Cathode material of hollow cathode zinc lamp and preparation method thereof
Technical Field
The invention relates to a hollow cathode zinc lamp cathode material and a preparation method thereof, belonging to the technical field of analytical test instruments.
Background
The hollow cathode zinc lamp is used for atomic absorption spectrum analysis, atomic fluorescence spectrum analysis, molecular absorption spectrum analysis and other zinc sharp line light sources in instruments which need to use line spectrum light sources and reference wavelengths.
The selection and forming of the hollow cathode lamp cathode of transition element zinc generally uses pure metal zinc, because of the poor conductivity of zinc, the hollow cathode zinc lamp has low energy and short service life, especially the improvement of the sensitivity of atomic absorption spectrum analysis and atomic fluorescence analysis instruments, and requires longer service life, which depends on the improvement of light source part to a great extent, some analysis and test units require the hollow cathode zinc lamp to have high strength and high stability for pursuing the sensitivity of instruments, the service life is long, the melting point of zinc simple substance is relatively low, easy to volatilize and poor conductivity,
the energy-saving device cannot be used under a large current, and only the current can be increased to obtain high energy.
Disclosure of Invention
The invention aims to provide a hollow cathode zinc lamp cathode material which has better conductivity, higher light intensity, better stability and longer service life.
The invention also aims to provide a preparation method of the cathode material of the hollow cathode zinc lamp.
In order to achieve the purpose, the invention adopts the following technical scheme:
the cathode material of the hollow cathode zinc lamp is copper-zinc alloy, wherein the mass percent of zinc is 15-85%, and the mass percent of copper is 15-85%.
A preparation method of the cathode material of the hollow cathode zinc lamp comprises the following steps:
(1) weighing metal copper and metal zinc according to the proportion;
(2) putting the weighed copper and zinc into a melting crucible of a vacuum induction melting furnace, and vacuumizing until the vacuum degree of a hearth is lower than 1 multiplied by 10-3Pa;
(3) Starting induction heating, heating copper and zinc in a crucible to 800-1500 ℃, melting the raw materials, and simultaneously performing rapid electromagnetic stirring for 15-180 min;
(4) and after the smelting is finished, pouring the copper-zinc alloy liquid into a forced cooling casting mold, wherein the cooling speed is 15-100 ℃/min, and demolding to obtain the copper-zinc alloy.
Preferably, the purity of the metallic copper is greater than 99.99%. The purity of the metal zinc is more than 99.99%.
Preferably, the melting crucible is a copper crucible, a graphite crucible or an alumina crucible. The casting mould is a copper casting mould or a graphite casting mould.
The invention has the advantages that:
the invention adopts copper-zinc alloy to replace pure metal zinc as the cathode material of the hollow cathode zinc lamp, the copper-zinc alloy has higher melting point than zinc and better conductivity, and the hollow cathode zinc lamp using the copper-zinc alloy as the cathode has higher light intensity, better stability and longer service life compared with the hollow cathode zinc lamp using pure metal zinc as the cathode. Specifically, (1) stability drift < ± 0.6% (after half an hour of preheating); (2) compared with zinc as cathode, the service life is prolonged by more than 50%.
Detailed Description
The present invention is further illustrated by the following specific embodiments, which are not meant to limit the scope of the invention.
Example 1
The cathode material copper-zinc alloy for hollow cathode zinc lamp has copper content of 70% and zinc content of 30%. The preparation method comprises the following steps:
(1) weighing metal copper and metal zinc according to the proportion, wherein the metal copper and the metal zinc are in a block shape, and the purity of the metal copper and the metal zinc is more than 99.99 percent;
(2) putting copper and zinc raw materials into a copper crucible, putting the crucible into a vacuum induction melting furnace, and vacuumizing a hearth to a vacuum degree of 9.2 multiplied by 10-4Pa;
(3) And starting induction heating, heating to 950 ℃, melting the raw materials, carrying out strong electromagnetic stirring simultaneously, wherein the melting time is 30min, pouring the melted copper-zinc 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 25 ℃/min, cooling to room temperature, and taking out to obtain the copper-zinc alloy.
