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A method for determining niobium content in titanium-niobium alloy

A titanium-niobium alloy and content technology, applied in the field of chemical analysis, can solve the problems that the detection method cannot be applied, the niobium content cannot be detected, and the popularization and application of memory alloy materials are restricted, and the effect of clarification and stability of the sample solution is achieved.

Active Publication Date: 2019-11-05
CHENGDU AIRCRAFT INDUSTRY GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, there is no unified and mature detection technology for the determination of memory alloys NiTiNb and Ti45Nb in China, and it is urgent to study the detection technology.
[0003] Especially for the detection technology of 40.0% to 50.0% high content of niobium in Ti45Nb memory alloy material, there is no open and feasible standard at home and abroad.
Generally, the public detection techniques are all for the detection of niobium in ferroniobium, tantalum ore, niobium ore, steel and alloys, etc. The limitations of the detection method are: 1) The existing detection method usually detects a constant niobium content , cannot detect niobium content as high as 40.0% to 50.0%
For example, HB 5220.34-2008 "Determination of niobium content by chlorosulfonol C absorbance photometry" can only measure 0.10% to 3.00% of niobium content in superalloys; GB / T4698.22-1996 "5-Br-PADAP spectrophotometric measurement "Niobium content" can only measure 0.20% ~ 3.00% niobium content in titanium and titanium alloys; GB / T 223.38-1985 "Ion exchange separation-gravimetric determination of niobium content" can only measure 1.00% ~ 5.00% niobium content in steel ; Such as ISO 9441 "PAR Spectrophotometric Determination of Niobium Content" can only measure the niobium content of 0.005% to 1.3% in iron and steel; such as ΓΟCT 12361 "PAR Spectrophotometric Determination of Niobium Content" can only measure the content of niobium in alloy steel and high alloy steel Niobium content of 0.01 % to 8.00 %
2) The types of target materials detected by existing detection methods are only steel, alloy steel, niobium ore, etc. These types of materials are very different from Ti45Nb memory alloy materials and cannot be used directly
Such as HB5220.33-2008 "Chemical Analysis Method of Superalloys for the Determination of Niobium Content by Tetraphenylarsenic Chloride Hydrochloride Gravimetric Method", the measurement range is >1.00%, but because the target material is a superalloy, the chemical composition of the superalloy is different from that of Ti45Nb. The composition of elemental alloys is very different, and its detection method cannot be applied
[0004] Due to the limitations of the existing domestic technology restricting the promotion and application of memory alloy materials, it can be seen that a unified, high-precision, and repeatable detection method has been developed to accurately determine the content of 40.0% to 50.0% in Ti45Nb memory alloy materials. % high niobium content is not only conducive to the development of new materials but also ensures the application of materials in products

Method used

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  • A method for determining niobium content in titanium-niobium alloy
  • A method for determining niobium content in titanium-niobium alloy
  • A method for determining niobium content in titanium-niobium alloy

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Experimental program
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Effect test

Embodiment 1

[0062] 3 sample test material

[0063] Weigh 0.0998g sample material, accurate to 0.0001g.

[0064] 4 Preparation of test solution

[0065] 4.1 Put the sample (3) in a 150 mL polytetrafluoroethylene beaker, add 5 mL of nitric acid (2.1), dropwise add 1 mL of hydrofluoric acid (2.3), heat at low temperature until the sample dissolves, cool slightly, add 20 mL of sulfuric acid (2.5), heat at low temperature until the volume of the solution is about 20mL, remove it, transfer it into a 250mL beaker, heat until sulfuric acid fumes are emitted, and heat until the first sulfuric acid fumes are emitted for about 3~4min, remove the beaker and cool slightly, and then pour into the beaker Blow in a small amount of water, heat until the second sulfuric acid fume is emitted for about 2~3 minutes, cool, add 20 mL tartaric acid solution (2.6), 5 mL ammonium fluoride solution (2.7), boil for 2~3 minutes, take it off, add 10 Continue to boil mL of saturated boric acid solution (2.8), cool to...

Embodiment 2

[0082] 3 sample test material

[0083] Weigh 0.1998 g sample material, accurate to 0.0001 g.

[0084] 4 Preparation of test solution

[0085]4.1 Put the sample (3) in a 150 mL polytetrafluoroethylene beaker, add 10 mL of nitric acid (2.1), dropwise add 2 mL of hydrofluoric acid (2.3), heat at low temperature until the sample dissolves, cool slightly, add 25 mL of sulfuric acid (2.5), heat at low temperature until the volume of the solution is about 20mL, remove it, transfer it into a 250mL beaker, heat until sulfuric acid fumes are emitted, and heat until the first sulfuric acid fumes are emitted for about 3~4min, remove the beaker and cool slightly, and then pour into the beaker Blow in a small amount of water, heat until the second sulfuric acid fume is emitted for about 2~3 minutes, cool, add 20 mL tartaric acid solution (2.6), 5 mL ammonium fluoride solution (2.7), boil for 2~3 minutes, take it off, add 10 Continue to boil mL of saturated boric acid solution (2.8), cool ...

Embodiment 3

[0102] 3 samples

[0103] Weigh 0.1502g sample material, accurate to 0.0001g.

[0104] 4 Preparation of test solution

[0105] 4.1 Put the sample (3) in a 150 mL polytetrafluoroethylene beaker, add 8 mL of nitric acid (2.1), dropwise add 2 mL of hydrofluoric acid (2.3), heat at low temperature until the sample dissolves, cool slightly, add 23 mL of sulfuric acid (2.5), heat at low temperature until the volume of the solution is about 20mL, remove it, transfer it into a 250mL beaker, heat until sulfuric acid fumes are emitted, and heat until the first sulfuric acid fumes are emitted for about 3~4min, remove the beaker and cool slightly, and then pour into the beaker Blow in a small amount of water, heat until the second sulfuric acid fume is emitted for about 2~3 minutes, cool, add 20 mL tartaric acid solution (2.6), 5 mL ammonium fluoride solution (2.7), boil for 2~3 minutes, take it off, add 10 Continue to boil mL of saturated boric acid solution (2.8), cool to room tempera...

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Abstract

The invention discloses a method for determining the niobium content in a titanium-niobium alloy. The method comprises: preparing a Ti45Nb sample solution; taking the Ti45Nb sample solution, and developing the color with a PAR solution; measuring the absorbance of the developed solution at a wavelength of 520-530 nm on a spectrophotometer; preparing a niobium standard solution; preparing a titanium base solution; preparing a series of standard solutions for establishing the niobium concentrations from 0.00%-0.25*10<-3>% of a curve, wherein the solutions are corresponding to the niobium concentrations from 0-50% in the sample; establishing a working curve, wherein a series of standard solutions of S6 are subjected to color development, the absorbance values are measured, and the working curve using the concentrations as a abscissa and the absorbance values as an ordinate is established; and dissolving the Ti45Nb sample, developing the color, determining the absorbance value, and obtaining the corresponding concentration value in the established working curve by using the determined absorbance value so as to obtain the niobium content in the Ti45Nb memory alloy material. According to the present invention, the method has advantages of stable color development, satisfactory working curve, and good data repeatability.

Description

technical field [0001] The invention relates to a chemical analysis method, in particular to a method for determining the content of metal niobium in alloys by absorbance photometry. Background technique [0002] Memory alloy materials include NiTiNb, Ti45Nb, etc. In order to ensure the reversible phase transition performance of the material, high content of niobium Nb, titanium Ti, nickel Ni and other elements are added to the material, which is rare in other conventional materials. The change of the content of these elements in the material will directly affect the performance of the material. Therefore, only by accurately grasping the exact content of these elements in each batch of materials can the physical properties and process performance of the materials be further guaranteed. However, at present, there is no unified and mature detection technology for the determination of memory alloys NiTiNb and Ti45Nb in China, and research on detection technology is urgently ne...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/78G01N21/31
CPCG01N21/31G01N21/78
Inventor 吴旻李东升孙涛李刚杨春晟陈莉王璐璐王巧利刘默涵何六一
Owner CHENGDU AIRCRAFT INDUSTRY GROUP
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