CN102866047A - Method for preparing metallographic display sample made of Ti-Al laminated composite material - Google Patents
Method for preparing metallographic display sample made of Ti-Al laminated composite material Download PDFInfo
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- CN102866047A CN102866047A CN2012103683769A CN201210368376A CN102866047A CN 102866047 A CN102866047 A CN 102866047A CN 2012103683769 A CN2012103683769 A CN 2012103683769A CN 201210368376 A CN201210368376 A CN 201210368376A CN 102866047 A CN102866047 A CN 102866047A
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- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 229910004349 Ti-Al Inorganic materials 0.000 title claims abstract description 35
- 229910004692 Ti—Al Inorganic materials 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title abstract description 14
- 238000005498 polishing Methods 0.000 claims abstract description 44
- 239000004744 fabric Substances 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000005520 cutting process Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 238000002360 preparation method Methods 0.000 claims description 16
- 239000002826 coolant Substances 0.000 claims description 15
- 239000000314 lubricant Substances 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 229920000742 Cotton Polymers 0.000 claims description 10
- 235000013312 flour Nutrition 0.000 claims description 10
- 238000003801 milling Methods 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000000356 contaminant Substances 0.000 claims description 5
- 238000007598 dipping method Methods 0.000 claims description 5
- 239000003292 glue Substances 0.000 claims description 5
- 230000008520 organization Effects 0.000 claims description 5
- 230000002269 spontaneous effect Effects 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 4
- -1 polytetrafluoroethylene Polymers 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000013618 particulate matter Substances 0.000 abstract 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract 1
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 11
- 239000010936 titanium Substances 0.000 description 11
- 229910052719 titanium Inorganic materials 0.000 description 11
- 239000008399 tap water Substances 0.000 description 10
- 235000020679 tap water Nutrition 0.000 description 10
- 229910001069 Ti alloy Inorganic materials 0.000 description 5
- 239000004411 aluminium Substances 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910000838 Al alloy Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 239000004836 Glue Stick Substances 0.000 description 1
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 1
- 241000720974 Protium Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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Abstract
The invention provides a method for preparing a metallographic display sample made of a Ti-Al laminated composite material. The method comprises the following steps of: capturing and treating the sample, bonding a polytetrafluoroethylene material to the surface of the treated Ti-Al laminated composite material through an adhesive, gradually grinding a surface for displaying a tissue from thick to thin, performing rough polishing by polishing cloth, then performing fine polishing, treating by corrosion solutions, and drying to obtain the metallographic display sample made of the Ti-Al laminated composite material. According to the method, working procedures of capturing the test sample through an organic mechanical linear cutting method, grinding the test sample for many times, performing metallographic polishing and the like are combined; two corrosion solutions are adopted; the shortcomings of hard particle pollution and surface scratches which are caused by the conventional polishing paste are overcome; the prepared test sample can be suitable to metallographic observation and scanning electron microscope tissue observation; the method is simple; a microscopic tissue of a combined interface of the Ti-Al laminated composite material can be effectively displayed; and the sample is high in definition.
Description
Technical field
The invention belongs to technical field of metallographic sample preparation, be specifically related to a kind of preparation method of the metallographic show sample for the larger Ti-Al laminar composite of matrix mechanical property difference.
Background technology
Relatively many other non-ferrous metals, titanium (or titanium alloy), aluminium (or aluminium alloy) are larger metal (alloy) materials of mechanical property difference such as intensity, hardness, wearing quality, bring very large difficulty for the preparation of sample metallographic sample preparation.
Incident subject matter when 1, tradition prepares the titanium or titanium alloy sample:
(1) metallographic sample preparation of titanium or titanium alloy is more difficult than steel, and its polishing and polishing efficiency are very low;
(2) excessively violent cutting and polishing process all can α mutually in the generation deformation twin;
(3) it is more suitable to adopt cold method of inlaying to inlay than thermal pressure for the relatively high pure titanium of purity, because thermal pressure is inlaid with content and the distribution that may change protium in the pure titanium;
(4) especially for pure titanium, in the sample preparation process, want to remove cut and plastic flow is very difficult.
Incident subject matter when 2, tradition prepares aluminium and aluminum alloy specimen:
(1) darker by intercepting and grind the distortion that causes;
(2) at a lower temperature, will occur to reply and precipitation process such as 180 ~ 250 ℃, and in sample making course, be easy to be raised to such temperature;
(3) be difficult to eliminate polishing road trace and be easy to occur between Second Phase Particles embossment.
