CN109030148A - 一种铁基合金粉末ebsd检测试样的制备方法 - Google Patents
一种铁基合金粉末ebsd检测试样的制备方法 Download PDFInfo
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- CN109030148A CN109030148A CN201810846725.0A CN201810846725A CN109030148A CN 109030148 A CN109030148 A CN 109030148A CN 201810846725 A CN201810846725 A CN 201810846725A CN 109030148 A CN109030148 A CN 109030148A
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- Prior art keywords
- powder
- iron
- base powder
- preparation
- detection sample
- Prior art date
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- 239000000843 powder Substances 0.000 title claims abstract description 182
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 159
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 80
- 238000001887 electron backscatter diffraction Methods 0.000 title claims abstract description 73
- 238000001514 detection method Methods 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 46
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 62
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000000243 solution Substances 0.000 claims abstract description 47
- 239000000126 substance Substances 0.000 claims abstract description 39
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 36
- 239000000956 alloy Substances 0.000 claims abstract description 36
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 31
- 238000012545 processing Methods 0.000 claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 25
- 230000004913 activation Effects 0.000 claims abstract description 14
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000010792 warming Methods 0.000 claims abstract description 8
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 40
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 24
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 20
- 229960000583 acetic acid Drugs 0.000 claims description 17
- 239000010949 copper Substances 0.000 claims description 16
- 235000011187 glycerol Nutrition 0.000 claims description 16
- 229910052802 copper Inorganic materials 0.000 claims description 15
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 14
- 238000005551 mechanical alloying Methods 0.000 claims description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 11
