of particles. Crystalline interface (slip-prone surface). Therefore, these sliders are not consistent.
- the slider array prepared by the invention has uniform sliding surface and height.
- Fig. 1 is the typical expected result schematic diagram of the nondestructive three-dimensional inspection of highly oriented pyrolytic graphite of the present invention
- Fig. 2 is the schematic diagram of the sample after coating and patterning photoresist of the present invention.
- FIG. 3 is a schematic diagram of a sample after the etching substrate of the present invention forms an island array
- [Correction 28.07.2020 according to Rule 91] 4 is a schematic diagram of the present invention removing residual photoresist, and after processing the sample, the graphite island array has a uniform high slip surface;
- 5 is a schematic diagram of a sample with a tie layer after coating and patterning the photoresist of the present invention
- 6 is a schematic diagram of the present invention showing a sample after etching the connecting layer and the substrate to form an island array;
- FIG. 7 is a schematic diagram of a sample with a connection layer after the processing of the present invention is completed.
- Step 1 select highly oriented pyrolytic graphite (HOPG), so that the highly oriented pyrolytic graphite material has a relatively flat surface and layered structure, and has a large single crystal size and thickness.
- HOPG highly oriented pyrolytic graphite
- step 2 the crystal grains near the graphite surface, especially the non-destructive testing of the three-dimensional grain structure near the surface, are detected by means of material non-destructive testing, and the polycrystalline structure near the graphite surface is obtained.
- the non-destructive testing means can be, for example, electron backscatter diffraction technology, X-ray scattering technology, elliptically polarized light technology, etc.
- An example of expected measurement results is shown in Figure 1.
- Highly oriented graphite has a "brick-like" polycrystalline mosaic structure, including several longitudinal grain boundaries 1 extending from the graphite surface to the interior, and several horizontal grain boundaries 2 inside the graphite , the position of these grain boundaries can be accurately measured by non-destructive three-dimensional inspection technology.
- a single crystal region 3 with a large area can be accurately selected on the surface of the highly oriented pyrolytic graphite for use in subsequent preparation steps.
- Step 3 sequentially covering the HOPG with photoresist, and the photoresist can be covered by spin coating.
- Step 4 patterning the photoresist, leaving a plurality of photoresist islands.
- the step of patterning the photoresist determines the layout of the island-like structures formed in the subsequent steps.
- the photoresist can be patterned by an electron beam etching method, and the photoresist islands formed can be, for example, with an average diameter of 1 ⁇ m to 30 ⁇ m, the average spacing between photoresist islands is a square or circular array of 1 ⁇ m to 100 ⁇ m, so that the etched island structures also have the corresponding average diameter and average spacing, as shown in Figure 2. Show.
- the substrate is etched to remove part of the substrate that is not protected by the photoresist, thereby forming a plurality of island-like structures.
- the etching method may be, for example, reactive ion etching. Based on the measurement data in step 2, especially the grain thickness data in the area where the island structure is located, the time of reactive ion etching is strictly controlled during the etching process, so that the etching depth is just larger than the outermost grain of graphite thickness, as shown in Figure 3.
- Step 6 remove the residual photoresist, and after the processing is completed, a batch of graphite island slider arrays are obtained.
- the horizontal grain boundaries in the original graphite now become unified slip planes in the graphite island array, as shown in FIG. 4 .
- Different graphite islands within the same batch of arrays will slide away from the same height when sliding, so there is consistency.
- each graphite island slider can also have a connecting layer, such as SiO2.
- the specific preparation method is:
- Step 1 select highly oriented pyrolytic graphite, which has a flat surface and layered structure, and a large single crystal size and thickness.
- step 2 the crystal grains near the graphite surface are detected by means of material nondestructive testing, especially the nondestructive testing of the three-dimensional grain structure near the surface, and the polycrystalline structure near the graphite surface is obtained, as shown in FIG. 1 .
- a single crystal region 3 with a large area can be accurately selected on the surface of the highly oriented pyrolytic graphite for subsequent preparation.
- connection layer may be SiO2, and the thickness may be, for example, 50 nm to 500 nm nm, the SiO2 connecting layer can be deposited by plasma chemical vapor deposition.
- the photoresist can be covered by spin coating.
- Step 4 patterning the photoresist, leaving a plurality of photoresist islands.
- the photoresist can be patterned by an electron beam etching method, and the photoresist islands formed can be, for example, with an average diameter of 1 ⁇ m to 30 ⁇ m, and an average interval between the photoresist islands of 1 ⁇ m to 100 ⁇ m. , so that the etched island structures also have corresponding average diameters and average intervals.
- the sample after completing the patterned photoresist is shown in Figure 5.
- Step 5 the connecting layer and the graphite substrate are sequentially etched, so as to remove the connecting layer and part of the graphite that are not protected by the photoresist, thereby forming a plurality of island-like structures with connecting layers.
- the etching may be, for example, reactive ion etching.
- the time of reactive ion etching is strictly controlled, and based on the measurement data in step 2, the etching depth is just greater than the thickness of the topmost grain of graphite, and less than the thickness from the topmost layer to the second grain. The height of the bottom. As shown in Figure 6.
