CN110455846A - A kind of display methods of attritive powder section microscopic structure - Google Patents
A kind of display methods of attritive powder section microscopic structure Download PDFInfo
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- CN110455846A CN110455846A CN201910764739.2A CN201910764739A CN110455846A CN 110455846 A CN110455846 A CN 110455846A CN 201910764739 A CN201910764739 A CN 201910764739A CN 110455846 A CN110455846 A CN 110455846A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—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
- 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
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—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
- 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
- G01N23/225—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 using electron or ion
- G01N23/2251—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 using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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Abstract
The present invention relates to a kind of display methods of attritive powder section microscopic structure.The display methods includes: to prepare metallographic specimen: mixing sample and the embedding powder of hot insert, and the embedding powder of heating fusing hot insert obtains metallographic specimen；Grinding and polishing metallographic specimen: waterproof abrasive paper and polishing fluid grinding and polishing metallographic specimen are used；Corrode metallographic specimen: using the metallographic specimen after corrosion corrosion grinding and polishing；Display microscopic structure: microscopic structure is carried out to the metallographic specimen after corrosion using Electronic Speculum and is shown.The display methods operating process of attritive powder section microscopic structure of the invention is simple, low in cost, as a result reliably, is applicable to various alloy powders, provides valuable reference frame for the performance of pulverulent product.
Description
Technical field
Present invention relates generally to analysis detection fields, and in particular to a kind of display side of attritive powder section microscopic structure
Method.
Background technique
With increasing material manufacturing, the extensive use of powder metallurgy product, each field proposes the requirement of higher performance to product, this
Difficulty is equally increased to the analysis of properties of product.The main raw material in the fields such as increasing material manufacturing, powder metallurgy are various materials
Powder, powder tissue morphology internal after preparation forming has tissue topography, the mechanical property etc. of subsequent sample important
Influence, however the small powder interior tissue of granularity is difficult to observe.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for observing attritive powder section microscopic structure, solve existing various conjunctions
The golden undetectable problem of attritive powder section tissue.
The present invention provides a kind of display methods of attritive powder section microscopic structure, wherein includes:
Prepare metallographic specimen: mixing sample and the embedding powder of hot insert, heating melt the embedding powder of the hot insert and obtain metallographic specimen；
Grinding and polishing metallographic specimen: using metallographic specimen described in waterproof abrasive paper and polishing fluid grinding and polishing；
Corrode metallographic specimen: using the metallographic specimen after corrosion corrosion grinding and polishing；
Display microscopic structure: microscopic structure is carried out to the metallographic specimen after corrosion using Electronic Speculum and is shown.
Optionally, according to display methods above-mentioned, wherein the embedding powder of hot insert is phenolic moulding powder or urea-formaldehyde moulding powder.
Optionally, according to display methods above-mentioned, wherein the partial size of the embedding powder of hot insert is 50-100 μm.
Optionally, according to display methods above-mentioned, wherein prepared in metallographic specimen described, the sample and the heat
The volume ratio for inlaying powder is 1:1-1:3.
Optionally, it according to display methods above-mentioned, is prepared in metallographic specimen described, the heating temperature is 130-160
DEG C, the heating time is 5-9min.
Optionally, according to display methods above-mentioned, wherein in the grinding and polishing metallographic specimen, successively using 600# and
Then metallographic specimen described in 1200# liquid honing carries out rough polishing using 30 μm of polishing fluids, finally carried out using 50nm polishing fluid
Essence is thrown.
Optionally, according to display methods above-mentioned, wherein the display microscopic structure includes determining to corrode the fine powder
Last granulometric range and the observation attritive powder particle erosion pattern.
Optionally, according to display methods above-mentioned, wherein the corrosive liquid is the dedicated corrosive liquid of sample.The corrosive liquid
Dosage is adjusted according to the metallographic specimen volume.The corrosive liquid dosage is 15-30ml.Etching time is 5-20s.
Optionally, according to display methods above-mentioned, wherein when the sample be GH3536 alloy, the corrosive liquid be with
20mlHCl:4gCuSO4: 20mlH2The mixed liquor of O ratio preparation, dosage 15-30ml, etching time 5-10s.
Optionally, according to display methods above-mentioned, wherein when the sample is AlSi10Mg, the corrosive liquid be with
95mlH2O:2.5mlHNO3: the mixed liquor of 1.5mlHCl:1.0mlHF ratio preparation, dosage 15-30ml, etching time 10-
20s。
It is to mention for the production of increasing material manufacturing, powder metallurgy etc., R&D process the invention shows the beneficial effect of method
For a kind of new powder microstructure morphology analysis method, operating process is simple, low in cost, as a result reliably, is applicable to
Various alloy powders provide valuable reference frame for the performance of pulverulent product.
Detailed description of the invention
Fig. 1 is embodiment 1GH3536 superalloy powder section microscopic structure；
Fig. 2 is embodiment 2AlSi10Mg powder section microscopic structure.
Specific embodiment
Below in conjunction with drawings and examples, a specific embodiment of the invention is described in more details, so as to energy
The advantages of enough more fully understanding the solution of the present invention and its various aspects.However, specific embodiments described below and reality
It applies example to be for illustrative purposes only, rather than limiting the invention.
Experimental method in following embodiments is unless otherwise specified conventional method.Examination as used in the following examples
Material is tested, is that conventional reagent shop is commercially available unless otherwise specified.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
Each step executes sequence in the method being mentioned above, unless otherwise indicated, however it is not limited to the text institute body of this paper
Reveal the sequence come, that is to say, that the execution sequence of each step can change, and between two steps as needed
Other steps can be inserted.
Attritive powder described herein refers to that partial size is 10-65 μm of material, such as powder metallurgy superalloy.
The present invention provides a kind of display methods of attritive powder section microscopic structure, comprising:
Prepare metallographic specimen: the embedding powder of hot insert is melted in mixing sample (the i.e. described attritive powder) and the embedding powder of hot insert, heating
Obtain metallographic specimen.The embedding powder of hot insert used has preferable edge retention and higher hardness, while having weak inductive, can
For sem analysis with inlaying sample.Phenolic moulding powder or urea-formaldehyde moulding powder specifically can be used.
Grinding and polishing metallographic specimen: using metallographic specimen described in waterproof abrasive paper and polishing fluid grinding and polishing.Using liquid honing, without making
It is polished with coarse sandpaper, inlaying samples inside metallographic specimen is avoided to fall off.
Corrode metallographic specimen: using the metallographic specimen after corrosion corrosion grinding and polishing.Corrosive liquid used needs that gold can be covered
Some or all of one surface of phase sample is to carry out etch.
Display microscopic structure: microscopic structure is carried out to the metallographic specimen after corrosion using Electronic Speculum and is shown.
In some embodiments, the partial size of the embedding powder of the hot insert is 50-100 μm.It is preferred that small with sample powder partial size difference
And the embedding powder of hot insert of partial size fine uniform, powder diameter difference is smaller, sample particle can be made uniformly to disperse, be more advantageous to tissue
Observation.Sieve, such as 160 mesh screens can be used, the embedding powder of hot insert is sieved to obtain the embedding powder of aforementioned hot insert.
In some embodiments, it is prepared in metallographic specimen described, the volume ratio of the sample and the embedding powder of the hot insert is
The quantity of sample particle can be improved using biggish volume ratio by 1:1-1:3, and quantity is bigger in the visual field, and testing result is more quasi-
Really.The heating temperature is 130-160 DEG C, and the heating time is 5-9min.The heating temperature can make the embedding powder of hot insert sufficiently molten
Change, inlayed mixed-powder sample is stronger, avoids subsequent grinding and polishing process sample shed powder.If heating temperature is too low, sample is inlayed
After, powder combine it is insecure, be easy to dissipate；And heating temperature is excessively high, then the embedding powder mobility of hot insert is big, damages mounting press.
In some embodiments, in the grinding and polishing metallographic specimen, using metallographic described in 600#, 1200# liquid honing
Sample, then rough polishing and essence throwing are carried out using 30 μm, 50nm polishing fluid.
In some embodiments, in the corrosion metallographic specimen, the corrosive liquid is the dedicated corrosive liquid of sample.The corruption
Erosion liquid dosage is adjusted according to the metallographic specimen volume.The corrosive liquid dosage is 15-30ml.Etching time is 5-20s.
Specifically, in the corrosion metallographic specimen, when the sample be GH3536 alloy when, the corrosive liquid be with
20ml HCl:4g CuSO4: 20ml H2The mixed liquor of the ratio preparation of O, corrosive liquid dosage are 15-30ml, etching time 5-
10s.When the sample is AlSi10When Mg alloy, the corrosive liquid is Keller's corrosive agent, and corrosive liquid dosage is 15-30ml,
Etching time is 10-20s.
In some embodiments, the display microscopic structure includes determining to corrode the attritive powder granulometric range and observation
The attritive powder particle erosion pattern.Specifically, corrosive particles range is determined using metallographic microscope, is seen using scanning electron microscope
Examine particle erosion pattern.
Embodiment 1
The present embodiment is a kind of method for observing increasing material manufacturing GH3536 superalloy powder section microscopic structure, specifically
Method implementation process sequentially includes the following steps:
1) prepared by powder metallographic specimen: phenolic moulding powder is sieved into the powder of fine uniform, phenolic moulding powder used with 160 mesh screens
With weak inductive.GH3536 superalloy powder 10ml, the embedding powder 10ml of hot insert, according to volume ratio are measured respectively with 25ml graduated cylinder
1:1 is put into mortar and is mixed, and the granularity of superalloy powder used is 15~53 μm, is made after mixing using mounting press
It is insert-molded to obtain and inlay sample block (i.e. metallographic specimen).The heating temperature of mounting press is 160 DEG C, heating-up time 4min, heat preservation
Time 5min.
2) powder metallographic specimen grinding and polishing: sample block is inlayed using 600#, 1200# liquid honing, then is polished using 30 μm, 50nm
Liquid carries out rough polishing and essence throws and inlays sample block.
3) powder metallographic specimen corrosion observation: by the edge sample block after grinding and polishing use 25ml corrosive liquid (with 20mlHCl:
4gCuSO4: 20mlH2The preparation of O ratio) corrode 5s.Corrosive particles are marked under Axio Imager A2 metallographic microscope (Zeiss)
Range, then use Zeiss scanning electron microscopic observation powder particle erosion profile instead.
Specific erosion profile is shown in Fig. 1.Microcosmic group of powder can clearly, be accurately observed using the display methods of the application
It knits, provides accurate support for GH3536 high temperature alloy product performance boost.
Embodiment 2
The present embodiment is a kind of observation increasing material manufacturing AlSi10The method of Mg alloy powder section microscopic structure, specific side
Method implementation process sequentially includes the following steps:
1) prepared by powder metallographic specimen: phenolic moulding powder is sieved into the powder of fine uniform with 160 mesh screens.With 25ml graduated cylinder
AlSi is measured respectively10Mg alloy powder 10ml, phenolic moulding powder 20ml is put into mortar according to volume ratio 1:2 and is mixed, used
AlSi10The granularity of Mg alloy powder is 15~43 μm, is insert-molded it using mounting press after mixing to obtain edge sample block
(i.e. metallographic specimen).The heating temperature of mounting press is 130 DEG C, heating-up time 3min, soaking time 3min.
2) powder metallographic specimen grinding and polishing: sample block is inlayed using 600#, 1200# liquid honing, then is polished using 30 μm, 50nm
Liquid carries out rough polishing and essence throws and inlays sample block.
3) powder metallographic specimen corrosion observation: use 25ml Keller's corrosive agent (with 95ml the edge sample block after grinding and polishing
Water: 2.5mlHNO3: the preparation of 1.5mlHcl:1.0mlHF ratio) 15s is corroded, in Axio Imager A2 metallographic microscope
(Zeiss) corrosive particles range is marked under, then uses Zeiss scanning electron microscopic observation powder particle erosion profile instead.
Specific erosion profile is shown in Fig. 2.Microcosmic group of powder can clearly, be accurately observed using display methods of the invention
It knits, is AlSi10Mg increasing material manufacturing product properties, which is promoted, provides accurately support.
Finally, it should be noted that obviously, the above embodiment is merely an example for clearly illustrating the present invention, and simultaneously
The non-restriction to embodiment.For those of ordinary skill in the art, it can also do on the basis of the above description
Other various forms of variations or variation out.There is no necessity and possibility to exhaust all the enbodiments.And thus drawn
The obvious changes or variations that Shen goes out are still in the protection scope of this invention.
Claims (10)
1. a kind of display methods of attritive powder section microscopic structure characterized by comprising
Prepare metallographic specimen: mixing sample and the embedding powder of hot insert, heating melt the embedding powder of the hot insert and obtain metallographic specimen；
Grinding and polishing metallographic specimen: using metallographic specimen described in waterproof abrasive paper and polishing fluid grinding and polishing；
Corrode metallographic specimen: using the metallographic specimen after corrosion corrosion grinding and polishing；
Display microscopic structure: microscopic structure is carried out to the metallographic specimen after corrosion using Electronic Speculum and is shown.
2. display methods according to claim 1, which is characterized in that the embedding powder of hot insert is phenolic moulding powder or urea-formaldehyde moulding powder.
3. display methods according to claim 1, which is characterized in that the partial size of the embedding powder of hot insert is 50-100 μm.
4. display methods according to claim 1, which is characterized in that it is prepared in metallographic specimen described,
The volume ratio of the sample and the embedding powder of the hot insert is 1:1-1:3.
5. display methods according to claim 1, which is characterized in that prepared in metallographic specimen described, the heating temperature
Degree is 130-160 DEG C, and the heating time is 5-9min.
6. display methods according to claim 1, which is characterized in that in the grinding and polishing metallographic specimen,
Successively using metallographic specimen described in 600# and 1200# liquid honing, rough polishing then is carried out using 30 μm of polishing fluids, finally
Smart throwing is carried out using 50nm polishing fluid.
7. -6 any display methods according to claim 1, which is characterized in that the display microscopic structure includes determining corruption
It loses the attritive powder granulometric range and observes the attritive powder particle erosion pattern.
8. -6 any display methods according to claim 1, which is characterized in that the corrosive liquid is the dedicated corrosion of sample
Liquid, the corrosive liquid dosage are 15-30ml, etching time 5-20s.
9. display methods according to claim 8, which is characterized in that
When the sample is GH3536 alloy, the corrosive liquid is with 20mlHCl:4gCuSO4: 20mlH2The mixing of O ratio preparation
Liquid, dosage 15-30ml, etching time 5-10s.
10. display methods according to claim 8, which is characterized in that
When the sample is AlSi10Mg, the corrosive liquid are with 95mlH2O:2.5mlHNO3: 1.5mlHCl:1.0mlHF ratio system
Standby mixed liquor, dosage 15-30ml, etching time 10-20s.
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Cited By (2)
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| CN111965205A (en) * | 2020-07-31 | 2020-11-20 | 中国航发北京航空材料研究院 | Sample preparation method for nickel-based powder superalloy in-situ sample micro-area observation SEM + EBSD |
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