CN113560960A - Diffuse reflection type calibration plate and preparation method thereof - Google Patents
Diffuse reflection type calibration plate and preparation method thereof Download PDFInfo
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- CN113560960A CN113560960A CN202010347388.8A CN202010347388A CN113560960A CN 113560960 A CN113560960 A CN 113560960A CN 202010347388 A CN202010347388 A CN 202010347388A CN 113560960 A CN113560960 A CN 113560960A
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- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000005498 polishing Methods 0.000 claims abstract description 107
- 238000000227 grinding Methods 0.000 claims abstract description 89
- 238000000034 method Methods 0.000 claims abstract description 82
- 239000011521 glass Substances 0.000 claims abstract description 75
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000011651 chromium Substances 0.000 claims abstract description 44
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 44
- 230000007797 corrosion Effects 0.000 claims abstract description 36
- 238000005260 corrosion Methods 0.000 claims abstract description 36
- 239000005357 flat glass Substances 0.000 claims abstract description 29
- 238000000576 coating method Methods 0.000 claims abstract description 28
- 239000003292 glue Substances 0.000 claims abstract description 28
- 238000001259 photo etching Methods 0.000 claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 239000002184 metal Substances 0.000 claims abstract description 15
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 13
- 239000004065 semiconductor Substances 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 10
- 239000007888 film coating Substances 0.000 claims abstract description 10
- 238000009501 film coating Methods 0.000 claims abstract description 10
- 238000005520 cutting process Methods 0.000 claims description 31
- 229920002120 photoresistant polymer Polymers 0.000 claims description 27
- 239000000758 substrate Substances 0.000 claims description 20
- 230000003746 surface roughness Effects 0.000 claims description 20
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 19
- 238000004544 sputter deposition Methods 0.000 claims description 18
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000004528 spin coating Methods 0.000 claims description 9
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 7
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 7
- 238000013016 damping Methods 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 6
- 229920002635 polyurethane Polymers 0.000 claims description 6
- 239000004814 polyurethane Substances 0.000 claims description 6
- 238000000059 patterning Methods 0.000 claims description 4
- 238000002310 reflectometry Methods 0.000 abstract description 2
- 239000004576 sand Substances 0.000 abstract 1
- 239000011859 microparticle Substances 0.000 description 12
- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical compound [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 description 10
- 239000000919 ceramic Substances 0.000 description 9
- 238000003698 laser cutting Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005488 sandblasting Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 229910001651 emery Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention discloses a preparation method of a diffuse reflection type calibration plate, which comprises the following steps: grinding the upper surface and/or the lower surface of the polishing sheet/original glass for 10-40min by using 20-60% DN95 carborundum solution with the grain diameter of less than 10 microns to obtain a first grinding surface, wherein the upper surface of the polishing sheet/original glass is a first grinding surface or plane; processing and manufacturing a graph on the upper surface of the polished wafer/original plate glass by adopting a semiconductor mask graph manufacturing process flow, and sequentially carrying out film coating, glue coating, photoetching, developing and corrosion to prepare a metal chromium layer; the invention adopts grinding process to make the frosted effect, which satisfies the requirement of high flatness, the sand grain is fine and controllable, and the reflectivity is less than 0.1%.
Description
Technical Field
The invention relates to the field of calibration plates, in particular to a diffuse reflection type calibration plate and a preparation method thereof.
Background
In the applications of machine vision, image measurement, photogrammetry, three-dimensional reconstruction and the like, a geometric model for camera imaging needs to be established for correcting lens distortion, determining a conversion relation between a physical size and a pixel and determining a mutual relation between a three-dimensional geometric position of a certain point on the surface of a space object and a corresponding point in an image. The camera shoots the array flat plate with the fixed-spacing pattern, and a geometric model of the camera can be obtained through calculation of a calibration algorithm, so that high-precision measurement and reconstruction results are obtained. However, under the condition of a front light source, the glass calibration plate can reflect light.
There are several prior art at present to solve the problem that the reflection of light appears in glass material calibration plate:
1) ceramic is used as a base material, chromium plating is carried out on the ceramic sheet, and the ceramic base material is not reflective. However, alumina and zirconia ceramics are more expensive than glass and have poorer flatness than glass. The general thickness of the ceramic substrate is only 1mm, the maximum size capable of being processed is about 200mm, the glass substrate can be in various thicknesses and large sizes, and the maximum polishing equipment in China can reach 1 meter at present.
2) The surface of the glass is coated with a high polymer material film, and the film layer is not reflective. However, the adhesion of the polymer film coated on the glass surface is inferior to that of the chromium film formed by magnetron sputtering, and the glass is not resistant to weather, high temperature, acid and alkali.
