CN116893157A - Analysis method for low carbon content in ultra-high purity titanium - Google Patents
Analysis method for low carbon content in ultra-high purity titanium Download PDFInfo
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- CN116893157A CN116893157A CN202310966121.0A CN202310966121A CN116893157A CN 116893157 A CN116893157 A CN 116893157A CN 202310966121 A CN202310966121 A CN 202310966121A CN 116893157 A CN116893157 A CN 116893157A
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000010936 titanium Substances 0.000 title claims abstract description 45
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 36
- 238000004458 analytical method Methods 0.000 title claims abstract description 10
- 239000007789 gas Substances 0.000 claims abstract description 67
- 238000005554 pickling Methods 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 33
- 238000012360 testing method Methods 0.000 claims abstract description 24
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 23
- 239000011593 sulfur Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000126 substance Substances 0.000 claims abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 36
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 30
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 22
- 229910052742 iron Inorganic materials 0.000 claims description 18
- AWXLLPFZAKTUCQ-UHFFFAOYSA-N [Sn].[W] Chemical compound [Sn].[W] AWXLLPFZAKTUCQ-UHFFFAOYSA-N 0.000 claims description 17
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 16
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 16
- 229910052802 copper Inorganic materials 0.000 claims description 16
- 239000010949 copper Substances 0.000 claims description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 15
- 239000006184 cosolvent Substances 0.000 claims description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims description 15
- 238000002329 infrared spectrum Methods 0.000 claims description 10
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 229920000742 Cotton Polymers 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000004566 IR spectroscopy Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 9
- 230000000052 comparative effect Effects 0.000 description 19
- 238000001514 detection method Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000004907 flux Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000013077 target material Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- DBGSRZSKGVSXRK-UHFFFAOYSA-N 1-[2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]acetyl]-3,6-dihydro-2H-pyridine-4-carboxylic acid Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)N1CCC(=CC1)C(=O)O DBGSRZSKGVSXRK-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010128 melt processing Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
- G01N2021/3568—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor applied to semiconductors, e.g. Silicon
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
- G01N2021/3572—Preparation of samples, e.g. salt matrices
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The application provides an analysis method for low carbon content in ultra-high purity titanium, which comprises the following steps: pickling the ultra-high purity titanium, heating and melting the ultra-high purity titanium in an oxygen atmosphere, collecting generated gas, and removing water in the gas to obtain gas to be detected; and testing the sulfur content in the gas to be tested, removing sulfur-containing substances in the gas to be tested, and testing the carbon content in the gas to be tested. The method can accurately test the carbon content (< 5 ppm) in the ultra-high purity titanium, and solves the problem of stable analysis of the ultra-low carbon content in the high purity titanium material.
Description
Technical Field
The application belongs to the field of analytical chemistry, and relates to a method for analyzing low carbon content in ultra-high purity titanium.
Background
As an important functional thin film material in the field of electronic information, the demand for high-purity titanium has rapidly increased in recent years with the rapid development of industries such as integrated circuits, flat panel displays, solar energy and the like in China. The magnetron sputtering technology (PVD) technology is one of key technologies for preparing thin film materials, and the high-purity titanium sputtering target material is a key consumable in the magnetron sputtering technology, so that the method has a wide market application prospect. The titanium target material is used as a coating material with high added value, and has strict requirements on chemical purity, tissue performance and the like.
The target acts as a cathode source in sputtering, and the impurity elements and gas Kong Gaza in the material are the main sources of contamination for the deposited film. The air hole inclusions can be basically removed in the nondestructive inspection process of the cast ingot, and the air hole inclusions which are not removed can generate a point discharge phenomenon (alignment) in the sputtering process, so that the quality of the film is affected. It is therefore particularly important to control the gaseous elements in the material.
Quantitative analysis of these elements is required during materials research, production and use. Since carbon, oxygen, nitrogen, and hydrogen are usually in a gaseous state at normal temperature and pressure, if these elements are present in the metal, they are called gaseous elements in the metal. Even carbon, sulfur is also referred to as a gaseous element in metals because it is in a form similar to hydrogen, nitrogen, and the assay method converts it into a gaseous compound.
Disclosure of Invention
In order to solve the technical problems in the prior art, the application provides the method for analyzing the content of low carbon in the ultra-high purity titanium, which can accurately test the carbon content (< 5 ppm) in the ultra-high purity titanium and solve the problem of stable analysis of the ultra-low carbon content in the high purity titanium material.
In order to achieve the technical effects, the application adopts the following technical scheme:
the application provides an analysis method for low carbon content in ultra-high purity titanium, which comprises the following steps:
pickling the ultra-high purity titanium, heating and melting the ultra-high purity titanium in an oxygen atmosphere, collecting generated gas, and removing water in the gas to obtain gas to be detected;
and testing the sulfur content in the gas to be tested, removing sulfur-containing substances in the gas to be tested, and testing the carbon content in the gas to be tested.
