CN112126814B - Copper-bismuth alloy for hollow cathode bismuth lamp cathode and preparation method thereof - Google Patents
Copper-bismuth alloy for hollow cathode bismuth lamp cathode and preparation method thereof Download PDFInfo
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- CN112126814B CN112126814B CN201910553858.3A CN201910553858A CN112126814B CN 112126814 B CN112126814 B CN 112126814B CN 201910553858 A CN201910553858 A CN 201910553858A CN 112126814 B CN112126814 B CN 112126814B
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- 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
- G01N21/3103—Atomic absorption analysis
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
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Abstract
The invention relates to a copper-bismuth alloy for a cathode of a hollow cathode bismuth lamp and a preparation method thereof, belonging to the technical field of analytical test instruments. The mass fraction of bismuth in the copper-bismuth alloy is 8-70 wt%, and the mass fraction of copper is 30-92 wt%. Firstly, weighing metal copper and metal bismuth according to mass fraction; putting copper and bismuth into a melting crucible of a vacuum induction melting furnace, and vacuumizing; starting induction heating, heating the copper and the bismuth in the crucible, heating to a smelting temperature, melting the copper and the bismuth into alloy liquid, and simultaneously starting high-speed electromagnetic stirring for induction smelting; and after the completion, pouring the copper-bismuth alloy liquid into a forced cooling casting mold, cooling, and demolding to obtain a copper-bismuth alloy ingot. Compared with a bismuth lamp adopting a pure bismuth cathode material, the bismuth lamp adopting the alloy as the cathode has good stability, the drift is less than 0.6%, the service life is prolonged by more than 50%, and the problems of overlarge stability drift and short service life of the bismuth lamp in atomic absorption and atomic fluorescence analysis are obviously improved.
Description
Technical Field
The invention belongs to the technical field of analytical test instruments, and particularly relates to a copper-bismuth alloy for a cathode material of a hollow cathode bismuth lamp and a preparation method thereof.
Background
The hollow cathode bismuth lamp is used for atomic absorption spectrum analysis, atomic fluorescence spectrum analysis, molecular absorption spectrum analysis and other bismuth sharp line light sources in instruments needing to use line spectrum light sources and reference wavelengths.
Conventionally, pure bismuth processed moldings have been generally used for selection and processing of hollow cathode lamp cathodes of transition element bismuth, and since the resistivity of bismuth is relatively large and the electrical conductivity is poor, the electrical conductivity of the bismuth moldings is poor, the hollow cathode bismuth lamp has low energy, large stability drift, and short service life. The improvement of the sensitivity of modern atomic absorption spectrum analysis and atomic fluorescence analysis instruments and the requirement of longer service life depend on the improvement of a light source part to a great extent, some analysis and test units require a hollow cathode bismuth lamp to have high strength and high stability and longer service life in order to pursue the sensitivity of the instruments, the bismuth metal has larger resistivity and poor conductivity and is difficult to use under large current, and the problems of poor stability, easy damage, short service life and the like are caused because the high energy is required to be obtained during analysis and test and only the current is increased.
Disclosure of Invention
The invention provides a copper-bismuth alloy for a cathode material of a hollow cathode bismuth lamp and a preparation method thereof, aiming at solving the problems of low energy, large stability drift and short service life of the hollow cathode bismuth lamp in the prior art.
The invention adopts the copper-bismuth alloy cathode to replace the pure bismuth processing formed body cathode, the copper-bismuth alloy has lower resistivity than bismuth and better conductivity, and the hollow cathode bismuth lamp using the copper-bismuth alloy cathode has better stability and longer service life compared with the hollow cathode bismuth lamp using the pure bismuth forming body as the cathode.
The purpose of the invention is realized by the following technical scheme:
the cathode material copper-bismuth alloy for hollow cathode bismuth lamp has bismuth in 8-70 wt% and copper in 30-92 wt%.
Preferably, the mass fraction of bismuth in the copper-bismuth alloy is 15 wt% -65 wt%, and the mass fraction of copper is 35 wt% -85 wt%.
Preferably, the mass fraction of bismuth in the copper-bismuth alloy is 20 wt% -60 wt%, and the mass fraction of copper is 40 wt% -80 wt%.
More preferably, the mass fraction of bismuth in the copper-bismuth alloy is 25 wt% to 55 wt%, and the mass fraction of copper is 45 wt% to 75 wt%.
