CN116840227A - Metallographic display method of Ln series element doped In-Zn based oxide target material - Google Patents
Metallographic display method of Ln series element doped In-Zn based oxide target material Download PDFInfo
- Publication number
- CN116840227A CN116840227A CN202310691431.6A CN202310691431A CN116840227A CN 116840227 A CN116840227 A CN 116840227A CN 202310691431 A CN202310691431 A CN 202310691431A CN 116840227 A CN116840227 A CN 116840227A
- Authority
- CN
- China
- Prior art keywords
- polishing
- based oxide
- oxide target
- minutes
- metallographic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000013077 target material Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000005498 polishing Methods 0.000 claims abstract description 255
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 63
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 244000137852 Petrea volubilis Species 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000011010 flushing procedure Methods 0.000 claims abstract description 3
- 229910003460 diamond Inorganic materials 0.000 claims description 32
- 239000010432 diamond Substances 0.000 claims description 32
- 239000002245 particle Substances 0.000 claims description 30
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical group [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 28
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 28
- 238000005260 corrosion Methods 0.000 claims description 17
- 230000007797 corrosion Effects 0.000 claims description 17
- 238000005530 etching Methods 0.000 claims description 12
- 238000007517 polishing process Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000003384 imaging method Methods 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 description 43
- 239000000243 solution Substances 0.000 description 39
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 15
- 229910017604 nitric acid Inorganic materials 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 229910000925 Cd alloy Inorganic materials 0.000 description 7
- 238000000227 grinding Methods 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 239000000110 cooling liquid Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
-
- 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
- B24B19/00—Single-purpose machines or devices for particular grinding operations not covered by any other main group
-
- 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
- B24B29/00—Machines or devices for polishing surfaces on work by means of tools made of soft or flexible material with or without the application of solid or liquid polishing agents
- B24B29/02—Machines or devices for polishing surfaces on work by means of tools made of soft or flexible material with or without the application of solid or liquid polishing agents designed for particular workpieces
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The application belongs to the technical field of target detection, and discloses a metallographic display method of an Ln series element doped In-Zn based oxide target, which comprises the following steps of polishing by using sand paper, polishing by using a polishing solution, corroding by using a corrosive solution, flushing after corroding, drying, and observing the surface of the Ln series element doped In-Zn based oxide target under a metallographic microscope to obtain a metallographic structure image; the corrosive liquid is prepared from hydrofluoric acid, hydrochloric acid and water, and the volume ratio of the hydrofluoric acid to the hydrochloric acid to the water is 1-1.2: 1 to 1.2:20, performing metallographic display by the method to obtain a metallographic structure image of the Ln series element doped In-Zn based oxide target material with accurate imaging and clear grain boundary.
Description
Technical Field
The application relates to the technical field of target detection, in particular to a metallographic display method of an Ln series element doped In-Zn based oxide target.
Background
The Ln series element can be used as an excellent additive of a target material due to the unique optical, electrical and magnetic properties, and the Ln series element is widely applied to various fields as an additive at present. The sintering temperature, carrier concentration, resistivity and the like of the target can be improved by adding a proper amount of Ln series elements in the preparation process of the semiconductor oxide target; oxide semiconductor targets are relatively brittle and easy to crack due to the characteristics of the oxide semiconductor targets, and ZrO 2 The material itself has higher toughness and high bending resistance, so that a small amount of ZrO is added 2 The hardness and the bending strength of the target material can be enhanced.
Parameters such as grain size, grain orientation and the like of the target material have very important influences on physical properties, mechanical properties, photoelectric properties and the like of the sputtered film. To obtain high performance films, it is particularly important to characterize and control the grain size and grain orientation of the sputtering target. The grain size of the target is obtained by analyzing a metallographic image, and in the prior art, the target is required to be subjected to metallographic corrosion firstly, and then the metallographic structure of the target is observed by a metallographic microscope to obtain the metallographic image of the target; however, since different materials have different corrosion resistance to different acids, the composition and the ratio of the corrosive liquid of different materials are often different.