- 239000012362 glacial acetic acid Substances 0.000 claims description 11
- 238000005498 polishing Methods 0.000 claims description 11
- 239000003792 electrolyte Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 7
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 7
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 7
- 150000001298 alcohols Chemical class 0.000 claims description 7
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 7
- 239000001632 sodium acetate Substances 0.000 claims description 7
- 235000017281 sodium acetate Nutrition 0.000 claims description 7
- 239000001509 sodium citrate Substances 0.000 claims description 7
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 7
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 7
- 239000001384 succinic acid Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 241000254173 Coleoptera Species 0.000 claims description 2
- 238000012387 aerosolization Methods 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 238000000498 ball milling Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 230000001476 alcoholic effect Effects 0.000 claims 1
- 238000003801 milling Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- 238000012512 characterization method Methods 0.000 abstract description 2
- 238000007747 plating Methods 0.000 description 34
- 238000004140 cleaning Methods 0.000 description 15
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 7
- 229910010271 silicon carbide Inorganic materials 0.000 description 7
- 238000002604 ultrasonography Methods 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 229910052804 chromium Inorganic materials 0.000 description 4
- 239000011651 chromium Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 229910052745 lead Inorganic materials 0.000 description 3
- 229910052718 tin Inorganic materials 0.000 description 3
- 102000004160 Phosphoric Monoester Hydrolases Human genes 0.000 description 2
- 108090000608 Phosphoric Monoester Hydrolases Proteins 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000320 mechanical mixture Substances 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- LCDFWRDNEPDQBV-UHFFFAOYSA-N formaldehyde;phenol;urea Chemical compound O=C.NC(N)=O.OC1=CC=CC=C1 LCDFWRDNEPDQBV-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 210000001161 mammalian embryo Anatomy 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000012913 prioritisation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
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- 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
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C18/1635—Composition of the substrate
- C23C18/1637—Composition of the substrate metallic substrate
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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- C23C18/1646—Characteristics of the product obtained
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C18/168—Control of temperature, e.g. temperature of bath, substrate
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
- C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
-
- 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
- C23F17/00—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
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
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- C25F3/02—Etching
- C25F3/06—Etching of iron or steel
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/22—Polishing of heavy metals
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- G01N1/36—Embedding or analogous mounting of samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/203—Measuring back scattering
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
- C25F1/02—Pickling; Descaling
- C25F1/04—Pickling; Descaling in solution
- C25F1/06—Iron or steel
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- G—PHYSICS
- G01—MEASURING; TESTING
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- 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
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- G—PHYSICS
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- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/053—Investigating materials by wave or particle radiation by diffraction, scatter or reflection back scatter
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pathology (AREA)
- General Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
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Abstract
本发明涉及一种铁基合金粉末EBSD检测试样的制备方法,属于材料表征技术领域。所述制备方法包括下述步骤:在电解液中对铁基合金粉末进行电解活化处理;然后用无水乙醇和/或无水甲醇溶液超声清洗,干燥,得到备用粉末;将备用粉末加入到化学包埋溶液中超声分散;超声分散后,进行A处理;然后再升温至80~92℃,反应,得到包覆有镍的铁基合金块体。所述A处理为:以静置、搅拌,再静置为一个周期;实施至少一个周期的操作,即完成A处理。对所得包覆有镍的铁基合金块体进行打磨、电解抛光,得到所述铁基合金粉末EBSD检测试样。本发明首次实现了对铁基合金粉末EBSD检测试样的制备。
Description
技术领域
本发明涉及一种铁基合金粉末EBSD检测试样的制备方法,属于特种材料表征技术领域。
背景技术
电子背散射衍射(Elecrton Backscatter Diffraction,简称EBSD)技术是基于扫描电镜中电子束在倾斜样品表面激发出并形成的衍射菊池带的分析从而确定晶体结构、取向及相关信息的方法。
氧化物弥散强化合金粉末是制备高性能氧化物弥散强化合金的原料,其显微组织形貌、结构与取向分布、成分分布是决定合金性能的关键。制备高质量合金粉末(包括铁磁性合金粉末)EBSD检测试样是获得合金粉末显微组织形貌、结构与取向分布的关键。目前绝大部分EBSD研究工作主要涉及块体材料和薄膜材料,而关于粉体(≤150μm)材料的EBSD研究分析未见报道,这主要由于粉体材料的EBSD试样制备困难。
EBSD检测对检测试样的要求有:(1)样品观察面与载物台之间要有有效的导电连接;(2)样品观察面要求光亮平整;(3)样品观察面至样品内部1~5μm深度范围内无残余应力。
目前,制备粉体EBSD检测试样的方法主要采用树脂(酚醛树脂或导电树脂)镶嵌粉末,对镶嵌后粉末进行打磨、机械抛光、振动抛光,得到EBSD检测试样。其中,采用不导电酚醛树脂镶嵌粉末经振动抛光后需要对样品表面进行镀碳膜处理,为了保证在EBSD检测时有清晰的菊池线条带信号,样品表面所镀碳膜厚度要求小于5nm,而普通镀碳设备无法满足该条件。
中国专利CN107228870A公开了一种硬质合金(WC)粉末EBSD制样方法,将硬质合金粉末和电解Cu粉按一定比例混合,压胚,烧结,得到烧结试样;对烧结试样进行镶嵌、研磨和抛光、表面清洁,得到EBSD试样。该方法预先将硬质合金粉末与铜粉混合、预烧结,该过程会改变粉末原始显微组织,仅适用于高熔点难熔金属及合金;EBSD分析通常要求保持粉末原始显微组织状态,特别是机械合金化粉末/球磨粉末,因此无法采用上述方法制备EBSD试样。
针对以上问题,本发明首次提出了一种采用化学镀镍包埋铁基粉末再进行磨抛、电解抛光的方法,适用于雾化合金粉末和机械合金化粉末的EBSD检测试样的制备。本发明一种铁基合金粉末EBSD检测试样的制备方法,解决了粉末EBSD检测时样品导电性的问题;解决了粉末EBSD检测样品制备过程中抛光困难的问题,高效解决粉末EBSD检测样品表面残余应力的问题;填补了合金粉末EBSD检测试样制备方法的空缺。目前,国内外未见相关研究成果的公开报道。
发明内容
本发明提供了一种铁基合金粉末EBSD检测试样的制备方法。
本发明在开发过程中遇到的关键技术问题有:
(1)铁基合金粉末的镶嵌体系设计
本发明在开发过程中,针对铁基合金粉末设计了多种镶嵌方案,包括物理粘接:树脂冷镶/热镶,电木粉温热镶,快干胶冷粘接,Pb、Sn等低熔点金属熔融粘接;机械混合压制:采用Pb、Sn、Cu、Al等金属粉末混合压制。化学粘接:采用化学元素,包括Fe、Cr、Cu、Al、Ni等化学包埋。
所述的物理粘接,或无法形成有效的界面粘接,导致粉末脱落;或因加热,改变了粉末的状态;或不导电,无法进行有效的表征。
所述的机械混合压制,采用Pb、Sn、Cu等易变形金属粉末混合压制,一方面使铁基合金粉末变形,另一方面粉末之间界面结合强度低,导致粉末脱落,无法完成样品制备。
所述的化学粘接,采用Fe、Cr、Cu、Al、Ni等化学包埋;其中,采用Fe、Cr、Cu、Al等化学镀包埋,一方面难以在铁基粉末表面形成有效沉积,包埋效果差,无法进行电解抛光;采用电镀的方法在铁基粉末表面镀Fe、Cr、Cu、Al,当镀层达到1μm时就发生镀层脱落现象,难以制备符合要求的样品。
针对上述问题,设计了电镀、化学镀等多种工艺方案,以及多种溶液体系,并实施综合实验,最终设计了本发明技术方案,采用Ni进行化学镀包覆。
(2)粉末表面活化
在开发过程中,出现包埋不致密和镀层脱落的现象,最终在化学镀之前对粉末作表面活化预处理,使得粉末表面能和镀层发生紧密的化学结合。
(3)化学镀温度的控制
在开发过程中发现不同温度条件下镀层生成的速度有很大差异,温度过低反应速度过慢,无法产生有效镀层;温度过高反应速度快,会出现镍在溶液中自形核长大,而无法在粉末表面生长。
(4)化学镀时粉末的铺设
在开发过程中发现粉末铺设密度对最终包埋致密度有重大影响,因此要求在包埋前将粉末铺设厚度均匀。
本发明在解决上述问题的过程中逐渐形成本发明的方案以及优化方案。
本发明一种铁基合金粉末EBSD检测试样的制备方法,包括下述步骤:
步骤一
在电解液中,对铁基合金粉末进行电解活化处理;电解活化处理后用无水醇和/或无水甲醇溶液超声清洗,干燥,得到备用粉末;
步骤二
将备用粉末加入到化学包埋溶液中,超声分散;超声分散后,进行A处理;然后再升温至80~92℃、优选88~92℃,反应,得到包覆有镍的铁基合金块;所述A处理为:以静置、搅拌,再静置为一个周期;实施至少一个周期的操作,即完成A处理;所述化学包埋溶液包括下述组分:
氯化镍28-32g/L、优选为30g/L;
次亚磷酸钠15-30g/L;
