CN106596214A - Efficient preparation method of high purity aluminum gold-phase sample - Google Patents
Efficient preparation method of high purity aluminum gold-phase sample Download PDFInfo
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- CN106596214A CN106596214A CN201610932032.4A CN201610932032A CN106596214A CN 106596214 A CN106596214 A CN 106596214A CN 201610932032 A CN201610932032 A CN 201610932032A CN 106596214 A CN106596214 A CN 106596214A
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- sample
- polishing
- metallographic
- rafifinal
- preparation
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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
-
- 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
-
- 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
- G01N1/32—Polishing; Etching
-
- 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
- G01N2001/2873—Cutting or cleaving
Abstract
The invention relates to the technical field of preparation of gold-phase samples, in particular to an efficient preparation method of a high purity aluminum gold-phase sample. The preparation method comprises the steps of sampling, coarse grinding, precision grinding, electrolytic polishing, mechanical polishing, electrolytic polishing and chemical etching. According to the technical scheme, the preparation method of the gold-phase sample is achieved by combining mechanical polishing with electrolytic polishing and then conducting chemical etching, the technical scheme is short in time, simple, efficient and free of requirements on the preparation environment temperature, the polishing effect of the gold-phase sample and the working environment of operators can be effectively improved, no grind surface scratch is generated, grain boundary corrosion is clear, and the method is convenient, practical and suitable for further application and popularization.
Description
Technical field
The present invention relates to the preparing technical field of metallographic sample, more particularly, it relates to a kind of rafifinal metallographic sample
High efficiency preparation method.
Background technology
The material properties such as the organizational structure inside metal material and intensity, hardness, ductility have it is close contact, metallographic
Observation is to research and analyse the maximally efficient direct method of metal material internal organizational structure, and metallographic refers to the chemistry of metal or alloy
The physical state and chemical state of composition and various composition inside metal or alloy.
Metallographic observation is carried out, first has to make the crystal boundary structure of metal to show, then with metallography microscope sem observation metallographic
Tissue, crystal boundary is that structure is identical and the section that is orientated between different crystal grain, namely the contact surface between crystal grain and crystal grain.It is high-purity
Aluminum and aluminium and the aluminium alloy containing a small amount of alloying element, this class material is either processed or annealed condition, due to its material spy
Point and low hardness, are easy to leave cut during prepared by sample, and metallographic preparation process and display are all more difficult.I.e.
Make to be to corrode out its tissue to also tend to the incomplete of display；Especially purity is miscellaneous 99.999% and its rafifinal of the above
Matter is few, and forming core is difficult, and metallographic can be made to show that crystal boundary is imperfect, or even can not differentiate crystal boundary.
It is in the prior art, general as a example by metallographic observation for use as the rafifinal (purity is 99.999%) of target
Method is：From correct position on aluminum target a part is cut as sample；Sand paper grinding, flannelette are carried out successively to described sample
Mechanical polishing/electrobrightening, chemical etching/electro-etching；Then the metallographic structure using metallurgical microscope to the sample is entered
Row observation.In the past few decades, there are many researchs with regard to metallographic, but the research of the metallographic of high pure metal is less.For
The heterogeneous microstructure of research high pure metal, have also been made both at home and abroad the research of some related metallographics, such as Chinese patent application, Shen
Please number：201310720695.6, denomination of invention：A kind of rafifinal metallographic specimen preparation method, proposes to be thrown using grinding-electrolysis
The preparation method of optical-electronic solution overlay film.In all kinds of preparation methoies, the problem that presently, there are is that electrolysis time is longer, is polished and rotten
Electrolysis installation is all used in erosion, and the time of worker exposure's chemical reagent is relatively long, there is potential safety hazard, operation inconvenience；Corrosion
Time is longer, and work efficiency is relatively low；Grain surface has cut, and grain boundary corrosion is unintelligible.For the problems referred to above, exploitation is a kind of high-purity
The high efficiency preparation method of aluminum metallographic sample is those skilled in the art's technical problem urgently to be resolved hurrily.
