CN108663257A - A kind of metallographic etching agent and method for displaying metallographic structure of Nitinol - Google Patents
A kind of metallographic etching agent and method for displaying metallographic structure of Nitinol Download PDFInfo
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- CN108663257A CN108663257A CN201810415690.5A CN201810415690A CN108663257A CN 108663257 A CN108663257 A CN 108663257A CN 201810415690 A CN201810415690 A CN 201810415690A CN 108663257 A CN108663257 A CN 108663257A
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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
- G01N1/32—Polishing; Etching
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
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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
- 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
- G01N1/34—Purifying; Cleaning
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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
- G01N1/36—Embedding or analogous mounting of 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
- 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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- 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
- G01N1/36—Embedding or analogous mounting of samples
- G01N2001/364—Embedding or analogous mounting of samples using resins, epoxy
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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
- G01N1/36—Embedding or analogous mounting of samples
- G01N2001/366—Moulds; Demoulding
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Abstract
The present invention relates to a kind of metallographic etching agent of Nitinol and method for displaying metallographic structure, compared to the perchloric acid as conventional corrosion agent, nitric acid in the corrosive agent of the present invention is diluted with hydrofluoric acid by a large amount of deionized water, substantially reduce the concentration of nitric acid and hydrofluoric acid in metallographic etching agent, the corrosivity and oxidisability of metallographic etching agent are reduced simultaneously, and the security risks such as health hazard and environmental pollution to operating personnel are preferably minimized；Corrosive agent configuration is simple, and cost is also cheaper, and key is that corrosive effect is good, and the metallographic structure of sample just can be effectively shown after corrosion 40s；Corrode that the metallographic structure is clearly shrewd in the present invention, is conducive to scientific research personnel and more detailed exploratory development is carried out for the structural constituent of Nitinol.In addition method for displaying metallographic structure is simple and convenient, and the metallographic structure of observation is clearly shrewd, is conducive to scientific research personnel and carries out more detailed exploratory development for the structural constituent of Nitinol.
Description
Technical field
The present invention relates to a kind of metallographic etching agent of Nitinol and method for displaying metallographic structure, belong to etching pit technology
Field.
Background technology
Nitinol be studied in current marmem most comprehensively, memory performance is best, the strongest alloy of practicability
Material, its own corrosion resistance protrude, and memory effect is notable, functional reliability is high and certain bioactivity, shows very
Good development prospect, is especially widely used in medical domain.
However the metallographic of Nitinol is not easy to be made, this just brings resistance to the research Optimization Progress of nickel-titanium alloy material
Hinder.Corrosive agent conventional selection currently used for preparing Nitinol metallographic is perchloric acid, but perchloric acid is expensive, and crystalline phase is shown
As a result also more general, and it is great that itself there is strong oxidizing property, strong corrosive and strong oxidizing property to be constituted to environment and human body
Security risk.
Invention content
The purpose of the present invention is to overcome the above shortcomings, and from corrosive agent prepare it is simple, of low cost, environmentally friendly and efficiently
It angularly sets out, provides a kind of metallographic etching agent and method for displaying metallographic structure of Nitinol.
The object of the present invention is achieved like this：
A kind of metallographic etching agent of Nitinol, the corrosive agent ingredient are hydrofluoric acid, nitric acid and deionized water, and each component contains
The volume ratio of amount is 1:2:5, hydrofluoric acid, nitric acid and deionized water are poured into specified containers successively, are stood after uniform stirring, are obtained
Corrosive agent.
A kind of method for displaying metallographic structure of Nitinol, this method are as follows：
1) Nitinol sample is put into above the lower die in pointing machine, the phenolic resin inlay being then filled with covers
Upper mold carries out heating pressurization, is taken out after sample is fully cooled to room temperature after heat preservation；
2) sample inlayed is placed on grinder and passes through multiple sand paper mechanical lapping, then carried out on sand paper manual
Grinding, until the cut of a upper procedure is override, new cut direction is consistent；
3) polishing flannelet is finished changing on turntable, uniformly the upper polishing fluid of sprinkling, then ground sample is placed on polishing cloth
Upper polishing is thrown to surface no marking；Then one piece of new polishing cloth is changed, polishing fluid is uniformly sprayed, repeats above-mentioned polishing step
It is rapid, sample is finally taken out, is dried up after cleaning for use；
4) sample obtained is first put into supersonic wave cleaning machine and is cleaned, taken out later and sample surfaces are blown to water stain-free
；
5) hydrofluoric acid, nitric acid, deionized water are measured respectively with graduated cylinder, pours into specified containers stood after uniform stirring successively
Obtain corrosive agent；
6) the etch time first is set with timer, then grips sample with tweezers, so that it is completely immersed in corrosive agent, press
Timer takes out sample after timer sound；
7) deionized water cleaning sample, cleaned just drying is used to stand；
8) sample after drying is positioned on metallographic microscope objective table, observes its metallographic structure.