Chinese patent application 202210298167.5 discloses a metallographic display method of cadmium alloy, comprising the steps of: (1) Providing a cadmium alloy metallographic sample, and cutting according to a gold phase sample preparation standard to obtain a cadmium alloy sample; (2) Polishing the end face to be detected of the cadmium alloy sample obtained in the step (1) by using silicon carbide water-based sand paper until the surface of the end face is flat and close to a mirror surface; (3) Mechanically polishing the end face to be detected of the cadmium alloy sample polished in the step (2) until the surface of the end face is a mirror face; (4) And (3) carrying out metallographic chemical corrosion treatment on the end face to be detected of the cadmium alloy sample subjected to mechanical polishing in the step (3) to form a metallographic display surface.
The scheme mainly relates to a metallographic display method for cadmium alloy, wherein the corrosive liquid is prepared by adopting nitric acid alcohol solution, the volume fraction of the nitric acid alcohol solution is 2-5%, and as can be seen from comparative examples 1 and 2 of the scheme, when the corrosive liquid is changed from the nitric acid alcohol solution into nitric acid aqueous solution, the corrosion speed is difficult to control, and even if the volume fraction of nitric acid in the aqueous solution is greatly reduced, excessive corrosion still occurs.
Chinese patent application 202011317843.6 discloses a method for displaying high purity aluminum metallographic phase comprising the steps of:
(1) Sampling, namely turning the surface of the sample flat;
(2) Sequentially grinding with water-based sand paper with gradually smaller granularity;
(3) Fine grinding is carried out by adopting aqueous sand paper with smaller granularity than that in the step (2), and absolute ethyl alcohol is used as cooling liquid for fine grinding;
(4) Polishing the surface of the sample after fine grinding;
(5) And (3) chemically corroding the polished sample surface, cleaning with a cleaning agent, and drying.
As can be seen from the instruction book of the scheme, the corrosive agent in the scheme is a mixture of hydrofluoric acid, nitric acid and hydrochloric acid, wherein the volume ratio of the hydrofluoric acid, the nitric acid and the hydrochloric acid is: nitric acid: hydrochloric acid = 1:4 to 6:9 to 10, the mass concentration of HF in hydrofluoric acid is 40 to 49 percent, HNO in nitric acid 3 The mass concentration of HCl in hydrochloric acid is 60-68%, and the raw material in the scheme is high-purity aluminum material.
As can be seen from the above comparison document, for different materials, the corrosion resistance to acid is different, and in the corrosion process, not only the factors of raw materials, but also the factors of the type, the proportion, the concentration and the like of the acid are considered, so that the result of sufficient corrosion and excessive corrosion can be obtained, and metallographic structure metallographic observation is facilitated.
The problem that this scheme needs to solve: how to provide a metallographic display method of an Ln series element doped In-Zn based oxide target.
Disclosure of Invention
The application aims to provide a metallographic display method of an Ln series element doped In-Zn based oxide target, which is characterized In that the metallographic structure image of the Ln series element doped In-Zn based oxide target with clear crystal boundary and accurate imaging is obtained through steps of grinding, polishing, corrosion and the like.
In order to achieve the aim, the application discloses a metallographic display method of an Ln series element doped In-Zn based oxide target, which is characterized by comprising the following steps:
step 1: polishing by using sand paper;
step 2: polishing by using a polishing solution;
step 3: corroding by using a corrosive liquid;
step 4: washing, drying and observing the surface of the Ln series element doped In-Zn based oxide target material under a metallographic microscope to obtain a metallographic structure image;
the corrosive liquid is prepared from hydrofluoric acid, hydrochloric acid and water, and the volume ratio of the hydrofluoric acid to the hydrochloric acid to the water is 1-1.2: 1 to 1.2:20.
preferably, the sandpaper is silicon carbide sandpaper;
the polishing liquid is diamond polishing liquid.
Preferably, the step 1 specifically comprises:
primary polishing: the silicon carbide sand paper with 180 meshes is used for carrying out primary polishing, the rotating speed of the primary polishing is 240-260 r/min, and the primary polishing time is 2-4 minutes;
secondary polishing: carrying out secondary polishing by using 320-mesh silicon carbide sand paper, wherein the rotating speed of the secondary polishing is 290-310 r/min, and the secondary polishing time is 4-6 minutes;
and (3) polishing for three times: three times of polishing are carried out by using 500-mesh silicon carbide sand paper, the rotating speed of the three times of polishing is 290-310 r/min, and the time of the three times of polishing is 9-11 minutes;
four times of polishing: the silicon carbide sand paper with 1200 meshes is used for four times of polishing, the rotating speed of the four times of polishing is 340-360 r/min, and the four times of polishing time is 19-21 minutes;
five times of polishing: five times of polishing are carried out by using 3000-mesh silicon carbide sand paper, the rotating speed of the five times of polishing is 340-360 r/min, and the time of the five times of polishing is 19-21 minutes.