As a preferable technical scheme of the application, the pickling solution used for pickling is a mixed aqueous solution of hydrofluoric acid and nitric acid.
Preferably, the volume ratio of hydrofluoric acid to water in the pickling solution is 1:5-7, such as 1:5.2, 1:5.5, 1:5.8, 1:6, 1:6.2, 1:6.5 or 1:6.8, but is not limited to the listed technical scheme, and other non-listed values in the numerical range are equally applicable.
Preferably, the volume ratio of nitric acid to water in the pickling solution is 1:5-7, such as 1:5.2, 1:5.5, 1:5.8, 1:6, 1:6.2, 1:6.5 or 1:6.8, but is not limited to the listed technical scheme, and other non-listed values in the numerical range are equally applicable.
Preferably, the number of times of pickling is not less than 3, and the time of each pickling is not less than 1min.
According to the application, before the ultra-high purity titanium is subjected to melt processing, the ultra-high purity titanium is subjected to acid cleaning treatment, and the acid cleaning liquid with a special formula is adopted, so that impurities which are shielded for carbon element and sulfur element detection in the ultra-high purity titanium can be effectively removed, and the accuracy of the test is improved.
The number of times of pickling may be 4 times, 5 times, 6 times, 7 times, 8 times, 9 times, 10 times, or the like, and the time of pickling may be 2 minutes, 3 minutes, 4 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes, or 10 minutes, or the like, but the present application is not limited to the above-mentioned technical scheme, and other non-listed values in the above-mentioned numerical ranges are equally applicable.
As a preferable technical scheme of the application, the cosolvent is added in the heating and melting process.
As a preferable technical scheme of the application, the cosolvent is a mixture composed of tungsten tin, iron and copper.
Preferably, the mass ratio of the tungsten tin, the iron and the copper is 3-4:1:2-3, such as 3.1:1:2.1, 3.2:1:2.2, 3.3:1:2.3, 3.4:1:2.4, 3.5:1:2.5, 3.6:1:2.6, 3.7:1:2.7, 3.8:1:2.8 or 3.9:1:2.9, etc., but not limited to the listed technical scheme, and other non-listed values in the numerical range are equally applicable.
The existing national standard uses tungsten particles and tin particles as cosolvent, although the carbon content is low, when the detection blank is made, the blank slightly fluctuates due to the high blank, namely the analysis stability of the carbon content below the detection limit of 5ppm is reduced. The fluxing agent provided by the application can ensure the full combustion of the blank sample, the detection background is stable, and the detection limit of equipment and the detection stability of a sample are improved.
As a preferred embodiment of the present application, the method for removing moisture from the gas comprises passing the gas through anhydrous magnesium chloride.
In the present application, in addition to anhydrous magnesium chloride, other desiccants not containing sulfur or carbon may be used to remove moisture from the gas.
As a preferable technical scheme of the application, the method for testing the sulfur content in the gas to be tested is an infrared spectrometry.
According to the preferable technical scheme, the method for removing the sulfur-containing substances in the gas to be detected is to convert sulfur dioxide in the gas to be detected into sulfur trioxide, and absorbent cotton is adopted to absorb the sulfur trioxide.
In the present application, the conversion of sulfur dioxide to sulfur trioxide can be performed by any method in the prior art without introducing other carbon elements, and will not be described in detail herein.
As a preferable technical scheme of the application, the method for testing the carbon content in the gas to be tested is an infrared spectrometry.
As a preferable technical scheme of the application, the purity of the titanium in the ultra-high purity titanium is more than 99.995 percent.
As a preferable technical scheme of the application, the method for analyzing the content of low carbon in the ultra-high purity titanium comprises the following steps:
the ultra-high purity titanium is pickled by using a mixed aqueous solution of hydrofluoric acid and nitric acid, wherein the volume ratio of the hydrofluoric acid to water in the pickling solution is 1:5-7, the volume ratio of the nitric acid to water in the pickling solution is 1:5-7, the pickling times are not less than 3 times, and the pickling time is not less than 1min each time;
adding a cosolvent, heating and melting the ultra-high purity titanium in an oxygen atmosphere, and collecting generated gas, wherein the cosolvent is a mixture of tungsten tin, iron and copper, the mass ratio of the tungsten tin to the iron to the copper is 3-4:1:2-3, and removing water in the gas through anhydrous magnesium chloride to obtain gas to be detected;
and testing the sulfur content in the gas to be tested by using infrared spectrum, converting sulfur dioxide in the gas to be tested into sulfur trioxide, absorbing the sulfur trioxide by using absorbent cotton, removing sulfur-containing substances in the gas to be tested, and testing the carbon content in the gas to be tested by using infrared spectrum.
