CN102268669A - WC-TiC-Co cemented carbide metallographic staining agent and treatment method - Google Patents
WC-TiC-Co cemented carbide metallographic staining agent and treatment method Download PDFInfo
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- CN102268669A CN102268669A CN2011102315568A CN201110231556A CN102268669A CN 102268669 A CN102268669 A CN 102268669A CN 2011102315568 A CN2011102315568 A CN 2011102315568A CN 201110231556 A CN201110231556 A CN 201110231556A CN 102268669 A CN102268669 A CN 102268669A
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Abstract
The invention discloses a WC-TiC-Co cemented carbide metallographic staining agent which is prepared from the following components: 5-50 g of ferric chloride and 1-15 ml of nitric acid in per 100ml of water. The invention also discloses a pretreatment method of a specimen for metallographic display by utilizing the metallographic staining agent, and the pretreatment method comprises the following steps of: preparing the WC-TiC-Co cemented carbide metallographic staining agent; pre-preparing the specimen according to a microstructure inspection method; continuously immersing the treated specimen in the prepared staining agent with the polished surface upwards to stain for 1-1.5 hours; and washing the stained specimen with water, and then blow-drying the specimen with a hair dryer toward one direction, thereby the specimen can be used for metallurgical examination. By the method disclosed by the invention, the surface of the specimen is only slightly etched, and the identification capability of the optical metallographic examination is significantly improved.
Description
Technical field
The invention belongs to materials science field, relate to a kind of WC-TiC-Co series hard metal metallographic staining agent, the invention still further relates to and a kind ofly utilize this WC-TiC-Co series hard metal metallographic staining agent that test specimen is carried out metallographic to show pretreated method.
Background technology
Along with the common development of Materials science and industry-by-industry, also more and more higher to the requirement of material, this with regard to the research that requires material and producers exactly display material microstructure and obtain corresponding useful information.Conventional black and white metallurgical analysis method generally all is to rely on chemical reagent etching metallic surface to cause relief, the black and white contrast of utilizing catoptrical strong and weak difference to cause is differentiated tissue or phase, often because metallic surface microstructure contrast deficiency, feature are clear inadequately, quantity of information is less and be not easily distinguishable and differentiate, even also can enlarge because of etching causes the alloy structure profile, or the generation illusion, organize really thereby distorted various alloys.
Summary of the invention
The purpose of this invention is to provide a kind of WC-TiC-Co series hard metal metallographic staining agent, solved in the prior art because metallic surface microstructure contrast deficiency, feature are clear inadequately, quantity of information is less, the problem that causes alloy structure not to be easily distinguishable and differentiate.
Another object of the present invention is, provides a kind of and utilizes this WC-TiC-Co series hard metal metallographic staining agent that test specimen is carried out metallographic to show pretreated method.
The technical solution adopted in the present invention is, a kind of WC-TiC-Co series hard metal metallographic staining agent is formulated by following component: as in the water of every 100ml, to be mixed with the iron trichloride of 5～50g and the nitric acid of 1～15ml.
Another technical scheme of the present invention is, a kind ofly utilizes aforesaid WC-TiC-Co series hard metal metallographic staining agent that test specimen is carried out metallographic to show pretreated method, and this method is implemented according to following steps:
Step 1, in the water of 100ml, the iron trichloride that adds earlier 5～50g fully stirs, the nitric acid that adds 1～15ml more fully stirs, and obtains WC-TiC-Co series hard metal metallographic staining agent;
Step 2, according to the prefabricated sample of the microstructure method of inspection, comprise polish, the technology of corase grind, fine grinding, rough polishing, finishing polish, sample, hand, frock or grinding and polishing machine clamp must be cleaned up between each passage of mill, throwing, sample all need rotate 90 ° when following passage mill, throwing;
Step 3, the sample polished surface that step 2 is handled well immerse up in the staining agent that step 1 prepares and dye, and continue to soak 1～1.5 hour; With the flushing of the sample water after the dyeing, dry up sample with blower along a direction then, sample promptly can be used in metallographic and detects.
The invention has the beneficial effects as follows, make sample surfaces only be subjected to slight etching, the main film interference that relies on, produce colored contrast and differentiate tissue or phase, overcome the most of deficiency in traditional black and white metallographic, improve the distinguishing ability of optics metallographic, can observe general the display packing tissue that can't differentiate and the details that can't see, the less and easy identification of illusion occurred.
Description of drawings
Fig. 1 is the color metallograph that utilizes after staining agent of the present invention is anticipated YT15 carbide-tipped milling cutter head.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
WC-TiC-Co series hard metal metallographic staining agent of the present invention, formulated by following component: in the water of every 100ml, add the iron trichloride of 5～50g and the nitric acid of 1～15ml, the concentration of this nitric acid is 65%-68%.
The inventive method has adopted chemical reagent etching deposit embrane method, makes sample surfaces produce one deck interference thin film, utilizes film interference and complementary color principle, makes each composition of different nature in the sample produce distinct colors, thus the internal information of show sample.
