CN101943640A - Metallographic etchant for medical beta titanium alloy and etching method - Google Patents
Metallographic etchant for medical beta titanium alloy and etching method Download PDFInfo
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- CN101943640A CN101943640A CN2009100124145A CN200910012414A CN101943640A CN 101943640 A CN101943640 A CN 101943640A CN 2009100124145 A CN2009100124145 A CN 2009100124145A CN 200910012414 A CN200910012414 A CN 200910012414A CN 101943640 A CN101943640 A CN 101943640A
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- metallographic
- titanium alloy
- corrosive liquid
- etchant
- medical beta
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 20
- 239000000956 alloy Substances 0.000 title claims abstract description 20
- 238000005530 etching Methods 0.000 title claims abstract description 19
- 229910001040 Beta-titanium Inorganic materials 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 15
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004310 lactic acid Substances 0.000 claims abstract description 11
- 235000014655 lactic acid Nutrition 0.000 claims abstract description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims description 26
- 238000005260 corrosion Methods 0.000 claims description 13
- 230000007797 corrosion Effects 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008399 tap water Substances 0.000 claims description 6
- 235000020679 tap water Nutrition 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 229910001069 Ti alloy Inorganic materials 0.000 abstract description 10
- 238000000137 annealing Methods 0.000 abstract description 10
- 239000010955 niobium Substances 0.000 abstract description 10
- 229910052758 niobium Inorganic materials 0.000 abstract description 9
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 abstract description 8
- 238000012545 processing Methods 0.000 abstract description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract 2
- 239000000463 material Substances 0.000 description 11
- 239000003518 caustics Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 210000000988 bone and bone Anatomy 0.000 description 3
- 239000007943 implant Substances 0.000 description 3
- 210000001519 tissue Anatomy 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
The invention relates to the field of metallographic etching of the titanium alloy, in particular to a metallographic etchant for the medical beta titanium alloy and an etching method, which are particularly suitable for the metallographic etching of the novel medical beta titanium alloy with high niobium content. The etchant consists of 10 to 50 volume parts of lactic acid, 5 to 30 volume parts of nitric acid and 1 to 10 volume parts of hydrofluoric acid; and a polished metallographic sample is soaked in the etchant for a certain period of time. The metallographic etchant and the etching method can realize metallographic etching of novel medical beta titanium alloy boards, bars and wires with high niobium content in the processing condition and the annealing condition, and the obtained metallographic structure is clear and complete.
Description
Technical field:
The present invention relates to titanium alloy etching pit field, be specially a kind of metallographic etchant and caustic solution of medical beta-titanium alloy, be particularly suitable for the etching pit of the new medical beta-titanium alloy of high content of niobium.
Background technology:
Titanium alloy has advantages such as high human compatibility, low-density, low elastic modulus, high strength, anti-human body fluid corrosion, substitutes stainless steel and cobalt-base alloys gradually and becomes hard tissue substituting materials such as bone and tooth.At present, be widely used in clinical medical medical titanium alloy and be mainly type alpha+beta Ti-6Al-4V and Ti-6Al-7Nb, its elastic modulus only is half of stainless steel and cobalt-base alloys, reduced embedded material and bone modulus difference, alleviated the stress shielding effect and caused that bone tissue is absorbed and the risk of the loosening and fracture of implant.Owing to contain Al and V titanium alloy behind long-term implant into body, because of wearing and tearing and corrosion discharge and have cytotoxicity and neurovirulent Al and V ion, developed countries such as the U.S. and Japan are devoted to develop the metastable β type medical titanium alloy with better human compatibility in middle nineteen nineties.Because elements such as Nb, Ta, Zr are nontoxic, and all be beta stable element, therefore the medical beta-titanium alloy of developing on the recent international mostly contains a large amount of Nb, Ta etc., as Ti-13Nb-13Zr (ASTM F1713), the Ti-35Nb-5Ta-7Zr of the U.S., and the Ti-29Nb-13Ta-4.6Zr of Japan etc.A kind of Ti-24Nb-4Zr-8Sn high strength multifunctional titanium (application number: 200410092858.1) of Metal Inst., Chinese Academy of Sciences's development with independent intellectual property right, its elastic modulus and skeleton are complementary, the skeleton of its super-elasticity and damping capacity and porous structure is similar, characteristics such as its high strength, corrosion-resistant, inanimate object toxicity can satisfy human body and implant demand for a long time, wherein also contain a large amount of Nb elements.