Compared with the prior art, the application has at least the following beneficial effects:
the application provides a method for analyzing the content of low carbon in ultra-high purity titanium, which can accurately test the carbon content (< 5 ppm) in the ultra-high purity titanium and solve the problem of stable analysis of the ultra-low carbon content in a high purity titanium material.
Drawings
FIG. 1 is a schematic flow chart of the method for analyzing the low carbon content in the ultra-high purity titanium.
The present application will be described in further detail below. The following examples are merely illustrative of the present application and are not intended to represent or limit the scope of the application as defined in the claims.
Detailed Description
The technical scheme of the application is further described below by the specific embodiments with reference to the accompanying drawings.
For a better illustration of the present application, which is convenient for understanding the technical solution of the present application, exemplary but non-limiting examples of the present application are as follows:
example 1
The embodiment provides a method for analyzing the content of low carbon in ultra-high purity titanium, the flow of which is shown in fig. 1, the method comprises the following steps:
the ultra-high purity titanium is pickled by using a mixed aqueous solution of hydrofluoric acid and nitric acid, wherein the volume ratio of the hydrofluoric acid to water in the pickling solution is 1:6, the volume ratio of the nitric acid to water in the pickling solution is 1:6, the pickling times are 3, and the pickling time is 1min each time;
adding a cosolvent, heating and melting the ultra-high purity titanium in an oxygen atmosphere, and collecting generated gas, wherein the cosolvent is a mixture of tungsten tin, iron and copper, the mass ratio of the tungsten tin to the iron to the copper is 3:1:2, and removing water in the gas through anhydrous magnesium chloride to obtain gas to be detected;
and testing the sulfur content in the gas to be tested by using infrared spectrum, converting sulfur dioxide in the gas to be tested into sulfur trioxide, absorbing the sulfur trioxide by using absorbent cotton, removing sulfur-containing substances in the gas to be tested, and testing the carbon content in the gas to be tested by using infrared spectrum, wherein the results are shown in table 1.
Example 2
The embodiment provides a method for analyzing the content of low carbon in ultra-high purity titanium, the flow of which is shown in fig. 1, the method comprises the following steps:
the ultra-high purity titanium is pickled by using a mixed aqueous solution of hydrofluoric acid and nitric acid, wherein the volume ratio of the hydrofluoric acid to water in the pickling solution is 1:7, the volume ratio of the nitric acid to water in the pickling solution is 1:7, the pickling times are 5, and the pickling time is 2min each time;
adding a cosolvent, heating and melting the ultra-high purity titanium in an oxygen atmosphere, and collecting generated gas, wherein the cosolvent is a mixture of tungsten tin, iron and copper, the mass ratio of the tungsten tin to the iron to the copper is 4:1:3, and removing water in the gas through anhydrous magnesium chloride to obtain gas to be detected;
and testing the sulfur content in the gas to be tested by using infrared spectrum, converting sulfur dioxide in the gas to be tested into sulfur trioxide, absorbing the sulfur trioxide by using absorbent cotton, removing sulfur-containing substances in the gas to be tested, and testing the carbon content in the gas to be tested by using infrared spectrum, wherein the results are shown in table 1.
Example 3
The embodiment provides a method for analyzing the content of low carbon in ultra-high purity titanium, the flow of which is shown in fig. 1, the method comprises the following steps:
the ultra-high purity titanium is pickled by using a mixed aqueous solution of hydrofluoric acid and nitric acid, wherein the volume ratio of the hydrofluoric acid to water in the pickling solution is 1:5, the volume ratio of the nitric acid to water in the pickling solution is 1:5, the pickling times are 6, and the pickling time is 1.5min each time;
adding a cosolvent, heating and melting the ultra-high purity titanium in an oxygen atmosphere, and collecting generated gas, wherein the cosolvent is a mixture of tungsten tin, iron and copper, the mass ratio of the tungsten tin to the iron to the copper is 3.5:1:2.5, and removing water in the gas through anhydrous magnesium chloride to obtain gas to be detected;
and testing the sulfur content in the gas to be tested by using infrared spectrum, converting sulfur dioxide in the gas to be tested into sulfur trioxide, absorbing the sulfur trioxide by using absorbent cotton, removing sulfur-containing substances in the gas to be tested, and testing the carbon content in the gas to be tested by using infrared spectrum, wherein the results are shown in table 1.
Comparative example 1
The comparative example was conducted in the same manner as in example 1, except that the pickling solution was an aqueous hydrofluoric acid solution.
Comparative example 2
The comparative example was conducted in the same manner as in example 1 except that the pickling solution was an aqueous nitric acid solution.
Comparative example 3
The comparative example was conducted in the same manner as in example 1, except that the pickling operation was not conducted.