The present invention utilizes this WC-TiC-Co series hard metal metallographic staining agent that test specimen is carried out metallographic to show pretreated method, implement according to following steps:
Step 1, in the water of 100ml, the iron trichloride that adds earlier 5～50g fully stirs, the nitric acid that adds 1～15ml more fully stirs, the concentration of this nitric acid is 65%-68%, obtains WC-TiC-Co series hard metal metallographic staining agent;
Step 2, according to the prefabricated sample of the microstructure method of inspection, comprise polish, the technology of corase grind, fine grinding, rough polishing, finishing polish, between each passage of mill, throwing, sample, hand, frock or grinding and polishing machine clamp must be cleaned up, following passage mill, sample all need rotate 90 ° (the conventional requirement of sample making technology grinds off preceding one polishing scratch when throwing.The polishing process commentaries on classics helps for 90 ° eliminating dragging tail, reduces illusion).
Step 3, the sample polished surface that step 2 is handled well immerse up in the staining agent that step 1 prepares and dye, and continue to soak 1～1.5 hour; With the flushing of the sample water after the dyeing, dry up sample with blower along a direction then, sample is used further to metallographic and detects.
Embodiment 1
Step 1) is according to the proportioning preparation staining agent of water 100ml, iron trichloride 30g, nitric acid 10ml.In 100ml water, add 30 gram iron trichlorides and fully stir, add nitric acid 10ml then and mix.
Step 2) YT15 carbide-tipped milling cutter head is inlayed, according to polish → roughly grind → order of fine grinding → rough polishing → finishing polish operates.Corase grind and correct grinding adopt diamond disk, and rough polishing adopts 9 μ m, 6 μ m, 3 μ m, 1 μ m diamond polishing agent and supporting polishing cloth to polish successively, the polishing of finish polishing 0.05 μ m aluminum oxide rumbling compound.After the polishing sample is cleaned up, dry up along a direction with blower then,, do not have sample preparation defective such as cut to be qualified sample at test under microscope.
The sample that step 3) is thrown essence after qualified directly is immersed in the staining agent for preparing, and the sample glazed surface takes out after at room temperature 1 hour up, and water is rinsed well, dries up the dyeing course end then along a direction with blower.
Can observe after microscope adjusted,, proceed dyeing if dyeing inadequately can the proper extension time; If painted overweight, reuse the polishing of 0.05 μ m aluminum oxide rumbling compound, dyeing again then is till satisfaction.Carry out electronic image capture after dyeing is satisfied, in the image acquisition process with parameter adjustments such as light, contrast gradient, saturation ratio and colors to optimum regime, analyze then, operations such as photograph, data logging and view data processing.
Embodiment 2
Step 1) is according to the proportioning preparation staining agent of water 100ml, iron trichloride 5g, nitric acid 15ml.In 100ml water, add 5 gram iron trichlorides and fully stir, add nitric acid 15ml then and mix.
Step 2) YT15 carbide-tipped milling cutter head is inlayed, according to polish → roughly grind → order of fine grinding → rough polishing → finishing polish operates.Corase grind and correct grinding adopt diamond disk, and rough polishing adopts 9 μ m, 6 μ m, 3 μ m, 1 μ m diamond polishing agent and supporting polishing cloth to polish successively, the polishing of finish polishing 0.05 μ m aluminum oxide rumbling compound.After the polishing sample is cleaned up, dry up along a direction with blower then,, do not have sample preparation defective such as cut to be qualified sample at test under microscope.
The sample that step 3) is thrown essence after qualified directly is immersed in the staining agent for preparing, and the sample glazed surface takes out after at room temperature 1.5 hours up, and water is rinsed well, dries up the dyeing course end then along a direction with blower.
Embodiment 3
Step 1) is according to the proportioning preparation staining agent of water 100ml, iron trichloride 50g, nitric acid 1ml.In 100ml water, add 50 gram iron trichlorides and fully stir, add nitric acid 1ml then and mix.
Step 2) YT15 carbide-tipped milling cutter head is inlayed, according to polish → roughly grind → order of fine grinding → rough polishing → finishing polish operates.Corase grind and correct grinding adopt diamond disk, and rough polishing adopts 9 μ m, 6 μ m, 3 μ m, 1 μ m diamond polishing agent and supporting polishing cloth to polish successively, the polishing of finish polishing 0.05 μ m aluminum oxide rumbling compound.After the polishing sample is cleaned up, dry up along a direction with blower then,, do not have sample preparation defective such as cut to be qualified sample at test under microscope.
The sample that step 3) is thrown essence after qualified directly is immersed in the staining agent for preparing, and the sample glazed surface takes out after at room temperature 1.5 hours up, and water is rinsed well, dries up the dyeing course end then along a direction with blower.
Embodiment 4
Step 1) is according to the proportioning preparation staining agent of water 100ml, iron trichloride 10g, nitric acid 5ml.In 100ml water, add 10 gram iron trichlorides and fully stir, add nitric acid 5ml then and mix.