(4) The prepared copper-zinc alloy is used as a cathode material to manufacture a hollow cathode zinc lamp for an atomic absorption spectrometer, and the test conditions are as follows: the slit is 0.2nm, the wavelength is 213.9nm, and compared with the old lamp (cathode material is pure zinc, the purity is 99.99%), the performance is shown in table 2, and the table shows that the performance of the hollow cathode zinc lamp made of the copper-zinc alloy cathode material prepared by the invention is obviously superior to that of the old lamp.
Example 2
The cathode material copper-zinc alloy for hollow cathode zinc lamp has copper content of 60 wt% and zinc content of 40 wt%. The preparation method comprises the following steps:
(1) weighing metal copper and metal zinc according to the proportion, wherein the metal copper and the metal zinc are in a block shape, and the purity of the metal copper and the metal zinc is more than 99.99 percent;
(2) putting copper and zinc raw materials into a copper crucible, putting the crucible into a vacuum induction melting furnace, and vacuumizing a hearth to a vacuum degree of 8.7 multiplied by 10-4Pa;
(3) Starting induction heating, heating to 1150 ℃, melting the raw materials, simultaneously carrying out strong electromagnetic stirring, wherein the melting time is 40min, pouring the melted copper-zinc 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 cooling speed of 35 ℃/min, cooling to room temperature, and taking out to obtain the copper-zinc alloy.
(4) The prepared copper-zinc alloy is used as a cathode material to manufacture a hollow cathode zinc lamp for an atomic absorption spectrometer, and the test conditions are as follows: the slit is 0.2nm, the wavelength is 213.9nm, and compared with the old lamp (cathode material is pure zinc, the purity is 99.99%), the performance is shown in table 2, and the table shows that the performance of the hollow cathode zinc lamp made of the copper-zinc alloy cathode material prepared by the invention is obviously superior to that of the old lamp.
Example 3
The cathode material copper-zinc alloy for hollow cathode zinc lamp has copper content of 55% and zinc content of 45%. The preparation method comprises the following steps:
(1) weighing metal copper and metal zinc according to the proportion, wherein the metal copper and the metal zinc are in a block shape, and the purity of the metal copper and the metal zinc is more than 99.99 percent;
(2) putting copper and zinc raw materials into a copper crucible, putting the crucible into a vacuum induction melting furnace, and vacuumizing a hearth to a vacuum degree of 9.4 multiplied by 10-4Pa;
(3) Starting induction heating, heating to 1250 ℃, melting the raw materials, simultaneously carrying out strong electromagnetic stirring, wherein the melting time is 60min, pouring the melted copper-zinc 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, controlling the cooling speed to be 45 ℃/min, cooling to room temperature, and taking out to obtain the copper-zinc alloy.
(4) The prepared copper-zinc alloy is used as a cathode material to manufacture a hollow cathode zinc lamp for an atomic absorption spectrometer, and the test conditions are as follows: the slit is 0.2nm, the wavelength is 213.9nm, and compared with the old lamp (cathode material is pure zinc, the purity is 99.99%), the performance is shown in table 2, and the table shows that the performance of the hollow cathode zinc lamp made of the copper-zinc alloy cathode material prepared by the invention is obviously superior to that of the old lamp.
Performance test methods and results
(1) Stability testing method
Preheating for 30min under the condition of spectral bandwidth of 0.2nm, and recording zero drift (calculated by taking the starting point as a reference) in corresponding time by using an instantaneous measurement mode or a time constant of not more than 0.5s and using a sensitive line wavelength of 213.9nm and a current of 8 mA.
(2) Life test method
a. And (3) detection period: 2000mA · h, 3000mA · h, 3500mA · h, 4000mA · h, 4500mA · h.
b. End of life determination
The determination of the end of life of the hollow cathode lamp is shown in table 1.
TABLE 1 determination table for the end of life of hollow cathode lamp
(3) Hollow cathode zinc lamp performance test results
The performance test data of the hollow cathode zinc lamp are shown in the table 2, and the performance of the hollow cathode zinc lamp is obviously superior to that of the old lamp.
TABLE 2 comparison of the Performance of hollow cathode Zinc lamps