CN115595585A - Preparation method of special metallographic polishing agent for easily-oxidized metal - Google Patents
Preparation method of special metallographic polishing agent for easily-oxidized metal Download PDFInfo
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- CN115595585A CN115595585A CN202211404909.4A CN202211404909A CN115595585A CN 115595585 A CN115595585 A CN 115595585A CN 202211404909 A CN202211404909 A CN 202211404909A CN 115595585 A CN115595585 A CN 115595585A
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- 238000005498 polishing Methods 0.000 title claims abstract description 78
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 28
- 239000002184 metal Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 70
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 56
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 39
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000002244 precipitate Substances 0.000 claims abstract description 21
- 238000000498 ball milling Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 125000003158 alcohol group Chemical group 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 7
- 239000012266 salt solution Substances 0.000 claims abstract description 7
- 239000006185 dispersion Substances 0.000 claims abstract description 6
- 150000000703 Cerium Chemical class 0.000 claims abstract description 5
- 150000002603 lanthanum Chemical class 0.000 claims abstract description 5
- 239000012716 precipitator Substances 0.000 claims abstract description 5
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- 239000002243 precursor Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical group NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 3
- 239000001099 ammonium carbonate Substances 0.000 claims description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 3
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 3
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims 1
- 235000017550 sodium carbonate Nutrition 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 6
- 150000002739 metals Chemical class 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 5
- 230000035882 stress Effects 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000002344 surface layer Substances 0.000 abstract description 3
- 238000007517 polishing process Methods 0.000 abstract description 2
- 229910000861 Mg alloy Inorganic materials 0.000 description 13
- 229910000881 Cu alloy Inorganic materials 0.000 description 7
- 235000011187 glycerol Nutrition 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 4
- 229920003081 Povidone K 30 Polymers 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- -1 magnesium alloy Chemical class 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 101150096185 PAAS gene Proteins 0.000 description 1
- DRVWBEJJZZTIGJ-UHFFFAOYSA-N cerium(3+);oxygen(2-) Chemical class [O-2].[O-2].[O-2].[Ce+3].[Ce+3] DRVWBEJJZZTIGJ-UHFFFAOYSA-N 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
- C23F3/02—Light metals
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
A preparation method of a special metallographic polishing agent for easily oxidized metals comprises nano cerium oxide or lanthanum oxide abrasive particles, a dispersing agent, a PH regulator and an alcohol group or oil-based/alcohol-based mixed liquid. The preparation method comprises the following steps: adding a precipitator into the cerium salt or lanthanum salt solution, aging to generate precipitates, washing, drying and roasting to obtain the cerium oxide or lanthanum oxide abrasive particles. Grinding the abrasive particles into nano-grade abrasive particles by ball milling; adding a dispersing agent, a pH regulator and an alcohol group or oil-based/alcohol-based mixed liquid, and uniformly mixing in a high-speed cutting dispersion machine to obtain the special metallographic polishing agent for the easily-oxidized metal. The invention adopts oil base or oil base/alcohol base mixed liquid as a dispersion system, which can prevent the oxidation of the easily oxidized metal in the polishing process; in a weakly alkaline environment, the polishing agent abrasive particles can effectively remove stress layers and oxide films on the surface layers of easily oxidized metal samples.
Description
Technical Field
The invention relates to a polishing agent and a preparation method thereof, in particular to a preparation method of a special metallographic polishing agent for easily-oxidized metal, belonging to the technical field of polishing agents.
Background
With the rapid development of science and technology and industry, magnesium alloy is applied more and more in the fields of aerospace, textile, instruments and the like at present, and compared with other metal materials, the magnesium alloy has the advantages of low density, radiation resistance, high specific strength and specific stiffness, good vibration damping performance and the like, and has wide application prospects in the fields of electronics, automobiles, aerospace and the like. The magnesium alloy can form texture in the processing process, and the crystal grains can have preferred orientation.
