CN107228870A - A kind of cemented carbide powder EBSD method for making sample - Google Patents
A kind of cemented carbide powder EBSD method for making sample Download PDFInfo
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- CN107228870A CN107228870A CN201710414677.3A CN201710414677A CN107228870A CN 107228870 A CN107228870 A CN 107228870A CN 201710414677 A CN201710414677 A CN 201710414677A CN 107228870 A CN107228870 A CN 107228870A
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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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- 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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- 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
- G01N1/32—Polishing; Etching
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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
- G01N1/38—Diluting, dispersing or mixing samples
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
- G01N23/203—Measuring back scattering
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/053—Investigating materials by wave or particle radiation by diffraction, scatter or reflection back scatter
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
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- G01N2223/312—Accessories, mechanical or electrical features powder preparation
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Abstract
The invention discloses a kind of cemented carbide powder EBSD method for making sample, including powder sample mix, it is compressing, sinter, inlay, grind and polish and sample cleaning.The present invention is sufficiently mixed hard alloy material powder and Cu powder uniformly; and it is accurate and have and be sintered in the thermal analyzer of protective atmosphere in temperature control; hard alloy material powder is solidified using Cu phases; realize the good dispersion effect of WC raw material granules simultaneously; optimization EBSD grinds and polished the optimal parameter of sample preparation, can obtain good EBSD test results；Experimentation instead of the application of large scale equipment, greatlys save compacting and sintering cost, shortens experimental period.
Description
Technical field
The present invention relates to the EBSD of alloy powder (EBSD) method for making sample, more particularly to a kind of hard alloy
Powder EBSD method for making sample.
Background technology
EBSD technology (EBSD) turns into the new method of testing of crystalline material Micro-Structure Analysis, and wide
It is general to be applied to various crystalline materials, such as metal, ceramics, geology and mineral.EBSD technical methods can show the micro- of material simultaneously
Pattern, structure and distribution of orientations information are seen, and obtains the results such as accurate crystallite dimension, crystal grain orientation, interface feature, texture.
At present, most EBSD research work relate generally to block materials and thin-film material, and on powder (1-100 μm) material
EBSD, which is researched and analysed, has no report, and this prepares relatively difficult mainly due to the EBSD samples of powder body material.
Hard alloy cutter combination property is directly influenceed by WC raw materials, Ball-milling Time, sintering process etc., therefore for WC
Material internal heterogeneous microstructure is analyzed under the different phases such as powder stock, ball milling and sintering, different technology conditions,
Macro-mechanical performance to raising hard alloy cutter is particularly significant.And existing sample preparation and test analysis on EBSD is special
Profit report and documents and materials are generally steel and alloy zone material, and method for making sample is mainly electrobrightening, mechanical polishing, particle beams throwing
Light etc., the academic documents and report in related hard alloy field are relatively fewer, are related to hard alloy WC raw materials and compound powder
EBSD sample preparations be not yet reported that so far.
The content of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art that EBSD technologies are applied successfully there is provided one kind
In the cemented carbide powder EBSD method for making sample of powder body material.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of cemented carbide powder EBSD method for making sample, comprises the following steps：
S1, dispensing：Cemented carbide powder and electrolysis Cu powder are mixed by a certain percentage；
S2, shaping：Mixed powder is compressing, obtain pressure embryo；
S3, sintering：By the sample for pressing embryo to cut into certain size, sample is sintered；
S4, inlay：Sample after sintering is inlayed；
S5, grinding and polishing：Sample after to inlaying is ground and polished；
S6, cleaning：Specimen surface is cleaned.
It is used as the further improvement of above-mentioned technical proposal：
The proportioning of cemented carbide powder and electrolysis Cu powder is weight percentage 1 in the step S1：1.5~1.5：1.
Using mosaicker that mixed powder is compressing in the step S2, pressing pressure is 16KN~20KN, presses embryo diameter
For 25mm~30mm.
The step of being sintered in the step S3 includes：
S31, sample is put into thermal analyzer DSC Al2O3Crucible；
S32, close cavity and to being vacuumized in cavity；
S33, protected using Ar, be rapidly heated with 5K/min~10K/min programming rate to 1050 DEG C, then with 2K/
Min~10K/min programming rate is to slowly warm up to 1100 DEG C~1150 DEG C, then with 2K/min~5K/min cooling rate
It is cooled to 1050 DEG C；
S34, Temperature fall.
In the step S4, the sample sintered is put into mosaicker, amount of conductive resin is dosed and inlays powder, inlayed
It is embedding, inlay a diameter of 25mm~30mm.
