CN105506638A - Polishing liquid for metallographic analysis and preparation method and application method thereof - Google Patents

Polishing liquid for metallographic analysis and preparation method and application method thereof Download PDF

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Publication number
CN105506638A
CN105506638A CN201510966672.2A CN201510966672A CN105506638A CN 105506638 A CN105506638 A CN 105506638A CN 201510966672 A CN201510966672 A CN 201510966672A CN 105506638 A CN105506638 A CN 105506638A
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polishing fluid
metallurgical analysis
powder
polishing
aluminum oxide
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CN105506638B (en
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黄志华
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23FNON-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
    • C23F3/00Brightening metals by chemical means
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching

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  • Chemical & Material Sciences (AREA)
  • Immunology (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Pathology (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

The invention discloses polishing liquid for metallographic analysis. Aluminum oxide powder and mullite powder serve as polishing powder; sodium dodecyl sulfate, nonyl phenol polyoxyethylene ether, tripolyglycerol monostearate, triethanolamine, potassium pyrophosphate and potassium tripolyphosphate serve as additives; and anhydrous ethanol and water serve as dispersion mediums. The polishing liquid for metallographic analysis is suitable for metallographic sample preparation polishing of hard alloys; solid particles of the polishing liquid are exquisite, and are high in hardness; and the polishing liquid can effectively and finely polish the hard alloys, and is excellent in fluidity, low in cost and incapable of causing the dyeing trouble to metallographic test surfaces.

Description

A kind of metallurgical analysis polishing fluid and preparation method thereof, using method
Technical field
The present invention relates to a kind of polishing fluid containing polishing powder, be specifically related to a kind of polishing fluid being applicable to hard alloy metallographic polishing.
Background technology
Metallurgical analysis is one of main method of research metal and alloy internal structural flaw, occupies very consequence in metallic substance research field.Specimen method 50-1500 doubly can be studied the tissue of metal and alloy by metaloscope, is the most basic a kind of experimental technique of research metallic substance microtexture.The process of metallographic sample preparation can be divided into several operations, comprises cutting sampling, edge sample, mechanical mill, mechanical polishing four procedure.Cutting sampling operation cuts by the metal sample of required inspection, and cutting is namely needing the metal block carrying out analyzing to be cut into the size being applicable to inlaying.Edge sample can use metallographic pointing machine to carry out heat and inlay the method that also can use cold edge, insert in metal pattern by heat cured resin-oatmeal, metal sample to be analyzed is inserted in resin-oatmeal, then pass through metal pattern heating and pressurizing or add solidifying agent, making resin-oatmeal curing molding.Need to polish metal sample tested surface after edge sample completes, then polishing, selects suitable corrosive fluid to carry out etch or wiping after polishing, obtain the microcosmic grain structure of metal covering to be measured.
The object of mechanical mill and polishing is to obtain smooth surface, so that metallographic phase can intactly be presented in microscope after corrosion.In general, first with sand paper, plane is ground into for metallographic sample, then use more fine and smooth sand paper fine grinding, finally utilize rubbing paste to carry out rubbing down, the effect making metallographic test surfaces reach required by meticulous rubbing down again and again.The rubbing paste adopted in prior art is that the conventional powder such as cerium oxide, chromic oxide is as rubbing paste, commercially available rubbing paste mostly is yellow, in the process of actual metallographic sample preparation, test surfaces very easily dyes by colored polishing powder, or the seam crossing concealed in metal sample and inlay, being dissolved out when corroding, affecting corroded surface effect.These rubbing pastes are because ensureing stability and homogeneity simultaneously, and often lotion thickness, not easily disperses, and is difficult to all effectively be scattered on polishing cloth in polishing process, causes great waste, also easily causes the precision of polishing low, can not carry out meticulous polishing.Also have the rubbing paste using bortz powder as polishing powder, but price is extremely expensive.
Summary of the invention
For the deficiencies in the prior art part, the invention provides a kind of polishing fluid being applicable to the polishing of Wimet metallographic sample preparation, this polishing fluid solid particulate is fine and smooth and hardness is large, effectively can carry out meticulous polishing to Wimet, simultaneously this polishing fluid good fluidity, cheap, can not to metallographic test surfaces cause dyeing puzzlement.
Technical problem to be solved by this invention is achieved by the following technical programs:
Component and the content of the metallurgical analysis polishing fluid in the present invention are:
Aluminum oxide powder 200-240g/L
Mullite powder 30-50g/L
Sodium laurylsulfonate 8-12g/L
Polyoxyethylene nonylphenol ether 5-8g/L
Tripolyglycerol monostearates 2-4g/L
Trolamine 3-6g/L
Potassium pyrophosphate 2-4g/L
Potassium tripolyphosphate 2-4g/L
Dehydrated alcohol 90-120ml/L
Water surplus.
The mode that polishing powder in the present invention selects aluminum oxide powder and mullite powder to be used in combination.When the present inventor finds to use aluminum oxide powder to match with mullite powder in practice, better as the effect of polishing powder than single aluminum oxide to the removal effect of carbide surface fine scratches.Aluminum oxide powder is one of conventional polishing powder, and the mullite mineral that to be silicate at high temperature generate, wherein containing stable Al 2o 3-SiO 2symbiotic compound, Mohs' hardness can reach about 8, effectively can not only promote the hardness of aluminum oxide powder after appropriate interpolation, and other mineral elements contained in mullite powder there is very large promoter action to the stable suspersion of polishing powder in water and ethanolic soln.Meanwhile, aluminum oxide powder and mullite powder are in white, and inclined light gray, very easily cleans removing, can not cause the problem that sample surfaces dyes.
Can effectively be scattered in the mixing solutions of water and ethanol for making aluminum oxide powder and mullite powder, interpolation sodium laurylsulfonate and polyoxyethylene nonylphenol ether are as tensio-active agent, improve the condition of surface of polishing powder, make powder surface present hydrophily, make it more easily be disperseed in preparation process.Tripolyglycerol monostearates and trolamine then can promote the hydrophilic improvement in polishing powder surface further, go back the viscosity of polishing fluid in adjustable invention simultaneously.Potassium pyrophosphate and Potassium tripolyphosphate solvability splendid, simultaneously the ability of adjust ph and conformable metallic ion is strong, is added with the electrobalance type helping keep polishing fluid entirety in right amount, makes polishing fluid more stable.Meanwhile, for making each component balanced dispersion of polishing fluid adopt water and the two component dispersion medium of ethanol.
Further preferably, component and the content of the metallurgical analysis polishing fluid in the present invention are:
Aluminum oxide powder 220-230g/L
Mullite powder 35-45g/L
Sodium laurylsulfonate 10-12g/L
Polyoxyethylene nonylphenol ether 7-8g/L
Tripolyglycerol monostearates 3-4g/L
Trolamine 3-5g/L
Potassium pyrophosphate 3-4g/L
Potassium tripolyphosphate 3-4g/L
Dehydrated alcohol 110-120ml/L
Water surplus.
Again further preferably, component and the content of the metallurgical analysis polishing fluid in the present invention are:
Aluminum oxide powder 225g/L
Mullite powder 40g/L
Sodium laurylsulfonate 12g/L
Polyoxyethylene nonylphenol ether 8g/L
Tripolyglycerol monostearates 3g/L
Trolamine 4g/L
Potassium pyrophosphate 4g/L
Potassium tripolyphosphate 4g/L
Dehydrated alcohol 120ml/L
Water surplus.
The preparation method of the polishing fluid in the present invention is as follows:
(1) sodium laurylsulfonate, polyoxyethylene nonylphenol ether, Tripolyglycerol monostearates, trolamine are dissolved in dehydrated alcohol;
(2) potassium pyrophosphate and Potassium tripolyphosphate are dissolved in the water;
(3) ethanolic soln and aqueous solution are stirred;
(4) aluminum oxide powder and mullite powder are dropped in above-mentioned mixing solutions;
(5) said mixture is dropped in high speed dispersor, with the Rate Dispersion 2-4 hour of 3500-4500r/min;
(6) mixture after dispersion is dropped in shredder, solid particulate is ground to 0.5-3.5 μm, obtains described brightening solution for stainless steel.
Remove carbide surface cut when using the metallurgical analysis polishing fluid solid particulate granularity obtained by preparation method in the present invention to be 1 μm best, grain graininess is excessive, cannot carry out meticulous polishing, too small then cannot throwing sample surfaces.Consider the cost of polishing fluid, in the present invention, the granularity of aluminum oxide powder and mullite powder raw material is 30-50 μm.
Metallurgical analysis polishing fluid in the present invention is used for the meticulous polishing in Wimet metallurgical analysis sample making course, and described Wimet refers to stainless steel, high temperature steel, die steel, superalloy, expansion alloy.
The present invention has following beneficial effect:
1, the metallurgical analysis polishing fluid in the present invention is used for the meticulous polishing in Wimet metallurgical analysis sample making course, can have extraordinary removal effect to the fine scratches on Wimet metallographic sample rubbing down face;
2, the metallurgical analysis in the present invention is fine and smooth with polishing fluid solid particulate, good fluidity;
3, the metallurgical analysis in the present invention is with polishing fluid in white, and slightly light gray, easy cleaning, can not cause the problem that sample tested surface dyes.
4, the metallurgical analysis polishing fluid in the present invention is cheap, is applicable to suitability for industrialized production.
Embodiment
Below by embodiment, content of the present invention is conducted further description.
Stainless steel polishing cream composition in embodiment and content as shown in the table, the dispersion medium of surplus adopts deionized water.
Aluminum oxide powder in its Raw, the mean particle size of mullite powder are 30 μm, and rubbing paste preparation method is as follows:
(1) sodium laurylsulfonate, polyoxyethylene nonylphenol ether, Tripolyglycerol monostearates, trolamine are dissolved in dehydrated alcohol;
(2) potassium pyrophosphate and Potassium tripolyphosphate are dissolved in deionized water;
(3) ethanolic soln and aqueous solution are stirred;
(4) aluminum oxide powder and mullite powder are dropped in above-mentioned mixing solutions;
(5) said mixture is dropped in high speed dispersor, with the Rate Dispersion 4 hours of 4500r/min;
(6) mixture after dispersion is dropped in shredder, solid particulate is ground to 1 μm, obtains described polishing fluid.
Wherein, the shredder used in above-mentioned steps is ball mill, uses ball mill grinding can promote the homogeneity of polishing fluid further.
Polishing fluid finished product in above-described embodiment is homogeneous latex emulsion, overall white light gray partially, less than commercially available tubular polishing cream viscosity, therefore dispersing property is good, can load in container, drop on polishing cloth time to be used, can disperse on polishing cloth in seconds rapidly, can not reunite.
Depositing 90 days by being placed in warehouse under the polishing fluid normal temperature and pressure in embodiment, being all homogeneous latex emulsion shape after taking-up, not stratified suspension of not reuniting is good.
Wimet such as the Vickers' hardnesses such as stainless steel, high temperature steel, die steel, superalloy, expansion alloy reach the alloy of more than HV400, after utilizing common commercially available cerium oxide or chromic oxide rubbing paste (1.5 μm) burnish gold phase tested surface, the many tiny cuts of remained on surface, utilize the polishing fluid in the present invention in embodiment 6 to coordinate canvas polishing cloth to carry out polishing, polishing can remove tiny cut in about 1 minute.
Finally it should be noted that, above embodiment is only in order to illustrate the technical scheme of the embodiment of the present invention but not to be limited, although be described in detail the embodiment of the present invention with reference to preferred embodiment, those of ordinary skill in the art is to be understood that and still can modifies to the technical scheme of the embodiment of the present invention or equivalent replacement, and these are revised or be equal to the scope that replacement also can not make amended technical scheme disengaging embodiment of the present invention technical scheme.

Claims (8)

1. a metallurgical analysis polishing fluid, is characterized in that the component of described polishing fluid and content are:
Aluminum oxide powder 200-240g/L
Mullite powder 30-50g/L
Sodium laurylsulfonate 8-12g/L
Polyoxyethylene nonylphenol ether 5-8g/L
Tripolyglycerol monostearates 2-4g/L
Trolamine 3-6g/L
Potassium pyrophosphate 2-4g/L
Potassium tripolyphosphate 2-4g/L
Dehydrated alcohol 90-120ml/L
Water surplus.
2. metallurgical analysis polishing fluid as claimed in claim 1, is characterized in that: the granularity of described aluminum oxide powder and mullite powder raw material is 30-50 μm.
3. metallurgical analysis polishing fluid as claimed in claim 1, is characterized in that the component of described polishing fluid and content are:
Aluminum oxide powder 220-230g/L
Mullite powder 35-45g/L
Sodium laurylsulfonate 10-12g/L
Polyoxyethylene nonylphenol ether 7-8g/L
Tripolyglycerol monostearates 3-4g/L
Trolamine 3-5g/L
Potassium pyrophosphate 3-4g/L
Potassium tripolyphosphate 3-4g/L
Dehydrated alcohol 110-120ml/L
Water surplus.
4. metallurgical analysis polishing fluid as claimed in claim 1, is characterized in that the component of described polishing fluid and content are:
Aluminum oxide powder 225g/L
Mullite powder 40g/L
Sodium laurylsulfonate 12g/L
Polyoxyethylene nonylphenol ether 8g/L
Tripolyglycerol monostearates 3g/L
Trolamine 4g/L
Potassium pyrophosphate 4g/L
Potassium tripolyphosphate 4g/L
Dehydrated alcohol 120ml/L
Water surplus.
5. prepare as arbitrary in claim 1-4 as described in the method for metallurgical analysis polishing fluid, it is characterized in that comprising the steps:
Sodium laurylsulfonate, polyoxyethylene nonylphenol ether, Tripolyglycerol monostearates, trolamine are dissolved in dehydrated alcohol;
Potassium pyrophosphate and Potassium tripolyphosphate are dissolved in the water;
Ethanolic soln and aqueous solution are stirred;
Aluminum oxide powder and mullite powder are dropped in above-mentioned mixing solutions;
Said mixture is dropped in high speed dispersor, with the Rate Dispersion 2-4 hour of 3500-4500r/min;
Mixture after dispersion is dropped in shredder, solid particulate is ground to 0.5-3.5 μm, obtains described brightening solution for stainless steel.
6. the preparation method of metallurgical analysis polishing fluid as claimed in claim 5, is characterized in that: obtained metallurgical analysis polishing fluid solid particulate granularity is 1 μm.
7. a using method for metallurgical analysis polishing fluid as described in as arbitrary in claim 1-4, is characterized in that: described metallurgical analysis polishing fluid is used for the meticulous polishing in Wimet metallurgical analysis sample making course.
8. a using method for metallurgical analysis polishing fluid as claimed in claim 7, is characterized in that: described Wimet is stainless steel, high temperature steel, die steel, superalloy, expansion alloy.
CN201510966672.2A 2015-12-21 2015-12-21 A kind of Metallographic Analysis polishing fluid and preparation method thereof, application method Expired - Fee Related CN105506638B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106337183A (en) * 2016-06-05 2017-01-18 山东军沃科技有限公司 Stainless steel polishing solution used for magnetic grinders
CN106370489A (en) * 2016-08-24 2017-02-01 江西稀有稀土金属钨业集团有限公司 Sample production method used for hard alloy metallographic detection
CN106497435A (en) * 2016-10-21 2017-03-15 过冬 A kind of Metallographic Analysis polishing fluid and preparation method thereof, using method
CN107604363A (en) * 2017-08-14 2018-01-19 肥西县通力机械有限公司 A kind of method for lifting hard alloy stamping parts surface gloss

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1368912A (en) * 1999-05-28 2002-09-11 圣戈本磨料股份有限公司 Abrasive tools for grinding electronic components
US20100219269A1 (en) * 2002-09-17 2010-09-02 Imerys Minerals Limited Grinding method for inorganic particulate material
CN101831244A (en) * 2010-05-10 2010-09-15 上海高纳粉体技术有限公司 High-precision alumina polishing solution and preparation method thereof
CN102250585A (en) * 2011-08-19 2011-11-23 永州皓志稀土材料有限公司 Preparation method of zirconia grinding fluid
CN104559798A (en) * 2014-12-24 2015-04-29 上海新安纳电子科技有限公司 Alumina-based chemical mechanical polishing slurry

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1368912A (en) * 1999-05-28 2002-09-11 圣戈本磨料股份有限公司 Abrasive tools for grinding electronic components
US20100219269A1 (en) * 2002-09-17 2010-09-02 Imerys Minerals Limited Grinding method for inorganic particulate material
CN101831244A (en) * 2010-05-10 2010-09-15 上海高纳粉体技术有限公司 High-precision alumina polishing solution and preparation method thereof
CN102250585A (en) * 2011-08-19 2011-11-23 永州皓志稀土材料有限公司 Preparation method of zirconia grinding fluid
CN104559798A (en) * 2014-12-24 2015-04-29 上海新安纳电子科技有限公司 Alumina-based chemical mechanical polishing slurry

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106337183A (en) * 2016-06-05 2017-01-18 山东军沃科技有限公司 Stainless steel polishing solution used for magnetic grinders
CN106370489A (en) * 2016-08-24 2017-02-01 江西稀有稀土金属钨业集团有限公司 Sample production method used for hard alloy metallographic detection
CN106370489B (en) * 2016-08-24 2019-04-12 江西江钨硬质合金有限公司 The method for making sample of hard alloy metallographic detection
CN106497435A (en) * 2016-10-21 2017-03-15 过冬 A kind of Metallographic Analysis polishing fluid and preparation method thereof, using method
CN107604363A (en) * 2017-08-14 2018-01-19 肥西县通力机械有限公司 A kind of method for lifting hard alloy stamping parts surface gloss

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