The content of the invention
The technical problem to be solved is：The technical problem mentioned in overcome above-mentioned background technology, now provides
A kind of work efficiency is higher, grain boundary corrosion clearly rafifinal preparation method of metallographic sample.
The technical solution adopted for the present invention to solve the technical problems is：A kind of efficient preparation side of rafifinal metallographic sample
Method, the method comprises the steps：
(1) sampling is sampled using saw blade hand sample or Water Cutting, and range estimation makes sample facet regular and smooth；Will
The sample test face of asking is vertical with side, and size is easy to grind away；
(2) corase grind is ground off the burr of each corner of sample and saw kerf face with water mill coarse sandpaper in the scaife of polished machine；
(3) fine grinding grinds the silicon carbide paper that step (2) gained sample is gradually reduced successively with granularity；
(4) electrobrightening
The sample that step (3) has been refined is connected with polishing instrument positive source, and iron plate is connected with polishing instrument power cathode, will
Sample and iron plate are put in the electrolytic polishing liquid for preparing simultaneously, and polishing voltage is 20 ± 2V, and polishing time is 20-30s, electrolysis
Sample is rinsed successively with water and ethanol after polishing, is rapidly dried up flour milling with hair-dryer；
(5) antiscuffing paste is applied in after step (4) gained sample surfaces and is polished on buffing machine by mechanical polishing, until sample
Product surface is smooth and forms angle with the front cut direction of polishing without direction till fine scratches, is polished；
(6) electrobrightening
The sample that step (5) has been mechanically polished with polishing instrument power supply positive pole be connected, iron plate with polish instrument power cathode
Connection, sample and iron plate are put in the electrolytic polishing liquid for preparing simultaneously, and polishing voltage is 20 ± 2V, and polishing time is 20-
30s, sample is rinsed successively after electrobrightening with water and ethanol, is rapidly dried up flour milling with hair-dryer；
(7) chemical etching
The good sample of step (6) electrobrightening is put in the etchant for preparing according to the mode that test is faced upwards and is soaked
Erosion, taking-up after etch is finished rinsed well with water, then with alcohol washes, hair-dryer dries up rapidly, is put into culture dish and treats that metallographic is examined
Survey；The etch time is 40-80s.
Further, in above-mentioned technical proposal, the rotating speed of the polished machine in the step (2) and step (3) is 500-
1000r/min, the rotating speed of buffing machine is 500-1000r/min in step (5)；Water mill coarse sandpaper is 150# in the step (2)
Carborundum；Silicon carbide paper is followed successively by 600#, 1000#, 2000#, 2500# carborundum paper in step (3).
Further, in above-mentioned technical proposal, the composition and volume ratio of polishing fluid formula is in the step (4)：Anhydrous second
Alcohol：Perchloric acid=(93-97):5；Antiscuffing paste is w2.5 types in step (5)；In the step (6) composition of polishing fluid formula and
Volume ratio is：Dehydrated alcohol：Perchloric acid=(93-97):5；The composition and volume ratio of etchant is in step (7)：Pure water:Hydrogen
Fluoric acid=50:(45-55).
Beneficial effect：Compared with prior art, the technical scheme is that a kind of will mechanical polishing and electrobrightening knot
Altogether, the metallographic specimen preparation method of chemical etching is then carried out again, technical scheme innovative point is that the consuming time is shorter, letter
It is single efficiently to preparing ambient temperature no requirement (NR), the polishing effect of metallographic specimen and the working environment of operator to be effectively improved,
Without flour milling cut, grain boundary corrosion is more clear, convenient and practical, suitable further genralrlization application.
Description of the drawings
Fig. 1 show the metallographic spectrogram obtained by the preparation method using embodiment one；
Fig. 2 show the metallographic spectrogram obtained by the preparation method using embodiment two.
