CN110286012A - It is a kind of for characterizing the sample and preparation method thereof of increasing material manufacturing non-ferrous metal performance - Google Patents
It is a kind of for characterizing the sample and preparation method thereof of increasing material manufacturing non-ferrous metal performance Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
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- B33Y80/00—Products made by additive manufacturing
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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
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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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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N23/20—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
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
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- 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
- G01N2001/2866—Grinding or homogeneising
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Abstract
The present invention provides a kind of for characterizing the sample and preparation method thereof of increasing material manufacturing non-ferrous metal performance, belongs to material microarrays techniques field.This method comprises: coating sample to be processed using cold mosaic mode, is then successively ground, mechanically polished and ion polishing with the region remnants to be measured for completely removing sample to be processed prepares stressor layers.Heating pressurization is not carried out to sample to be processed in cold mosaic process.This method perfect can eliminate specimen surface remnants and prepare stressor layers, it solves the problems, such as that back scattering diffraction technology and Nanoindentation measurement fathom less than surface deformation thickness degree to be measured and lead to measurement result inaccuracy, achievees the effect that each mechanical property of accurate characterization increasing material manufacturing non-ferrous metal and microstructure.The test zone remnants preparation stressor layers of the sample of this method preparation meet electron backscattered technology and the measurement of nano-hardness tester technology to the rigors of sample, achieve the purpose that accurate characterization material microstructure and mechanical property with a thickness of zero.
Description
Technical field
The present invention relates to material microarrays techniques fields, coloured for characterizing increasing material manufacturing in particular to one kind
Sample of metallicity and preparation method thereof.
Background technique
Increasing material manufacturing (3D printing) non-ferrous metal, there is its unique distinction: first is that size is finer, second is that usually thin-walled is empty
Between irregular part, it is difficult to cut on original part meet conventional mechanical property detection sample；Third is that increasing material manufacturing (3D printing) material
Larger in the printing direction of growth and vertical printing direction of growth performance difference, microstructure and mechanical property exist obvious respectively to different
Property.These features determine that increasing material manufacturing (3D printing) non-ferrous metal characterizes microstructure and mechanical property difficulty by conventional means
It is larger.
EBSD technology and Nanoindentation are nearly 20 years micrometerings to grow up and structural analysis
Technology.It is widely used in investigation of materials field in recent years because technologically advanced.Electron backscatter diffraction can be in micro/nano level to grade
Material is mutually identified in scale, mutually the crystallographic datas such as distribution, phase content characterize, Nanoindentation passes through calculating
Machine control load, on-line monitoring nano-indentators be pressed into depth of material, pass through sensor real-time measurement and record nano-indentators with to
Material surface contact situation is surveyed, analysis unloading curve obtains the mechanical property parameters such as the hardness and elastic modulus of material, has and survey
The high feature of accuracy of measurement.
EBSD technology and Nanoindentation are because investigation depth is nanoscale, to material region table to be characterized
Face requirement is harsh, and the examination for meeting electron backscattered technology and nano-hardness tester technology measurement request can be prepared at present by not having also
The method of sample.
Summary of the invention
The first object of the present invention include provide it is a kind of for characterizing the preparation of the sample of increasing material manufacturing non-ferrous metal performance
Method, which perfect can eliminate specimen surface remnants and prepare stressor layers, to solve back scattering diffraction technology and receive
Rice indentation measurement fathoms less than surface deformation thickness degree to be measured and leads to measurement result inaccuracy problem, reaches accurate
Characterize the effect of increasing material manufacturing non-ferrous metal each mechanical property and microstructure.
The second object of the present invention is coloured including providing a kind of characterization increasing material manufacturing prepared by the preparation method
The sample of metallicity, the test zone remnants preparation stressor layers of the sample with a thickness of zero, meet electron backscattered technology and
Nano-hardness tester technology measures the rigors to sample, achievees the purpose that accurate characterization material microstructure and mechanical property.
The present invention solves its technical problem and adopts the following technical solutions to realize:
The present invention proposes a kind of for characterizing the preparation method of the sample of increasing material manufacturing non-ferrous metal performance, including following step
It is rapid:
Using cold mosaic mode cladding non-ferrous metal sample to be processed, then successively ground, mechanically polish and from
Son polishing prepares stressor layers with the region remnants to be measured for completely removing sample to be processed.
Wherein, heating pressurization is not carried out to sample to be processed in cold mosaic process.
In some embodiments, above-mentioned increasing material manufacturing non-ferrous metal include manufactured in a manner of precinct laser fusion-it is coloured
Metal and its alloy, non-ferrous metal include any one in Al, Ti, Cu, Ag, Au, Pt, Pd, Sn, Pb, W and Mo.
In some embodiments, cold inlay includes: to inlay agent by cold and coat examination to be processed under negative pressure, normal temperature condition
Sample is then stood.