Step 2) YT15 carbide-tipped milling cutter head is inlayed, according to polish → roughly grind → order of fine grinding → rough polishing → finishing polish operates.Corase grind and correct grinding adopt diamond disk, and rough polishing adopts 9 μ m, 6 μ m, 3 μ m, 1 μ m diamond polishing agent and supporting polishing cloth to polish successively, the polishing of finish polishing 0.05 μ m aluminum oxide rumbling compound.After the polishing sample is cleaned up, dry up along a direction with blower then,, do not have sample preparation defective such as cut to be qualified sample at test under microscope.
The sample that step 3) is thrown essence after qualified directly is immersed in the staining agent for preparing, and the sample glazed surface takes out after at room temperature 1.2 hours up, and water is rinsed well, dries up the dyeing course end then along a direction with blower.
As shown in Figure 1, be method according to embodiment 1, the actual colour picture after YT15 carbide-tipped milling cutter head is dyeed, WC has been dyed blueness in Fig. 1, and Co is dyed black, and WC+TiC is dyed other multicolour.WC+TiC mutually in other multicolour relevant with WC with TiC proportion difference.
The prescription of staining agent of the present invention is verified through the stain test of multiple Wimet, good reproducibility, and highly versatile, the metallographic specimen shelf time after the dyeing is long, and the metallographic structure of sample is clear, contains much information, and illusion is few.Wimet colour metallograpy staining agent of the present invention and color display method thereof, it is simple to have operating process, do not need to increase special equipment, do not need to carry out pre-etching, only prepare a kind of staining agent and just can show Wimet WC phase, WC+TiC phase and Co simultaneously mutually, distinguishing ability is strong, tissue shows accurately, quantity of information is abundant, remedy the deficiency of traditional white and black displays method, the potentiality of optics metallography microscope technology can have fully been excavated, for Wimet metallurgical analysis in the research of reality and production process provides effective means.
Claims (4)
1. WC-TiC-Co series hard metal metallographic staining agent, its characteristics are: formulated by following component: in the water of every 100ml, be mixed with the iron trichloride of 5～50g and the nitric acid of 1～15ml.
2. WC-TiC-Co series hard metal metallographic staining agent according to claim 1, its characteristics are: the concentration of described nitric acid is 65%-68%.
3. one kind is utilized the described WC-TiC-Co series hard metal of claim 1 metallographic staining agent that test specimen is carried out metallographic to show pretreated method, and its characteristics are that this method is implemented according to following steps:
Step 1, in the water of 100ml, the iron trichloride that adds earlier 5～50g fully stirs, the nitric acid that adds 1～15ml more fully stirs, and obtains WC-TiC-Co series hard metal metallographic staining agent;
Step 2, according to the prefabricated sample of the microstructure method of inspection, comprise polish, the technology of corase grind, fine grinding, rough polishing, finishing polish, sample, hand, frock or grinding and polishing machine clamp must be cleaned up between each passage of mill, throwing, sample all need rotate 90 ° when following passage mill, throwing;
Step 3, the sample polished surface that step 2 is handled well immerse up in the staining agent that step 1 prepares and dye, and continue to soak 1～1.5 hour; With the flushing of the sample water after the dyeing, dry up sample with blower along a direction then, sample promptly can be used in metallographic and detects.
4. metallographic according to claim 3 shows pretreated method, and its characteristics are: the concentration of described nitric acid is 65%-68%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105067414A (en) * | 2015-08-17 | 2015-11-18 | 江西稀有稀土金属钨业集团有限公司 | System and method for observing hard alloy structure with scanning electron microscope |
| CN106995921A (en) * | 2017-05-25 | 2017-08-01 | 齐鲁工业大学 | A kind of (Ti, W) C base ceramic cutting tool materials corrosive liquid and caustic solution |
| CN110530701A (en) * | 2019-08-19 | 2019-12-03 | 江苏师范大学 | It is a kind of for metallographic etching agent of stainless steel and preparation method thereof, caustic solution |
-
2011
- 2011-08-12 CN CN2011102315568A patent/CN102268669A/en active Pending
Non-Patent Citations (2)
| Title |
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| > 19980630 万美珍，李华飞 钢显微组织快速简易浸蚀方法 78-80 1-4 第20卷, 第2期 * |
| 万美珍，李华飞: "钢显微组织快速简易浸蚀方法", <<武汉化工学院学报>> * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105067414A (en) * | 2015-08-17 | 2015-11-18 | 江西稀有稀土金属钨业集团有限公司 | System and method for observing hard alloy structure with scanning electron microscope |
| CN106995921A (en) * | 2017-05-25 | 2017-08-01 | 齐鲁工业大学 | A kind of (Ti, W) C base ceramic cutting tool materials corrosive liquid and caustic solution |
| CN110530701A (en) * | 2019-08-19 | 2019-12-03 | 江苏师范大学 | It is a kind of for metallographic etching agent of stainless steel and preparation method thereof, caustic solution |
| CN110530701B (en) * | 2019-08-19 | 2021-12-03 | 江苏师范大学 | Metallographic corrosive agent for stainless steel, preparation method and corrosion method thereof |
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Application publication date: 20111207 |