The holding temperature of pointing machine is 400 DEG C in step 1), and soaking time is 14 minutes, waits for 20 points after heat preservation again
Clock waits for that sample is completely cooling.
Sample in step 2) on the sand paper of 600,800,1000,1200,1500 mesh successively by carrying out mechanical lapping, so
Hand-ground is carried out on the sand paper of 2500,5000 mesh afterwards, is needed when changing sand paper every time by 90 ° of rotary sample, and grinding every time
After need with clear water rinse sample to remove remained on surface impurity.
Step 3) finishes changing polishing flannelet on turntable, uniformly sprays 0.5 μm of polishing fluid, then ground sample is placed
It is polished on polishing cloth；Then one piece of new polishing cloth is changed, 0.25 μm of polishing fluid is uniformly sprayed.
Sample obtained is first put into supersonic wave cleaning machine and cleans 2 minutes by step 4).
Measure hydrofluoric acid 10ml, nitric acid 20ml in step 5) respectively with graduated cylinder, deionized water 50ml pours into specified appearance successively
It in device, is stood after uniform stirring, obtains corrosive agent.
Step 6) Timer sets 40 seconds etch time.
The scavenging period of step 7) deionized water cleaning sample is 1 minute.
The display multiple of metallographic microscope in step 8) is in 400X.
Compared with prior art, the beneficial effects of the invention are as follows：
The metallographic etching agent and method for displaying metallographic structure of a kind of this Nitinol are compared to the height as conventional corrosion agent
Chloric acid, the nitric acid in corrosive agent of the invention are diluted with hydrofluoric acid by a large amount of deionized water, substantially reduce metallographic etching agent
The concentration of middle nitric acid and hydrofluoric acid, while the corrosivity and oxidisability of metallographic etching agent are reduced, it endangers to the health of operating personnel
The security risks such as evil and environmental pollution are preferably minimized；Corrosive agent configuration is simple, and cost is also cheaper, and key is corrosive effect
Well, the metallographic structure of sample just can be effectively shown after corrosion 40s；It is clearly bright to corrode the metallographic structure in the present invention
It distinguishes, is conducive to scientific research personnel and more detailed exploratory development is carried out for the structural constituent of Nitinol.In addition metallographic structure is aobvious
Show that method is simple and convenient, the metallographic structure of observation is clearly shrewd, be conducive to scientific research personnel for Nitinol structural constituent into
The more detailed exploratory development of row.
Description of the drawings
Fig. 1 is a kind of metallographic etching agent of Nitinol of the present invention and the flow diagram of method for displaying metallographic structure.
Fig. 2 handles the Nitinol sample crystalline phase organization chart of gained with general corrosion agent (perchloric acid).
Fig. 3 is the metallographic structure figure of sample surfaces in the present invention.
Specific implementation mode
The present invention relates to a kind of metallographic etching agent of Nitinol and method for displaying metallographic structure, this Nitinol sample
Method for displaying metallographic structure uses following corrosive agent and its technique.
Referring to Fig. 1 to Fig. 3, a method for displaying metallographic structure of Nitinol is as follows：
1, Nitinol sample is put into above the lower die in pointing machine, is then filled with suitable phenolic resin inlay,
Upper mold is covered, heating pressurization is carried out, holding temperature is 400 DEG C, and soaking time is 14 minutes, waits for 20 points after heat preservation again
Clock takes out after sample is fully cooled to room temperature.
2, the sample inlayed is placed on to the sand paper machine for passing through 600,800,1000,1200,1500 mesh on grinder successively
Tool is ground, and is then carried out hand-ground on the sand paper of 2500,5000 mesh, is needed when changing sand paper every time by 90 ° of rotary sample, directly
To the cut of a upper procedure is override, new cut direction is consistent, and need after grinding every time with clear water rinse sample with
Remove remained on surface impurity.
3, polishing flannelet is finished changing on turntable, uniformly sprays 0.5 μm of polishing fluid, then ground sample is placed on throwing
It is polished on light cloth, rotary speed is 150 revs/min, is thrown to surface no marking；Then one piece of new polishing cloth is changed, is uniformly sprayed
0.25 μm of polishing fluid is spilt, above-mentioned polishing step is repeated, finally takes out sample, is dried up after cleaning for use.
4, sample obtained is first put into supersonic wave cleaning machine and is cleaned 2 minutes, taking-up later dries rifle with ion and is blown to sample
Product surface water stain-free.
5, hydrofluoric acid 10ml, nitric acid 20ml are measured respectively with graduated cylinder, deionized water 50ml is poured into specified containers successively,
It is stood after even stirring, obtains corrosive agent.