醋酸钠14-16g/L、优选为15g/L;
柠檬酸钠14-16g/L、优选为15g/L;
丁二酸4-6g/L、优选为5g/L;
氨基乙酸5-15g/L;
丙三醇1-3vol.%;
冰醋酸1-3vol.%、优选为2vol.%;
所述包埋溶液的pH值为3.5~5.4、优选为4.0~5.4;
步骤三
对步骤二所得包覆有镍的铁基合金块进行打磨、电解抛光,得到所述铁基合金粉末EBSD检测试样。
本发明一种铁基合金粉末EBSD检测试样的制备方法,所述铁基合金粉末为气雾化Fe基合金粉末,或机械合金化铁基合金粉末,或经球磨处理的铁基合金粉末。
本发明一种铁基合金粉末EBSD检测试样的制备方法,所述铁基合金粉末的粒度小于等于150μm。
本发明一种铁基合金粉末EBSD检测试样的制备方法,在工业上应用时,步骤一中所述电解活化处理为:将铁基合金粉末装入勺形铜容器电极中,进行电解活化粉末表面,活化后粉末利用无水乙醇和超声波清洗仪清洗并干燥待后续使用。在本发明中,经步骤一处理后,可以实现Ni的化学镀。
本发明一种铁基合金粉末EBSD检测试样的制备方法,步骤一中所述电解液由下述组分构成:高氯酸0.5~1wt%、丙三醇0.05~0.15wt%,余量为无水乙醇或无水甲醇。
本发明一种铁基合金粉末EBSD检测试样的制备方法,步骤一中:电解活化的时间为30-60s、温度为25-30℃。
本发明一种铁基合金粉末EBSD检测试样的制备方法,步骤一中:超声清洗时间为10~15min,其中更换2~3次无水乙醇和/或无水甲醇。
本发明一种铁基合金粉末EBSD检测试样的制备方法,步骤二中:按固液质量比1-3:500,将备用粉末加入到化学包埋溶液中。
本发明一种铁基合金粉末EBSD检测试样的制备方法,步骤二中:所述超声分散时间为10~15min
本发明一种铁基合金粉末EBSD检测试样的制备方法,步骤二中:单次静置的时间为30-60min;搅拌速度为100-120r/min,单次搅拌时间为3-5min;单次再静置的时间为30-60min。通过A处理,实现了粉末在化学镀容器底部的均匀沉积。上述工作为后续升温镀镍得到块体提供了必要条件。
本发明一种铁基合金粉末EBSD检测试样的制备方法,步骤二中:进行A处理后,升温至80~92℃、优选88~92℃,反应2-3.5小时;反应时控制镍的生长速度30~50μm/h。在工业上应用时,当化学包埋溶液成分确定后,通过严格控制温度来控制镍的生长速度。在本发明探索过程中,发现镍太快生成或太慢生成均不利于得到致密的块体,导致无法制备符合要求的EBSD检测样品。
本发明一种铁基合金粉末EBSD检测试样的制备方法,包埋完成后合金块体的尺寸调整成10×10mm,厚度50~200μm。
本发明一种铁基合金粉末EBSD检测试样的制备方法,包覆有镍的铁基合金块利用400~2000目水磨砂纸进行打磨平整,最后采用2000~3000目SiC金相砂纸打磨光亮,样品表面无明显划痕。
本发明一种铁基合金粉末EBSD检测试样的制备方法,步骤三中所述电解抛光溶液为:高氯酸3~10wt%、冰醋酸1~2wt%、磷酸0.5~1wt%、丙三醇1~2wt%,余量为无水甲醇和/或无水乙醇。
本发明一种铁基合金粉末EBSD检测试样的制备方法,所述电解抛光过程以不锈钢板作阴极,尺寸为5×3cm,以待电解抛光的合金试样块为阳极,样品夹具为纯铜,抛光面正对阴极板,恒电压电解,电压3~6V,室温条件电解10~30s,获得用于EBSD检测的粉末试样。
本发明的优点和积极效果:
(1)本发明一种铁基合金粉末EBSD检测试样的制备方法,首次提出利用化学镀镍的方法包埋铁基金属粉末,并利用电解抛光工艺制备铁基粉末EBSD检测试样,解决了无法制备粉末(尤其是铁基金属粉末)EBSD检测样品的问题。
(2)本发明一种铁基合金粉末EBSD检测试样的制备方法,利用电解抛光工艺制备铁基粉末EBSD检测试样,适用于雾化铁基粉末和机械合金化粉末,该工艺能获得平整光亮的样品待测表面,并完全消除粉末EBSD检测样品待测面存在的残余应力,为EBSD检测提供良好的试样。
(3)本发明一种铁基合金粉末EBSD检测试样的制备方法,利用电解法对粉末预先进行表面活化,解决了化学包埋时,包埋金属与粉末表面结合问题。
(4)本发明一种铁基合金粉末EBSD检测试样的制备方法,通过严格控制化学镀镍工艺及沉降方式,得到了结合紧密的致密块体材料,将粉末无损块体化,解决了粉末无法进行电解抛光的问题。
(5)本发明一种铁基合金粉末EBSD检测试样的制备方法,通过严格控制沉降方式、反应温度及包埋反应溶液含量,能有效调控包埋速率,可获得粉末包埋厚度可控的块体材料。
(6)本发明一种铁基合金粉末EBSD检测试样的制备方法,通过选用镍对铁基粉末进行包埋,在电解抛光过程中能对包埋粉末进行有效抛光。
附图说明
图1为本发明实施例1所制备的铁基粉末化学镀镍包埋样品经打磨后试样的OM图像。
图2为本发明实施例1所制备的铁基粉末化学镀镍包埋样品经电解抛光后粉末表面的SEM图像。
图3为本发明实施例1粉末的EBSD图像。
从图1中能看出铁粉被包埋致密,其中打磨光亮的部分不存在空隙,该区域在后续检测中作为主要观察面。
从图2中能看出粉末经电解抛光后,其球磨粉末的层状结构被凸显。
图3为粉末经EBSD检测获得的IPF图像,不同色彩代表粉末晶粒不同取向,其中大尺寸晶粒为本发明所用铁基材料,而细小晶粒区域为包埋镍材料,从IPF图中我们可以获得粉末晶粒尺寸分布和晶粒取向分布。
具体实施方式
实施例1:
首先,称取Fe-14Cr-3W-0.4Ti-0.5Y2O3机械合金化粉末2g,在无水乙醇中利用超声波清洗仪清洗10min,期间更换2次无水乙醇,将清洗完毕的粉末过滤后干燥。然后进行以下操作:
步骤一:将清洗、干燥的粉末装入勺形铜电极中,浸没在活化电解液中,进行电解活化处理,所用活化电解液为:高氯酸0.5%、丙三醇0.1%,余量为无水甲醇,活化30s。电解活化处理后用无水醇和/或无水甲醇溶液超声清洗10min,过滤,干燥,得到备用粉末;
步骤二:将备用粉末加入到化学镀镍溶液中,超声分散10min,所用化学镀镍溶液为:氯化镍30g、次亚磷酸钠15g、醋酸钠15g、柠檬酸钠15g、丁二酸5g、氨基乙酸5g、丙三醇10ml、冰醋酸20ml、蒸馏水970ml,溶液pH=4.0。超声分散后,进行A处理,所用A处理为:超声分散10min,随后静置0.5h,再以100转/min的搅拌速率搅拌3min;然后再静置0.5h。然后将完成A处理后的含有铁基合金粉末的化学镀镍溶液升温至85±5℃;反应2h后获得包覆有镍的铁基合金块,调整金块体尺寸为10×10mm,厚度115μm。
步骤三:对步骤二所得包覆有镍的铁基合金块利用400~2000目水磨砂纸将样品打磨平整,再利用2000目SiC金相砂纸将样品打磨光亮。然后将合金块体浸没在电解液中进行电解抛光,得到Fe-14Cr-3W-0.4Ti-0.5Y2O3机械合金化粉末EBSD检测试样。该步骤所用电解抛光溶液为:高氯酸6ml、冰醋酸2ml、磷酸1ml、丙三醇2ml,无水甲醇89ml;该步骤电解抛光采用合金试样块为阳极,不锈钢板作阴极(尺寸为5×3cm),样品夹具为纯铜,抛光面正对阴极板,恒电压电解,电压3V,室温条件电解15s。
附图1为本实施例所制备的铁基粉末化学镀镍包埋样品经打磨后试样的OM图像。
附图2为本实施例所制备的铁基粉末化学镀镍包埋样品经电解抛光后粉末表面的SEM图像。其中出现花纹状凸起为球磨粉末由多个粉末冷焊造成的。
附图3为本实施例粉末的EBSD图像。
实施例2:
首先,称取Fe-14Cr-3W-0.4Ti-1Y2O3机械合金化粉末2g,在无水乙醇中利用超声波清洗仪清洗10min,期间更换2次无水乙醇,将清洗完毕的粉末过滤后干燥。然后进行以下操作:
步骤一:将清洗、干燥的粉末装入勺形铜电极中,浸没在活化电解液中,进行电解活化处理,所用活化电解液为:高氯酸1%、丙三醇0.1%,余量为无水甲醇,活化60s。电解活化处理后用无水醇和/或无水甲醇溶液超声清洗10min,过滤,干燥,得到备用粉末;
步骤二:将备用粉末加入到化学镀镍溶液中,超声分散10min,所用化学镀镍溶液为:氯化镍28g、次亚磷酸钠15g、醋酸钠14g、柠檬酸钠14g、丁二酸4g、氨基乙酸4g、丙三醇10ml、冰醋酸20ml、蒸馏水970ml,溶液pH=5.4。超声分散后,进行A处理,所用A处理为:超声分散10min,随后静置0.5h,再以100转/min的搅拌速率搅拌3min;然后再静置0.5h。然后将完成A处理后的含有铁基合金粉末的化学镀镍溶液升温至85±5℃;反应1h后获得包覆有镍的铁基合金块,调整金块体尺寸为10×10mm,厚度45μm。
步骤三:对步骤二所得包覆有镍的铁基合金块利用400~2000目水磨砂纸将样品打磨平整,再利用2000目SiC金相砂纸将样品打磨光亮。然后将合金块体浸没在电解液中进行电解抛光,得到Fe-14Cr-3W-0.4Ti-1Y2O3机械合金化粉末EBSD检测试样。该步骤所用电解抛光溶液为:高氯酸6ml、冰醋酸2ml、磷酸1ml、丙三醇2ml,无水甲醇89ml;该步骤电解抛光采用合金试样块为阳极,不锈钢板作阴极(尺寸为5×3cm),样品夹具为纯铜,抛光面正对阴极板,恒电压电解,电压6V,室温条件电解20s。
对比例1:
首先,称取Fe-14Cr-3W-0.4Ti-0.25Y2O3机械合金化粉末2g,在无水乙醇中利用超声波清洗仪清洗10min,期间更换2次无水乙醇,将清洗完毕的粉末过滤后干燥。然后进行以下操作:
步骤一:将备用粉末加入到化学镀镍溶液中,超声分散10min,所用化学镀镍溶液为:氯化镍30g、次亚磷酸钠15g、醋酸钠15g、柠檬酸钠15g、丁二酸5g、氨基乙酸5g、丙三醇10ml、冰醋酸20ml、蒸馏水970ml,溶液pH=4.0。超声分散后,进行A处理,所用A处理为:超声分散10min,随后静置0.5h,再以100转/min的搅拌速率搅拌3min;然后再静置0.5h。然后将完成A处理后的含有铁基合金粉末的化学镀镍溶液升温至85±5℃;反应2h。
由于没有对粉末进行活化处理,在包埋过程中粉末无法结块,反应2h后仍是松散粉末,包埋失败。
对比例2:
首先,称取Fe-14Cr-3W-0.4Ti-1Y2O3机械合金化粉末2g,在无水乙醇中利用超声波清洗仪清洗10min,期间更换2次无水乙醇,将清洗完毕的粉末过滤后干燥。然后进行以下操作:
步骤一:将清洗、干燥的粉末装入勺形铜电极中,浸没在活化电解液中,进行电解活化处理,所用活化电解液为:高氯酸0.5%、丙三醇0.1%,余量为无水甲醇,活化30s。电解活化处理后用无水醇和/或无水甲醇溶液超声清洗10min,过滤,干燥,得到备用粉末;
步骤二:将备用粉末加入到化学镀镍溶液中,超声分散10min,随后静置0.5h。所用化学镀镍溶液为:氯化镍30g、次亚磷酸钠15g、醋酸钠15g、柠檬酸钠15g、丁二酸5g、氨基乙酸5g、丙三醇10ml、冰醋酸20ml、蒸馏水970ml,溶液pH=4.0。将含有铁基合金粉末的化学镀镍溶液升温至85±5℃;反应4h。