Preferably, step 2 specifically comprises:
primary polishing: performing primary polishing by using a diamond polishing solution with the particle size of 15 microns, wherein the rotating speed of the primary polishing is 340-360 r/min, and the primary polishing time is 38-42 minutes;
secondary polishing: performing secondary polishing by using diamond polishing solution with the particle size of 6 microns, wherein the rotating speed of the secondary polishing is 340-360 r/min, and the secondary polishing time is 18-22 minutes;
and (3) polishing for three times: and (3) polishing for three times by using diamond polishing liquid with the particle size of 0.25 microns, wherein the rotating speed of the polishing for three times is 340-360 r/min, and the polishing time for three times is 18-22 minutes.
Preferably, the angle of the In-Zn-based oxide target doped with the Ln series element is adjusted when the gap is polished once, polished twice, polished three times, polished four times and polished five times, the In-Zn-based oxide target doped with the Ln series element is rotated by 90 degrees after each polishing, and each rotation is the same as the direction of the previous rotation.
Preferably, the angle of the Ln element doped In-Zn-based oxide target is adjusted at the time of the gap of the primary polishing, the secondary polishing, and the tertiary polishing, and after each polishing, the Ln element doped In-Zn-based oxide target is rotated by 90 °, and each rotation is the same as the direction of the previous rotation.
Preferably, in the primary polishing process, diamond polishing liquid with the same particle size is supplemented every 2 minutes, and the volume of the supplemented polishing liquid is 1-2 ml;
in the secondary polishing process, the diamond polishing liquid with the same particle size is replenished every 2 minutes, and the volume of the replenished polishing liquid is 1-2 ml;
in the three polishing processes, every 2 minutes, the diamond polishing liquid with the same particle size is supplemented, and the volume of the supplemented polishing liquid is 1-2 ml.
Preferably, the step 3 specifically comprises:
mixing hydrofluoric acid, hydrochloric acid and water according to a volume ratio to prepare an etching solution;
immersing the polished surface of the Ln series element doped In-Zn based oxide target material into corrosive liquid for corrosion for 8-12 seconds, flushing with deionized water after corrosion, drying, and observing the surface of the Ln series element doped In-Zn based oxide target material under a microscope to obtain a metallographic structure image.
The beneficial effects of the application are as follows: the application obtains metallographic structure images of the Ln series element doped In-Zn based oxide target material with clear crystal boundary and accurate imaging through steps of grinding, polishing, corrosion and the like, and simultaneously obtains the corrosive liquid which is particularly suitable for the Ln series element doped In-Zn based oxide target material through controlling various kinds of acid, proportion and other variables.
Drawings
FIG. 1 is a metallographic image obtained in example 1;
FIG. 2 is a metallographic image obtained in example 2;
FIG. 3 is a metallographic image obtained in example 3;
FIG. 4 is a metallographic image obtained in comparative example 1;
FIG. 5 is a metallographic image obtained in comparative example 3;
FIG. 6 is a metallographic image obtained in comparative example 5.
Detailed Description
The present application will be described more fully hereinafter with reference to the accompanying drawings, in which specific conditions, either conventional or manufacturer-suggested, are not explicitly shown. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The target material of the following examples for metallographic display operation was an in—zn-based oxide target material doped with Pr element, wherein the mass fraction of Pr element In the target material was 6%.