- step 6 the residual photoresist is removed, the processing is completed, and a batch of graphite island slider arrays with connecting layers are obtained, and they have uniform sliding surfaces, as shown in FIG. 7 .
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- Inorganic Chemistry (AREA)
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Abstract
Description
图4为本发明去除残余光刻胶,加工完成后的样品,石墨岛阵列具有统一高度易滑移面的示意图;
图5为本发明的涂覆并构图光刻胶后的带连接层样品的示意图;
图6为本发明示出刻蚀连接层及基底形成岛状阵列后的样品的示意图;
从石墨表面延伸向内部的纵向晶界1 | 石墨内部的水平晶界2 |
面积较大的单晶区域3 | 已构图后的光刻胶4 |
石墨岛中的易滑移面5 | 石墨岛基底6 |
石墨岛滑块7 | 连接层8 |
石墨岛顶部的连接层9 |
Claims (10)
- 一种石墨岛滑块阵列的制备方法,包括以下步骤,步骤一:在高定向热解石墨上至少覆盖光刻胶;步骤二:构图所述光刻胶,保留多个光刻胶岛;步骤三:刻蚀所述高定向热解石墨,去除未被光刻胶保护的部分高定向热解石墨,形成多个岛状结构;步骤四:去除残余的光刻胶,得到所述石墨岛滑块阵列;其特征在于,在步骤一之前,对高定向热解石墨表面附近的三维晶粒结构进行检测,得到石墨表面附近的多晶结构的晶粒信息;步骤三中,基于上述检测的多晶结构的晶粒信息,控制所述刻蚀,使得刻蚀后的石墨岛滑块(7)仅包括一层水平晶界。
- 根据权利要求1所述的制备方法,其特征在于,步骤一中所述光刻胶优选为通过旋转涂布的方式进行覆盖。
- 根据权利要求1或2所述的制备方法,其特征在于,步骤二中所形成的光刻胶岛的平均直径优选为1μm~30μm,光刻胶岛之间的平均间隔优选为1μm~100μm。
- 根据权利要求1-3任一项所述的制备方法,其特征在于,步骤三中所述刻蚀是反应离子刻蚀。
- 根据权利要求1-4任一项所述的制备方法,其特征在于,所述检测是电子背散射衍射、X射线散射或椭圆偏振光检测。
- 根据权利要求1-5任一项所述的制备方法,其特征在于,所述晶粒信息是晶粒厚度。
- 根据权利要求6所述的制备方法,其特征在于,控制所述刻蚀的时间,使刻蚀深度恰好大于石墨最表层一块晶粒的厚度,小于从最表层到第二块晶粒底部的高度。
- 根据权利要求1-7任一项所述的制备方法,其特征在于,每个石墨岛滑块(7)顶部具有一个石墨岛顶部的连接层(9)。
- 根据权利要求8所述的制备方法,其特征在于,所述石墨岛顶部的连接层(9)是通过等离子体化学气相沉积法将连接层(8)沉积在所述高定向热解石墨上。
- 根据权利要求9所述的制备方法,其特征在于,所述连接层(8)的材料优选为SiO2,厚度优选为50nm~500nm。
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
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PCT/CN2020/098477 WO2022000120A1 (zh) | 2020-06-28 | 2020-06-28 | 一种石墨岛滑块阵列的制备方法 |
JP2022559676A JP7384368B2 (ja) | 2020-06-28 | 2020-06-28 | グラファイトアイランドスライディングブロックアレイの調製方法 |
KR1020227038944A KR20220166315A (ko) | 2020-06-28 | 2020-06-28 | 그래파이트 아일랜드 슬라이딩 블록 어레이의 제조방법 |
US17/923,254 US20240043266A1 (en) | 2020-06-28 | 2020-06-28 | Manufacturing method for graphite slider arrays |
CN202080092510.XA CN115003620A (zh) | 2020-06-28 | 2020-06-28 | 一种石墨岛滑块阵列的制备方法 |
EP20942675.8A EP4112536A4 (en) | 2020-06-28 | 2020-06-28 | MANUFACTURING PROCESS FOR NETWORKS OF SLIDING BLOCKS IN ISLANDS OF GRAPHITE |
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US (1) | US20240043266A1 (zh) |
EP (1) | EP4112536A4 (zh) |
JP (1) | JP7384368B2 (zh) |
KR (1) | KR20220166315A (zh) |
CN (1) | CN115003620A (zh) |
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CN113582125A (zh) * | 2021-07-21 | 2021-11-02 | 深圳清华大学研究院 | 一种超滑封装器件及其封装方法 |
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- 2020-06-28 EP EP20942675.8A patent/EP4112536A4/en active Pending
- 2020-06-28 WO PCT/CN2020/098477 patent/WO2022000120A1/zh active Application Filing
- 2020-06-28 US US17/923,254 patent/US20240043266A1/en active Pending
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CN115003620A (zh) | 2022-09-02 |
US20240043266A1 (en) | 2024-02-08 |
EP4112536A1 (en) | 2023-01-04 |
KR20220166315A (ko) | 2022-12-16 |
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