Comparative example 4
This comparative example was conducted in the same manner as in example 1 except that a mixture of metallic tungsten and metallic tin (mass ratio: 4:1) was used as the flux.
Comparative example 5
This comparative example was conducted under the same conditions as in example 1 except that the flux was free of metallic copper (the mass ratio of tungsten tin to iron and the total mass added were the same as in example 1).
Comparative example 6
This comparative example was conducted under the same conditions as in example 1 except that the flux was free of metallic iron (the mass ratio of tungsten tin to iron and the total mass added were the same as in example 1).
The purities of tungsten tin, iron and copper in the fluxes used in examples 1 to 3 and comparative examples 1 to 6 were 99.99% or more, and the purities of an oxygen atmosphere were 99.999% or more.
TABLE 1
| C content/ppm | |
| Example 1 | 3 |
| Example 2 | 4 |
| Example 3 | 3 |
| Comparative example 1 | 11 |
| Comparative example 2 | 13 |
| Comparative example 3 | 25 |
| Comparative example 4 | 9 |
| Comparative example 5 | 11 |
| Comparative example 6 | 15 |
The applicant states that the detailed structural features of the present application are described by the above embodiments, but the present application is not limited to the above detailed structural features, i.e. it does not mean that the present application must be implemented depending on the above detailed structural features. It should be apparent to those skilled in the art that any modifications of the present application, equivalent substitutions of selected components of the present application, addition of auxiliary components, selection of specific modes, etc., are within the scope of the present application and the scope of the disclosure.
The preferred embodiments of the present application have been described in detail above, but the present application is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present application within the scope of the technical concept of the present application, and all the simple modifications belong to the protection scope of the present application.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the application can be made without departing from the spirit of the application, which should also be considered as disclosed herein.
Claims (10)
1. An analysis method for low carbon content in ultra-high purity titanium, which is characterized by comprising the following steps:
pickling the ultra-high purity titanium, heating and melting the ultra-high purity titanium in an oxygen atmosphere, collecting generated gas, and removing water in the gas to obtain gas to be detected;
and testing the sulfur content in the gas to be tested, removing sulfur-containing substances in the gas to be tested, and testing the carbon content in the gas to be tested.
2. The method according to claim 1, wherein the pickling solution used for pickling is a mixed aqueous solution of hydrofluoric acid and nitric acid;
preferably, the volume ratio of hydrofluoric acid to water in the pickling solution is 1:5-7;
preferably, the volume ratio of nitric acid to water in the pickling solution is 1:5-7;
preferably, the number of times of pickling is not less than 3, and the time of each pickling is not less than 1min.
3. The method of claim 1 or 2, wherein the heat and melt process incorporates a co-solvent.
4. The method of claim 3, wherein the cosolvent is a mixture of tungsten tin, iron, and copper;
preferably, the mass ratio of the tungsten tin to the iron to the copper is 3-4:1:2-3.
5. The method of any one of claims 1-4, wherein the removing moisture from the gas comprises passing the gas through anhydrous magnesium chloride.
6. The method according to any one of claims 1 to 5, wherein the method for measuring the sulfur content in the gas to be measured is infrared spectroscopy.
7. The method according to any one of claims 1 to 6, wherein the method for removing sulfur-containing substances in the test gas is to convert sulfur dioxide in the test gas into sulfur trioxide and absorb the sulfur trioxide with absorbent cotton.
8. The method according to any one of claims 1 to 7, wherein the method for measuring the carbon content in the gas to be measured is infrared spectroscopy.
9. The method according to any one of claims 1 to 8, wherein the purity of titanium in the ultra-high purity titanium is 99.995% or more.
10. The method of any one of claims 1-9, wherein the method of analysis comprises:
the ultra-high purity titanium is pickled by using a mixed aqueous solution of hydrofluoric acid and nitric acid, wherein the volume ratio of the hydrofluoric acid to water in the pickling solution is 1:5-7, the volume ratio of the nitric acid to water in the pickling solution is 1:5-7, the pickling times are not less than 3 times, and the pickling time is not less than 1min each time;
adding a cosolvent, heating and melting the ultra-high purity titanium in an oxygen atmosphere, and collecting generated gas, wherein the cosolvent is a mixture of tungsten tin, iron and copper, the mass ratio of the tungsten tin to the iron to the copper is 3-4:1:2-3, and removing water in the gas through anhydrous magnesium chloride to obtain gas to be detected;
and testing the sulfur content in the gas to be tested by using infrared spectrum, converting sulfur dioxide in the gas to be tested into sulfur trioxide, absorbing the sulfur trioxide by using absorbent cotton, removing sulfur-containing substances in the gas to be tested, and testing the carbon content in the gas to be tested by using infrared spectrum.
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