CN102980794A - Metallographic erosion method for displaying cobalt-chromium alloy structure - Google Patents
Metallographic erosion method for displaying cobalt-chromium alloy structure Download PDFInfo
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- CN102980794A CN102980794A CN2012104418493A CN201210441849A CN102980794A CN 102980794 A CN102980794 A CN 102980794A CN 2012104418493 A CN2012104418493 A CN 2012104418493A CN 201210441849 A CN201210441849 A CN 201210441849A CN 102980794 A CN102980794 A CN 102980794A
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Abstract
The present invention describes a metallographic erosion method for displaying a cobalt-chromium alloy structure, including: preparing aqua regia; placing the aqua regia at a certain temperature for a specified time to make the aqua regia reach the chroma meet the requirements; dipping in the aqua regia with a flexible material to wipe a sample, wherein the wiping time is 30-90 seconds; removing the surface aqua regia; and drying to get a etched sample surface. The method of the present invention is clearly, completely and accurately displays the metallographic structure of the cobalt-chromium alloy. The good erosion effect of the reagent is reflected by a test of a cobalt-chromium alloy human body implantable material. According to the present invention, the cobalt-chromium alloy etchant is prepared by a conventional metallographic etchant, good erosion effect of cobalt-chromium alloy is achieved by using that the erosion abilities of the etchant during different periods are different, thus a clear, complete and accurate metallographic structure is displayed.
Description
Technical field
The present invention relates to a kind of metallographic etching method, particularly a kind of metallographic etching method that shows the cochrome tissue.
Background technology
Cochrome proportion is little, light weight, and fusing point is high, stable chemical performance, corrosion resistivity is strong, has good mechanical property, to the body nonirritant, is widely used at present the human body planting material.Owing to be difficult to corrosion, so metallographic sample preparation is a difficult point, by consulting many metallographic sample preparation technical information, do not find the concrete corrosion method of cochrome, only have the etchant of cobalt-base alloys to be mainly totally four kinds in hydrochloric acid+water+acetic acid+nitric acid+solution, alcohol+hydrofluorite+nitric acid, hydrochloric acid+sulphuric acid copper liquor and lactic acid+heavy water+nitric acid.But through the author test, this several etchants or do not corrode, or poor effect.。
Summary of the invention
Technical matters to be solved by this invention provides a kind of metallographic etching method that shows the cochrome tissue, the problem that exists for the metallographic etching of cochrome, utilize the activity of severe corrosive and the different times of chloroazotic acid, the examination face of making is limpid, tissue shows intact, accurate, simultaneously also be tested material in China's industrial and agricultural production, accurately and reliably foundation is provided in the practical application of the development of defense-related science and technology.
For the purpose that realizes solving the problems of the technologies described above, the present invention has adopted following technical scheme:
A kind of metallographic etching method that shows the cochrome tissue of the present invention is characterised in that technological process is:
(1), proportionally prepares chloroazotic acid;
(2), chloroazotic acid is placed the stipulated time in uniform temperature, make chloroazotic acid reach satisfactory colourity:
Wherein, in the time of-5 ℃ ~ 5 ℃, be the standing time of chloroazotic acid: 8 ~ 15 minutes;
In the time of 5 ℃ ~ 15 ℃, be the standing time of chloroazotic acid: 5 ~ 10 minutes;
In the time of 15 ℃ ~ 25 ℃, be the standing time of chloroazotic acid: 2 ~ 7 minutes;
In the time of 25 ℃ ~ 35 ℃, be the standing time of chloroazotic acid: 0.5 ~ 3 minute;
Described ceiling temperature does not all contain this value;
(3), dip chloroazotic acid wiping sample with flexible material, the wiping time was 30 ~ 90 seconds; When specimen surface light no longer, burnt hair a little, this moment, erosion effect was best;
(4), wipe the chloroazotic acid of specimen surface with flexible material, and water is rinsed specimen surface well; Perhaps sample is placed on and washes the chloroazotic acid of removing the surface in the water; Then dry up, namely obtain the specimen surface that is corroded.