Specific embodiment
With reference to embodiment, the present invention is further described, and the full content of the composition represented by example below is not limited
Necessary to the solution as the invention described in claim.
Embodiment one
A kind of high efficiency preparation method of rafifinal metallographic sample, the method comprises the steps：
(1) sampling is sampled using Water Cutting, and range estimation makes sample facet regular and smooth；Sample Width is to be tested
Sheet metal thickness, thickness of sample about 7mm, height of specimen about 10mm；
(2) corase grind is ground off the burr of each corner of sample and saw kerf face with water mill coarse sandpaper in the scaife of polished machine；
(3) fine grinding grinds the silicon carbide paper that step (2) gained sample is gradually reduced successively with fineness；
(4) sample that electrobrightening has refined step (3) is connected with polishing instrument positive source, and iron plate is electric with polishing instrument
Source negative pole connection, sample and iron plate are put in the electrolytic polishing liquid for preparing simultaneously, and polishing voltage is 20V, and polishing time is
20s, sample is rinsed successively after electrobrightening with water and ethanol, is rapidly dried up flour milling with hair-dryer；
(5) antiscuffing paste is applied in after step (4) gained sample surfaces and is polished on buffing machine by mechanical polishing, until sample
Product surface is smooth and forms 45 ° of angle with the front cut direction of polishing without direction till fine scratches, is polished；
(6) electrobrightening
The sample that step (5) has been mechanically polished with polishing instrument power supply positive pole be connected, iron plate with polish instrument power cathode
Connection, sample and iron plate are put in the electrolytic polishing liquid for preparing simultaneously, and polishing voltage is 20V, and polishing time is 20s, electricity
Sample is rinsed successively with water and ethanol after solution polishing, is rapidly dried up flour milling with hair-dryer；
(7) chemical etching
The good sample of step (6) electrobrightening is put in the etchant for preparing according to the mode that test is faced upwards and is soaked
Erosion, taking-up after etch is finished rinsed well with water, then with alcohol washes, hair-dryer dries up rapidly, is put into culture dish and treats that metallographic is examined
Survey；The etch time is 40s.
In above-mentioned technical proposal, the rotating speed of the polished machine in the step (2) and step (3) is 950r/min, step
(5) rotating speed of buffing machine is 800r/min in；Water mill coarse sandpaper is 150# carborundums in the step (2)；Water mill in step (3)
Sand paper is followed successively by 600#, 1000#, 2000#, 2500# carborundum paper；The composition and body of polishing fluid formula in the step (4)
Accumulating ratio is：Dehydrated alcohol：Perchloric acid=95:5；Antiscuffing paste is w2.5 types in step (5)；Polishing fluid formula in the step (6)
Composition and volume ratio be：Dehydrated alcohol：Perchloric acid=95:5；The composition and volume ratio of etchant is in step (7)：It is pure
Water:Fluohydric acid .=50:50.
Embodiment two
The preparation that the step of the present embodiment applicant adopts above-described embodiment one (1), (2), (3), (4), (5), (7) are formed
Method.
By using the method for above-described embodiment one and embodiment two gained sample collecting fractograph, as a result such as the He of accompanying drawing 1
Shown in accompanying drawing 2, from accompanying drawing 1 and accompanying drawing 2, there is obvious cut in accompanying drawing 2, can using the high efficiency preparation method of the present invention
Obtain preferable collection of illustrative plates effect.