6,40 seconds etch time first is set with timer, then grips sample with tweezers, it is made to be completely immersed in corrosive agent,
It presses timer and takes out sample after timer sound.
7, with deionized water cleaning sample, scavenging period 1 minute is stood after drying.
8, the sample after drying is positioned on metallographic microscope objective table, its metallographic structure is observed at 400X, Fig. 1 is
With the Nitinol sample of general corrosion agent processing gained, Fig. 2 is with the sample obtained by the present invention, and Fig. 2 comes with respect to Fig. 1
It says, the crystalline phase in Nitinol is more easy to distinguish, sample tissue is clearly shrewd, and crystal boundary is clearly demarcated；Thus deduce, using NiTi of the present invention
Microstructure of the alloy corrosive agent, Crystallization Phases that will not be in excessive corrosion alloy, and can fast and efficiently corrode the metallographic group for sample
It knits, is conducive to the quality for evaluating Nitinol product.
The configuration of the metallographic etching agent of Nitinol in the present invention：Corrosive agent main component be hydrofluoric acid, nitric acid and go from
The volume ratio of sub- water, each component content is 1:2:5.
Sample in the present invention, which need to first pass through, to be inlayed, and is ground, and is polished, then cleaning is impregnated, later in above-mentioned corrosive agent
Cleaning is taken out, drying is finally taken and observes its metallographic structure on the objective table of metallographic microscope.
Sample is embedding by phenolic resin progress hot insert in the present invention.
Be ground to mechanical lapping and hand-ground involved in the present invention, the sand paper needed for mechanical lapping include 600,
800,1000,1200,1500,2000 mesh (according to the arrangement of grinding sequencing), the sand paper needed for hand-ground is 2500,5000
Mesh.
Polishing involved in the present invention is using silk polishing cloth and 0.5 μm, 0.25 μm of polishing fluid, rotary speed 150
Rev/min.
The ingredient of corrosive agent in the present invention includes that hydrofluoric acid, nitric acid are that analysis is pure, and the time of sample etches is 40 seconds.
Claims (10)
1. a kind of metallographic etching agent of Nitinol, it is characterised in that：The corrosive agent ingredient is hydrofluoric acid, nitric acid and deionization
The volume ratio of water, each component content is 1:2:5, hydrofluoric acid, nitric acid and deionized water are poured into specified containers successively, uniform stirring
After stand, obtain corrosive agent.
2. a kind of method for displaying metallographic structure of Nitinol, it is characterised in that：This method is as follows：
1) Nitinol sample is put into above the lower die in pointing machine, the phenolic resin inlay being then filled with covers upper mold
Heating pressurization is carried out, is taken out after sample is fully cooled to room temperature after heat preservation；
2) sample inlayed is placed on grinder and passes through multiple sand paper mechanical lapping, then ground manually on sand paper
Mill, until the cut of a upper procedure is override, new cut direction is consistent；
3) polishing flannelet is finished changing on turntable, uniformly the upper polishing fluid of sprinkling, then ground sample is placed on polishing cloth upthrow
Light is thrown to surface no marking；Then one piece of new polishing cloth is changed, polishing fluid is uniformly sprayed, repeating above-mentioned polishing step is
Can, sample is finally taken out, is dried up after cleaning for use；
4) sample obtained is first put into supersonic wave cleaning machine and is cleaned, taken out later and sample surfaces are blown to water stain-free i.e.
It can；
5) hydrofluoric acid, nitric acid, deionized water are measured respectively with graduated cylinder, pours into specified containers to stand after uniform stirring successively and obtains
Corrosive agent；
6) the etch time first is set with timer, then grips sample with tweezers, so that it is completely immersed in corrosive agent, press timing
Device takes out sample after timer sound；
7) deionized water cleaning sample, cleaned just drying is used to stand；
8) sample after drying is positioned on metallographic microscope objective table, observes its metallographic structure.
3. a kind of method for displaying metallographic structure of Nitinol according to claim 2, it is characterised in that：Edge in step 1)
The holding temperature of embedding machine is 400 DEG C, and soaking time is 14 minutes, is waited for again after heat preservation and waits within 20 minutes that sample is completely cooling.
4. a kind of method for displaying metallographic structure of Nitinol according to claim 2, it is characterised in that：In step 2)
Sample on the sand paper of 600,800,1000,1200,1500 mesh successively by carrying out mechanical lapping, then in 2500,5000 purposes
Hand-ground is carried out on sand paper, is needed when changing sand paper every time by 90 ° of rotary sample, and is needed every time with clear water lavage specimens after grinding
Product are to remove remained on surface impurity.
5. a kind of method for displaying metallographic structure of Nitinol according to claim 2, it is characterised in that：Step 3) is turning
Polishing flannelet is finished changing on disk, uniformly sprays 0.5 μm of polishing fluid, then ground sample is placed on polishing cloth and is polished；So
One piece of new polishing cloth is changed afterwards, uniformly sprays 0.25 μm of polishing fluid.