3, lightweight based on the relative titanium or titanium alloy of aluminium, conduct electricity, cost is low, and titanium or titanium alloy corrosion-resistant good complementarity in sulfate that non-ferrous metal electrodeposition extracts and chlorate medium solution, CN101319333A discloses a kind of titanium-coated aluminium laminated composite plate and preparation method thereof, comprise and adopt welding, founding, it is compound to explode, rolling, with one or more Ti-Al composite plates that preparation titanium coats aluminium fully or part coats in the heat pressing process, and has good conductivity, corrosion stability is good, low cost and other advantages, the alternative titanium inert anode plate that is used at present electrolysis, reduce the tank voltage 0.1～0.8V of inert anode, it is substrate that this stratiform composite anode has changed at elemental metals or multicomponent alloy, apply again the traditional structural design of coating, so that the internal resistance in the inert anode plate reduces, homogenising distribution of current, reduced thermal value, prolong the serviceable life of positive plate, and improved production efficiency and the energy efficient of electrolytic production.For further investigating its interfacial characteristics, also to overcome the metallurgical integrated technical barrier that afterwards interface topography is imposed protection and true visualize tissue.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of Ti-Al laminar composite metallographic show sample, easy to operate, but complete display ground shows the tissue of its combination interface.
The present invention realizes by following technical proposal: a kind of preparation method of Ti-Al laminar composite metallographic show sample, and following each step of process:
A, intercepting and processing sample: the Ti-Al laminar composite is cut into required size, cleaned sample surfaces 2～10 minutes with soaked in absolute ethyl alcohol again, then use the acetone wiping, until surface and oil contaminant is dispelled totally, wash down with distilled water again, in air, naturally dry, then with the transversal section filing, stick with glue agent polytetrafluoroethylmaterial material is bonded in Ti-Al laminar composite surface after the whole processing, place at last on the shiny surface in air spontaneous curing 6～8 hours;
B, grind: make lubricant and cooling medium with water, use successively the metallographic waterproof abrasive paper of 320#, 400#, 800#, 1000#, 1200#, 1500# and seven grades of 2000#, sample after steps A solidified from thick, to carefully progressively grinding the surface that needs display organization, after each grade grinds and finishes all with ultrasonic cleaning once;
C, rough polishing: for making lubricant and cooling medium, the sample after step B ground was with polishing cloth polishing 30～40 minutes with water;
D, fine polishing:, for making lubricant and cooling medium the sample after the step C rough polishing is polished under rotating speed 1000～1500r/min with new polishing cloth with water, every polishing 1～3 minute just dips HCl(1.19g/cm with absorbent cotton
3) 70～80mL+HNO
3The wiping 10～25 seconds on flour milling of the etchant of 20～30mL, and water washes down rapidly, dipping the HF(mass concentration with absorbent cotton again is 40%) 1～3mL+Fe (NO
3)
39H
2O 8～12g+H
2C
2O
430～40g+H
2The wiping 10～15 seconds on flour milling of the etchant of O 200mL, and water washes down rapidly; Polish altogether with this that water washes down after 45 minutes, dry up the metallographic show sample that namely obtains the Ti-Al laminar composite through cold wind again.
The cutting of described steps A is to cut with wire cut electric discharge machine.
The tackifier of described steps A is the by volume potpourri of 1 ︰ 1 of epoxy resin and hardening agent.
The HNO of described step D
3, Fe (NO
3)
39H
2O, H
2C
2O
4Be the pure or chemical pure of commercial analysis.
H in the etchant of described step D
2O is distilled water.
Compare with prior art and the invention has the advantages that: the present invention has taked the operation combinations such as mechanical wire cutting method intercepting sample, multiple tracks grind, metallurgical polishing, and preferred two kinds of etchants, solved the defective of hard particles pollution, scratch surface in traditional antiscuffing paste, the sample of preparing can supply metallographic observation and scanning electron microscope microstructure observation, its method is easy, and the microstructure that can effectively show Ti-Al laminar composite combination interface, the sample sharpness is high.