In addition, doing within one day 100 calculating of metallographic sample according to 1 people, 1 complete equipment, the time of front 3 step similar operations is removed,
The patent of Application No. 201310720695.6：4th, 5 one-step electrolysis add overlay film time be 250-450s, time most short needs
250*100/ (60*60)=7h, most long 450*100/ (60*60)=12.5h, that is, need 7h-12.5h, along with corase grind, essence
Mill, mechanical polishing and the time for preparing, sample preparation is far longer than the 8h working times total time.Efficiency is low, meanwhile, staff's length
Time contacts electrolyte, the overlay film liquid of strong acid, serious to body harm；In the present invention, the time being electrolysed twice is 40-60s, and
Chemical etching once (can be negligible all samples together etch), then prepare 100 samples, electrolysis plus chemistry
The time of etch is most short for 40*100/ (60*60)=1h, up to 60*100/ (60*60)=1.7h, chemical etching it is most short
Time be (5 samples corrode together, totally 20 times), 40*20/ (60*60)=0.2h, maximum duration be 80*20/ (60*60)=
0.4h, i.e. total time are 1.2h-2.1h, therefore, work efficiency can be significantly improved using the method for the present invention, shorten working hours
(being up to 12.5/1.2=10.4 times), simultaneously because with electrobrightening twice, the requirement to mechanically polishing is reduced, to the people that works
The body harm of member is substantially reduced, suitable further genralrlization application.
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or using the present invention.
Various modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope for causing.
Claims (7)
1. a kind of high efficiency preparation method of rafifinal metallographic sample, it is characterised in that：The method comprises the steps：
(1) sample
Sampled using Water Cutting, range estimation makes sample facet regular and smooth；
(2) roughly grind
In the scaife of polished machine the burr of each corner of sample and saw kerf face is ground off with water mill coarse sandpaper；
(3) refine
The silicon carbide paper that step (2) gained sample is gradually reduced successively with granularity is ground；
(4) electrobrightening
The sample that step (3) has been refined is connected with polishing instrument positive source, and iron plate is connected with polishing instrument power cathode, by sample
It is put in the electrolytic polishing liquid for preparing simultaneously with iron plate, polishing voltage is 20 ± 2V, polishing time is 20-30s, electrobrightening
Afterwards sample is rinsed successively with water and ethanol, rapidly dried up flour milling with hair-dryer；
(5) mechanically polish
Antiscuffing paste is applied in after step (4) gained sample surfaces and is polished on buffing machine, until sample surfaces are smooth and do not have
Till fine scratches, polishing direction forms angle with the front cut direction of polishing；
(6) electrobrightening
The sample that step (5) has been mechanically polished is connected with the positive pole of polishing instrument power supply, and iron plate is connected with polishing instrument power cathode,
Sample and iron plate are put in the electrolytic polishing liquid for preparing simultaneously, polishing voltage is 20 ± 2V, and polishing time is 20-30s, electricity
Sample is rinsed successively with water and ethanol after solution polishing, is rapidly dried up flour milling with hair-dryer；
(7) chemical etching
The good sample of step (6) electrobrightening is put into into etch in the etchant for preparing according to the mode that test is faced upwards, is soaked
Taking-up after erosion is finished is rinsed well with water, then with alcohol washes, hair-dryer is dried up rapidly, is put into culture dish and is treated that metallographic is detected；Institute
The etch time is stated for 40-80s.
2. a kind of high efficiency preparation method of rafifinal metallographic sample as claimed in claim 1, it is characterised in that：The step
(2) rotating speed of the polished machine and in step (3) is 500-1000r/min, and the rotating speed of buffing machine is 500- in step (5)
1000r/min。
3. a kind of high efficiency preparation method of rafifinal metallographic sample as claimed in claim 1, it is characterised in that：The step
(2) water mill coarse sandpaper is 150# carborundums in；Silicon carbide paper is followed successively by 600#, 1000#, 2000#, 2500# carbonization in step (3)
Silica sand paper.
4. a kind of high efficiency preparation method of rafifinal metallographic sample as claimed in claim 1, it is characterised in that：The step
(4) composition and volume ratio of polishing fluid formula is in：Dehydrated alcohol：Perchloric acid=(93-97):5.
5. a kind of high efficiency preparation method of rafifinal metallographic sample as claimed in claim 1, it is characterised in that：The step
(5) antiscuffing paste is w2.5 types in.