由于没有对含有铁基合金粉末的化学镀镍溶液进行多道次搅拌、静置,所得粉末铺设不均匀,即使反应4h也没有形成致密包埋金属块,包埋失败。
对比例3:
首先,称取Fe-14Cr-3W-0.4Ti-0.5Y2O3机械合金化粉末2g,在无水乙醇中利用超声波清洗仪清洗10min,期间更换2次无水乙醇,将清洗完毕的粉末过滤后干燥。然后进行以下操作:
步骤一:将清洗、干燥的粉末装入勺形铜电极中,浸没在活化电解液中,进行电解活化处理,所用活化电解液为:高氯酸0.5%、丙三醇0.1%,余量为无水甲醇,活化30s。电解活化处理后用无水醇和/或无水甲醇溶液超声清洗10min,过滤,干燥,得到备用粉末;
步骤二:将备用粉末加入到化学镀镍溶液中,超声分散10min,所用化学镀镍溶液为:氯化镍30g、次亚磷酸钠15g、醋酸钠15g、柠檬酸钠15g、丁二酸5g、氨基乙酸5g、丙三醇10ml、冰醋酸20ml、蒸馏水970ml,溶液pH=4.0。超声分散后,进行A处理,所用A处理为:超声分散10min,随后静置0.5h,再以100转/min的搅拌速率搅拌3min;然后再静置0.5h。然后将完成A处理后的含有铁基合金粉末的化学镀镍溶液升温至95±5℃;反应2h后获得包覆有镍的铁基合金块,调整金块体尺寸为10×10mm,厚度132μm。
步骤三:对步骤二所得包覆有镍的铁基合金块利用400~2000目水磨砂纸将样品打磨平整,在打磨过程中样品破碎。
由于包埋温度过高,粉末样品表面镀层松散,粉末之间有大量孔隙,在打磨过程中粉末均从包埋基体上脱落,最终导致样品破碎。
Claims (10)
1.一种铁基合金粉末EBSD检测试样的制备方法,其特征在于:包括下述步骤:
步骤一
在电解液中,对铁基合金粉末进行电解活化处理;电解活化处理后用无水乙醇和/或无水甲醇溶液超声清洗,干燥,得到备用粉末;
步骤二
将备用粉末加入到化学包埋溶液中,超声分散;超声分散后,进行A处理;然后再升温至80~92℃,反应,得到包覆有镍的铁基合金块;所述A处理为:以静置、搅拌,再静置为一个周期;实施至少一个周期的操作,即完成A处理;所述化学包埋溶液包括下述组分:
氯化镍 28-32g/L;
次亚磷酸钠 15-30g/L;
醋酸钠 14-16g/L;
柠檬酸钠 14-16g/L;
丁二酸 4-6g/L;
氨基乙酸 5-15g/L;
丙三醇 1-3vol.%;
冰醋酸 1-3vol.%;
所述包埋溶液的pH值为3.5~5.4;
步骤三
对步骤二所得包覆有镍的铁基合金块进行打磨、电解抛光,得到所述铁基合金粉末EBSD检测试样。
2.根据权利要求1所述的一种铁基合金粉末EBSD检测试样的制备方法,其特征在于:所述铁基合金粉末为气雾化Fe基合金粉末,或机械合金化铁基合金粉末,或经球磨处理的铁基合金粉末。
3.根据权利要求1所述的一种铁基合金粉末EBSD检测试样的制备方法,其特征在于:所述铁基合金粉末的粒度小于等于150μm。
4.根据权利要求1所述的一种铁基合金粉末EBSD检测试样的制备方法,其特征在于:
步骤一中所述电解活化处理为:将铁基合金粉末装入勺形铜容器电极中,进行电解活化粉末表面,活化后粉末利用无水乙醇和超声波清洗仪清洗并干燥待后续使用;
步骤一中所述电解液由下述组分构成:高氯酸0.5~1wt%、丙三醇0.05~0.15wt%,余量为无水乙醇或无水甲醇;
步骤一中,电解活化的时间为30-60s、温度为25-30℃;
步骤一中,超声清洗时间为10~15min,其中更换2~3次无水乙醇和/或无水甲醇。
5.根据权利要求1所述的一种铁基合金粉末EBSD检测试样的制备方法,其特征在于:
步骤二中:按固液质量比1-3:500;将备用粉末加入到化学包埋溶液中;
步骤二中:所述超声分散时间为10~15min。
6.根据权利要求1所述的一种铁基合金粉末EBSD检测试样的制备方法,其特征在于:步骤二中,单次静置的时间为30-60min;搅拌时,搅拌速度为100-120r/min单次搅拌时间为3-5min;单次再静置的时间为30-60min。
7.根据权利要求1所述的一种铁基合金粉末EBSD检测试样的制备方法,其特征在于:步骤二中,进行A处理后,升温至88~92℃,反应2-3.5小时;反应时控制镍的生长速度30~50μm/h。
8.根据权利要求1所述的一种铁基合金粉末EBSD检测试样的制备方法,其特征在于:包埋完成后合金块体的尺寸调整成10×10mm,厚度50~200μm;然后利用400~2000目水磨砂纸进行打磨平整,最后采用2000~3000目SiC金相砂纸打磨光亮,样品表面无明显划痕。
9.根据权利要求1所述的一种铁基合金粉末EBSD检测试样的制备方法,其特征在于:步骤三中,所述电解抛光溶液为:高氯酸3~10wt%、冰醋酸1~2wt%、磷酸0.5~1wt%、丙三醇1~2wt%,余量为无水甲醇和/或无水乙醇。
10.根据权利要求1所述的一种铁基合金粉末EBSD检测试样的制备方法,其特征在于:步骤三中,所述电解抛光过程以不锈钢板作阴极,尺寸为5×3cm,以待电解抛光的合金试样块为阳极,样品夹具为纯铜,抛光面正对阴极板,恒电压电解,电压3~6V,室温条件电解10~30s,获得所述的粉末EBSD检测试样。
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