Example 1
Step 1: primary polishing: the silicon carbide sand paper with 180 meshes is used for carrying out primary polishing, the rotating speed of the primary polishing is 240r/min, and the primary polishing time is 2 minutes;
secondary polishing: carrying out secondary polishing by using 320-mesh silicon carbide sand paper, wherein the rotating speed of the secondary polishing is 290r/min, and the secondary polishing time is 4 minutes;
and (3) polishing for three times: three times of polishing are carried out by using 500-mesh silicon carbide sand paper, the rotating speed of the three times of polishing is 290r/min, and the time of the three times of polishing is 9 minutes;
four times of polishing: four times of polishing are carried out by using 1200-mesh silicon carbide sand paper, the rotating speed of the four times of polishing is 340r/min, and the four times of polishing time is 19 minutes;
five times of polishing: five times of polishing are carried out by using 3000-mesh silicon carbide sand paper, the rotating speed of the five times of polishing is 340r/min, and the time of the five times of polishing is 19 minutes;
step 2: primary polishing: performing primary polishing by using a diamond polishing solution with the particle size of 15 microns, wherein the rotating speed of the primary polishing is 340r/min, and the primary polishing time is 38 minutes; the diamond polishing solution with the same particle size is replenished every 2 minutes, and the volume of the replenished polishing solution is 1ml;
secondary polishing: performing secondary polishing by using diamond polishing solution with the particle size of 6 microns, wherein the rotating speed of the secondary polishing is 340r/min, and the time of the secondary polishing is 18 minutes; the diamond polishing solution with the same particle size is replenished every 2 minutes, and the volume of the replenished polishing solution is 1ml;
and (3) polishing for three times: performing three times of polishing by using diamond polishing liquid with the particle size of 0.25 micron, wherein the rotating speed of the three times of polishing is 340r/min, and the time of the three times of polishing is 18 minutes; the diamond polishing solution with the same particle size is replenished every 2 minutes, and the volume of the replenished polishing solution is 1ml;
step 3: the volume ratio of hydrofluoric acid, hydrochloric acid and water is 1.1:1.1:20, wherein the concentration of hydrofluoric acid is 40% and the concentration of hydrochloric acid is 78%;
and clamping the polished Ln element doped In-Zn-based oxide target material by using tweezers, immersing the polished surface In etching liquid for 10 seconds, cleaning the polished surface by using deionized water after etching, drying, and observing the etched Ln element doped In-Zn-based oxide target material by using a metallographic microscope after drying to obtain a metallographic structure image, wherein the grain boundary contour on the obtained metallographic structure image is clear, and the phases are obviously different.
Example 2
Step 1: primary polishing: the silicon carbide sand paper with 180 meshes is used for polishing once, the rotating speed of the polishing once is 260r/min, the polishing time once is 4 minutes, and after polishing once, the Ln series element doped In-Zn based oxide target material is rotated anticlockwise for 90 degrees;
secondary polishing: carrying out secondary polishing by using 320-mesh silicon carbide sand paper, wherein the rotating speed of the secondary polishing is 310r/min, and the secondary polishing time is 6 minutes; after secondary polishing, rotating the Ln series element doped In-Zn based oxide target material by 90 degrees anticlockwise;
and (3) polishing for three times: three times of polishing are carried out by using 500-mesh silicon carbide sand paper, the rotating speed of the three times of polishing is 310r/min, and the time of the three times of polishing is 11 minutes; after three times of polishing, rotating the Ln series element doped In-Zn based oxide target material by 90 degrees anticlockwise;
four times of polishing: four times of polishing are carried out by using 1200-mesh silicon carbide sand paper, the rotating speed of the four times of polishing is 360r/min, and the four times of polishing time is 21 minutes; after four times of polishing, rotating the Ln series element doped In-Zn based oxide target material by 90 degrees anticlockwise;
five times of polishing: five times of polishing are carried out by using 3000-mesh silicon carbide sand paper, the rotating speed of the five times of polishing is 360r/min, and the time of the five times of polishing is 21 minutes; after five times of polishing, the Ln series element doped In-Zn based oxide target material is rotated anticlockwise for 90 degrees;
step 2: primary polishing: performing primary polishing by using a diamond polishing solution with the particle size of 15 microns, wherein the rotating speed of the primary polishing is 360r/min, and the time of the primary polishing is 42 minutes; after primary polishing, rotating the Ln series element doped In-Zn based oxide target material by 90 degrees anticlockwise; the diamond polishing solution with the same particle size is replenished every 2 minutes, and the volume of the replenished polishing solution is 1.5ml;