More specifically, be the standing time after chloroazotic acid configuration is complete: in the time of-5 ℃ ~ 5 ℃, be the standing time of chloroazotic acid: 10 ~ 15 minutes; In the time of 5 ℃ ~ 15 ℃, be the standing time of chloroazotic acid: 5 ~ 10 minutes; In the time of 15 ℃ ~ 25 ℃, be the standing time of chloroazotic acid: 3 ~ 5 minutes; In the time of 25 ℃ ~ 35 ℃, be the standing time of chloroazotic acid: 0.5 ~ 2 minute.
The described chloroazotic acid of this patent refers to that mass concentration is that 55 ~ 70% nitric acid and mass concentration are 30 ~ 37% hydrochloric acid, according to nitric acid: the mixed liquor of hydrochloric acid volume ratio=1:2.5 ~ 4.
Preferably, described chloroazotic acid refers to that mass concentration is that 60 ~ 70% nitric acid and mass concentration are 33 ~ 37% hydrochloric acid, according to nitric acid: the mixed liquor of hydrochloric acid volume ratio=1:3 ~ 3.5.
Preferred chloroazotic acid refers to that mass concentration is that 65 ~ 69% nitric acid and mass concentration are 33 ~ 37% hydrochloric acid, according to nitric acid: the mixed liquor of hydrochloric acid volume ratio=1:3.Most preferred chloroazotic acid refers to that mass concentration is that 69% nitric acid and mass concentration are 36.5% hydrochloric acid, according to nitric acid: the mixed liquor of hydrochloric acid volume ratio=1:3.
Described cochrome specifically refers to the L605 alloy.This alloy composition is: C:0.05-0.15; Mg:1.00-2.00; Si :≤0.40; P :≤0.040; S :≤0.030; Cr:19-21; Ni:9-11; W:14-16; Fe :≤3; Surplus is Co and inevitable impurity.
For the cochrome metallographic etchant, key is to make examination face limpid, and tissue shows intact, accurate.Technical matters mainly contains: 1) how to make specimen erodes; 2) the tissue demonstration is intact, examination face is limpid; 3) tissue shows accurately.
What at first will solve is the erosion problem of sample, because cochrome stable chemical performance, corrosion resistivity is strong, so general etchant is difficult to corrode to cochrome, chloroazotic acid has strong corrosive attack, metal to the overwhelming majority has the burn into dissolution, therefore can select chloroazotic acid as etchant.
Also different with its erosion performance of the length of standing time with the difference of temperature after the chloroazotic acid configuration, erosional competency weakens after increasing first grow standing time gradually with the rising of temperature grow gradually.The power of chloroazotic acid erosional competency shows on the color of reagent, just the chloroazotic acid color of configuration is water white, with increasing standing time, two kinds of reagent mix gradually, color becomes pale yellow, deep yellow, reddish brown, pale yellow, water white transparency gradually, erosional competency is the strongest when being rufous for stainless steel and high temperature alloy class material color, and takes second place when yellow, and is the poorest when colourless.Different just because of chloroazotic acid different times erosional competency, so the corresponding best erosion of different materials is also different opportunity, when using chloroazotic acid as etchant, holding its best erosion opportunity for a kind of specific material is the key of specimen erodes.Cochrome is different, does not corrode when chloroazotic acid just disposes, and sample or do not corrode when color is faint yellow, or excessive erosion even surface dissolution and can't obtain preferably metallographic structure be not in any case corrode when chloroazotic acid becomes rufous yet.When chloroazotic acid corrodes the erosion effect that sample can obtain by yellowish becoming in this deep yellow time period.This patent is exactly to design in accordance with this principle, control.
By adopting technique scheme, the present invention has following beneficial effect:
A kind of metallographic etching method that shows the cochrome tissue of the present invention is clear, complete, shown and the metallographic structure of cochrome by the cochrome human body being implanted the test with material, embodied the good erosion effect of this reagent exactly; The present invention utilizes the difference of etchant different times erosional competency to reach the erosion effect good to cochrome, thereby demonstrates clear, complete, accurately metallographic structure with the etchant of metallographic etchant configuration cochrome commonly used.