In titanium alloy, the resistance to corrosion of β phase is apparently higher than the α phase.In addition, the niobium element also can significantly improve the resistance to corrosion of titanium alloy.Therefore, the metallographic specimen of high content of niobium new medical beta-titanium alloy is difficult to corrosion, and the etching pit reagent of general titanium alloy all is not suitable for this type of alloy.And be that the tissue of understanding material is formed and form, metallographic observation is a kind of simple and reliable means, is vast research work, slip-stick artist and analytical test personnel common method.
Summary of the invention:
The metallographic etchant and the caustic solution that the purpose of this invention is to provide a kind of new medical beta-titanium alloy use the metallographic specimen of the high content of niobium new medical of the corrosion beta-titanium alloy that this corrosive liquid and caustic solution can be easily and effectively, and the metallographic structure that obtains is clear accurately.
Technical scheme of the present invention is:
The invention provides a kind of metallographic etchant of medical beta-titanium alloy, corrosive liquid consists of lactic acid, nitric acid and hydrofluorite, umber meter by volume, and in the described corrosive liquid, lactic acid content is 10~50 parts, and nitric acid content is 5~30 parts, and fluohydric acid content is 1~10 part.
In the described corrosive liquid, liquid water content is 0ml.
In the described corrosive liquid, lactic acid, nitric acid and hydrofluorite are analytical reagent.
The present invention also provides the etching pit method of medical beta-titanium alloy, and polished metallographic specimen is soaked certain hour in described corrosive liquid.
Described etching pit method, state soaks 3~8h in corrosive liquid per sample.
Described etching pit method, corrosion is at room temperature carried out, and need not heat.
Described etching pit method is soaked sample in the corrosion process in corrosive liquid, corrosion finishes back taking-up sample cleans with tap water earlier at once, cleans with absolute ethyl alcohol then, dries up with hair-dryer cold wind at last.
The invention has the beneficial effects as follows:
1, employing the present invention can realize processing the etching pit of high content of niobium new medical beta-titanium alloy sheet material, bar and the silk material of attitude, annealed state, the metallographic structure complete display that obtains.
2, the invention provides a kind of etching pit method of simple and effective high content of niobium new medical beta-titanium alloy, can accurately understand the tissue of this type of material, thus the control material performance, to development with to use this type of new medical titanium alloy significant.
Description of drawings:
Fig. 1 is the metallographic structure of Ti-24Nb-4Zr-8Sn hot rolled plate;
Fig. 2 is the metallographic structure of Ti-24Nb-4Zr-8Sn annealing bar;
Fig. 3 is the metallographic structure of Ti-24Nb-4Zr-8Sn annealing sheet material;
Fig. 4 is the metallographic structure of Ti-29Nb-13Ta-4.6Zr annealing bar.
Embodiment:
Embodiment 1
With analyzing pure lactic acid, nitric acid and hydrofluorite is the ratio preparation corrosive liquid of raw material in 30ml: 10ml: 5ml, at ambient temperature, polished Ti-24Nb-4Zr-8Sn hot rolled plate metallographic specimen is immersed in the corrosive liquid 4 hours, take out sample subsequently, clean with tap water at once, clean with absolute ethyl alcohol then, dry up with hair-dryer cold wind subsequently, the sheet material metallographic structure pattern of gained is seen Fig. 1.As can be seen from Figure 1, the metallographic structure complete display that obtains.
Embodiment 2
With analyzing pure lactic acid, nitric acid and hydrofluorite is the ratio preparation corrosive liquid of raw material in 20ml: 20ml: 10ml, at ambient temperature, polished Ti-24Nb-4Zr-8Sn annealing bar metallographic specimen is immersed in the corrosive liquid 5 hours, take out sample subsequently, clean with tap water at once, clean with absolute ethyl alcohol then, dry up with hair-dryer cold wind subsequently, the annealing bar metallographic structure pattern of gained is seen Fig. 2.As can be seen from Figure 2, the metallographic structure complete display that obtains.
Embodiment 3
With analyzing pure lactic acid, nitric acid and hydrofluorite is the ratio preparation corrosive liquid of raw material in 40ml: 10ml: 10ml, at ambient temperature, polished Ti-24Nb-4Zr-8Sn annealing sheet material metallographic specimen is immersed in the corrosive liquid 7 hours, take out sample subsequently, clean with tap water at once, clean with absolute ethyl alcohol then, dry up with hair-dryer cold wind subsequently, the annealing sheet material metallographic structure pattern of gained is seen Fig. 3.As can be seen from Figure 3, the metallographic structure complete display that obtains.