Most preferably, the mass fraction of bismuth in the copper-bismuth alloy is 28-42 wt%, and the mass fraction of copper is 58-72 wt%.
The preparation method of the cathode material copper-bismuth alloy of the hollow cathode bismuth lamp comprises the following steps:
(1) weighing metal copper and metal bismuth according to the mass fraction;
(2) putting copper and bismuth into a melting crucible of a vacuum induction melting furnace, and vacuumizing;
(3) starting induction heating, heating the copper and the bismuth in the crucible, heating to a smelting temperature, melting the copper and the bismuth into alloy liquid, and simultaneously starting high-speed electromagnetic stirring for induction smelting;
(4) and after the smelting is finished, pouring the copper-bismuth alloy liquid into a forced cooling casting mold, cooling, and demolding to obtain a copper-bismuth alloy ingot.
Preferably, in the step (1), the purity of the copper is more than or equal to 99.99 wt%, and the purity of the bismuth is more than or equal to 99.99 wt%; the metal copper and the metal bismuth can be in the form of blocks or particles.
Preferably, in the step (2), the crucible can be a graphite crucible, a magnesia crucible or an alumina crucible; in the vacuum induction melting furnace, the vacuum degree of a hearth is required to be controlled to be lower than 1 xl 0-3Pa。
Preferably, in the step (3), the induction melting may adopt medium-frequency induction melting or high-frequency induction melting. The smelting temperature is 850-1450 ℃, and more preferably 1200-1360 ℃; the melting time is 20min to 200min, and more preferably 30min to 60 min.
Preferably, in step (4), the mold may be a copper mold or a graphite mold. The cooling rate is 30 ℃/min to 170 ℃/min, and more preferably 30 ℃/min to 80 ℃/min.
The invention discloses an application of a copper-bismuth alloy in preparing a cathode material of a hollow cathode bismuth lamp, which comprises the following steps:
the cathode material of the hollow cathode bismuth lamp is prepared by adopting the copper-bismuth alloy. Compared with a hollow cathode bismuth lamp with pure bismuth as a cathode, the hollow cathode bismuth lamp adopting the cathode material has better stability and longer service life, and has the following performances:
(1) stability drift < 0.6%;
(2) the service life is prolonged by more than 50%.
The invention has the beneficial effects that: the hollow cathode bismuth lamp using the copper-bismuth alloy as the cathode has higher light intensity, higher stability and longer service life.
Compared with the pure bismuth cathode material, the copper-bismuth alloy of the invention has good stability, drift is less than 0.6%, the service life is prolonged by more than 50%, and the problems of overlarge stability drift and short service life of the bismuth lamp in atomic absorption and atomic fluorescence analysis are obviously improved.
Detailed Description
The mass fraction of bismuth in the copper-bismuth alloy is 8-70 wt%, and the mass fraction of copper is 30-92 wt%. The copper-bismuth alloy can replace pure bismuth to be used as a cathode material of a hollow cathode bismuth lamp.
The invention relates to a preparation method of a copper-bismuth alloy for a cathode of a hollow cathode bismuth lamp, which comprises the following steps:
(1) weighing metal copper (blocks or particles) and metal bismuth (blocks or particles) according to the proportion; the purity of the metallic copper and the metallic bismuth is more than 99.99 wt%.
(2) Putting the weighed copper and bismuth into a melting crucible of a vacuum induction melting furnace, and vacuumizing until the vacuum degree of a hearth is lower than 1 xl 0-3Pa; the crucible used for vacuum medium-frequency induction melting is a graphite crucible, a magnesia crucible or an alumina crucible.
(3) Starting induction heating, heating the copper and the bismuth in the crucible to 850-1450 ℃, melting the raw materials of the copper and the bismuth, and simultaneously performing high-speed electromagnetic stirring on the alloy liquid for 20-200 min; the alloy liquid is subjected to high-speed electromagnetic stirring while induction smelting, so that the chemical components of the alloy liquid are uniform and consistent. The copper-bismuth alloy smelting can use vacuum medium-frequency induction smelting or vacuum high-frequency induction smelting.
(4) After the smelting is finished, pouring the copper-bismuth alloy liquid into a forced cooling casting mold, wherein the casting mold used for casting ingots after the copper-bismuth alloy is smelted is a copper casting mold or a graphite casting mold, the cooling speed is 30-170 ℃/min, and the copper-bismuth alloy is obtained after demolding and is used as a raw material for processing hollow cathode bismuth lamps.