Description of drawings
Fig. 1 is the faint yellow chloroazotic acid wiping cochrome metallographic structure in 30 seconds, 200 *.
Fig. 2 is the faint yellow chloroazotic acid wiping cochrome metallographic structure in 50 seconds, 200 *.
Fig. 3 is 2 minutes cochrome metallographic structure of red chloroazotic acid wiping, 100 *.
Fig. 4 is 50 seconds cochrome metallographic structure of buff chloroazotic acid wiping, 200 *.
Embodiment
Below in conjunction with accompanying drawing this patent is further explained.But the protection domain of this patent is not limited to concrete embodiment.
Embodiment 1
Test material is human body implantation cochrome tubing.Alloy proportion is: C:0.05-0.15; Mg:1.00-2.00; Si :≤0.40; P :≤0.040; S :≤0.030; Cr:19-21; Ni:9-11; W:14-16; Fe :≤3; Surplus is Co and inevitable impurity.
The chloroazotic acid of embodiment 1 refers to that mass concentration is that 69% nitric acid and mass concentration are 36.5% hydrochloric acid, according to nitric acid: the mixed liquor of hydrochloric acid volume ratio=1:3.
28 ℃ of room temperatures, when the chloroazotic acid for preparing was placed 7 minutes, the chloroazotic acid color was buff, and begin to dip the wiping sample with cotton this moment, and the wiping time was about for 50 seconds.No longer bright when examination face, to shade a little, this moment, erosion effect was best, and specimen surface is limpid, and crystal boundary is clear, is organized as twin α, sees Fig. 4.
Embodiment 2
Test material is that the human body implantation is: C:0.05-0.15 with cochrome tubing alloy proportion; Mg:1.00-2.00; Si :≤0.40; P :≤0.040; S :≤0.030; Cr:19-21; Ni:9-11; W:14-16; Fe :≤3; Surplus is Co and inevitable impurity.
The chloroazotic acid of embodiment 2 refers to that mass concentration is that 69% nitric acid and mass concentration are 36.5% hydrochloric acid, according to nitric acid: the mixed liquor of hydrochloric acid volume ratio=1:3.
28 ℃ of room temperatures, when the chloroazotic acid for preparing was placed 1 minute, the chloroazotic acid color was buff, and begin to dip the wiping sample with cotton this moment, and the wiping time was about for 60 seconds.No longer bright when examination face, to shade a little, this moment, erosion effect was best, and specimen surface is limpid, and crystal boundary is clear, is organized as twin α.
Claims (6)
1. metallographic etching method that shows the cochrome tissue is characterized in that technological process is:
(1), proportionally prepares chloroazotic acid;
(2), chloroazotic acid is placed the stipulated time in uniform temperature, make chloroazotic acid reach satisfactory colourity:
Wherein, in the time of-5 ℃ ~ 5 ℃, be the standing time of chloroazotic acid: 8 ~ 15 minutes;
In the time of 5 ℃ ~ 15 ℃, be the standing time of chloroazotic acid: 5 ~ 10 minutes;
In the time of 15 ℃ ~ 25 ℃, be the standing time of chloroazotic acid: 2 ~ 7 minutes;
In the time of 25 ℃ ~ 35 ℃, be the standing time of chloroazotic acid: 0.5 ~ 3 minute;
Described ceiling temperature does not all contain this value;
(3), dip chloroazotic acid wiping sample with flexible material, the wiping time was 30 ~ 90 seconds;
(4), wipe the chloroazotic acid of specimen surface with flexible material, and water is rinsed specimen surface well; Perhaps sample is placed on and washes the chloroazotic acid of removing the surface in the water; Then dry up, namely obtain the specimen surface that is corroded.