The Electron backscattering Diffraction (EBSD) technique is a research and analysis method for determining crystal structure orientation and related information assembled in a scanning Electron microscope. It plays an extremely important role in studying the microstructure of materials and controlling their properties, and is called a "new weapon" for the microstructure study of materials. However, the EBSD analysis has high requirements on the surface quality of the sample, and requires that the surface of the sample has no residual stress layer, no oxide film, no pollution, good conductivity and proper size. The preparation of EBSD samples is the basis and difficulty of EBSD detection. The chemical-mechanical polishing method is a method for preparing the EBSD sample with high efficiency, safety, economy and wide application range. However, no chemical-mechanical polishing agent special for easily oxidized metals such as magnesium alloy, copper alloy and the like is produced and sold at present in China. At present, the magnesium alloy and copper alloy EBSD samples are mainly prepared by electrolytic polishing, and the electrolytic polishing has the defects of complex process, narrow application range, toxicity and danger of electrolyte, low safety and the like.
The metallographic polishing agent prepared aiming at the EBSD analysis sample in China has few types, and has the problems of being not suitable for polishing of easily oxidized metals such as magnesium alloy, copper alloy and the like, and the severe oxidation occurs when the magnesium alloy and the copper alloy are polished. The general metallographic polishing agent cannot remove stress layers and oxide films on the surface layers of magnesium alloy and copper alloy samples, and has the problem of low polishing efficiency.
Disclosure of Invention
The invention aims to provide a preparation method of a special metallographic polishing agent for easily-oxidized metals, aiming at the problems of metallographic polishing agents prepared from EBSD analysis samples, and particularly the problem that the polishing of easily-oxidized metals such as magnesium alloys and copper alloys cannot be solved.
The technical scheme is that the preparation method of the special metallographic polishing agent for the easily oxidized metal comprises nano cerium oxide or lanthanum oxide abrasive particles, a dispersing agent, a PH regulator and an alcohol group or oil-based/alcohol-based mixed liquid; wherein, the dispersant is 1.5 percent, the PH regulator is 0.7 to 0.8 percent, the abrasive particles are 5 to 20 percent, and the balance is alcohol group or oil-based alcohol group mixed liquid.
The preparation method comprises the following steps:
adding Ce 4+ Salt or La 3+ Mixing salt with a polyvinylpyrrolidone (PVP K30) solution or a hydrochloric acid solution to prepare a cerium salt or lanthanum salt solution, adding a precipitator, standing and aging at 50-100 ℃ until a precipitate is generated, cleaning the precipitate with deionized water or ethanol, then drying in vacuum to obtain a cerium oxide precursor or a lanthanum oxide precursor, roasting the cerium oxide precursor or the lanthanum oxide precursor to generate cerium oxide or lanthanum oxide abrasive particles with certain crystallinity, and ball-milling the cerium oxide or the lanthanum oxide precursor into nano-scale cerium oxide particles by a ball mill; adding a dispersing agent, a pH regulator and an alcohol group or oil-based/alcohol-based mixed liquid, mixing in a high-speed cutting dispersion machine, and uniformly dispersing to obtain the special metallographic polishing agent for the easily-oxidized metal.
The method adopts a planetary ball mill to perform ball milling on the abrasive particles for 1-3 hours, 3-5 hours and 5-10 hours; respectively obtaining polishing agent abrasive particles with the particle sizes of 0.06 mu m, 0.05 mu m and 0.02 mu m; the nano cerium oxide particles with different particle sizes can be independently used as polishing agent abrasive particles, and the cerium oxide particles with different particle sizes can be mixed to be used as the polishing agent abrasive particles; cerium oxides of 0.02 μm and 0.05 μm/0.06 μm particle diameters were mixed in accordance with a ratio of 2.
The oil base is glycerol or silicone oil, and the alcohol group is ethanol or methanol; the oil-based/alcohol-based mixed liquid comprises the following components in percentage by weight of 1.
The dispersant is polyvinylpyrrolidone (PVP K30), sodium Polyacrylate (PAAS) or magnesium aluminum silicate.
The PH regulator is ethanolamine, sodium hydroxide or sodium methoxide.
The roasting temperature of the cerium oxide particles or the lanthanum oxide particles with certain crystallinity is 800-950 ℃.