Example 1
The cathode material copper-bismuth alloy of the hollow cathode bismuth lamp comprises 76 wt% of copper and 24 wt% of bismuth. The preparation steps are as follows:
(1) weighing metal copper and metal bismuth according to the proportion, wherein the metal copper and the metal bismuth are blocky and have the purity of more than 99.99 wt%;
(2) putting copper and bismuth raw materials into a graphite crucible, putting the crucible into a vacuum induction melting furnace, and vacuumizing a hearth until the vacuum degree is 8.8 xl 0-4Pa；
(3) Starting induction heating, heating to 1270 ℃, melting the raw materials, simultaneously carrying out strong electromagnetic stirring, wherein the melting time is 36min, pouring the melted copper-bismuth alloy liquid into a copper casting mold with a cooling pipe after the melting is finished, introducing water into the cooling pipe for cooling, controlling the water flow, cooling at the speed of 34 ℃/min, cooling to room temperature, and taking out to obtain the copper-bismuth alloy ingot.
(4) The prepared copper-bismuth alloy is used as a cathode material to manufacture a hollow cathode bismuth lamp for an atomic absorption spectrometer, and the test conditions are as follows: the slit is 0.2nm, the wavelength is 306.8nm, the preheating is carried out for 30min, compared with the old lamp (the cathode material is a pure bismuth forming body, the purity is 99.99 wt%), the performance is shown in the table l, and the performance of the hollow cathode bismuth lamp manufactured by the copper-bismuth alloy cathode material prepared by the invention is obviously superior to the old lamp.
Example 2
The cathode material copper-bismuth alloy of the hollow cathode bismuth lamp comprises 68 wt% of copper and 32 wt% of bismuth. The preparation steps are as follows:
(1) weighing metal copper and metal bismuth according to the proportion, wherein the metal copper and the metal manganese are particles, and the purity of the metal copper and the metal manganese is more than 99.99 wt%;
(2) putting copper and bismuth raw materials into a magnesia crucible, putting the crucible into a vacuum induction melting furnace, and vacuumizing a hearth until the vacuum degree is 7.6 xl 0-4Pa；
(3) Starting induction heating, heating to 1220 ℃, melting the raw materials, simultaneously carrying out strong electromagnetic stirring, wherein the melting time is 42min, pouring the melted copper-bismuth alloy liquid into a graphite casting mold with a cooling pipe after the melting is finished, introducing water into the cooling pipe for cooling, controlling the water flow, cooling at the cooling speed of 48 ℃/min, cooling to room temperature, and taking out to obtain the copper-bismuth alloy ingot.
(4) The prepared copper-bismuth alloy is used as a cathode material to manufacture a hollow cathode bismuth lamp for an atomic absorption spectrometer, and the test conditions are as follows: the slit is 0.2nm, the wavelength is 306.8nm, the preheating is carried out for 30min, compared with the old lamp (the cathode material is a pure bismuth metal forming body, the purity is 99.99 wt%), the performance is shown in the table l, and the performance of the hollow cathode bismuth lamp manufactured by the copper-bismuth alloy cathode material prepared by the invention is obviously superior to the old lamp.
Example 3
A cathode material copper-bismuth alloy of a hollow cathode bismuth lamp is provided, wherein the mass of copper is 63 wt%, and the mass fraction of bismuth is 37 wt%. The preparation steps are as follows:
(1) weighing metal copper and metal bismuth according to the proportion, wherein the metal copper and the metal bismuth are blocky and have the purity of more than 99.99 wt%;
(2) putting copper and bismuth raw materials into an alumina crucible, putting the crucible into a vacuum induction melting furnace, and vacuumizing a hearth until the vacuum degree is 6.8 xl 0-4Pa；
(3) Starting induction heating, heating to 1310 ℃, melting the raw materials, simultaneously carrying out strong electromagnetic stirring, wherein the melting time is 35min, pouring the melted copper-bismuth alloy liquid into a copper casting mold with a cooling pipe after the melting is finished, introducing water into the cooling pipe for cooling, controlling the water flow, cooling at the speed of 58 ℃/min, cooling to room temperature, and taking out to obtain the copper-bismuth alloy ingot.
(4) The prepared copper-bismuth alloy is used as a cathode material to manufacture a hollow cathode bismuth lamp for an atomic absorption spectrometer, and the test conditions are as follows: the slit is 0.2nm, the wavelength is 306.8nm, the preheating is carried out for 30min, compared with the old lamp (the cathode material is a pure bismuth forming body, the purity is 99.99 wt%), the performance is shown in the table l, and the performance of the hollow cathode bismuth lamp manufactured by the copper-bismuth alloy cathode material prepared by the invention is obviously superior to the old lamp.
TABLE 1 comparison of the Performance of New and old hollow cathode bismuth lamps
As can be seen from Table 1, the hollow cathode bismuth lamp using the Cu-Bi alloy prepared by the invention as the cathode material has stability drift of less than 0.6% and service life improved by more than 50% compared with the pure bismuth cathode material, so that the stability drift of the bismuth lamp in atomic absorption and atomic fluorescence analysis is greatly reduced and the service life is greatly improved.
The above embodiments are only used for illustrating but not limiting the technical solutions of the present invention, and although the above embodiments describe the present invention in detail, those skilled in the art should understand that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention and any modifications and equivalents may fall within the scope of the claims.
Claims (8)
1. The application of the copper-bismuth alloy in preparing the cathode material of the hollow cathode bismuth lamp is characterized in that: the mass fraction of bismuth in the copper-bismuth alloy is 8-70 wt%, and the mass fraction of copper is 30-92 wt%.
2. The use of the copper-bismuth alloy of claim 1 in the preparation of cathode materials for hollow cathode bismuth lamps, characterized in that: the preparation method of the copper-bismuth alloy comprises the following steps:
(1) weighing metal copper and metal bismuth according to the mass fraction;
(2) putting copper and bismuth into a melting crucible of a vacuum induction melting furnace, and vacuumizing;
(3) starting induction heating, heating the copper and the bismuth in the crucible, heating to a smelting temperature of 850-1450 ℃, melting the copper and the bismuth into alloy liquid, and simultaneously starting high-speed electromagnetic stirring for induction smelting;
(4) and after the smelting is finished, pouring the copper-bismuth alloy liquid into a forced cooling casting mold, cooling at the cooling speed of 30-170 ℃/min, and demolding to obtain the copper-bismuth alloy ingot.
3. The use of the copper-bismuth alloy of claim 2 in the preparation of cathode materials for hollow cathode bismuth lamps, characterized in that: the purity of the copper is more than or equal to 99.99 wt%, and the purity of the bismuth is more than or equal to 99.99 wt%.
4. The use of the copper-bismuth alloy of claim 2 in the preparation of cathode materials for hollow cathode bismuth lamps, characterized in that: the crucible is a graphite crucible, a magnesia crucible or an alumina crucible.
5. The use of the copper-bismuth alloy of claim 2 in the preparation of cathode materials for hollow cathode bismuth lamps, characterized in that: the vacuum degree in the vacuum induction smelting furnace is lower than 1 xl 0-3Pa。
6. The use of the copper-bismuth alloy of claim 2 in the preparation of cathode materials for hollow cathode bismuth lamps, characterized in that: the induction melting is medium-frequency induction melting or high-frequency induction melting.
7. The use of the copper-bismuth alloy of claim 6 in the preparation of cathode materials for hollow cathode bismuth lamps, wherein: the smelting time is 20 min-200 min.
8. The use of the copper-bismuth alloy of claim 2 in the preparation of cathode materials for hollow cathode bismuth lamps, characterized in that: the casting mould is a copper casting mould or a graphite casting mould.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101770925A (en) * | 2008-12-30 | 2010-07-07 | 北京有色金属研究总院 | Cathode material of hollow-cathode lamp and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4437038A (en) * | 1979-05-29 | 1984-03-13 | Westinghouse Electric Corp. | Hollow cathode lamp with improved stability alloy for the cathode |
| EP0246248A1 (en) * | 1985-11-28 | 1987-11-25 | Photron Pty. Ltd. | Hollow cathode assembly and lamp |
| CN109909511B (en) * | 2019-03-22 | 2022-05-03 | 中国工程物理研究院化工材料研究所 | Preparation method and application of bismuth-based hollow nano material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101770925A (en) * | 2008-12-30 | 2010-07-07 | 北京有色金属研究总院 | Cathode material of hollow-cathode lamp and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| Constraints imposed upon theories of the vacuum arc cathode region by specific ion energy measurements;H.Craig Miller;《Journal of Applied Physics》;19810731;4523-4530 * |
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