Description of drawings
Fig. 1 is the contour structures synoptic diagram of Ti-Al laminar composite;
Fig. 2 is the microstructure picture that the metallographic show sample of embodiment 1 gained Ti-Al laminar composite arrives at scanning electron microscopic observation;
Fig. 3 is the microstructure picture that the metallographic show sample of embodiment 2 gained Ti-Al laminar composites arrives at scanning electron microscopic observation;
The width in the somewhere, interface that observes when 5000 multiples amplify as seen in Figure 2 is about 2.24 μ m, and the interface is clear; The width in somewhere, interface is about 1 μ m when 10000 multiples amplify as seen in Figure 3, and the interface is clear.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Selecting technique is 500 ℃ of temperature, pressure 6MPa, the Ti-Al laminar composite for preparing under the heat-insulation pressure keeping time 1h condition
A, intercepting and processing sample: the Ti-Al laminar composite is cut into required size with wire cut electric discharge machine, cleaned sample surfaces 5 minutes with soaked in absolute ethyl alcohol again, then use the acetone wiping, until surface and oil contaminant is dispelled totally, wash down with distilled water again, in air, naturally dry, then with the transversal section filing, stick with glue agent polytetrafluoroethylmaterial material is bonded in Ti-Al laminar composite surface after the whole processing, place at last on the shiny surface in air spontaneous curing 7 hours; Wherein, tackifier is the by volume potpourri of 1 ︰ 1 of epoxy resin and hardening agent; The senior general double-tube glue stick that this routine tackifier adopts southwest, Jiangxi Province chemical industry company limited to produce;
B, grind: make lubricant and cooling medium with tap water, use successively the metallographic waterproof abrasive paper of 320#, 400#, 800#, 1000#, 1200#, 1500# and seven grades of 2000#, sample after steps A solidified from thick, to carefully progressively grinding the surface that needs display organization, after each grade grinds and finishes all with ultrasonic cleaning once;
C, rough polishing: for making lubricant and cooling medium, the sample after step B ground was with polishing cloth polishing 35 minutes with tap water;
D, fine polishing:, for making lubricant and cooling medium the sample after the step C rough polishing is polished under rotating speed 1350r/min with new polishing cloth with tap water, every polishing 2 minutes just dips HCl(1.19g/cm with absorbent cotton
3) 75mL+HNO
3The wiping 15 seconds on flour milling of the etchant of (analyzing pure) 25mL, and wash down with tap water rapidly, dipping the HF(mass concentration with absorbent cotton again is 40%) 2mL+Fe (NO
3)
39H
2O(analyzes pure) 10g+H
2C
2O
4(analyzing pure) 35g+H
2O(distilled water) etchant of 200mL wiping 10 seconds on flour milling, and wash down with tap water rapidly; Polish altogether with this that water washes down after 45 minutes, dry up the metallographic show sample that namely obtains the Ti-Al laminar composite through cold wind again.
Embodiment 2
A, intercepting and processing sample: the Ti-Al laminar composite is cut into required size with wire cut electric discharge machine, cleaned sample surfaces 10 minutes with soaked in absolute ethyl alcohol again, then use the acetone wiping, until surface and oil contaminant is dispelled totally, wash down with distilled water again, in air, naturally dry, then with the transversal section filing, stick with glue agent polytetrafluoroethylmaterial material is bonded in Ti-Al laminar composite surface after the whole processing, place at last on the shiny surface in air spontaneous curing 6 hours;
B, grind: make lubricant and cooling medium with water, use successively the metallographic waterproof abrasive paper of 320#, 400#, 800#, 1000#, 1200#, 1500# and seven grades of 2000#, sample after steps A solidified from thick, to carefully progressively grinding the surface that needs display organization, after each grade grinds and finishes all with ultrasonic cleaning once;
C, rough polishing: for making lubricant and cooling medium, the sample after step B ground was with polishing cloth polishing 30 minutes with water;
D, fine polishing:, for making lubricant and cooling medium the sample after the step C rough polishing is polished under rotating speed 1500r/min with new polishing cloth with water, every polishing 1 minute just dips HCl(1.19g/cm with absorbent cotton
3) 80mL+HNO
3The wiping 25 seconds on flour milling of the etchant of (chemical pure) 20mL, and water washes down rapidly, dipping the HF(mass concentration with absorbent cotton again is 40%) 1mL+Fe (NO
3)
39H
2The O(chemical pure) 8g+H
2C
2O
4(chemical pure) 30g+H
2The wiping 15 seconds on flour milling of the etchant of O 200mL, and water washes down rapidly; Polish altogether with this that water washes down after 45 minutes, dry up the metallographic show sample that namely obtains the Ti-Al laminar composite through cold wind again.