The step of grinding and polish in the step S5 includes：
S51, sample top layer is quickly removed using diamond disk；
S52, successively select 9 μm~1 μm polishing cloth polish step by step, until specimen surface it is smooth, without fine scratches.
The step of being cleaned in the step S6 includes：
S61, specimen surface is cleaned multiple times using cleaning agent manually；
S62, cleaned with alcohol and deionized water ultrasonic activation.
The cemented carbide powder is WC material powders.
In the step S3, the size of sample is 3mm~10mm.
Compared with prior art, the advantage of the invention is that：
(1) cemented carbide powder EBSD method for making sample of the invention, realizes EBSD technologies and is successfully applied to powder body material,
From electrolysis Cu powder as dispersed phase, the effect that hard alloy material granule spreads out is reached.
(2) cemented carbide powder EBSD method for making sample of the invention, holds the ratio of Cu powder and hard alloy raw material powder body,
While ensureing that hard alloy material powder granule dispersion effect is good, hard alloy in EBSD gathered datas visual field in turn ensure that
The quantity of material powder granule.
(3) cemented carbide powder EBSD method for making sample of the invention, be widely used in 1 micron it is hard to some tens of pm granularity
Matter alloy raw material powder sample.
(4) cemented carbide powder EBSD method for making sample of the invention, method for making sample is convenient, remove from large scale equipment application and
Device parameter gropes work, cost-effective, and test repeatability is high, easily realizes；First, application conventional metallographic equipment mosaicker generation
For large powder press equipment, and the pressing parameter of hard alloy material powder and Cu powder compounds need not be groped, save equipment
Cost and test period；Second, it is accurate and have the thermal analyzer equipment of protective atmosphere using temperature control, test and burn instead of large-scale vacuum
Freezing of a furnace, saves sintering cost and experimental period.
Brief description of the drawings
The sample that Fig. 1 is the present invention uses ESEM and EBSD comparative result figures (multiplying power 4000X).
The sample that Fig. 2 is the present invention uses ESEM and EBSD comparative result figures (multiplying power 8000X).
Embodiment
The present invention is described in further detail below in conjunction with Figure of description and specific embodiment.
The cemented carbide powder EBSD method for making sample of the present invention, comprises the following steps：
S1, dispensing：Cemented carbide powder and electrolysis Cu powder are mixed by a certain percentage；
S2, shaping：Mixed powder is compressing, obtain pressure embryo；
S3, sintering：By the sample for pressing embryo to cut into certain size, sample is sintered；
S4, inlay：Sample after sintering is inlayed；
S5, grinding and polishing：Sample after to inlaying is ground and polished；
S6, cleaning：Specimen surface is cleaned.
In above-mentioned steps S1, applying electronic balance weighs hard alloy material powder (1 μm~100 μm) and Cu powder, is
Reach that hard alloy material powder granule spreads out in Cu phases and keeps visual field area ratio/occupancy ratio, hard alloy material powder
It is 1.5 with being electrolysed the percentage by weight of Cu powder:1~1:1.5, then grinding is sufficiently mixed.
Using mosaicker that mixed powder is compressing in above-mentioned steps S2, pressing pressure is 16KN~20KN, and pressure embryo is straight
Footpath is 25mm~30mm.Here the conventional metallographic equipment mosaicker of application replaces large powder press equipment, and need not grope hard
The pressing parameter of alloy raw material powder and Cu powder compounds, saves equipment cost and test period.
In above-mentioned steps S3, pressure embryo is taken out and about 3mm~10mm blocks are cut, STA449F3 thermal analyzers are put into
DSC Al2O3It is sintered, includes the step of sintering in crucible：
S31, sample is put into thermal analyzer DSC Al2O3 crucibles；
S32, close cavity and to being vacuumized in cavity；
S33, protected using Ar, be rapidly heated with 5K/min~10K/min programming rate to 1050 DEG C, then with 2K/
Min~10K/min programming rate is to slowly warm up to 1100 DEG C~1150 DEG C, then with 2K/min~5K/min cooling rate
It is cooled to 1050 DEG C；1100 DEG C~1150 DEG C be higher than copper 1084 DEG C of fusing point, and at 1150 DEG C not with cemented carbide powder
WC, Co etc. chemically react, it is ensured that Cu phases melt and immersed between WC granules, WC granules is spread out；This method
It is accurate and have the thermal analyzer equipment of protective atmosphere using temperature control, sintering furnace is tested instead of large-scale vacuum, sintering cost has been saved,
Shorten experimental period；
S34, Temperature fall.
In above-mentioned steps S4, the sample sintered is put into mosaicker, amount of conductive resin is dosed and inlays powder, inlayed
It is embedding, inlay a diameter of 25mm~30mm.
In above-mentioned steps S5, using the special grinding and polishing apparatus of EBSD sample preparations and the special consumptive materials of EBSD, the step of grinding and polish
Including：
S51, sample top layer is quickly removed using diamond disk；
S52, successively select 9 μm~1 μm polishing cloth polish step by step, until specimen surface it is smooth, without fine scratches.Consider
Cu phases and hard alloy phase mechanical property difference great disparity, sample preparation using slow-speed of revolution 180r/min~150r/min, small pressure 30N~
15N weakens step by step, and each step grinding and polishing set of time is 3min~10min.
Include in above-mentioned steps S6, the step of cleaning：
S61, specimen surface is cleaned multiple times using cleaning agent manually：The conscientious various impurity that thoroughly clean surface is stained with,
Such as abrasive particle, polishing suspension other compositions, paraffin wax lubricants, edge sample powder, alloyed powder, examination is cleaned multiple times using cleaning agent manually
Sample surface；
S62, cleaned with alcohol and deionized water ultrasonic activation：Cleaned with absolute alcohol ultrasonic activation 2min~
5min.Finally cleaned with deionized water, and surface is dried with hair-dryer.
In concrete application example, after step S6, in addition to sample is fixed, the step that sample is fixed is：Will
Sample is placed on EBSD and fixed on sample stage, fixes sample by screws clamp, sample finally is put into SEM
(SEM), debugging tilts sample stage, setup test manually.
Embodiment
Cemented carbide powder chooses 5 μm of WC material powder samples, system by taking 5 μm of WC material powders as an example in the present embodiment
Standby EBSD samples are simultaneously tested, and as a result as depicted in figs. 1 and 2, are concretely comprised the following steps：
Dispensing：Applying electronic balance by weight percentage 1:1 weighs 5 μm of WC material powders and the analysis electrolysis of 200 mesh respectively
Cu powder (Ke Miou reagents) each 10g, and it is fully ground mixing 30min in mortar.
It is compressing：It is using Struer Citopress-1 mosaickers that the WC/Cu mixed powders matched is compressing, pressure
Pressing pressure about 20KN, a diameter of 25mm of pressure embryo.
Sintering：From the block of cut lengths about 3mm on compacting pressure embryo, thermal analyzer DSC Al are put into2O3In crucible, then
It is put on STA449F3 thermal analyzer supports, closes cavity.Vacuumize, then protected using Ar, with 10K/min in cavity first
Programming rate rise to 1050 DEG C, then rise to 1150 DEG C with 5K/min speed, then 1050 DEG C are cooled to 5K/min, finally
End program Temperature fall.
Inlay：The coupon sintered is put into Struer citopress-1 mosaickers, appropriate polyfast is dosed and leads
Electric resin inlays powder, is inlayed, a diameter of 25mm.
Grinding and polishing：The sample inlayed is ground on the full-automatic grinding and polishing apparatus of Struer Tegramin-25 and
Polishing, prepares EBSD samples, it is contemplated that the performance difference of WC material powders and Cu powder, and sample preparation parameter and program set such as table 1 below
It is shown, the different types of grinding fluid of mill correspondence of different model.
Table 1
Sample is cleaned：Specimen surface is cleaned multiple times using cleaning agent manually, then alcohol ultrasonic activation cleaning 3min, and
Cleaned with deionized water, last hair-dryer dries up surface.
Sample is fixed：Specimen size is inlayed in consideration and weight is larger, and sample is placed on into EBSD fixes sample stage (inside straight
Footpath φ=25.5mm) on, screws clamp, which is fixed, inlays sample, and sample stage is tilted manually, sample is inclined to 70 ° of angles.Substitution is led
The mode of electric glue adhered test sample, can effectively suppress image drift, the problems such as electron beam is unstable, obtain good experiment effect, most
Sample is put into SEM, setup test afterwards.
Fig. 1 is 5 μm of WC material powder EBSD test results, and multiplying power 4000X, granule dispersion effect is good, in single granule
Portion's crystal boundary is clear：(a) it is scanning electron microscope electron image；(b) for using band contrast figures of the EBSD to sample progress test acquisition
(Band Contrast Map), from (b) it can be seen that clearly crystal boundary inside granule, i.e., netted lines are partitioned into different crystal grain.
Fig. 2 be the single granule EBSD test results of 5 μm of WC material powders, multiplying power 8000X, the agglomerates intragranular portion is by more
Individual monocrystalline composition, crystal boundary is clear, and orientation is clear and definite：(c) scanning electron microscope electron image；(d) it is that sample is tested using EBSD
The band contrast figure (Band Contrast Map) of acquisition, from (d) it can be seen that clearly crystal boundary, netted lines point inside granule
Cut out different crystal grain.
Although the present invention is disclosed above with preferred embodiment, but is not limited to the present invention.It is any to be familiar with ability
The technical staff in domain, in the case where not departing from technical solution of the present invention scope, all using the technology contents pair of the disclosure above
Technical solution of the present invention makes many possible variations and modification, or is revised as the equivalent embodiment of equivalent variations.Therefore, it is every
Without departing from the content of technical solution of the present invention, according to the technology of the present invention essence to any simple modification made for any of the above embodiments,
Equivalent variations and modification, all should fall in the range of technical solution of the present invention protection.
Claims (9)
1. a kind of cemented carbide powder EBSD method for making sample, it is characterised in that comprise the following steps：
S1, dispensing：Cemented carbide powder and electrolysis Cu powder are mixed by a certain percentage；
S2, shaping：Mixed powder is compressing, obtain pressure embryo；
S3, sintering：By the sample for pressing embryo to cut into certain size, sample is sintered；
S4, inlay：Sample after sintering is inlayed；
S5, grinding and polishing：Sample after to inlaying is ground and polished；
S6, cleaning：Specimen surface is cleaned.
2. cemented carbide powder EBSD method for making sample according to claim 1, it is characterised in that in the step S1, firmly
The proportioning of matter alloy powder and electrolysis Cu powder is weight percentage 1:1.5~1.5:1.
3. cemented carbide powder EBSD method for making sample according to claim 1, it is characterised in that in the step S2, adopt
With mosaicker that mixed powder is compressing, pressing pressure is 16KN~20KN, a diameter of 25mm~30mm of pressure embryo.
4. cemented carbide powder EBSD method for making sample according to claim 1, it is characterised in that sintered in the step S3
The step of include：
S31, sample is put into thermal analyzer DSC Al2O3Crucible；
S32, close cavity and to being vacuumized in cavity；
S33, protected using Ar, be rapidly heated with 5K/min~10K/min programming rate to 1050 DEG C, then with 2K/min~
10K/min programming rate is to slowly warm up to 1100 DEG C~1150 DEG C, then is cooled to 2K/min~5K/min cooling rate
1050℃；
S34, Temperature fall.
5. cemented carbide powder EBSD method for making sample according to claim 1, it is characterised in that in the step S4, will
The sample sintered is put into mosaicker, doses amount of conductive resin and inlays powder, inlayed, inlays a diameter of 25mm~30mm.
6. cemented carbide powder EBSD method for making sample according to claim 1, it is characterised in that ground in the step S5
The step of with polishing, includes：
S51, sample top layer is quickly removed using diamond disk；
S52, successively select 9 μm~1 μm polishing cloth polish step by step, until specimen surface it is smooth, without fine scratches.
7. cemented carbide powder EBSD method for making sample according to claim 1, it is characterised in that cleaned in the step S6
The step of include：
S61, specimen surface is cleaned multiple times using cleaning agent manually；
S62, cleaned with alcohol and deionized water ultrasonic activation.
8. the cemented carbide powder EBSD method for making sample according to claim 1 to 7 any one, it is characterised in that described
Cemented carbide powder is WC material powders.
9. the cemented carbide powder EBSD method for making sample according to claim 1 to 7 any one, it is characterised in that described
In step S3, the size of sample is 3mm~10mm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108760782A (en) * | 2018-06-06 | 2018-11-06 | 广东省新材料研究所 | A kind of electron backscatter diffraction sample of column crystal zirconia coating and preparation method thereof |
| CN109030148A (en) * | 2018-07-27 | 2018-12-18 | 中南大学 | A kind of preparation method of iron(-)base powder EBSD detection sample |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108760782A (en) * | 2018-06-06 | 2018-11-06 | 广东省新材料研究所 | A kind of electron backscatter diffraction sample of column crystal zirconia coating and preparation method thereof |
| CN109030148A (en) * | 2018-07-27 | 2018-12-18 | 中南大学 | A kind of preparation method of iron(-)base powder EBSD detection sample |
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