secondary polishing: performing secondary polishing by using diamond polishing solution with the particle size of 6 microns, wherein the rotating speed of the secondary polishing is 360r/min, and the time of the secondary polishing is 22 minutes; after secondary polishing, rotating the Ln series element doped In-Zn based oxide target material by 90 degrees anticlockwise; the diamond polishing solution with the same particle size is replenished every 2 minutes, and the volume of the replenished polishing solution is 1.5ml;
and (3) polishing for three times: the diamond polishing solution with the particle size of 0.25 micron is used for three times of polishing, the rotating speed of the three times of polishing is 360r/min, and the time of the three times of polishing is 22 minutes. After three times of polishing, rotating the Ln series element doped In-Zn based oxide target material by 90 degrees anticlockwise; the diamond polishing solution with the same particle size is replenished every 2 minutes, and the volume of the replenished polishing solution is 1.5ml;
step 3: the volume ratio of hydrofluoric acid, hydrochloric acid and water is 1.1:1.1:20, wherein the concentration of hydrofluoric acid is 40% and the concentration of hydrochloric acid is 78%;
and clamping the polished Ln element doped In-Zn-based oxide target material by using tweezers, immersing the polished surface In etching liquid for 8 seconds, cleaning the polished surface by using deionized water after etching, drying, and observing the etched Ln element doped In-Zn-based oxide target material by using a metallographic microscope after drying to obtain a metallographic structure image, wherein the grain boundary contour on the obtained metallographic structure image is clear, and the phases are obviously different.
Example 3
Step 1: primary polishing: the silicon carbide sand paper with 180 meshes is used for polishing once, the rotating speed of the polishing once is 250r/min, the polishing time once is 3 minutes, and after polishing once, the Ln series element doped In-Zn based oxide target material is rotated anticlockwise for 90 degrees;
secondary polishing: carrying out secondary polishing by using 320-mesh silicon carbide sand paper, wherein the rotating speed of the secondary polishing is 300r/min, and the secondary polishing time is 5 minutes; after secondary polishing, rotating the Ln series element doped In-Zn based oxide target material by 90 degrees anticlockwise;
and (3) polishing for three times: three times of polishing are carried out by using 500-mesh silicon carbide sand paper, the rotating speed of the three times of polishing is 300r/min, and the time of the three times of polishing is 10 minutes; after three times of polishing, rotating the Ln series element doped In-Zn based oxide target material by 90 degrees anticlockwise;
four times of polishing: four times of polishing are carried out by using 1200-mesh silicon carbide sand paper, the rotating speed of the four times of polishing is 350r/min, and the four times of polishing time is 20 minutes; after four times of polishing, rotating the Ln series element doped In-Zn based oxide target material by 90 degrees anticlockwise;
five times of polishing: five times of polishing are carried out by using 3000-mesh silicon carbide sand paper, the rotating speed of the five times of polishing is 350r/min, and the time of the five times of polishing is 20 minutes; after five times of polishing, the Ln series element doped In-Zn based oxide target material is rotated anticlockwise for 90 degrees;
step 2: primary polishing: performing primary polishing by using a diamond polishing solution with the particle size of 15 microns, wherein the rotating speed of the primary polishing is 350r/min, and the time of the primary polishing is 40 minutes; after primary polishing, rotating the Ln series element doped In-Zn based oxide target material by 90 degrees anticlockwise; the diamond polishing solution with the same particle size is replenished every 2 minutes, and the volume of the replenished polishing solution is 2ml;
secondary polishing: performing secondary polishing by using diamond polishing solution with the particle size of 6 microns, wherein the rotating speed of the secondary polishing is 350r/min, and the time of the secondary polishing is 20 minutes; after secondary polishing, rotating the Ln series element doped In-Zn based oxide target material by 90 degrees anticlockwise; the diamond polishing solution with the same particle size is replenished every 2 minutes, and the volume of the replenished polishing solution is 2ml;
and (3) polishing for three times: the diamond polishing solution with the particle size of 0.25 micron is used for three times of polishing, the rotating speed of the three times of polishing is 350r/min, and the time of the three times of polishing is 20 minutes. After three times of polishing, rotating the Ln series element doped In-Zn based oxide target material by 90 degrees anticlockwise; the diamond polishing solution with the same particle size is replenished every 2 minutes, and the volume of the replenished polishing solution is 2ml;
step 3: the volume ratio of hydrofluoric acid, hydrochloric acid and water is 1.1:1.1:20, wherein the concentration of hydrofluoric acid is 40% and the concentration of hydrochloric acid is 78%;
and clamping the polished Ln element doped In-Zn-based oxide target material by using tweezers, immersing the polished surface In corrosive liquid for 12 seconds, cleaning the polished surface by using deionized water after corrosion, drying, and observing the corroded Ln element doped In-Zn-based oxide target material by using a metallographic microscope after drying to obtain a metallographic structure image, wherein the grain boundary contour on the obtained metallographic structure image is clear, and the phases are obviously different.