Embodiment 3
A, intercepting and processing sample: the Ti-Al laminar composite is cut into required size with wire cut electric discharge machine, cleaned sample surfaces 2 minutes with soaked in absolute ethyl alcohol again, then use the acetone wiping, until surface and oil contaminant is dispelled totally, wash down with distilled water again, in air, naturally dry, then with the transversal section filing, stick with glue agent polytetrafluoroethylmaterial material is bonded in Ti-Al laminar composite surface after the whole processing, place at last on the shiny surface in air spontaneous curing 8 hours; Wherein, tackifier is the by volume potpourri of 1 ︰ 1 of epoxy resin and hardening agent;
B, grind: make lubricant and cooling medium with tap water, use successively the metallographic waterproof abrasive paper of 320#, 400#, 800#, 1000#, 1200#, 1500# and seven grades of 2000#, sample after steps A solidified from thick, to carefully progressively grinding the surface that needs display organization, after each grade grinds and finishes all with ultrasonic cleaning once;
C, rough polishing: for making lubricant and cooling medium, the sample after step B ground was with polishing cloth polishing 40 minutes with tap water;
D, fine polishing:, for making lubricant and cooling medium the sample after the step C rough polishing is polished under rotating speed 1000r/min with new polishing cloth with tap water, every polishing 3 minutes just dips HCl(1.19g/cm with absorbent cotton
3) 70mL+HNO
3The wiping 10 seconds on flour milling of the etchant of (analyzing pure) 30mL, and wash down with tap water rapidly, dipping the HF(mass concentration with absorbent cotton again is 40%) 3mL+Fe (NO
3)
39H
2O(analyzes pure) 12g+H
2C
2O
4(analyzing pure) 40g+H
2O(distilled water) etchant of 200mL wiping 12 seconds on flour milling, and wash down with tap water rapidly; Polish altogether with this that water washes down after 45 minutes, dry up the metallographic show sample that namely obtains the Ti-Al laminar composite through cold wind again.
Claims (5)
1. the preparation method of a Ti-Al laminar composite metallographic show sample is characterized in that through following each step:
A, intercepting and processing sample: the Ti-Al laminar composite is cut into required size, cleaned sample surfaces 2～10 minutes with soaked in absolute ethyl alcohol again, then use the acetone wiping, until surface and oil contaminant is dispelled totally, wash down with distilled water again, in air, naturally dry, then with the transversal section filing, stick with glue agent polytetrafluoroethylmaterial material is bonded in Ti-Al laminar composite surface after the whole processing, place at last on the shiny surface in air spontaneous curing 6～8 hours;
B, grind: make lubricant and cooling medium with water, use successively the metallographic waterproof abrasive paper of 320#, 400#, 800#, 1000#, 1200#, 1500# and seven grades of 2000#, sample after steps A solidified from thick, to carefully progressively grinding the surface that needs display organization, after each grade grinds and finishes all with ultrasonic cleaning once;
C, rough polishing: for making lubricant and cooling medium, the sample after step B ground was with polishing cloth polishing 30～40 minutes with water;
D, fine polishing:, for making lubricant and cooling medium the sample after the step C rough polishing is polished under rotating speed 1000～1500r/min with new polishing cloth with water, every polishing 1～3 minute just dips HCl(1.19g/cm with absorbent cotton
3) 70～80mL+HNO
3The wiping 10～25 seconds on flour milling of the etchant of 20～30mL, and water washes down rapidly, dipping the HF(mass concentration with absorbent cotton again is 40%) 1～3mL+Fe (NO
3)
39H
2O 8～12g+H
2C
2O
430～40g+H
2The wiping 10～15 seconds on flour milling of the etchant of O 200mL, and water washes down rapidly; Polish altogether with this that water washes down after 45 minutes, dry up the metallographic show sample that namely obtains the Ti-Al laminar composite through cold wind again.
2. the preparation method of Ti-Al laminar composite metallographic show sample according to claim 1, it is characterized in that: the cutting of described steps A is to cut with wire cut electric discharge machine.
3. the preparation method of Ti-Al laminar composite metallographic show sample according to claim 1 is characterized in that: the tackifier of described steps A is the by volume potpourri of 1 ︰ 1 of epoxy resin and hardening agent.
4. the preparation method of Ti-Al laminar composite metallographic show sample according to claim 1 is characterized in that: the HNO of described step D
3, Fe (NO
3)
39H
2O, H
2C
2O
4Be the pure or chemical pure of commercial analysis.
5. the preparation method of Ti-Al laminar composite metallographic show sample according to claim 1 is characterized in that: the H in the etchant of described step D
2O is distilled water.
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| CN104236981A (en) * | 2014-09-15 | 2014-12-24 | 温州瑞明工业股份有限公司 | Polishing method for metallographic sample of aluminum alloy |
| CN108061737A (en) * | 2017-12-06 | 2018-05-22 | 北京工业大学 | A kind of preparation method of the electron backscatter diffraction sample of tin-based solder interconnection solder joint |
| CN109211645A (en) * | 2017-07-06 | 2019-01-15 | 宁波江丰电子材料股份有限公司 | The metallographic etching agent of chromium tantalum-titanium alloy and its display methods of metallographic structure |
| CN111257092A (en) * | 2020-04-10 | 2020-06-09 | 昆明理工大学 | Fixing method for polished metal and mineral sheet samples |
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