At present, no technology for solving the problem of light reflection by treating the surface of a glass calibration plate exists, and the frosted effect of sand blasting is found to damage the surface of glass in the operation process, so that the glass is not suitable for processing sheet glass.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the diffuse reflection type calibration plate and the preparation method thereof solve the problems in the prior art, the grinding process is adopted to manufacture the frosted effect, the polishing process is adopted to meet the requirement of high flatness, and the semiconductor mask plate process is combined to meet the requirements of fine lines and high-precision processing.
The technical scheme adopted by the invention is as follows:
a method for preparing a diffuse reflection type calibration plate comprises the following steps:
grinding for the first time: grinding the upper surface of the polishing sheet/original glass for 10-40min by using 20-60% of DN95 carborundum solution with the grain diameter of less than 10 microns to obtain a first grinding surface, wherein the upper surface of the polishing sheet/original glass is the first grinding surface; or grinding the lower surface of the polishing sheet/original edition glass for 10-40min to obtain a first grinding surface, wherein the upper surface of the polishing sheet/original edition glass is a plane; or grinding the upper surface and the lower surface of the polishing sheet/original edition glass for 10-40min at the same time to obtain two first grinding surfaces, wherein the upper surface of the polishing sheet/original edition glass is the first grinding surface; the upper surface and/or the lower surface of the polishing sheet/master glass is preferably ground for 20-30min using 30% -50% DN95 carborundum solution with the grain diameter of less than 10 microns.
The key of the grinding step is that: the carborundum with different grain diameters is used for obtaining the roughness of different surfaces, and the surface roughness is controllable. By correcting the flatness of the surface of the grinding disc, high flatness (up to 5 microns) can be obtained.
Making a graph: processing and manufacturing a graph on the upper surface of the polished wafer/original plate glass by adopting a semiconductor mask graph manufacturing process flow, and sequentially carrying out film coating, glue coating, photoetching, developing and corrosion to prepare a metal chromium layer graph;
precision cutting: and performing precision cutting, wherein the size precision is +/-0.05 mm.
Further, the polishing step is also included between the first grinding step and the patterning step: and polishing a first grinding surface for 10-120min by using a cerium oxide polishing solution with 10-30% DN95 and the particle size of 0.5-1.5 microns to obtain a polished surface. Preferably, one of the first abrasive surfaces is polished for 50-80min by using a cerium oxide polishing solution with 20-30% DN95 and a particle size of 1-1.5 microns.
And further, polishing the other first grinding surface to obtain another polishing surface, and grinding one polishing surface for the second time to obtain a second grinding surface.
Further, the second grinding step is performed between the polishing step and the patterning step, or after the precision cutting step.
Further, the first grinding step of the lower surface of the polishing sheet/original glass follows the precision cutting step.
Further, the surface roughness Ra of the first grinding surface and/or the second grinding surface is 1-5 microns, and the surface micro-particle size is 6-8 microns. Preferably, the surface roughness Ra of the first grinding surface and/or the second grinding surface is 2-4 microns, and the surface micro-particle size is 7-8 microns.
Further, the polished surface has a surface roughness Ra of 0.005 to 0.015nm, preferably 0.01 to 0.015 nm.
Further, the coating process is that the polished wafer/original glass is put into a magnetron sputtering vacuum chamber after being cleaned and dried by ultrasonic, a layer of chromium film with the thickness of 80-120nm is coated on the front surface of the glass substrate by adopting a direct current magnetron sputtering process, and the proportion of Ar \ N2\ O2\ CO2 in the process gas in the sputtering process is 5-80: 0-50: 0-60: 0-80, the vacuum degree is 1-8 multiplied by 10 < -6 >, the sputtering power is 0.2-5kw, and the chromium film substrate is obtained; the preferred thickness is 100-120 nm.
The glue coating process adopts a spin coating process to spin to obtain a photoresist film with the glue thickness of 100 and 500nm, the uniformity can reach +/-0.5%, and the resolution can reach 1 micron; the preferred thickness is 200-300 nm.
The photoetching process is an exposure process by using an inlet photoetching machine with an I-line high-resolution lens, and lines can be made to be 1 micron;
and the developing corrosion is exposure, firstly, on a precise full-automatic developing corrosion device, 0.01-0.3% TMAH is utilized to react and remove the exposed photoresist, the solution temperature is controlled at 23-25 ℃, the developing time is controlled at 10-25s, then, a special corrosive liquid is utilized to remove and corrode the chromium layer exposed after the photoresist is removed by developing, the corrosion time is 40-60s, the solution temperature is 23-25 ℃, and the process requirement of 1 micron lines is met.
Further, the pressure applied during the polishing was 100-500 kgf;
polishing is carried out on polyurethane and damping cloth;
the pressure applied during polishing was 100-300 kgf.
Another aspect of the present invention relates to a diffusely reflective calibration plate made according to the above method.
Compared with the prior art, the invention has the following advantages:
1) the grain size of the frosted particles can be 7 microns, and the frosted effect is uniform.
2) The frosted surface reflects light diffusely, and the reflectivity is less than 0.1%.
3) By adopting the manufacturing process of the semiconductor mask, fine lines can be manufactured with high precision. The minimum line can be made to be 1 micron, the line control precision can reach 0.2 micron, and the pattern distance precision can be made to be 1 meter and have a deviation of 1 micron.
4) The flatness of the glass is higher than that of the ceramic plate, the flatness of the glass can reach 2 microns at most, and the flatness of the ceramic plate is about 50 microns in common use.
5) The glass has wide range of machinable size, and the size of the calibration plate can reach 1 m. The thickness of the glass can be customized and selected. Ceramic calibration plates are typically 1mm thick, and currently range in size up to about 200 mm.
6) The glass is suitable for a high-precision cutting process, is suitable for customized manufacturing by utilizing the existing product, reduces the development process and cost, and has high difficulty and high development cost in ceramic precision cutting.
7) The frosting effect of sand blasting is utilized, the glass surface is damaged, and the glass is not suitable for processing the thin glass. The glass sheet with the thickness of 0.3-1mm can be processed by grinding, and the surface of the glass can not be damaged.
8) The metal chromium film on the ground frosting is environment-resistant and more stable and wear-resistant than the high molecular film layer.
9) The grinding effect uniformity is good, and the sand blasting and grinding effect is uneven.
Drawings
FIG. 1 is a schematic structural view of a diffuse reflection type calibration plate in examples 1-2 of the present invention;
FIG. 2 is a schematic structural view of a diffuse reflection type calibration plate in example 3 of the present invention;
fig. 3 is a schematic structural view of a diffuse reflection type calibration plate in embodiment 7 of the present invention.
Detailed description of the preferred embodiments
In order to better understand the technical solution, the technical solution will be described in detail with reference to the drawings and the specific embodiments.
Example 1
For calibration plates with no requirement for flatness, polishing sheets/original glass can be used for direct grinding, and this embodiment is a method for preparing a diffuse reflection calibration plate with frosted double surfaces, which comprises the following steps:
grinding for the first time: the upper and lower surfaces of the polishing sheet/original glass were polished with a carborundum solution of 20% DN95 with a particle size of 10 μm or less under a pressure of 100kgf for 10min, respectively, to a first polished surface roughness Ra of 5 μm and a surface micro-particle size of 8 μm.
Making a graph: processing and manufacturing a graph on a first grinding surface of the upper surface of the polished wafer/original plate glass by adopting a semiconductor mask graph manufacturing process flow, and sequentially carrying out film coating, glue coating, photoetching, developing and corrosion to prepare a metal chromium layer graph;
the coating process is that the polished wafer/original glass is put into a magnetron sputtering vacuum chamber after being cleaned and dried by ultrasonic, a layer of 80nm chromium film is coated on the front surface of the glass substrate by adopting a direct current magnetron sputtering process, and the proportion of process gas Ar \ N2\ O2\ CO2 in the sputtering process is 35 sccm: 25 sccm: 0 sccm: 9sccm, the vacuum degree of 4 multiplied by 10 < -6 >, and the sputtering power of 1.2kw to obtain a chromium film substrate;
the glue coating process adopts a spin coating process to spin to obtain a photoresist film with the glue thickness of 100nm, the uniformity can reach +/-0.5%, and the resolution can reach 1 micron;
the photoetching process is an exposure process by using an inlet photoetching machine with an I-line high-resolution lens, and lines can be made to be 1 micron;
and the development corrosion is exposure, on an accurate full-automatic development corrosion device, firstly, 0.01% TMAH is utilized to remove the exposed photoresist by reaction, the solution temperature is controlled at 23 ℃, the development time is controlled at 10s, the special corrosive liquid adopts ceric ammonium nitrate, then the special corrosive liquid is utilized to remove and corrode the chromium layer exposed after the photoresist is removed by development, the corrosion time is controlled at 40s, the solution temperature is controlled at 23 ℃, and the process requirement of 1 micron line is met.
Precision cutting: precision cutting is carried out by adopting an automatic cutter wheel cutting machine positioned by the ccd, so that the squareness and the size precision are well controlled, and the size precision is +/-0.05 mm.
The prepared diffuse reflection type calibration plate with frosted double surfaces is shown in figure 1 and comprises a polishing sheet/original plate glass 1, wherein the upper surface and the lower surface of the polishing sheet/original plate glass 1 are both first grinding surfaces 2, and a metal chromium layer 3 is manufactured on the first grinding surface 2 of the upper surface of the polishing sheet/original plate glass.
Example 2
For calibration plates with no requirement for flatness, polishing sheets/original glass can be used for direct grinding, and this embodiment is a method for preparing a diffuse reflection calibration plate with frosted double surfaces, which comprises the following steps:
grinding for the first time: the upper surface of the polishing sheet/original glass was polished for 10min using 20% DN95 carborundum solution having a particle size of 10 μm or less with a pressure of 100kgf applied during polishing, and the first polished surface had a surface roughness Ra of 5 μm and a surface micro particle size of 8 μm.
Making a graph: processing and manufacturing a graph on a first grinding surface of the upper surface of the polished wafer/original plate glass by adopting a semiconductor mask graph manufacturing process flow, and sequentially carrying out film coating, glue coating, photoetching, developing and corrosion to prepare a metal chromium layer graph;
the coating process is that the polished wafer/original glass is put into a magnetron sputtering vacuum chamber after being cleaned and dried by ultrasonic, a layer of 80nm chromium film is coated on the front surface of the glass substrate by adopting a direct current magnetron sputtering process, and the proportion of process gas Ar \ N2\ O2\ CO2 in the sputtering process is 35 sccm: 25 sccm: 0 sccm: 9sccm, the vacuum degree of 4 multiplied by 10 < -6 >, and the sputtering power of 1.2kw to obtain a chromium film substrate;
the glue coating process adopts a spin coating process to spin to obtain a photoresist film with the glue thickness of 100nm, the uniformity can reach +/-0.5%, and the resolution can reach 1 micron;
the photoetching process is an exposure process by using an inlet photoetching machine with an I-line high-resolution lens, and lines can be made to be 1 micron;
and the development corrosion is exposure, on an accurate full-automatic development corrosion device, firstly, 0.01% TMAH is utilized to remove the exposed photoresist by reaction, the solution temperature is controlled at 23 ℃, the development time is controlled at 10s, the special corrosive liquid adopts ceric ammonium nitrate, then the special corrosive liquid is utilized to remove and corrode the chromium layer exposed after the photoresist is removed by development, the corrosion time is controlled at 40s, the solution temperature is controlled at 23 ℃, and the process requirement of 1 micron line is met.
Precision cutting: precision cutting is carried out by adopting an automatic cutter wheel cutting machine positioned by the ccd, so that the squareness and the size precision are well controlled, and the size precision is +/-0.05 mm.
Grinding for the first time: the lower surface of the polishing sheet/original glass was polished for 10min using 20% DN95 carborundum solution having a particle size of 10 μm or less with a pressure of 100kgf applied during polishing, and the first polished surface had a surface roughness Ra of 5 μm and a surface micro particle size of 8 μm.
The prepared diffuse reflection type calibration plate with frosted double surfaces is shown in figure 1 and comprises a polishing sheet/original plate glass 1, wherein the upper surface and the lower surface of the polishing sheet/original plate glass 1 are both first grinding surfaces 2, and a metal chromium layer 3 is manufactured on the first grinding surface 2 of the upper surface of the polishing sheet/original plate glass.
Example 3
For a calibration plate with flatness requirement of 10-30 microns, grinding by using a polishing sheet/original glass and then polishing the single surface, this embodiment is a preparation method of a diffuse reflection type calibration plate with frosted single surface, and the preparation method comprises the following steps:
grinding for the first time: the upper and lower surfaces of the polishing sheet/original glass were polished with a carborundum solution of 20% DN95 with a particle size of 10 μm or less under a pressure of 100kgf for 10min, respectively, to a first polished surface roughness Ra of 5 μm and a surface micro-particle size of 8 μm.
And (3) polishing: polishing the first grinding surface of the lower surface of the polished sheet/original glass for 10min by using a cerium oxide polishing solution with 10% DN95 and the particle size of 0.5 micron to obtain a polished surface; the polished surface had a surface roughness Ra of 0.015 nm. The polishing step is carried out on polyurethane and damping cloth; the pressure applied during polishing was 100 kgf.
Making a graph: processing and manufacturing a graph on a first grinding surface of the upper surface of the polished wafer/original plate glass by adopting a semiconductor mask graph manufacturing process flow, and sequentially carrying out film coating, glue coating, photoetching, developing and corrosion to prepare a metal chromium layer graph;
the coating process is that the polished wafer/original glass is put into a magnetron sputtering vacuum chamber after being cleaned and dried by ultrasonic, a layer of 80nm chromium film is coated on the front surface of the glass substrate by adopting a direct current magnetron sputtering process, and the proportion of process gas Ar \ N2\ O2\ CO2 in the sputtering process is 35 sccm: 25 sccm: 0 sccm: 9sccm, the vacuum degree of 4 multiplied by 10 < -6 >, and the sputtering power of 1.2kw to obtain a chromium film substrate;
the glue coating process adopts a spin coating process to spin to obtain a photoresist film with the glue thickness of 100nm, the uniformity can reach +/-0.5%, and the resolution can reach 1 micron;
the photoetching process is an exposure process by using an inlet photoetching machine with an I-line high-resolution lens, and lines can be made to be 1 micron;
and the development corrosion is exposure, on an accurate full-automatic development corrosion device, firstly, 0.01% TMAH is utilized to remove the exposed photoresist by reaction, the solution temperature is controlled at 23 ℃, the development time is controlled at 10s, the special corrosive liquid adopts ceric ammonium nitrate, then the special corrosive liquid is utilized to remove and corrode the chromium layer exposed after the photoresist is removed by development, the corrosion time is controlled at 40s, the solution temperature is controlled at 23 ℃, and the process requirement of 1 micron line is met.
Precision cutting: and (3) precisely cutting by adopting a laser cutting machine positioned by the ccd to obtain good squareness and size precision control, wherein the size precision is +/-0.05 mm.
The prepared diffuse reflection type calibration plate with frosted double surfaces is shown in figure 2 and comprises a polishing sheet/original plate glass 1, wherein the upper surface of the polishing sheet/original plate glass 1 is a first grinding surface 2, the lower surface of the polishing sheet/original plate glass 1 is a polishing surface 4, and a metal chromium layer 3 is manufactured on the first grinding surface 2 of the upper surface of the polishing sheet/original plate glass.
Example 4
For calibration plates with flatness requirement within 10 microns, polishing sheets/original glass are used for grinding, then double-sided polishing is carried out, and then single-sided grinding is carried out. The embodiment is a preparation method of a diffuse reflection type calibration plate with frosted single surface, which comprises the following steps:
grinding for the first time: the upper and lower surfaces of the polishing sheet/original glass were polished with a carborundum solution of 20% DN95 with a particle size of 10 μm or less under a pressure of 100kgf for 10min, respectively, to a first polished surface roughness Ra of 5 μm and a surface micro-particle size of 8 μm.
And (3) polishing: polishing the first grinding surfaces of the upper surface and the lower surface of the polishing sheet/original glass for 10min by using a cerium oxide polishing solution with 10 percent DN95 and the grain size of 0.5 micron to obtain polishing surfaces; the polished surface had a surface roughness Ra of 0.015 nm. The polishing step is carried out on polyurethane and damping cloth; the pressure applied during polishing was 100 kgf.
And (3) second grinding: the polished surface of the upper surface of the polished sheet/original glass was polished for 10 minutes using 20% DN95 emery solution with a particle size of 10 μm or less under a pressure of 100kgf to obtain a second polished surface having a surface roughness Ra of 5 μm and a surface micro particle size of 8 μm.
Making a graph: processing and manufacturing a graph on a second grinding surface of the upper surface of the polished wafer/original plate glass by adopting a semiconductor mask graph manufacturing process flow, and sequentially carrying out film coating, glue coating, photoetching, developing and corrosion to prepare a metal chromium layer graph;
the coating process is that the polished wafer/original glass is put into a magnetron sputtering vacuum chamber after being cleaned and dried by ultrasonic, a layer of 80nm chromium film is coated on the front surface of the glass substrate by adopting a direct current magnetron sputtering process, and the proportion of process gas Ar \ N2\ O2\ CO2 in the sputtering process is 35 sccm: 25 sccm: 0 sccm: 9sccm, the vacuum degree of 4 multiplied by 10 < -6 >, and the sputtering power of 1.2kw to obtain a chromium film substrate;
the glue coating process adopts a spin coating process to spin to obtain a photoresist film with the glue thickness of 100nm, the uniformity can reach +/-0.5%, and the resolution can reach 1 micron;
the photoetching process is an exposure process by using an inlet photoetching machine with an I-line high-resolution lens, and lines can be made to be 1 micron;
and the development corrosion is exposure, on an accurate full-automatic development corrosion device, firstly, 0.01% TMAH is utilized to remove the exposed photoresist by reaction, the solution temperature is controlled at 23 ℃, the development time is controlled at 10s, the special corrosive liquid adopts ceric ammonium nitrate, then the special corrosive liquid is utilized to remove and corrode the chromium layer exposed after the photoresist is removed by development, the corrosion time is controlled at 40s, the solution temperature is controlled at 23 ℃, and the process requirement of 1 micron line is met.
Precision cutting: and a scribing machine positioned by the ccd is adopted for precise cutting, so that the squareness and the size precision are well controlled, and the size precision is +/-0.05 mm.
Example 5
For calibration plates with flatness requirement within 10 microns, polishing sheets/original glass are used for grinding, then double-sided polishing is carried out, and then single-sided grinding is carried out. The embodiment is a preparation method of a diffuse reflection type calibration plate with frosted single surface, which comprises the following steps:
grinding for the first time: the upper and lower surfaces of the polishing sheet/original glass were polished with a carborundum solution of 20% DN95 with a particle size of 10 μm or less under a pressure of 100kgf for 10min, respectively, to a first polished surface roughness Ra of 5 μm and a surface micro-particle size of 8 μm.
And (3) polishing: polishing the first grinding surfaces of the upper surface and the lower surface of the polishing sheet/original glass for 10min by using a cerium oxide polishing solution with 10 percent DN95 and the grain size of 0.5 micron to obtain polishing surfaces; the polished surface had a surface roughness Ra of 0.015 nm. The polishing step is carried out on polyurethane and damping cloth; the pressure applied during polishing was 100 kgf.
Making a graph: processing and manufacturing a graph on the polishing surface of the upper surface of the polishing sheet/original plate glass by adopting a semiconductor mask graph manufacturing process flow, and sequentially carrying out film coating, glue coating, photoetching, developing and corrosion to prepare a metal chromium layer graph;
the coating process is that the polished wafer/original glass is put into a magnetron sputtering vacuum chamber after being cleaned and dried by ultrasonic, a layer of 80nm chromium film is coated on the front surface of the glass substrate by adopting a direct current magnetron sputtering process, and the proportion of process gas Ar \ N2\ O2\ CO2 in the sputtering process is 35 sccm: 25 sccm: 0 sccm: 9sccm, the vacuum degree of 4 multiplied by 10 < -6 >, and the sputtering power of 1.2kw to obtain a chromium film substrate;
the glue coating process adopts a spin coating process to spin to obtain a photoresist film with the glue thickness of 100nm, the uniformity can reach +/-0.5%, and the resolution can reach 1 micron;
the photoetching process is an exposure process by using an inlet photoetching machine with an I-line high-resolution lens, and lines can be made to be 1 micron;
after exposure, on a precise full-automatic developing corrosion device, firstly, 0.01% TMAH is used for removing the exposed photoresist by reaction, the solution temperature is controlled at 23 ℃, the developing time is controlled at 10s, the special corrosive liquid adopts ceric ammonium nitrate, then the special corrosive liquid is used for removing and corroding the chromium layer exposed after the photoresist is removed by development, the solution temperature is controlled at 23 ℃, the developing time is controlled at 10s, and the technological requirement of 1 micron lines is met.
Precision cutting: precision cutting is carried out by adopting an automatic cutter wheel cutting machine positioned by the ccd, so that the squareness and the size precision are well controlled, and the size precision is +/-0.05 mm.
And (3) second grinding: the surface of the polished surface of the lower surface of the polished sheet/original glass was polished for 10 minutes using 20% DN95 emery solution having a particle size of 10 μm or less under a pressure of 100kgf to obtain a second polished surface having a surface roughness Ra of 5 μm and a surface micro particle size of 8 μm.
Example 6
For calibration plates with no requirement for flatness, polishing sheets/original glass can be used for direct grinding, and this embodiment is a method for preparing a diffuse reflection type calibration plate with frosted single surface, and the method comprises the following steps:
grinding for the first time: grinding the upper surface of the polishing sheet/original plate glass for 40min by using 60% DN95 carborundum solution with the grain diameter of less than 10 microns and the applied pressure during grinding of 500kgf, wherein the upper surface of the polishing sheet/original plate glass is a first grinding surface; the first abrasive surface had a surface roughness Ra of 1 micron and a surface micro particle size of 6 microns.
Making a graph: processing a first grinding surface on the upper surface of the polished wafer/original plate glass by adopting a semiconductor mask pattern manufacturing process to manufacture a pattern, and sequentially carrying out film coating, glue coating, photoetching, developing and corrosion to prepare a metal chromium layer pattern;
the coating process is that the polished wafer/original glass is put into a magnetron sputtering vacuum chamber after being cleaned and dried by ultrasonic, a layer of 120nm chromium film is coated on the front surface of the glass substrate by adopting a direct current magnetron sputtering process, and the proportion of process gas Ar \ N2\ O2\ CO2 in the sputtering process is 35 sccm: 25 sccm: 0 sccm: 9sccm, the vacuum degree of 4 multiplied by 10 < -6 >, and the sputtering power of 1.2kw to obtain a chromium film substrate;
the glue coating process adopts a spin coating process to spin to obtain a photoresist film with the glue thickness of 500nm, the uniformity can reach +/-0.5%, and the resolution can reach 1 micron;
the photoetching process is an exposure process by using an inlet photoetching machine with an I-line high-resolution lens, and lines can be made to be 1 micron;
and the development corrosion is exposure, on an accurate full-automatic development corrosion device, firstly, 0.3% TMAH is utilized to remove the exposed photoresist by reaction, the solution temperature is controlled at 25 ℃, the development time is controlled at 25s, the special corrosive liquid adopts ammonium ceric nitrate, then the special corrosive liquid is utilized to remove and corrode the chromium layer exposed after the photoresist is removed by development, the corrosion time is controlled at 60s, the solution temperature is controlled at 25 ℃, and the line process requirement of 1 micron is met.
Precision cutting: and high-precision cutting equipment such as an automatic cutter wheel cutting machine, a laser cutting machine, a dicing saw and the like with specific ccd positioning is adopted for precision cutting, so that the squareness and the size precision are well controlled, and the size precision is +/-0.05 mm.
Example 7
For a calibration plate with flatness requirement of 10-30 microns, grinding by using a polishing sheet/original glass and then polishing the single surface, this embodiment is a preparation method of a diffuse reflection type calibration plate with frosted single surface, and the preparation method comprises the following steps:
a method for preparing a diffuse reflection type calibration plate comprises the following steps:
grinding for the first time: grinding the lower surface of the polishing sheet/original plate glass for 25min by using 40% DN95 carborundum solution with the grain diameter of less than 10 microns and the applied pressure during grinding of 300kgf to obtain a first grinding surface, wherein the upper surface of the polishing sheet/original plate glass is a plane; the first abrasive surface had a surface roughness Ra of 3 micrometers and a surface micro particle size of 7 micrometers.
And (3) polishing: polishing the upper surface of the polishing sheet/original glass for 60min by using a cerium oxide polishing solution with 20 percent DN95 and the particle size of 1 micron to obtain a polished surface; the polished surface had a surface roughness Ra of 0.01 nm. The polishing step is carried out on polyurethane and damping cloth; the pressure applied during polishing was 300 kgf.
Making a graph: processing and manufacturing a graph on the polishing surface of the upper surface of the polishing sheet/original plate glass by adopting a semiconductor mask graph manufacturing process flow, and sequentially carrying out film coating, glue coating, photoetching, developing and corrosion to prepare a metal chromium layer graph;
the coating process is that the polished wafer/original glass is put into a magnetron sputtering vacuum chamber after being cleaned and dried by ultrasonic, a layer of 100nm chromium film is coated on the front surface of the glass substrate by adopting a direct current magnetron sputtering process, and the proportion of process gas Ar \ N2\ O2\ CO2 in the sputtering process is 35 sccm: 25 sccm: 0 sccm: 9sccm, the vacuum degree of 4 multiplied by 10 < -6 >, and the sputtering power of 1.2kw to obtain a chromium film substrate;
the glue coating process adopts a spin coating process to spin to obtain a photoresist film with the glue thickness of 300nm, the uniformity can reach +/-0.5%, and the resolution can reach 1 micron;
the photoetching process is an exposure process by using an inlet photoetching machine with an I-line high-resolution lens, and lines can be made to be 1 micron;
after exposure, on a precise full-automatic developing corrosion device, firstly, 0.01-0.3% TMAH is used for removing the exposed photoresist in a reaction manner, the solution temperature is controlled at 24 ℃, the developing time is controlled at 15s, the special corrosion liquid adopts ammonium ceric nitrate, the chromium layer exposed after the photoresist is removed in the developing manner is removed by using the special corrosion liquid for removing corrosion, the corrosion time is controlled at 50s, the solution temperature is controlled at 24 ℃, and the technological requirement of 1 micron lines is met.
Precision cutting: and high-precision cutting equipment such as an automatic cutter wheel cutting machine, a laser cutting machine, a dicing saw and the like with specific ccd positioning is adopted for precision cutting, so that the squareness and the size precision are well controlled, and the size precision is +/-0.05 mm.
The prepared diffuse reflection type calibration plate with frosted double surfaces is shown in figure 3 and comprises a polishing sheet/original plate glass 1, wherein the upper surface of the polishing sheet/original plate glass 1 is a polishing surface 4, the lower surface of the polishing sheet/original plate glass 1 is a first grinding surface 2, and a metal chromium layer 3 is manufactured on the polishing surface 4 of the upper surface of the polishing sheet/original plate glass.
Claims (10)
1. A method for preparing a diffuse reflection type calibration plate is characterized by comprising the following steps:
grinding for the first time: grinding the upper surface of the polishing sheet/original glass for 10-40min by using 20-60% of DN95 carborundum solution with the grain diameter of less than 10 microns to obtain a first grinding surface, wherein the upper surface of the polishing sheet/original glass is the first grinding surface; or grinding the lower surface of the polishing sheet/original edition glass for 10-40min to obtain a first grinding surface, wherein the upper surface of the polishing sheet/original edition glass is a plane; or grinding the upper surface and the lower surface of the polishing sheet/original edition glass for 10-40min at the same time to obtain two first grinding surfaces, wherein the upper surface of the polishing sheet/original edition glass is the first grinding surface;
making a graph: processing and manufacturing a graph on the upper surface of the polished wafer/original plate glass by adopting a semiconductor mask graph manufacturing process flow, and sequentially carrying out film coating, glue coating, photoetching, developing and corrosion to prepare a metal chromium layer graph;
precision cutting: and performing precision cutting, wherein the size precision is +/-0.05 mm.
2. The method of claim 1, further comprising a polishing step between the first grinding step and the patterning step: and polishing a first grinding surface for 10-120min by using a cerium oxide polishing solution with 10-30% DN95 and the particle size of 0.5-1.5 microns to obtain a polished surface.
3. The method of claim 2, wherein the step of preparing the diffuse reflection type calibration plate comprises: and simultaneously polishing the other first grinding surface to obtain another polishing surface, and then grinding one polishing surface for the second time to obtain a second grinding surface.
4. The method of claim 3, wherein the step of preparing the diffusely reflective calibration plate comprises: the second grinding step is between the polishing step and the patterning step, or after the precision cutting step.
5. The method of claim 1, wherein the step of preparing the diffusely reflective calibration plate comprises: the first grinding step of the lower surface of the polishing sheet/master glass follows the precision cutting step.
6. The method of claim 3, wherein the step of preparing the diffusely reflective calibration plate comprises: the surface roughness Ra of the first grinding surface and/or the second grinding surface is 1-5 microns, and the surface micro-grain diameter is 6-8 microns.
7. The method for preparing a diffuse reflection type calibration plate according to any one of claims 2 to 4, wherein: the surface roughness Ra of the polished surface is 0.005-0.015 nm.
8. The method for preparing a diffuse reflection type calibration plate according to any one of claims 1 to 6, wherein:
the coating process is that the polished wafer/original glass is put into a magnetron sputtering vacuum chamber after being cleaned and dried by ultrasonic, a layer of chromium film with the thickness of 80-120nm is coated on the front surface of the glass substrate by adopting a direct current magnetron sputtering process, and the proportion of Ar, N2, O2 and CO2 in the process gas in the sputtering process is 5-80: 0-50: 0-60: 0-80, the vacuum degree is 1-8 multiplied by 10 < -6 >, the sputtering power is 0.2-5kw, and the chromium film substrate is obtained;
the glue coating process adopts a spin coating process to spin to obtain a photoresist film with the glue thickness of 100 and 500nm, the uniformity can reach +/-0.5%, and the resolution can reach 1 micron;
the photoetching process is an exposure process by using an imported photoetching machine with an I-line high-resolution lens;
after exposure, on a precise full-automatic developing corrosion device, firstly, 0.01-0.3% TMAH is used for removing the exposed photoresist by reaction, the solution temperature is controlled at 23-25 ℃, the developing time is controlled at 10-25s, then, a special corrosive liquid is used for removing the chromium layer exposed after the photoresist is removed by development, the corrosion time is 40-60s, and the solution temperature is 23-25 ℃.
9. The method for preparing a diffuse reflection type calibration plate according to any one of claims 1 to 6, wherein:
the pressure applied during the polishing is 100-;
grinding is carried out on polyurethane and damping cloth;
the pressure applied during polishing was 100-300 kgf.
10. A diffusely reflective calibration plate produced by the method of any one of claims 1 to 9.
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