Embodiment 4
With analyzing pure lactic acid, nitric acid and hydrofluorite is the ratio preparation corrosive liquid of raw material in 10ml: 20ml: 5ml, at ambient temperature, polished Ti-29Nb-13Ta-4.6Zr annealing bar metallographic specimen is immersed in the corrosive liquid 3 hours, take out sample subsequently, clean with tap water at once, clean with absolute ethyl alcohol then, dry up with hair-dryer cold wind subsequently, the annealing bar metallographic structure pattern of gained is seen Fig. 4.As can be seen from Figure 4, the metallographic structure complete display that obtains.
Claims (7)
1. the metallographic etchant of a medical beta-titanium alloy, it is characterized in that: corrosive liquid consists of lactic acid, nitric acid and hydrofluorite, umber meter by volume, in the described corrosive liquid, lactic acid content is 10~50 parts, and nitric acid content is 5~30 parts, and fluohydric acid content is 1~10 part.
2. according to the described metallographic etchant of claim 1, it is characterized in that: in the described corrosive liquid, liquid water content is 0ml.
3. according to the described metallographic etchant of claim 1, it is characterized in that: in the described corrosive liquid, lactic acid, nitric acid and hydrofluorite are analytical reagent.
4. an etching pit method of utilizing the medical beta-titanium alloy of the described corrosive liquid of claim 1 is characterized in that: polished metallographic specimen is soaked in described corrosive liquid.
5. according to the described etching pit method of claim 4, it is characterized in that: state per sample, soak 3~8h in corrosive liquid.
6. according to the described etching pit method of claim 4, it is characterized in that: corrosion is at room temperature carried out, and need not heat.
7. according to the described etching pit method of claim 4, it is characterized in that: in the corrosion process sample is soaked in corrosive liquid, corrosion finishes back taking-up sample cleans with tap water earlier at once, cleans with absolute ethyl alcohol then, dries up with hair-dryer cold wind at last.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102564830A (en) * | 2011-11-27 | 2012-07-11 | 西北有色金属研究院 | Chemical polishing agent |
CN102866048A (en) * | 2012-09-28 | 2013-01-09 | 昆明理工大学 | Preparation method of metallographic display sample of Ti-Cu laminar composite |
CN102928282A (en) * | 2012-11-02 | 2013-02-13 | 上海锅炉厂有限公司 | Method for solving problem of acid returning permeation of metal cracks subjected to corrosion of corrosives |
CN103484863A (en) * | 2012-06-07 | 2014-01-01 | 宁波江丰电子材料有限公司 | Metallographic corrosive, corrosion method for metallographic sample and display method for metallographic structure |
CN105750853A (en) * | 2014-12-15 | 2016-07-13 | 无锡市普尔换热器制造有限公司 | Cleaning technology for titanium alloy plate finned heat exchanger |
CN106702383A (en) * | 2016-07-05 | 2017-05-24 | 中国航空工业集团公司北京航空材料研究院 | Metallographic-phase corrosion liquid of beta titanium alloy and corrosion method |
CN107817149A (en) * | 2017-12-06 | 2018-03-20 | 湘潭大学 | A kind of caustic solution of high niobium titanium alloy |
CN113008650A (en) * | 2019-12-20 | 2021-06-22 | 中核北方核燃料元件有限公司 | Metallographic corrosive agent and metallographic corrosive method for UN fuel pellets |
-
2009
- 2009-07-08 CN CN2009100124145A patent/CN101943640A/en active Pending
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102564830A (en) * | 2011-11-27 | 2012-07-11 | 西北有色金属研究院 | Chemical polishing agent |
CN103484863A (en) * | 2012-06-07 | 2014-01-01 | 宁波江丰电子材料有限公司 | Metallographic corrosive, corrosion method for metallographic sample and display method for metallographic structure |
CN102866048A (en) * | 2012-09-28 | 2013-01-09 | 昆明理工大学 | Preparation method of metallographic display sample of Ti-Cu laminar composite |
CN102928282A (en) * | 2012-11-02 | 2013-02-13 | 上海锅炉厂有限公司 | Method for solving problem of acid returning permeation of metal cracks subjected to corrosion of corrosives |
CN105750853A (en) * | 2014-12-15 | 2016-07-13 | 无锡市普尔换热器制造有限公司 | Cleaning technology for titanium alloy plate finned heat exchanger |
CN106702383A (en) * | 2016-07-05 | 2017-05-24 | 中国航空工业集团公司北京航空材料研究院 | Metallographic-phase corrosion liquid of beta titanium alloy and corrosion method |
CN107817149A (en) * | 2017-12-06 | 2018-03-20 | 湘潭大学 | A kind of caustic solution of high niobium titanium alloy |
CN113008650A (en) * | 2019-12-20 | 2021-06-22 | 中核北方核燃料元件有限公司 | Metallographic corrosive agent and metallographic corrosive method for UN fuel pellets |
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