2. the metallographic etching method of described demonstration cochrome tissue according to claim 1 is characterized in that: be the standing time after the chloroazotic acid configuration is complete: in the time of-5 ℃ ~ 5 ℃, be the standing time of chloroazotic acid: 10 ~ 15 minutes; In the time of 5 ℃ ~ 15 ℃, be the standing time of chloroazotic acid: 5 ~ 10 minutes; In the time of 15 ℃ ~ 25 ℃, be the standing time of chloroazotic acid: 3 ~ 5 minutes; In the time of 25 ℃ ~ 35 ℃, be the standing time of chloroazotic acid: 0.5 ~ 2 minute.
3. the metallographic etching method of described demonstration cochrome tissue according to claim 1, it is characterized in that: described chloroazotic acid, refer to that mass concentration is that 55 ~ 70% nitric acid and mass concentration are 30 ~ 37% hydrochloric acid, according to nitric acid: the mixed liquor of hydrochloric acid volume ratio=1:2.5 ~ 4.
4. the metallographic etching method of described demonstration cochrome tissue according to claim 3, it is characterized in that: described chloroazotic acid refers to that mass concentration is that 60 ~ 70% nitric acid and mass concentration are 33 ~ 37% hydrochloric acid, according to nitric acid: the mixed liquor of hydrochloric acid volume ratio=1:3 ~ 3.5.
5. the metallographic etching method of described demonstration cochrome tissue according to claim 4 is characterized in that: described chloroazotic acid refers to that mass concentration is that 65 ~ 69% nitric acid and mass concentration are 33 ~ 37% hydrochloric acid, according to nitric acid: the mixed liquor of hydrochloric acid volume ratio=1:3.
6. the metallographic etching method of described demonstration cochrome tissue according to claim 5 is characterized in that: described chloroazotic acid refers to that mass concentration is that 69% nitric acid and mass concentration are 36.5% hydrochloric acid, according to nitric acid: the mixed liquor of hydrochloric acid volume ratio=1:3.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103487309A (en) * | 2013-08-27 | 2014-01-01 | 中国船舶重工集团公司第七二五研究所 | Method for displaying grain size of metal material |
| CN104062164A (en) * | 2014-06-30 | 2014-09-24 | 中国船舶重工集团公司第七二五研究所 | Erosion method of gold-phase metallographic structure of double-phase stainless steel |
| CN105241885A (en) * | 2015-09-30 | 2016-01-13 | 金川集团股份有限公司 | Forged magnetically soft alloy 1J50 alloy metallographic corrosive liquid and applications thereof |
| CN105699137A (en) * | 2014-11-25 | 2016-06-22 | 宁波江丰电子材料股份有限公司 | Displaying method for structure of metal chromium |
| JP2022513244A (en) * | 2018-12-14 | 2022-02-07 | テック メット インコーポレイテッド | Cobalt chrome etching method |
| CN114892172A (en) * | 2022-05-24 | 2022-08-12 | 先导薄膜材料（广东）有限公司 | Metallographic corrosive liquid and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103487309A (en) * | 2013-08-27 | 2014-01-01 | 中国船舶重工集团公司第七二五研究所 | Method for displaying grain size of metal material |
| CN104062164A (en) * | 2014-06-30 | 2014-09-24 | 中国船舶重工集团公司第七二五研究所 | Erosion method of gold-phase metallographic structure of double-phase stainless steel |
| CN105699137A (en) * | 2014-11-25 | 2016-06-22 | 宁波江丰电子材料股份有限公司 | Displaying method for structure of metal chromium |
| CN105241885A (en) * | 2015-09-30 | 2016-01-13 | 金川集团股份有限公司 | Forged magnetically soft alloy 1J50 alloy metallographic corrosive liquid and applications thereof |
| JP2022513244A (en) * | 2018-12-14 | 2022-02-07 | テック メット インコーポレイテッド | Cobalt chrome etching method |
| JP7247346B2 (en) | 2018-12-14 | 2023-03-28 | テック メット インコーポレイテッド | Cobalt chromium etching method |
| CN114892172A (en) * | 2022-05-24 | 2022-08-12 | 先导薄膜材料（广东）有限公司 | Metallographic corrosive liquid and application thereof |
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Application publication date: 20130320 |