Example 4
Substantially the same as in example 1, except that the etching solution was prepared from hydrofluoric acid, hydrochloric acid, and water in a volume ratio of 1:1.2:20, and the grain boundary contour on the finally obtained metallographic structure image is clear, and the phases are obviously distinguished.
Example 5
Substantially the same as in example 1, except that the etching solution was prepared from hydrofluoric acid, hydrochloric acid, and water in a volume ratio of 1.2:1:20, and the grain boundary contour on the finally obtained metallographic structure image is clear, and the phases are obviously distinguished.
Comparative example 1
Substantially the same as in example 1, except that the etching solution was prepared from hydrofluoric acid and water in a volume ratio of 2.2:20, preparing a mixed solution of 20; as the corrosive liquid does not have the participation of hydrochloric acid, the outline of the grain boundary of each part on the finally obtained metallographic structure image is not clear, and the phases are not obvious.
Comparative example 2
Substantially the same as in example 1, except that the corrosive liquid was prepared from nitric acid and water in a volume ratio of 2.2:20, preparing a mixed solution of 20; since nitric acid is not suitable for corrosion of the target, the outline of the grain boundary of each part on the finally obtained metallographic structure image is not clear, and the phases are not obvious.
Comparative example 3
Substantially the same as in example 1, except that the etching solution was composed of hydrofluoric acid, nitric acid, and water in a volume ratio of 1.1:1.1:20, preparing a mixed solution of 20; because hydrofluoric acid and nitric acid can not better synergistically corrode the target material, the outline of the grain boundary of each part on the finally obtained metallographic structure image is not clear, and the phases are not obvious
Comparative example 4
Substantially the same as in example 1, except that the volume ratio of the corrosive liquid to hydrochloric acid, nitric acid, and water was 1.1:1.1:20, preparing a mixed solution of 20; because hydrochloric acid and nitric acid can not better synergistically corrode the target, the contour of the grain boundary of each part on the finally obtained metallographic structure image is not clear, and the phases are not obvious.
Comparative example 5
Substantially the same as in example 1, except that the etching solution was prepared from hydrofluoric acid, hydrochloric acid, and water in a volume ratio of 1.5:1.5:20, preparing a mixed solution of 20; because the concentration of hydrochloric acid and hydrofluoric acid is too high, the outline of the grain boundary of each part on the finally obtained metallographic structure image is not clear, and the phases are not obvious.
Comparative example 6
Substantially the same as in example 1, except that the etching solution was composed of hydrofluoric acid, hydrochloric acid, and water in a volume ratio of 0.8:0.8:20, preparing a mixed solution of 20; because the concentration of hydrochloric acid and hydrofluoric acid is too low, the outline of the grain boundary of each part on the finally obtained metallographic structure image is not clear, and the phases are not obvious.
Comparative example 7
Substantially the same as In example 1, except that the Ln-based element-doped In-Zn-based oxide target was replaced with an undoped Ln-based element-doped In-Zn-based oxide target; as hydrochloric acid and hydrofluoric acid can cooperatively corrode the Ln series element doped In-Zn based oxide target material In a proper concentration ratio, when the type of the target material is changed, the outline of the grain boundary of each part on a finally obtained metallographic structure image is not clear, and the phases are not obvious.
Comparative example 8
Substantially the same as In example 1, except that an indium target was used instead of the Ln-based element-doped in—zn-based oxide target; as hydrochloric acid and hydrofluoric acid can cooperatively corrode the Ln series element doped In-Zn based oxide target material In a proper concentration ratio, when the type of the target material is changed, the outline of the grain boundary of each part on a finally obtained metallographic structure image is not clear, and the phases are not obvious.