Compared with the chemical-mechanical polishing agent in the current market, the polishing agent disclosed by the invention adopts oil base or oil base/alcohol base mixed liquid as a dispersion system instead of water, so that the oxidation of easily oxidized metal in the polishing process can be prevented; in addition, under a weakly alkaline environment, the polishing agent abrasive particles can effectively remove stress layers and oxide films on the surface layers of easily oxidized metal samples; the invention adopts cerium oxide and lanthanum oxide nano-scale particles as polishing agent abrasive particles, and has the advantages of high polishing efficiency, low sample surface roughness, high flatness and the like.
Compared with the currently commonly adopted electrolytic polishing method for preparing the EBSD sample of the easily-oxidized metal such as magnesium alloy, copper alloy and the like, the method for preparing the EBSD sample by adopting the special metallographic polishing agent for the easily-oxidized metal has the advantages of simple process, wide application range, no toxicity, no harm, good safety performance and the like.
Drawings
FIG. 1 is a block diagram of a metallographic polishing agent preparation process according to the present invention;
FIG. 2 is a magnesium alloy after polishing with a polishing agent according to an embodiment of the present invention;
FIG. 3 is a magnesium alloy after polishing with a conventional chemical-mechanical polishing agent;
FIG. 4 is a graph of pure copper after polishing with a polishing agent according to an embodiment of the invention;
figure 5 shows pure copper after polishing with a conventional chemical-mechanical polishing agent.
Detailed Description
Fig. 1 is a block diagram of a process for preparing a metallurgical polishing agent according to the present invention.
Example 1
1. Preparing nano cerium oxide abrasive particles:
（1）preparing raw materials: ce is mixed 4+ Mixing the salt with a polyvinylpyrrolidone (PVP K30) solution to prepare a cerium salt solution;
(2) And (3) generation of a precipitate: adding a precipitant sodium carbonate, standing and aging at 80 ℃ until precipitates are generated;
(3) Cleaning: washing the precipitate with deionized water or ethanol;
(4) And (3) drying: drying the precipitate in a vacuum drying oven at 200 ℃ for 2h to obtain a cerium oxide precursor;
(5) Roasting: placing the cerium oxide precursor in a muffle furnace, heating to 900 ℃, preserving heat for 2 hours, and roasting to generate cerium oxide particles with certain crystallinity;
(6) Ball milling: and (3) placing the cerium oxide particles in an agate ball milling tank, and carrying out ball milling for 5 hours by using a planetary ball mill to obtain cerium oxide particles with the particle size of 0.05 mu m, and carrying out ball milling for 10 hours to obtain cerium oxide particles with the particle size of 0.02 mu m.
2. Preparing a polishing solution:
mixing 0.02 μm with 0.05 μm cerium oxide particles according to 5; dispersing polyvinyl pyrrolidone serving as a dispersing agent in a total mass of 1.5%, ethanolamine serving as a pH regulator in a total mass of 0.8%, cerium oxide particles in a total mass of 10% and the rest of glycerin/ethanol mixed liquid (the ratio of glycerin to ethanol is 1.
Example 2
1. Preparing nano cerium oxide abrasive particles:
(1) Preparing raw materials: adding Ce 4+ Mixing salt and hydrochloric acid solution to prepare cerium salt solution;
(2) Precipitate formation: adding a precipitator ammonium bicarbonate, standing and aging at 70 ℃ until precipitates are generated;
(3) Cleaning: washing the precipitate with deionized water or ethanol;
(4) And (3) drying: drying the precipitate in a vacuum drying oven at 80 ℃ for 10h to obtain a cerium oxide precursor;
(5) Roasting: placing the cerium oxide precursor in a muffle furnace, heating to 850 ℃, preserving heat for 3 hours, and roasting to generate cerium oxide particles with certain crystallinity;
(6) Ball milling: and (3) placing the cerium oxide particles in an agate ball milling tank, and carrying out ball milling for 5 hours by using a planetary ball mill to obtain the cerium oxide particles with the particle size of 0.05 mu m.
2. Preparing a polishing solution:
dispersing polyvinyl pyrrolidone serving as a dispersing agent with the total mass of 1.0%, ethanolamine serving as a pH regulator with the total mass of 0.9%, cerium oxide particles with the total mass of 15% and the rest of glycerin/ethanol mixed liquid (the ratio of glycerin to ethanol is 1.
Example 3
1. Preparing nano lanthanum oxide abrasive particles:
(1) Preparing raw materials: la 3+ Mixing the salt with a polyvinylpyrrolidone (PVP K30) solution to prepare a lanthanum salt solution;
(2) Precipitate formation: adding a precipitator ammonium bicarbonate, standing and aging at 90 ℃ until precipitates are generated;
(3) Cleaning: washing the precipitate with deionized water or ethanol;
(4) And (3) drying: drying the precipitate in a vacuum drying oven at 120 ℃ for 6h to obtain a lanthanum oxide precursor;
(5) Roasting: placing the lanthanum oxide precursor in a muffle furnace, heating to 920 ℃, preserving the temperature for 2 hours, and roasting to generate lanthanum oxide particles with certain crystallinity;
(6) Ball milling: and placing the lanthanum oxide particles in an agate ball milling tank, carrying out ball milling for 3h by using a planetary ball mill to obtain lanthanum oxide particles with the particle size of 0.06 mu m, and carrying out ball milling for 7h to obtain lanthanum oxide particles with the particle size of 0.02 mu m.
2. Preparing a polishing solution:
mixing 0.02 μm with 0.06 μm lanthanum oxide particles according to 3; dispersing polyvinyl pyrrolidone serving as a dispersing agent in a total mass of 1.0%, ethanolamine serving as a pH regulator in a total mass of 1.0%, lanthanum oxide particles in a total mass of 10% and the rest of glycerin/methanol mixed liquid (the ratio of glycerin to methanol is 1.
Example 4
1. Preparing nano lanthanum oxide abrasive particles:
(1) Preparing raw materials: la 3+ Mixing salt and hydrochloric acid solution to prepare lanthanum salt solution;
(2) And (3) generation of a precipitate: adding oxalic acid as precipitant, and standing at 80 deg.C for aging to obtain precipitate;
(3) Cleaning: washing the precipitate with deionized water or ethanol;
(4) And (3) drying: drying the precipitate in a vacuum drying oven at 90 ℃ for 10h to obtain a lanthanum oxide precursor;
(5) Roasting: placing the lanthanum oxide precursor in a muffle furnace, heating to 900 ℃, preserving heat for 5 hours, and roasting to generate lanthanum oxide particles with certain crystallinity;
(6) Ball milling: and (3) placing the lanthanum oxide particles in an agate ball milling tank, and carrying out ball milling for 5 hours by using a planetary ball mill to obtain the lanthanum oxide particles with the particle size of 0.05 mu m.
2. Preparing a polishing solution:
dispersing sodium polyacrylate serving as a dispersing agent accounting for 1.0 percent of the total mass, sodium methoxide serving as a pH regulator accounting for 1.0 percent of the total mass, lanthanum oxide particles accounting for 5 percent of the total mass and the rest ethanol liquid in a high-speed cutting disperser in a high-shear manner, and uniformly mixing to obtain the special metallographic polishing agent for the easily oxidized metal.
Example 5 (test example)
The polishing agent and the common chemical-mechanical polishing agent are respectively adopted, vibroMet 2 vibration polishing machines are used for carrying out chemical-mechanical polishing on the magnesium alloy, and SEM detection is carried out on the polished material, and the results are shown in a figure 2 and a figure 3.
As can be seen from the detection results, compared with the common chemical-mechanical polishing agent, the polishing agent of the invention has no scratch and oxide layer on the surface of the material after being polished, and the polishing quality is obviously superior to that of the common chemical-mechanical polishing agent currently used.
Example 6 (test example)
The polishing agent and the common chemical-mechanical polishing agent are respectively adopted, vibroMet 2 vibration polishing machines are used for carrying out chemical-mechanical polishing on pure copper, and SEM detection is carried out on the polished material, and the results are shown in a figure 4 and a figure 5.
As can be seen from the detection results, compared with the common chemical-mechanical polishing agent, the polishing agent of the invention has no scratch and oxide layer on the surface of the material after being polished, and the polishing quality is obviously superior to that of the common chemical-mechanical polishing agent used at present.
Claims (9)
1. The preparation method of the special metallographic polishing agent for the easily oxidized metal is characterized in that the metallographic polishing agent comprises nano cerium oxide or lanthanum oxide abrasive particles, a dispersing agent, a pH regulator and an alcohol group or oil-based/alcohol-based mixed liquid; wherein, the dispersant is 0.1 to 1.5 percent, the PH regulator is 0.1 to 1.0 percent, the abrasive particles are 5 to 20 percent, and the balance is alcohol group or oil-based alcohol group mixed liquid;
the preparation method comprises the following steps:
(1) Preparing abrasive particles:
adding Ce 4+ Salt or La 3+ Mixing a salt with a polyvinylpyrrolidone solution or a hydrochloric acid solution to prepare a cerium salt or lanthanum salt solution, adding a precipitator, standing and aging at a certain temperature until precipitates are generated, cleaning the precipitates with deionized water or ethanol, then drying in vacuum to obtain a cerium oxide precursor or a lanthanum oxide precursor, and roasting the cerium oxide precursor or the lanthanum oxide precursor to generate cerium oxide or lanthanum oxide abrasive particles with certain crystallinity;
(2) Preparing a polishing agent:
grinding the cerium oxide or lanthanum oxide abrasive particles into nano cerium oxide or lanthanum oxide particles by a ball mill; adding a dispersing agent, a pH regulator and an alcohol group or an oil-based/alcohol-based mixed liquid, performing high-shear dispersion in a high-speed cutting dispersion machine, and uniformly mixing to obtain the special metallographic polishing agent for the easily-oxidized metal.
2. The preparation method of the easy-to-oxidize metal dedicated metallographic polishing agent according to claim 1, wherein the oil base is glycerol or silicone oil, and the alcohol base is ethanol or methanol; the oil-based/alcohol-based mixed liquid comprises the following components in percentage by weight of 1.
3. The method for preparing the special metallographic polishing agent for the easily-oxidizable metal according to claim 1, wherein the dispersing agent is polyvinylpyrrolidone, sodium polyacrylate or magnesium aluminum silicate.
4. The method for preparing the special metallographic polishing agent for the easily-oxidizable metal according to claim 1, wherein the pH regulator is ethanolamine, sodium hydroxide or sodium methoxide.
5. The preparation method of the special metallographic polishing agent for the easily-oxidized metal according to claim 1, wherein the method is characterized in that a planetary ball mill is adopted to perform ball milling on the abrasive particles for 1-3 hours, 3-5 hours and 5-10 hours; respectively obtaining polishing agent abrasive particles with the particle sizes of 0.06 mu m, 0.05 mu m and 0.02 mu m; the nano cerium oxide particles with different particle sizes can be independently used as polishing agent abrasive particles, and the cerium oxide particles with different particle sizes can be mixed to be used as the polishing agent abrasive particles; 0.02 μm and 0.05 μm/0.06 μm of particle size cerium oxide were mixed in accordance with 2.
6. The method for preparing the special metallographic polishing agent for the oxidizable metal according to claim 1, wherein the temperature of the aging is 50 ℃ to 100 ℃ during standing.
7. The method for preparing the special metallographic polishing agent for the easily-oxidizable metal according to claim 1, wherein the roasting temperature of the cerium oxide particles with a certain degree of crystallinity is 800 ℃ to 950 ℃.
8. The method for preparing the special metallographic polishing agent for the easily-oxidizable metal according to claim 1, wherein the metallographic polishing agent has a weak alkalinity with a pH value of 9-10.
9. The method for preparing the special metallographic polishing agent for the easily-oxidizable metal according to claim 1, wherein the precipitating agent is sodium carbonate, ammonium bicarbonate or oxalic acid.
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