6. a kind of method for displaying metallographic structure of Nitinol according to claim 2, it is characterised in that：Step 4) will be made
The sample obtained, which is first put into supersonic wave cleaning machine, to be cleaned 2 minutes.
7. a kind of method for displaying metallographic structure of Nitinol according to claim 2, it is characterised in that：It is used in step 5)
Graduated cylinder measures hydrofluoric acid 10ml respectively, and nitric acid 20ml, deionized water 50ml is poured into specified containers successively, quiet after uniform stirring
It sets, obtains corrosive agent.
8. a kind of method for displaying metallographic structure of Nitinol according to claim 2, it is characterised in that：Step 6) is fallen into a trap
When device set 40 seconds etch time.
9. a kind of method for displaying metallographic structure of Nitinol according to claim 2, it is characterised in that：Step 7) is spent
The scavenging period of ionized water cleaning sample is 1 minute.
10. a kind of method for displaying metallographic structure of Nitinol according to claim 2, it is characterised in that：In step 8)
Metallographic microscope display multiple be in 400X.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810415690.5A CN108663257A (en) | 2018-05-03 | 2018-05-03 | A kind of metallographic etching agent and method for displaying metallographic structure of Nitinol |
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| CN201810415690.5A CN108663257A (en) | 2018-05-03 | 2018-05-03 | A kind of metallographic etching agent and method for displaying metallographic structure of Nitinol |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109238814A (en) * | 2018-11-09 | 2019-01-18 | 成都先进金属材料产业技术研究院有限公司 | The preparation method of high-strength and high ductility beta titanium alloy metallographic specimen |
| CN109507005A (en) * | 2018-11-28 | 2019-03-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Vananum metallographic etching agent and caustic solution |
| CN110954388A (en) * | 2019-12-16 | 2020-04-03 | 中国民航大学 | Metallographic corrosive agent for laser cladding layer of titanium alloy containing rare earth and tissue display method |
| CN111579324A (en) * | 2020-05-26 | 2020-08-25 | 宁波江丰电子材料股份有限公司 | Chromium-titanium alloy treatment method and application thereof in metallographic structure display |
| CN111707513A (en) * | 2020-06-17 | 2020-09-25 | 宁波江丰电子材料股份有限公司 | Preparation method of NiV alloy metallographic specimen |
| CN113252411A (en) * | 2021-04-13 | 2021-08-13 | 江阴佩尔科技有限公司 | Method for displaying nonmetallic inclusion of nickel-titanium alloy |
| CN113969403A (en) * | 2021-10-27 | 2022-01-25 | 湖南工程学院 | Etching solution and method for nickel and titanium high-temperature alloy |
| CN114112606A (en) * | 2021-11-08 | 2022-03-01 | 陕西飞机工业有限责任公司 | Preparation method of titanium alloy bolt head crystal grain streamline sample |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109238814A (en) * | 2018-11-09 | 2019-01-18 | 成都先进金属材料产业技术研究院有限公司 | The preparation method of high-strength and high ductility beta titanium alloy metallographic specimen |
| CN109507005A (en) * | 2018-11-28 | 2019-03-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Vananum metallographic etching agent and caustic solution |
| CN110954388A (en) * | 2019-12-16 | 2020-04-03 | 中国民航大学 | Metallographic corrosive agent for laser cladding layer of titanium alloy containing rare earth and tissue display method |
| CN111579324A (en) * | 2020-05-26 | 2020-08-25 | 宁波江丰电子材料股份有限公司 | Chromium-titanium alloy treatment method and application thereof in metallographic structure display |
| CN111707513A (en) * | 2020-06-17 | 2020-09-25 | 宁波江丰电子材料股份有限公司 | Preparation method of NiV alloy metallographic specimen |
| CN111707513B (en) * | 2020-06-17 | 2023-09-08 | 宁波江丰电子材料股份有限公司 | Preparation method of NiV alloy metallographic specimen |
| CN113252411A (en) * | 2021-04-13 | 2021-08-13 | 江阴佩尔科技有限公司 | Method for displaying nonmetallic inclusion of nickel-titanium alloy |
| CN113969403A (en) * | 2021-10-27 | 2022-01-25 | 湖南工程学院 | Etching solution and method for nickel and titanium high-temperature alloy |
| CN113969403B (en) * | 2021-10-27 | 2023-10-31 | 湖南工程学院 | Etching solution and method for nickel-titanium superalloy |
| CN114112606A (en) * | 2021-11-08 | 2022-03-01 | 陕西飞机工业有限责任公司 | Preparation method of titanium alloy bolt head crystal grain streamline sample |
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