6. a kind of high efficiency preparation method of rafifinal metallographic sample as claimed in claim 1, it is characterised in that：The step
(6) composition and volume ratio of polishing fluid formula is in：Dehydrated alcohol：Perchloric acid=(93-97):5.
7. a kind of high efficiency preparation method of rafifinal metallographic sample as claimed in claim 1, it is characterised in that：The step
(7) composition and volume ratio of etchant is in：Pure water:Fluohydric acid .=50:(45-55).
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109187128A (en) * | 2018-09-11 | 2019-01-11 | 包头钢铁（集团）有限责任公司 | The preparation method of sample |
| CN109839393A (en) * | 2019-03-22 | 2019-06-04 | 南京理工大学 | Slicker solder and its composite material or its alloy electron backscatter diffraction sample preparation technique |
| CN111024697A (en) * | 2019-12-18 | 2020-04-17 | 新疆众和股份有限公司 | Preparation method of 6061 aluminum alloy metallographic specimen |
| CN111185854A (en) * | 2020-01-20 | 2020-05-22 | 武汉科技大学 | Spark spectrum analysis surface water jet cutting method |
| CN111650024A (en) * | 2020-05-27 | 2020-09-11 | 西安泰力松新材料股份有限公司 | Tinned copper wire/strip metallographic etchant and metallographic structure sample preparation method |
| CN112014195A (en) * | 2020-07-20 | 2020-12-01 | 新疆众和股份有限公司 | Erosion liquid for high-purity aluminum macrostructure detection and method thereof |
| CN112485084A (en) * | 2020-11-20 | 2021-03-12 | 先导薄膜材料（广东）有限公司 | Method for displaying high-purity aluminum-gold phase |
| CN112945676A (en) * | 2021-03-22 | 2021-06-11 | 西安交通大学 | Method for preparing pure aluminum metallographic sample by dielectric barrier discharge technology |
| CN113514311A (en) * | 2021-06-01 | 2021-10-19 | 先导薄膜材料有限公司 | Display method of pure tin metallographic phase |
| CN113866200A (en) * | 2021-09-29 | 2021-12-31 | 广西容创新材料产业研究院有限公司 | Preparation method of segregation-method high-purity aluminum EBSD sample |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109187128A (en) * | 2018-09-11 | 2019-01-11 | 包头钢铁（集团）有限责任公司 | The preparation method of sample |
| CN109839393A (en) * | 2019-03-22 | 2019-06-04 | 南京理工大学 | Slicker solder and its composite material or its alloy electron backscatter diffraction sample preparation technique |
| CN111024697A (en) * | 2019-12-18 | 2020-04-17 | 新疆众和股份有限公司 | Preparation method of 6061 aluminum alloy metallographic specimen |
| CN111185854A (en) * | 2020-01-20 | 2020-05-22 | 武汉科技大学 | Spark spectrum analysis surface water jet cutting method |
| CN111650024A (en) * | 2020-05-27 | 2020-09-11 | 西安泰力松新材料股份有限公司 | Tinned copper wire/strip metallographic etchant and metallographic structure sample preparation method |
| CN112014195A (en) * | 2020-07-20 | 2020-12-01 | 新疆众和股份有限公司 | Erosion liquid for high-purity aluminum macrostructure detection and method thereof |
| CN112485084A (en) * | 2020-11-20 | 2021-03-12 | 先导薄膜材料（广东）有限公司 | Method for displaying high-purity aluminum-gold phase |
| CN112945676A (en) * | 2021-03-22 | 2021-06-11 | 西安交通大学 | Method for preparing pure aluminum metallographic sample by dielectric barrier discharge technology |
| CN113514311A (en) * | 2021-06-01 | 2021-10-19 | 先导薄膜材料有限公司 | Display method of pure tin metallographic phase |
| CN113866200A (en) * | 2021-09-29 | 2021-12-31 | 广西容创新材料产业研究院有限公司 | Preparation method of segregation-method high-purity aluminum EBSD sample |
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Application publication date: 20170426 |