Comparative example 9
Substantially the same as In example 1, except that a zinc target was used In place of the Ln-based element-doped in—zn-based oxide target; as hydrochloric acid and hydrofluoric acid can cooperatively corrode the Ln series element doped In-Zn based oxide target material In a proper concentration ratio, when the type of the target material is changed, the outline of the grain boundary of each part on a finally obtained metallographic structure image is not clear, and the phases are not obvious.
The above examples are preferred embodiments of the present application, but the embodiments of the present application are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present application should be made in the equivalent manner, and the embodiments are included in the protection scope of the present application.
Claims (8)
1. A metallographic display method of an Ln series element doped In-Zn based oxide target material is characterized by comprising the following steps:
step 1: polishing by using sand paper;
step 2: polishing by using a polishing solution;
step 3: corroding by using a corrosive liquid;
step 4: washing, drying and observing the surface of the Ln series element doped In-Zn based oxide target material under a metallographic microscope to obtain a metallographic structure image;
the corrosive liquid is prepared from hydrofluoric acid, hydrochloric acid and water, and the volume ratio of the hydrofluoric acid to the hydrochloric acid to the water is 1-1.2: 1 to 1.2:20, a step of;
the concentration of hydrofluoric acid is 40%, and the concentration of hydrochloric acid is 78%.
2. The metallographic display method of the Ln-based element doped In-Zn-based oxide target material according to claim 1, wherein said sandpaper is silicon carbide sandpaper;
the polishing liquid is diamond polishing liquid.
3. The metallographic display method of the Ln-based element doped In-Zn-based oxide target material according to any one of claims 1-2, characterized In that said step 1 specifically is:
primary polishing: the silicon carbide sand paper with 180 meshes is used for carrying out primary polishing, the rotating speed of the primary polishing is 240-260 r/min, and the primary polishing time is 2-4 minutes;
secondary polishing: carrying out secondary polishing by using 320-mesh silicon carbide sand paper, wherein the rotating speed of the secondary polishing is 290-310 r/min, and the time of the secondary polishing is 4-6 minutes;
and (3) polishing for three times: three times of polishing are carried out by using 500-mesh silicon carbide sand paper, the rotating speed of the three times of polishing is 290-310 r/min, and the time of the three times of polishing is 9-11 minutes;
four times of polishing: the silicon carbide sand paper with 1200 meshes is used for four times of polishing, the rotating speed of the four times of polishing is 340-360 r/min, and the time of the four times of polishing is 19-21 minutes;
five times of polishing: five times of polishing are carried out by using 3000-mesh silicon carbide sand paper, the rotating speed of the five times of polishing is 340-360 r/min, and the time of the five times of polishing is 19-21 minutes.
4. The metallographic display method of the Ln-based element doped In-Zn-based oxide target material according to any one of claims 1-2, characterized In that said step 2 specifically is:
primary polishing: performing primary polishing by using a diamond polishing solution with the particle size of 15 microns, wherein the rotating speed of the primary polishing is 340-360 r/min, and the primary polishing time is 38-42 minutes;
secondary polishing: performing secondary polishing by using diamond polishing solution with the particle size of 6 microns, wherein the rotating speed of the secondary polishing is 340-360 r/min, and the secondary polishing time is 18-22 minutes;
and (3) polishing for three times: and (3) polishing for three times by using diamond polishing liquid with the particle size of 0.25 microns, wherein the rotating speed of the polishing for three times is 340-360 r/min, and the polishing time for three times is 18-22 minutes.
5. The method for displaying metallographic phase of an Ln-doped Zn-based oxide target according to claim 3, wherein the angle of the Ln-doped Zn-based oxide target is adjusted when the gap is between one polishing, two polishing, three polishing, four polishing, five polishing, and after each polishing, the Ln-doped In-Zn-based oxide target is rotated by 90 ° and each rotation is the same direction as the previous rotation.
6. The method for displaying metallographic phase of an Ln-doped Zn-based oxide target according to claim 4, wherein the angle of the Ln-doped Zn-based oxide target is adjusted at the time of the gap of the primary polishing, the secondary polishing, and the tertiary polishing, and after each polishing, the Ln-doped In-Zn-based oxide target is rotated by 90 ° and each rotation is the same direction as the previous rotation.