In some embodiments, the cold negative pressure inlayed is 1 × 10-2To 1 × 10-3MPa, more excellent is 1 × 10-3MPa。
In some embodiments, the cold temperature inlayed is 20-24 DEG C, and more excellent is 22 DEG C.
It is in some embodiments, cold that inlay agent include epoxy resin.
In some embodiments, time of repose 20-28h.
In some embodiments, the number of mechanical polishing is multiple, after the preceding load pressure once mechanically polished is higher than
The load pressure of one-time mechanical polishing.
In some embodiments, by sequencing is operated, the load pressure in mechanical polishing process reduces in gradient.
In some embodiments, the load pressure of mechanical polishing is 20-30N for the first time, last time mechanical polishing
Load pressure is 5N.
In addition, the invention also provides a kind of for characterizing the sample of increasing material manufacturing non-ferrous metal performance, by above-mentioned preparation
Method is prepared.The region remnants to be measured preparation stressor layers of the sample are with a thickness of 0.
The beneficial effect provided by the present application for being used to characterize sample of increasing material manufacturing non-ferrous metal performance and preparation method thereof
Include:
Preparation method provided by the present application is not by carrying out heating pressurization, a side to sample to be processed in cold mosaic process
Face effectively prevents sample tissue variation to be processed, maintains the pore structure of nonferrous materials script, on the other hand can also keep away
Exempt to generate new residual stress.Subsequent grinding, mechanical polishing and ion polishing are combined by above-mentioned cold mosaic technology, it can be complete
The full region remnants to be measured for removing sample prepare stressor layers, make the test zone remnants preparation stressor layers of sample obtained with a thickness of
Zero, to solve back scattering diffraction technology and Nanoindentation measurement fathoms less than surface deformation thickness degree to be measured and leads
Measurement result inaccuracy problem is caused, the effect of accurate characterization increasing material manufacturing non-ferrous metal each mechanical property and microstructure is reached
Fruit.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Below to provided by the embodiments of the present application for characterizing sample and its preparation side of increasing material manufacturing non-ferrous metal performance
Method is specifically described.
The preparation method of the sample of characterization increasing material manufacturing non-ferrous metal performance provided by the present application, comprising the following steps:
Using cold mosaic mode cladding non-ferrous metal sample to be processed, then successively ground, mechanically polish and from
Son polishing prepares stressor layers with the region remnants to be measured for completely removing sample to be processed, and sample is made.
Wherein, heating pressurization is not carried out to sample to be processed in cold mosaic process.
Optionally, above-mentioned increasing material manufacturing non-ferrous metal for example may include being manufactured-being had in a manner of precinct laser fusion
Non-ferrous metal and its alloy.Wherein, non-ferrous metal for example may include in Al, Ti, Cu, Ag, Au, Pt, Pd, Sn, Pb, W and Mo
Any one.
Characterization increasing material manufacturing non-ferrous metal performance mentioned in the application includes but are not limited to being parallel to for metal and beats
Print the direction of growth and microstructure and mechanical property perpendicular to the printing direction of growth.Wherein, microstructure includes using EBSD
The material phase constitution and distribution, mechanical property of method measurement include elasticity modulus, hardness and fracture toughness of material etc..
Can refer to ground, it is cold inlay before, the sample to be processed of preferred dimensions can be prepared in the following manner: in cutting revolving speed
Cutting interception non-ferrous metal is under conditions of being 0.03-0.04mm/s for 2000-2400rpm and feeding rate to obtain stand-by ruler
Very little sample to be processed.
In some preferred embodiments, cutting revolving speed is 2200rpm, feeding rate 0.035mm/s.Above-mentioned cutting
Diamond material tool (such as skive piece) progress can be used.
In the application, cold inlay for example may include: to inlay agent by cold and coat examination to be processed under negative pressure, normal temperature condition
Sample is then stood.Specifically, can make for the region surface to be measured of sample to be processed to be placed in downward in cold embedding die, in negative
Injected under pressure condition into mold it is cold inlay agent and make it is cold inlay agent natural coagulation, avoid heating, drying in the above process.
Inventors have found that conventional hot insert embedding technology is at a certain temperature and to impose certain pressure at present, temperature is usual
At 180 DEG C, in 20MPa between 30MPa, this condition is enough to cause nonferrous materials tissue change pressure, influences measurement table
Levy the Exact Travelling and objectivity of result.
In consideration of it, cold pressure of inlaying is arranged to 1 × 10 in the application-2To 1 × 10-3MPa, such as 1 × 10-3MPa、5×
10-3MPa or 1 × 10-2MPa etc., preferably 1 × 10-3MPa.By by cold mosaic process be defined under room temperature and condition of negative pressure into
Row, experiment proves that, metal material tissue variation, maximum journey during above-mentioned pressure condition can effectively avoid conventional hot insert embedding
Degree maintains its original performance.
Inventor also found, inlay embedding according to heat treatment mode, and hole and tissue in metal structure is be easy to cause to change
Become, and generates new stress.For example, after it uses hot insert embedding technology to handle, tissue morphology occurs obvious by taking copper pipe as an example
Variation, hardness reach 110HV, become hard state metal.
In consideration of it, in the application by the cold temperature setting inlayed be 20-24 DEG C, such as 20 DEG C, 21 DEG C, 22 DEG C, 23 DEG C or 24
DEG C, preferably 22 DEG C, higher than the cold setting time for inlaying agent can be extended lower than 20 DEG C, will lead to again higher than 24 DEG C material structure and
Performance changes.By carrying out under the conditions of above-mentioned temperature, the script tissue morphology of raw material can be effectively maintained.Pass through test
Verifying, with copper pipe material identical with above-mentioned copper pipe, the cold mosaic technology proposed using the application, tissue morphology is still protected
Original state is held, hardness remains as light and soft state metal, thus prove between 50-70HV, and what the application was proposed cold inlays packet
Covering mode can effectively avoid sample tissue to be processed or structure from changing and avoid to generate new residual stress really.
Optionally, mentioned by the application it is cold inlay agent for example can with but be not limited only to include epoxy resin.Using
Epoxy resin inlays agent not only cost inexpensively, and will not generate new remnants in above-mentioned cold mosaic process and answer as cold
Power, will not tissue to metal and performance have an impact.
In some embodiments, the cold time of repose inlayed can be 20-28h, such as 20h, 22h, for 24 hours, 26h or 28h,
Preferably for 24 hours.
Further, the sample to be processed after cold damascene process is ground and is mechanically polished, to be greatly decreased wait locate
It manages specimen surface remnants and prepares stressor layers thickness.Wherein, it is ground to mechanical lapping, namely the side crops industry in region to be measured is ground,
To achieve the purpose that influence of crust deformation layer is most shallow.The polish process for example may include grinding twice (corase grinding and fine grinding): adopt first
It is roughly ground with side crops industry to show complete sample to be tested region, reduces load fine grinding removal corase grinding scratch then to show region to be measured
Fine surface.
As reference, grinding includes grinding (corase grinding) for the first time, and the condition of grinding for example may include: grinding for the first time
Tool rotation speed is 280-320rpm (such as 280rpm, 290rpm, 300rpm, 310rpm or 320rpm), clamping head rotation
Speed be 130-170rpm (such as 130rpm, 140rpm, 150rpm, 160rpm or 170rpm), load pressure be 25-35N (such as
25N, 28N, 30N, 32N or 35N etc.), first time milling time is 0.2-0.3min (such as 0.2min, 0.25min or 0.3min
Deng).
It is preferably carried out in mode some, milling tool rotation speed is 300rpm, and clamping head rotation speed is
150rpm, load pressure 30N, milling time 0.2-0.25min.
Wherein, milling tool for example can be abrasive disk, similarly hereinafter.
Preferably, clamping head is identical as the direction of rotation of milling tool in first time process of lapping, grinding using sand paper into
Row.Sand paper for example may include the SiC sand paper including 320# SiC sand paper or 500# SiC sand paper.
Further, also added with the first cooling lubricant in first time process of lapping, which for example may be used
To include water.
Further, grinding includes second of grinding (fine grinding), and the condition of second of grinding for example may include: grinding work
Tool rotation speed is 130-170rpm (such as 130rpm, 140rpm, 150rpm, 160rpm or 170rpm), clamping head rotation speed
Degree is 120-170rpm (such as 120rpm, 130rpm, 140rpm, 150rpm, 160rpm or 170rpm), load pressure 20-
30N (such as 20N, 25N or 30N), second of milling time are 4-6min (such as 4min, 4.5min, 5min, 5.5min or 6min
Deng).
In some preferred embodiments, load pressure of the load pressure of second of grinding lower than grinding for the first time.
In some preferred embodiments, milling tool rotation speed is 150rpm, and clamping head rotation speed is
150rpm, load pressure 25N, milling time 4-5min.
Preferably, the direction of rotation of clamping head and milling tool is also identical in second of process of lapping, grinding uses Buddha's warrior attendant
Abrasive disk made from stone carries out.The particle diameter of diamond for example can be 8-10 μm, preferably 9 μm in abrasive disk.
Further, also added with the second cooling lubricant in second of process of lapping, the second cooling lubricant for example can be with
Including the suspension containing diamond particles.Preferably, diamond in the partial size and abrasive disk of diamond particles in suspension
Particle diameter is equal.
In the application, the number of mechanical polishing be it is multiple, the preceding load pressure once mechanically polished be higher than rear one-time mechanical
The load pressure of polishing.In some preferred embodiments, operation sequencing, the load pressure in mechanical polishing process are pressed
It reduces in gradient.In other words, above-mentioned mechanical polishing is mainly that the surface of the sample after mechanical lapping reduces load by gradient
Lotus and repeatedly polished, to achieve the purpose that maximum to reduce grinding deformation layer.
Preferably, by sequencing is operated, the load pressure in mechanical polishing process reduces in gradient.In some embodiment party
In formula, the load pressure of mechanical polishing is 20-30N for the first time, and the load pressure of last time mechanical polishing is 5N.
It can refer to ground, mechanical polishing for example may include: first using normal load (20-30N) normal time (1.5-
2.5min) polish sample to be processed, reduce load normal time fine sample surfaces again, then with lower load (such as
Can be using 10N as gradient) polishing sample 1-2min, until dropping to load pressure is 5N.
Specifically, mechanical polishing may include mechanically polishing for the first time, the condition of mechanical polishing includes: polishing tool for the first time
Rotation speed be 120-180rpm (such as 120rpm, 140rpm, 150rpm, 160rpm or 180rpm), the rotation of clamping head
Speed be 120-180rpm (such as 120rpm, 140rpm, 150rpm, 160rpm or 180rpm), load pressure be 20-30N (such as
20N, 25N or 30N etc.), first time polishing time is 2-2.5min (such as 2min, 2.2min or 2.5min).
It is preferably carried out in mode some, the rotation speed of polishing tool is 150rpm, folder in first time polishing process
The rotation speed for holding head is 150rpm, and load pressure 25N, first time polishing time is 2.3min.
Optionally, polishing tool used in first time polishing process can for example polish for wool plain fabric
Disk.
Preferably, clamping head is identical as the direction of rotation of polishing tool in first time polishing process.
Preferably, third cooling lubricant can for example be added in first time polishing process, third cooling lubricant may include
Suspension containing SiC particulate.Preferably, the partial size of SiC particulate can be 2-4 μm in suspension, and more excellent is 3 μm.
Further, mechanical polishing further includes second of mechanical polishing, and the condition of second of mechanical polishing includes: buffer
The rotation speed of tool is 120-180rpm (such as 120rpm, 140rpm, 150rpm, 160rpm or 180rpm), the rotation of clamping head
Rotary speed is 120-180rpm (such as 120rpm, 140rpm, 150rpm, 160rpm or 180rpm), load pressure 10-20N
(such as 10N, 15N or 20N), second polishing time be 1.5-2.5min (such as 1.5min, 1.8min, 2min, 2.2min or
2.5min etc.).
It is preferably carried out in mode some, the rotation speed of polishing tool is 150rpm, folder in second of polishing process
The rotation speed for holding head is 150rpm, and load pressure 15N, second of polishing time is 2min.
Optionally, polishing tool used in second of polishing process can be for example synthesis short wool suede polishing
Disk.
Preferably, the direction of rotation of clamping head and polishing tool is also identical in second of polishing process.
Preferably, the 4th cooling lubricant can be added in second of polishing process, the 4th cooling lubricant may include containing
The suspension of SiC particulate.Preferably, the partial size of SiC particulate can be 0.8-1 μm in suspension, and more excellent is 0.9 μm.
Further, mechanical polishing further includes that third time mechanically polishes, and the condition of third time mechanical polishing includes: buffer
The rotation speed of tool is 120-180rpm (such as 120rpm, 140rpm, 150rpm, 160rpm or 180rpm), the rotation of clamping head
Rotary speed is 120-180rpm (such as 120rpm, 140rpm, 150rpm, 160rpm or 180rpm), load pressure 5-10N
(5N or 10N), third time polishing time are 1-2min (such as 1min, 1.2min, 1.5min, 1.8min or 2min).
It is preferably carried out in mode some, the rotation speed of the polishing tool of third time is 150rpm, the rotation of clamping head
Rotary speed is 150rpm, and load pressure 10N, third time polishing time is 1.5min.
Optionally, polishing tool used in third time polishing process for example may be synthesis short wool suede polishing
Disk.
Preferably, the direction of rotation of clamping head and polishing tool is also identical in third time polishing process.
Preferably, can may include added with the 5th cooling lubricant, the 5th cooling lubricant in third time polishing process containing
The suspension of SiC particulate.Preferably, the partial size of SiC particulate can be 0.8-1 μm in suspension, and more excellent is 0.9 μm.
Further, mechanical polishing further includes the 4th mechanical polishing, and the condition of the 4th mechanical polishing includes: buffer
The rotation speed of tool is 120-180rpm (such as 120rpm, 140rpm, 150rpm, 160rpm or 180rpm), the rotation of clamping head
Rotary speed is 120-180rpm (such as 120rpm, 140rpm, 150rpm, 160rpm or 180rpm), load pressure 5N, the 4th
Secondary polishing time is 1-2min (such as 1min, 1.2min, 1.5min, 1.8min or 2min).
It is preferably carried out in mode some, the rotation speed of the 4th polishing tool is 150rpm, the rotation of clamping head
Rotary speed is that time polishing time of 150rpm, load pressure 5N, the 4th is 1.5min.
Optionally, polishing tool used in third time polishing process for example may be synthesis short wool suede polishing
Disk.
Preferably, the direction of rotation of clamping head and polishing tool is also identical in the 4th polishing process.
Preferably, the 6th cooling lubricant may include containing SiC added with the 6th cooling lubricant in the 4th polishing process
The suspension of particle.Preferably, the partial size of SiC particulate can be 0.8-1 μm in suspension, and more excellent is 0.9 μm.
Further, ion polishing is carried out to remove specimen surface after mechanical polishing to the sample to be processed after mechanical polishing
Remaining deformation layer.Optionally, ion sputtering method can be used in ion polishing.The depth of above-mentioned deformation layer is preferably
100nm。
In some embodiments, the time of ion polishing can be 50-70min, as 50min, 55min, 60min,
65min or 70min etc., preferably 60min.
In some embodiments, ion gun used in ion polishing and sample stage angle can be in 5.5-6.5 °, such as
5.5 °, 5.8 °, 6 °, 6.2 ° or 6.5 °, preferably 6 °.
By the ion polishing processing under above-mentioned condition, can effectively remove after mechanically polishing in specimen surface to be processed
It remains deformation layer (such as 100nm depth), achievees the effect that completely eliminate specimen surface deformation layer and expose metal material matrix.
In some embodiments, before ion polishing, further including that removing is cold inlays agent to expose whole metallic matrixes.
It holds, above-mentioned preparation method provided by the present application in cold mosaic process by not heating sample to be processed
On the one hand pressurization effectively prevents sample tissue variation to be processed, maintains the pore structure of nonferrous materials script, another party
Face, which is also avoided that, generates new residual stress.Through above-mentioned cold mosaic technology and subsequent grinding, mechanical polishing and ion polishing knot
It closes, completely removes the region remnants to be measured preparation stressor layers of sample, make the test zone remnants preparation stressor layers of sample obtained
With a thickness of zero, to solve back scattering diffraction technology and Nanoindentation measurement fathoms less than surface deformation thickness to be measured
It spends and leads to measurement result inaccuracy problem, reach each mechanical property of accurate characterization increasing material manufacturing non-ferrous metal and microstructure
Effect.
In addition, having coloured gold for characterizing increasing material manufacturing by what above-mentioned preparation method was prepared present invention also provides a kind of
The sample of attribute energy, the region remnants to be measured preparation stressor layers of the sample meet electron backscattered technology and nanometer with a thickness of 0
Impression instrument technology measures the rigors to sample, achievees the purpose that accurate characterization material microstructure and mechanical property.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of for characterizing the examination of increasing material manufacturing (3D printing) titanium alloy (Ti6Al4V) microstructure
Sample, preparation method include:
1, cutting is to obtain sample to be processed: cutting increasing material manufacturing (3D printing) titanium alloy, interception with skive piece
The sample to be processed of 8*5*3mm out, makes the face of 8*5 vertically print the direction of growth, and cutting wheel speed is 2200rpm, feed speed
Spend 0.035mm/s.
2, inlay sample: by the surface 8*5mm be placed in it is cold inlay in mould, cold mould of inlaying is placed in cold pointing machine, cold pointing machine
Negative pressure reaches 1*10-3Epoxy resin is injected when MPa, is stood 24 hours under the conditions of 22 DEG C of temperature after removing vacuum, is inlayed agent to cold
Natural coagulation does not heat up to cold pointing machine and pressurizes.
3, mechanical lapping sample to be processed:
1. carrying out first time grinding under the following conditions: 320# SiC sand paper is used, disc spin speed 300rpm is ground,
Upper clamping head rotation speed 150rpm, load pressure 30N, upper clamping head is relative to the equidirectional rotation of abrasive disk, milling time
0.25min, cooling lubricant are water；
2. carrying out second under the following conditions to grind: using particle diameter for 9 μm of diamond lap disk, grinding is spiraled
Rotary speed 150rpm, upper clamping head rotation speed 150rpm, load pressure 25N, upper clamping head relative to the equidirectional rotation of abrasive disk,
Milling time 5min, cooling lubricant are the suspension containing 9 μm of diamond particles.
4, sample to be processed is mechanically polished:
1. carrying out first time mechanical polishing under the following conditions: using wool plain fabric polishing disk, polish disc spins
Speed 150rpm, upper clamping head rotation speed 150rpm, load pressure 25N, upper clamping head are thrown relative to the equidirectional rotation of polishing disk
2.30min between light time, cooling lubricant are the suspension containing 3 μm of SiC particulates；
2. carrying out mechanically polishing for second under the following conditions: using synthesis short wool suede polishing disk, polishing disc spins speed
150rpm, upper clamping head rotation speed 150rpm, load pressure 15N are spent, upper clamping head is relative to the equidirectional rotation of polishing disk, polishing
Time 2.0min, cooling lubricant are the suspension containing 0.9 μm of SiC particulate；
3. carrying out third time mechanical polishing under the following conditions: using synthesis short wool suede polishing disk, polishing disc spins speed
150rpm, upper clamping head rotation speed 150rpm, load pressure 10N are spent, upper clamping head is relative to the equidirectional rotation of polishing disk, polishing
Time 1.5min, cooling lubricant are the suspension containing 0.9 μm of SiC particulate；
4. carrying out the 4th mechanical polishing under the following conditions: using synthesis short wool suede polishing disk, polishing disc spins speed
150rpm, upper clamping head rotation speed 150rpm, load pressure 5N are spent, upper clamping head is relative to the equidirectional rotation of polishing disk, polishing
Time 1.5min, cooling lubricant are the suspension containing 0.9 μm of SiC particulate.
5, using the sample to be processed after the mechanical polishing of precision gas cutting machine interception >=1mm thickness, cutting parameter are as follows: cutting
Wheel is SiC piece, cutting sheet revolving speed 2200rpm, feeding rate 0.035.Then ensuring carefully to go under the premise of not touching burnishing surface
Resin is inlayed except cladding is cold, exposes whole metallic matrixes.
6, to specimen surface ion polishing to be processed 60 minutes mechanically polished, ion gun and sample stage angle are 6 °.
It is used to characterize increasing material manufacturing (3D printing) titanium alloy (Ti6Al4V) microstructure through what the above method was prepared
The region remnants to be measured preparation stressor layers of sample are with a thickness of 0.
Embodiment 2
The present embodiment provides a kind of for measuring the sample of increasing material manufacturing (3D printing) copper alloy (TU) elasticity modulus, system
Preparation Method includes:
1, cutting is to obtain sample to be processed: cutting increasing material manufacturing (3D printing) copper alloy, interception with skive piece
The sample to be processed of 8*5*3mm out, makes the face of 8*5 print the direction of growth in parallel, and cutting wheel speed is 2200rpm, feed speed
Spend 0.035mm/s.
2, inlay sample: by the surface 8*5mm be placed in it is cold inlay in mould, cold mould of inlaying is placed in cold pointing machine, cold pointing machine
Negative pressure reaches 1*10-3Epoxy resin is injected when MPa, is stood 24 hours under the conditions of 24 DEG C of temperature after removing vacuum, is inlayed agent to cold
Natural coagulation must not heat up to cold pointing machine and pressurize.
3, mechanical lapping sample to be processed:
1. carrying out first time grinding under the following conditions: 500# SiC sand paper is used, disc spin speed 300rpm is ground,
Upper clamping head rotation speed 150rpm, load pressure 30N, upper clamping head is relative to the equidirectional rotation of abrasive disk, milling time
0.20min, cooling lubricant are water；
2. carrying out second under the following conditions to grind: using particle diameter for 9 μm of diamond lap disk, grinding is spiraled
Rotary speed 150rpm, upper clamping head rotation speed 150rpm, load pressure 25N, upper clamping head relative to the equidirectional rotation of abrasive disk,
Milling time 4min, cooling lubricant are the suspension containing 9 μm of diamond particles.
4, sample to be processed is mechanically polished:
1. carrying out first time mechanical polishing under the following conditions: using wool plain fabric polishing disk, polish disc spins
Speed 150rpm, upper clamping head rotation speed 150rpm, load pressure 25N, upper clamping head are thrown relative to the equidirectional rotation of polishing disk
2.30min between light time, cooling lubricant are the suspension containing 3 μm of SiC particulates；
2. carrying out mechanically polishing for second under the following conditions: using synthesis short wool suede polishing disk, polishing disc spins speed
150rpm, upper clamping head rotation speed 150rpm, load pressure 15N are spent, upper clamping head is relative to the equidirectional rotation of polishing disk, polishing
Time 2.0min, cooling lubricant are the suspension containing 0.9 μm of SiC particulate；
3. carrying out third time mechanical polishing under the following conditions: using synthesis short wool suede polishing disk, polishing disc spins speed
150rpm, upper clamping head rotation speed 150rpm, load pressure 10N are spent, upper clamping head is relative to the equidirectional rotation of polishing disk, polishing
Time 1.5min, cooling lubricant are the suspension containing 0.9 μm of SiC particulate；
4. carrying out the 4th mechanical polishing under the following conditions: using synthesis short wool suede polishing disk, polishing disc spins speed
150rpm, upper clamping head rotation speed 150rpm, load pressure 5N are spent, upper clamping head is relative to the equidirectional rotation of polishing disk, polishing
Time 1.5min, cooling lubricant are the suspension containing 0.9 μm of SiC particulate.
5, to specimen surface ion polishing has been mechanically polished 60 minutes, argon ion and sample stage angle are 6 °.
The sample for being used to measure increasing material manufacturing (3D printing) copper alloy (TU) elasticity modulus being prepared through the above method
Region remnants to be measured preparation stressor layers with a thickness of 0.
In conclusion the preparation method of the sample provided by the present application for characterizing increasing material manufacturing non-ferrous metal performance can
The perfect specimen surface remnants that eliminate prepare stressor layers, to solve back scattering diffraction technology and Nanoindentation measurement measurement deeply
Degree is less than surface deformation thickness degree to be measured and leads to measurement result inaccuracy problem, reaches accurate characterization increasing material manufacturing non-ferrous metal
The effect of each mechanical property and microstructure.The test zone remnants for the sample being prepared by this method prepare stress thickness
Degree is zero, meets electron backscattered technology and the measurement of nano-hardness tester technology to the rigors of sample, reaches accurate characterization
The purpose of material microstructure and mechanical property.
The foregoing is merely the preferred embodiment of the present invention, are not intended to restrict the invention, for this field
For technical staff, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any
Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of for characterizing the preparation method of the sample of increasing material manufacturing non-ferrous metal performance, which is characterized in that including following step
It is rapid:
Using cold mosaic mode cladding non-ferrous metal sample to be processed, then successively ground, mechanically polish and ion throw
Light prepares stressor layers with the region remnants to be measured for completely removing the sample to be processed, and the sample is made；
Wherein, heating pressurization is not carried out to the sample to be processed in cold mosaic process；
Preferably, the increasing material manufacturing non-ferrous metal includes that-non ferrous metal and their alloy is manufactured in a manner of precinct laser fusion, institute
Stating non-ferrous metal includes any one in Al, Ti, Cu, Ag, Au, Pt, Pd, Sn, Pb, W and Mo.
2. preparation method according to claim 1, which is characterized in that cold inlay includes: to inlay agent in negative pressure, room temperature for cold
Under the conditions of coat the sample to be processed, then stand；
Preferably, the cold negative pressure inlayed is 1 × 10-2To 1 × 10-3MPa, more excellent is 1 × 10-3MPa；
Preferably, the cold temperature inlayed is 20-24 DEG C, and more excellent is 22 DEG C；
It is preferably, described that cold to inlay agent include epoxy resin；
Preferably, time of repose 20-28h；
Preferably, it is cold inlay before, further include preparing the sample to be processed: in cutting revolving speed be 2000-2400rpm and to
Cutting interception non-ferrous metal is under conditions of being 0.03-0.04mm/s into speed to obtain the sample to be processed of stand-by size；
Preferably, cutting revolving speed is 2200rpm, feeding rate 0.035mm/s；
Preferably, cutting is carried out using diamond material tool.
3. preparation method according to claim 1, which is characterized in that grinding includes grinding for the first time, grinding for the first time
Condition includes: that milling tool rotation speed is 280-320rpm, and clamping head rotation speed is 130-170rpm, and load pressure is
25-35N, first time milling time are 0.2-0.3min；
Preferably, milling tool rotation speed is 300rpm, and clamping head rotation speed is 150rpm, load pressure 30N, grinding
Time is 0.2-0.25min；
Preferably, the clamping head is identical as the direction of rotation of the milling tool；
Preferably, grinding is carried out using sand paper；More preferably, the sand paper includes SiC sand paper, and more preferably, the SiC sand paper includes
No. 320 SiC sand paper or No. 500 SiC sand paper；
Preferably, being added in first time process of lapping has the first cooling lubricant；More preferably, first cooling lubricant includes
Water.
4. preparation method according to claim 3, which is characterized in that grinding includes second of grinding, second of grinding
Condition includes: that milling tool rotation speed is 130-170rpm, and clamping head rotation speed is 120-170rpm, and load pressure is
20-30N, second of milling time are 4-6min；
Preferably, load pressure of the load pressure of second of grinding lower than grinding for the first time；
Preferably, milling tool rotation speed is 150rpm, and clamping head rotation speed is 150rpm, load pressure 25N, grinding
Time is 4-5min；
Preferably, the clamping head is identical as the direction of rotation of the milling tool；
Preferably, grinding is carried out using abrasive disk made from diamond；More preferably, in the abrasive disk diamond particle diameter
It is 8-10 μm, more preferably, the particle diameter of the diamond is 9 μm；
Preferably, being added in second of process of lapping has the second cooling lubricant；More preferably, second cooling lubricant includes
Suspension containing diamond particles；More preferably, the partial size of diamond particles and Buddha's warrior attendant in the abrasive disk in the suspension
The particle diameter of stone is equal.
5. preparation method according to claim 1, which is characterized in that the number of mechanical polishing is multiple, preceding one-time mechanical
The load pressure of polishing is higher than the load pressure once mechanically polished afterwards；
Preferably, by sequencing is operated, the load pressure in mechanical polishing process reduces in gradient；
Preferably, the load pressure of mechanical polishing is 20-30N for the first time, and the load pressure of last time mechanical polishing is 5N；
Preferably, mechanical polishing includes mechanically polishing for the first time, and the condition of mechanical polishing includes: the rotation of polishing tool for the first time
Speed is 120-180rpm, and the rotation speed of clamping head is 120-180rpm, load pressure 20-30N, first time polishing time
For 1.5-2.5min；
Preferably, the rotation speed of polishing tool described in first time polishing process is 150rpm, and clamping head rotation speed is
150rpm, load pressure 25N, first time polishing time are 2.3min；
Preferably, the clamping head is identical as the direction of rotation of the polishing tool；
Preferably, polishing is carried out using wool plain fabric polishing disk for the first time；
Preferably, being added in first time polishing process has third cooling lubricant；More preferably, the third cooling lubricant includes
Suspension containing SiC particulate；More preferably, the partial size of SiC particulate is 2-4 μm, more preferably, the suspension in the suspension
The partial size of middle SiC particulate is 3 μm.
6. preparation method according to claim 5, which is characterized in that mechanical polishing further includes second of mechanical polishing, the
The condition of secondary mechanical polishing includes: that polishing tool rotation speed is 120-180rpm, and clamping head rotation speed is 120-
180rpm, load pressure 10-20N, second of polishing time is 1.5-2.5min；
Preferably, in second of polishing process, the rotation speed of the polishing tool is 150rpm, and the rotation speed of clamping head is
150rpm, load pressure 15N, second of polishing time is 2min；
Preferably, the clamping head is identical as the direction of rotation of the polishing tool；
Preferably, second of polishing is carried out using synthesis short wool suede polishing disk；
Preferably, being added in second of polishing process has the 4th cooling lubricant；More preferably, the 4th cooling lubricant includes
Suspension containing SiC particulate；More preferably, the partial size of SiC particulate is 0.8-1 μm, more preferably, the suspension in the suspension
The partial size of SiC particulate is 0.9 μm in liquid.
7. preparation method according to claim 6, which is characterized in that mechanical polishing further includes that third time mechanically polishes, the
The condition mechanically polished three times includes: that the rotation speed of polishing tool is 120-180rpm, and the rotation speed of clamping head is 120-
180rpm, load pressure 5-10N, third time polishing time are 1-2min；
Preferably, in third time polishing process, the rotation speed of the polishing tool is 150rpm, and the rotation speed of clamping head is
150rpm, load pressure 10N, third time polishing time are 1.5min；
Preferably, the clamping head is identical as the direction of rotation of the polishing tool；
Preferably, third time polishing is carried out using synthesis short wool suede polishing disk；
Preferably, being added in third time polishing process has the 5th cooling lubricant；More preferably, the 5th cooling lubricant includes
Suspension containing SiC particulate；More preferably, the partial size of SiC particulate is 0.8-1 μm, more preferably, the suspension in the suspension
The partial size of SiC particulate is 0.9 μm in liquid.
8. preparation method according to claim 7, which is characterized in that mechanical polishing further includes the 4th mechanical polishing, the
The condition of four mechanical polishinges includes: that the rotation speed of polishing tool is 120-180rpm, and the rotation speed of clamping head is 120-
180rpm, load pressure 5N, the 4th polishing time are 1-2min；
Preferably, in the 4th polishing process, the rotation speed of the polishing tool is 150rpm, and the rotation speed of clamping head is
150rpm, load pressure 5N, the 4th polishing time are 1.5min；
Preferably, the clamping head is identical as the direction of rotation of the polishing tool；
Preferably, the 4th polishing is carried out using synthesis short wool suede polishing disk；
Preferably, being added in the 4th polishing process has the 6th cooling lubricant；More preferably, the 6th cooling lubricant includes
Suspension containing SiC particulate；More preferably, the partial size of SiC particulate is 0.8-1 μm, more preferably, the suspension in the suspension
The partial size of SiC particulate is 0.9 μm in liquid.
9. preparation method according to claim 2, which is characterized in that ion polishing includes: to be removed using ion sputtering method
The deformation layer remained on surface of sample to be processed after going mechanical polishing；
Preferably, the time of ion polishing is 50-70min, preferably 60min；
Preferably, ion gun used in ion polishing and sample stage angle are in 5.5-6.5 °, and more excellent is 6 °；
It preferably, further include removing described cold to inlay agent to expose whole metallic matrixes before ion polishing.
10. a kind of for characterizing the sample of increasing material manufacturing non-ferrous metal performance, which is characterized in that by any one of claim 1 to 9
The preparation method is prepared；
The region remnants to be measured preparation stressor layers of the sample are with a thickness of 0.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112730484A (en) * | 2020-12-22 | 2021-04-30 | 广东省科学院新材料研究所 | Diamond film sample and preparation method and application thereof |
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2019
- 2019-07-02 CN CN201910588363.4A patent/CN110286012A/en active Pending
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| 吴小盼: "CuCoCrFeNi高熵合金激光焊接性研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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| CN112730484A (en) * | 2020-12-22 | 2021-04-30 | 广东省科学院新材料研究所 | Diamond film sample and preparation method and application thereof |
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