7. The metallographic display method of the Ln-based element doped In-Zn-based oxide target material according to claim 4, wherein In the primary polishing process, diamond polishing liquid with the same particle size is supplemented every 2 minutes, and the volume of the supplemented polishing liquid is 1-2 ml;
in the secondary polishing process, the diamond polishing liquid with the same particle size is replenished every 2 minutes, and the volume of the replenished polishing liquid is 1-2 ml;
in the three polishing processes, every 2 minutes, the diamond polishing liquid with the same particle size is supplemented, and the volume of the supplemented polishing liquid is 1-2 ml.
8. The metallographic display method of the Ln-based element doped In-Zn-based oxide target according to claim 3, wherein the step 3 is specifically:
mixing hydrofluoric acid, hydrochloric acid and water according to a volume ratio to prepare an etching solution;
immersing the polished surface of the Ln series element doped In-Zn based oxide target material into corrosive liquid for corrosion for 8-12 seconds, flushing with deionized water after corrosion, drying, and observing the surface of the Ln series element doped In-Zn based oxide target material under a microscope to obtain a metallographic structure image.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310691431.6A CN116840227A (en) | 2023-06-12 | 2023-06-12 | Metallographic display method of Ln series element doped In-Zn based oxide target material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310691431.6A CN116840227A (en) | 2023-06-12 | 2023-06-12 | Metallographic display method of Ln series element doped In-Zn based oxide target material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116840227A true CN116840227A (en) | 2023-10-03 |
Family
ID=88171604
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310691431.6A Pending CN116840227A (en) | 2023-06-12 | 2023-06-12 | Metallographic display method of Ln series element doped In-Zn based oxide target material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116840227A (en) |
-
2023
- 2023-06-12 CN CN202310691431.6A patent/CN116840227A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7452481B2 (en) | Polishing slurry and method of reclaiming wafers | |
| CN1967197A (en) | Method for preparing Al-Si-Cu-based alloy metallographic sample and displaying tissue thereof | |
| JP3820787B2 (en) | Sputtering target and manufacturing method thereof | |
| CN109211648B (en) | Preparation method of aluminum oxide dispersion strengthened copper alloy metallographic sample | |
| CN110823667B (en) | Metallographic corrosive agent for high-strength titanium alloy and preparation method of metallographic sample of high-strength titanium alloy | |
| CN110382730A (en) | The manufacturing method and sprayed manufacturing method of sprayed, spraying plating powder, spraying plating powder | |
| CN102419275A (en) | Method for observing metallographic structure of molybdenum-niobium alloy | |
| Githens et al. | Patterning corrosion‐susceptible metallic alloys for digital image correlation in a scanning electron microscope | |
| WO2023168780A1 (en) | Polishing solution having low abrasive material content and weak acidity for ultra-precise machining of optical glass, preparation method therefor | |
| CN110018028B (en) | Preparation method of metallographic section sample of sapphire substrate electronic component | |
| CN116840227A (en) | Metallographic display method of Ln series element doped In-Zn based oxide target material | |
| CN111040639A (en) | Chemical mechanical polishing liquid for processing optical surface of Ge-As-Se chalcogenide glass | |
| TW200813194A (en) | Alkaline etching solution for semiconductor wafer and alkaline etching method | |
| CN105699137B (en) | The structure display methods of crome metal | |
| CN115436134A (en) | Metallographic structure characterization method of high-purity yttrium target material | |
| CN116519416A (en) | Sample preparation method for industrial pure titanium metallographic structure observation | |
| CN113340690A (en) | Preparation method of high-purity aluminum gold phase sample | |
| CN111074279A (en) | Target corrosive agent and application method thereof | |
| CN113005457A (en) | Metallographic corrosive agent of aluminum alloy shear band, corrosion method and application | |
| CN112326377A (en) | Cadmium oxide metallographic specimen and preparation method thereof | |
| CN111537304B (en) | Sample preparation method and sample for Al-Li-Cu series deformation alloy | |
| CN113125481A (en) | Sample preparation method of EBSD sample of AlSc sputtering target material | |
| Schenk | Solid-solution hardening of bulk crystals | |
| CN113252411A (en) | Method for displaying nonmetallic inclusion of nickel-titanium alloy | |
| CN117721468A (en) | Corrosion solution and corrosion method for displaying metallographic structure of high-purity AL-0.5% Cu target material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |