CN114560624A - Glass pipeline device for preparing polarized helium three-glass gas chamber and preparation method of glass gas chamber - Google Patents
Glass pipeline device for preparing polarized helium three-glass gas chamber and preparation method of glass gas chamber Download PDFInfo
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- CN114560624A CN114560624A CN202210343282.XA CN202210343282A CN114560624A CN 114560624 A CN114560624 A CN 114560624A CN 202210343282 A CN202210343282 A CN 202210343282A CN 114560624 A CN114560624 A CN 114560624A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B23/00—Re-forming shaped glass
- C03B23/04—Re-forming tubes or rods
- C03B23/13—Reshaping combined with uniting or heat sealing, e.g. for making vacuum bottles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B31/00—Packaging articles or materials under special atmospheric or gaseous conditions; Adding propellants to aerosol containers
- B65B31/02—Filling, closing, or filling and closing, containers or wrappers in chambers maintained under vacuum or superatmospheric pressure or containing a special atmosphere, e.g. of inert gas
- B65B31/025—Filling, closing, or filling and closing, containers or wrappers in chambers maintained under vacuum or superatmospheric pressure or containing a special atmosphere, e.g. of inert gas specially adapted for rigid or semi-rigid containers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B51/00—Devices for, or methods of, sealing or securing package folds or closures; Devices for gathering or twisting wrappers, or necks of bags
- B65B51/10—Applying or generating heat or pressure or combinations thereof
- B65B51/14—Applying or generating heat or pressure or combinations thereof by reciprocating or oscillating members
- B65B51/142—Closing bottle necks or tubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B69/00—Unpacking of articles or materials, not otherwise provided for
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/10—Nuclear fusion reactors
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Abstract
The application discloses a glass pipeline device for preparing a polarized helium three-glass gas chamber. The glass pipeline device comprises a main glass pipeline and an alkali metal bifurcated pipe, wherein the alkali metal bifurcated pipe comprises an alkali metal ampoule test tube, an alkali metal purifying tube and an alkali metal storage tube which are communicated in sequence, and a free falling pipe arranged at the joint of the alkali metal purifying tube and the alkali metal ampoule test tube. When the alkali metal purification pipe is obliquely arranged, the free falling pipe is vertically arranged or is approximately vertically arranged; and the free falling body pipe is a closed pipe and is communicated with the alkali metal ampoule test tube through an opening, and a magnetic metal hammer capable of moving freely is placed in the free falling body pipe. The application also discloses a method for preparing the helium tri-neutron polarized glass gas chamber by adopting the glass pipeline device. The design of the glass pipeline in the application not only can realize the purification of alkali metal, but also can realize the simple recovery of the magnetic metal hammer, and the preparation period of the polarized helium three-glass gas chamber is shortened while the quality of the helium three-glass gas chamber is improved.
Description
Technical Field
The invention relates to a glass pipeline device for preparing a polarized helium three-glass gas chamber, in particular to a glass pipeline device for preparing the polarized helium three-glass gas chamber and a preparation method of the glass gas chamber.
Background
The polarized neutron technology is the only means capable of providing effective separation of nuclear, magnetic, coherent and incoherent scattering, and is an advanced experimental technology urgently needed for researching complex materials. The helium tri-neutron polarization technology has the advantages of large acceptance angle, high polarizability, low background, wide energy spectrum, uniform polarization and analysis capability and the like, and is a preferred scheme for developing the neutron polarization technology by three neutron sources in the future in China. The glass gas chamber which is packaged with helium tri-gas and alkali metals (potassium and rubidium) is a core element of helium tri-neutron polarization technology. When manufacturing the glass gas chamber, the glass gas chamber is required to be sintered on a glass tube, wherein one end of the glass tube is connected with a gas filling station, and the other end of the glass tube is connected with an alkali metal bifurcation tube. Alkali metal is then added to the alkali metal furcation tube and melted, purified and vaporized using a flame, causing the alkali metal to flow upward as a vapor, eventually falling into the glass gas cell. Among them, the purity of alkali metal has an important influence on the quality of the glass cell.
At present, all the alkali metals available on the market are glass ampoule packages, and when the alkali metals are added to a glass pipeline, the opening of the ampoule package needs to be knocked in the air to open the glass package, and then the ampoule is placed into an alkali metal test tube in a mode that the opening faces downwards. In the process, alkali metal is inevitably oxidized due to contact with air, and the cleanness of the inner environment in the glass pipeline is also reduced due to impurities introduced into the air environment, so that the quality of the prepared polarized helium three-glass gas chamber is influenced.
One of the ideas for solving the above problems is to open the alkali metal package in a clean environment. In view of this, the japanese proton accelerator research complex (J-PARC) proposed a solution based on magnetic metal hammer free fall hitting alkali metal ampoule to achieve clean unsealing. It should be noted that the magnetic metal hammer is first encapsulated in a glass capsule, since the ferromagnetic material greatly reduces the polarization lifetime of helium tri-gas in the polarized helium tri-gas chamber. Firstly, filling a magnetic alkali metal hammer and an alkali metal ampoule I into a pre-fired glass pipeline, sealing the glass pipeline and filling high-purity nitrogen; and then, pulling the magnetic metal hammer to a high position by using a magnet, immediately removing the magnet, enabling the magnetic metal hammer to make free-falling body motion under the action of gravity, and impacting an alkali metal ampoule arranged at the bottom to break glass so as to realize clean unsealing of the alkali metal. However, this solution has the problem that due to the design defect of the glass tube (as shown in fig. 1), the magnetic metal hammer will inevitably contaminate the alkali metal in the subsequent alkali metal vaporization stage, so that the magnetic alkali metal needs to be recycled after special treatment. This problem makes the proposed solution of J-PARC not very practical.
Disclosure of Invention
Aiming at the technical problems, the application provides a glass pipeline device for preparing a polarized helium three-glass gas chamber and a preparation method of the glass gas chamber, which can solve the problem of complicated magnetic alkali metal hammer recovery steps in the J-PARC technology, improve the practicability, reduce the process cost, and greatly shorten the hyperpolarization time3And (3) preparation period of the He gas chamber.
According to a first aspect, there is provided in one embodiment a glass tubing arrangement for use in the production of a polarized helium three-glass gas cell, comprising: the device comprises a main glass pipeline and alkali metal bifurcated pipes corresponding to the number of alkali metals;
the main glass pipeline is a glass pipeline with openings at two ends, one end of the two ends of the opening of the main glass pipeline is connected with the gas filling station, the other end of the opening of the main glass pipeline is connected with the alkali metal bifurcated pipe, and an opening connected with the glass gas chamber is further arranged in the middle of the main glass pipeline;
when the alkali metal bifurcated pipe is a plurality of sets, each set of alkali metal bifurcated pipe is independent and comprises an alkali metal storage pipe, an alkali metal purification pipe, an alkali metal ampoule test pipe and a free falling pipe arranged at the joint of the alkali metal purification pipe and the alkali metal ampoule test pipe, wherein the alkali metal storage pipe, the alkali metal purification pipe and the alkali metal ampoule test pipe are connected in sequence; the alkali metal storage tube of each set of alkali metal bifurcated tube is independently communicated with the main glass pipeline;
when the main glass pipeline is horizontally arranged, the alkali metal storage pipe and the main glass pipeline are on the same horizontal plane, and the alkali metal storage pipe is provided with a concave part for storing alkali metal; the alkali metal purification pipe is obliquely arranged; the side wall of the alkali metal ampoule test tube, which is close to the glass tube wall at the joint of the alkali metal ampoule test tube and the alkali metal purification tube, is provided with an opening, and the opening is connected with the free falling body tube, so that the free falling body tube is vertical or nearly vertical; the free falling body pipe is a closed pipe and is communicated with the alkali metal ampoule test tube through an opening, and a magnetic metal hammer capable of moving freely is placed in the free falling body pipe.
Further, the magnetic metal hammer is enclosed in a glass capsule, which can move freely inside the free fall tube.
Further, the length of the free falling pipe is 10-15 cm; the length of the alkali metal purification tube is 13-18 cm.
It should be noted that the purpose of designing the free-fall tube to be upright or nearly upright is to allow the glass capsule containing the magnetic metal hammer to fall freely within the free-fall tube after the magnet is removed, and the resulting impact force is able to break the alkali metal ampoule upon striking it.
It should be noted that the length of the free fall tube is not set too short, and if the length is set to be less than 10cm, the impact force generated by the glass capsule falling from the top of the free fall tube is insufficient, so that the magnetic metal hammer cannot crush the alkali metal ampoule.
Furthermore, the number of the alkali metal bifurcated pipes is two, and the two alkali metal bifurcated pipes are used for placing potassium metal and rubidium metal respectively.
According to a second aspect, an embodiment provides a method of making a polarized helium tri-glass gas cell, comprising enclosing an alkali metal and helium tri-gas into a glassware chamber using the glass line set-up of the first aspect.
Further, the method specifically comprises the following steps:
filling alkali metal: filling inert gas into the glass pipeline system, and continuously flushing the inert gas out; putting the ampoule packaged with the clean alkali metal into an alkali metal ampoule test tube; preheating an opening of an alkali metal ampoule test tube, softening and sealing the opening, stopping introducing inert gas immediately while sealing the opening of the alkali metal ampoule test tube, and annealing a seal; heating the gas filling station and the glass pipeline at constant temperature, starting a molecular pump of the gas filling station at the same time, and pumping out gas in the glass pipeline system until the glass pipeline system reaches a vacuum state;
unsealing the alkali metal ampoule: after the alkali metal is filled, stopping heating the alkali metal ampoule test tube, the free falling body tube, the alkali metal purifying tube and the alkali metal storage tube; adjusting the position of the alkali metal ampoule; fixing a magnetic metal hammer at the top end of the free falling body pipe by using a magnet, removing the magnet, and enabling the magnetic metal hammer to fall freely to break the alkali metal ampoule; then the magnet is reused to pull the magnetic metal hammer to a high position, and the magnet is used for fixing the magnetic metal hammer; filling inert gas into the glass pipeline system, and finally sealing and cutting off the free falling body pipe;
purification of alkali metals: after the alkali metal ampoule is unsealed, pumping out residual inert gas in the glass pipeline device; continuously starting the molecular pump to heat the alkali metal to melt and vaporize the alkali metal, enabling the alkali metal to flow upwards into the alkali metal purification tube, condensing the alkali metal in the alkali metal purification tube, and refluxing the alkali metal into the alkali metal ampoule test tube;
and (3) packaging the glass air chamber: after the purification of the alkali metal is finished, thermally driving the alkali metal to the corresponding alkali metal storage tube, fusing and cutting off the other parts except the alkali metal storage tube in the alkali metal bifurcated tube, sealing the opening of the alkali metal storage tube, and annealing the seal; and communicating the glass gas chamber with the main glass pipeline, thermally driving alkali metal in the alkali metal storage pipe into the glass gas chamber, filling helium gas into the glass gas chamber by using a gas filling station, and packaging the glass gas chamber to finish the preparation of the polarized helium gas chamber.
Further, the alkali metal purification step further comprises the steps of detecting the gas pumped by the molecular pump by using a gas analyzer, and judging the purification degree of the alkali metal according to the components and the content of the pumped gas.
Further, the alkali metal ampoule comprises a first glass tube, a bump and a spike-like synapse; one end of the first glass pipeline is sealed, and the other end of the first glass pipeline is connected with the bulge part; one end of the bulge part, which is far away from the first glass pipeline, is connected with the spike-shaped synapse; the first glass tube is used for storing alkali metal.
Further, the ridge may be ellipsoidal or spherical.
It should be noted that the glass tube wall of the bump in the alkali metal ampoule is thinner than that of the first glass tube, and the sharp synapse has a larger internal stress and can be broken after being simply knocked, which is determined by the firing method of the alkali metal ampoule.
Further, in the alkali metal filling step, the vacuum state of the glass line is: the vacuum degree of the pipeline system reaches 10- 9mbar level and H in the pipeline2In an amount of 10-8Torr level, H2The content of O is 10-9The Torr level;
preferably, in the alkali metal filling step, after the inert gas is filled, the gas pressure in the glass line apparatus is 0.3barg, and the purity of the inert gas is 99.999%;
preferably, in the step of enclosing the glass gas chamber, the flame temperature for thermally driving the alkali metal to the alkali metal reservoir tube and for thermally driving the alkali metal to the glass gas chamber are both 1000 ℃.
The invention has the beneficial effects that:
the alkali metal ampoule test tube and the free falling body tube are creatively arranged in the alkali metal bifurcated tube, so that the alkali metal ampoule test tube can be cleanly unsealed, and the magnetic metal hammer can be directly recycled through the free falling body tube after the alkali metal is unsealed, so that the phenomenon that the magnetic metal hammer is stained with the alkali metal in the subsequent alkali metal vaporization stage can be avoided.
Drawings
FIG. 1 is a schematic diagram of an unpackaged alkali metal ampoule;
FIG. 2 is a diagram showing a glass line set in example 1;
FIG. 3 is a schematic diagram of an alkali metal ampoule enclosing an alkali metal;
FIG. 4 is a drawing of a glass line set-up in example 2;
FIG. 5 is a partial internal structure diagram of an alkali furcation tube in example 2.
Detailed Description
The design key of the glass pipeline is the arrangement of the alkali metal ampoule test tube and the free falling body tube, and the arrangement of the alkali metal ampoule test tube can avoid the problem that the alkali metal ampoule is oxidized because the alkali metal ampoule is opened in the air; the free falling body pipe is arranged, so that the purpose of recovering the magnetic metal hammer can be achieved through simple sealing treatment after the magnetic metal hammer impacts the alkali metal ampoule.
In addition, in the solution proposed by the japanese proton accelerator research complex (J-PARC) based on the impact of free falling bodies of magnetic metal hammers on alkali metal ampoules to realize the clean unsealing of the alkali metal, there are also the following problems: because the alkali metal ampoules available on the market at present have the problem of over thick glass layers, when the magnetic metal hammer impacts the alkali metal ampoules as free falling bodies, the situation that the glass package of the magnetic metal hammer per se is broken and the alkali metal ampoules are still intact often occurs, therefore, the application also develops an alkali metal ampoule package which can be conveniently unsealed, and the alkali metal ampoule package is used for redistributing and packaging the alkali metals purchased on the market. Therefore, the use amount of alkali metal can be saved, and the purity of the alkali metal in the glass gas chamber can be further improved, so that the quality of the polarized helium three-glass gas chamber can be further improved.
The present application is described in further detail below with reference to specific embodiments and the attached drawings. The following examples are intended to be illustrative of the present application only and should not be construed as limiting the present application.
Example 1: redistribution, packaging of alkali metals
Early preparation:
(1) firstly, 4 Pyrex glass tubes with different sizes and numbers are prepared, 4 glass tubes with the first size are prepared: the outer diameter is 6mm, the wall thickness is 1mm, and the length is 7 cm; 1 glass tube of a second size: the outer diameter is 12mm, the wall thickness is 2mm, and the length is 50 cm; 1 glass tube of third size: the outer diameter is 15mm, the wall thickness is 2mm, and the length is 30 cm; 1 glass tube of fourth size: the outer diameter is 12mm, the wall thickness is 2mm, and the length is 75 cm; one Pyrex glass-stainless steel VCR straight-through adapter, wherein the outer diameter of the Pyrex glass end is 15mm, the wall thickness is 2mm, and the inner diameter of the stainless steel VCR end is 1/2 inches;
(2) cleaning the glass tubes and the straight-through adapters with the four sizes by using a Citranox cleaning agent for 5-6 times, and then rinsing with deionized water until foams are completely removed; sealing one end of each glass tube with the first size by using flame with the temperature of 1200 ℃, wherein one end with the sealed opening is a first glass pipeline 1413, burning the upper end of the glass tube by using the flame with the temperature of 900 ℃ to soften the glass tube, blowing air to the softened part to expand the glass tube until the softened part is in an ellipsoid shape, the part of the glass tube in the ellipsoid shape is a bulge part 1412, and the top end of the glass tube is a tubular opening, so as to prepare a 4-branch alkali metal ampoule 141 as shown in fig. 1; fusing the glass tube with the second size into two glass tubes from the middle by using flame with the temperature of 1200 ℃, respectively sealing fusing openings of the two glass tubes, and manufacturing two alkali metal test tubes 15 with equal length; fusing and not sealing the glass tube with the third size from the middle by using flame at the temperature of 1200 ℃ to obtain two glass tubes with equal length, softening and bending one end of each glass tube by using flame at the temperature of 1200 ℃ to obtain two first alkali metal glass tubes, wherein each first alkali metal glass tube comprises an alkali metal storage tube 13 and an alkali metal purification tube 14, the bent part is the alkali metal storage tube 13, the non-bent part is the alkali metal purification tube 14, and the length of the alkali metal purification tube 14 is 13-18 cm; a glass tube of a fourth size is used as the main glass duct 1;
the above glass tube is fired to form a glass line device as shown in fig. 2, which comprises: a main glass conduit 1 and two sets of alkali metal bifurcated pipes; the main glass pipeline 1 is a glass pipeline with openings at two ends; of the two ends of the opening, a first end 11 is used for being communicated with a gas filling station, and a second end 12 is communicated with an alkali metal bifurcation; the two sets of alkali metal bifurcated pipes are independent respectively and comprise an alkali metal test tube 15, an alkali metal purification tube 14 and an alkali metal storage tube 13 which are communicated in sequence; the alkali metal storage pipe 13 of each set of alkali metal bifurcated pipe is independently communicated with the main glass pipeline 1; when the main glass pipeline 1 is horizontally placed, the alkali metal storage pipe 13 of the alkali metal bifurcated pipe and the main glass pipeline 1 are on the same horizontal plane; the alkali metal purification pipe 14 is designed to be inclined downwards, one end of the alkali metal purification pipe 14 is communicated with the alkali metal storage pipe 13, and the other end of the alkali metal purification pipe is communicated with the alkali metal test tube 15; two alkali metal ampoules 141 are connected to the middle outer side wall of the alkali metal purification tube 14; the alkali metal test tube 15 is communicated with the alkali metal purification tube 14 through a port on the side wall thereof, and the open end of the alkali metal test tube 15 faces upward for loading the alkali metal;
(3) after the completion of the sintering of the glass pipe apparatus shown in fig. 2, annealing each sintering point using a flame at a temperature of 500 ℃; rinsing the fired glass pipeline with deionized water for 5-6 times, and then rinsing the glass pipeline with ethanol to remove residual deionized water; connecting and sealing the main glass pipeline 1 with a gas filling station by a Pyrex glass-stainless steel VCR through adapter;
(4) then preheating the open mouths of the two alkali metal test tubes 15 by using 500 ℃ flame, softening and sealing the two alkali metal test tubes by using 1200 ℃ flame, and then annealing the seal by using 500 ℃ flame;
(5) uniformly winding the gas filling station and the glass pipeline by using a heating belt, keeping the temperature of 200 ℃ constant for heating, starting the molecular pump of the gas filling station to discharge gas in the pipeline system and heating the gas from the pipeline systemImpurities released from the inner surface until the vacuum degree of the pipeline system reaches 10-9mbar level, hydrogen content up to 10-8The Torr level and the moisture content reach 10-9The Torr level.
Filling alkali metal:
(1) after the early preparation is finished, closing a molecular pump valve, isolating the molecular pump, and stopping heating the alkali metal test tube 15 at constant temperature;
(2) filling high-purity nitrogen of 0.3barg into the glass pipeline system, wherein the purity of the nitrogen is 99.999 percent; preheating the tail end of one alkali metal test tube 15 by using 500 ℃ flame, softening and opening the preheated part by using 1200 ℃ flame, rapidly adjusting the gas outlet pressure of nitrogen, keeping the gage pressure reading of 0.3barg, continuously punching the nitrogen out of the open port of the test tube, scratching one blank end of a metal potassium glass package by using a glass cutter, breaking the glass package along the nick, rapidly putting the open port downwards into the test tube 15, preheating the open port of the test tube 15 filled with the metal potassium by using 500 ℃ flame, softening and re-sealing the open port of the test tube 15 filled with the metal potassium by using 1200 ℃ flame, rapidly closing a nitrogen bottle pressure reducing valve before sealing, avoiding the seal of the test tube 15 from being broken and burst by the gas before solidification, and then annealing the seal by using 500 ℃ flame;
(3) step (2) is repeated except that the operation is carried out in another alkali metal test tube 15 and the alkali metal to be charged is rubidium metal.
(4) After the two alkali metal test tubes 15 are sealed and annealed, slowly opening a molecular pump valve, and pumping out gas in a pipeline system to realize high vacuum of the glass pipeline system; wherein, the high vacuum state is: the vacuum degree of the glass pipeline system reaches 10-9mbar level, hydrogen content up to 10-8The Torr level and the water content reach 10-9The Torr level.
Alkali metal purification:
(1) after the alkali metal is filled, stopping constant-temperature heating of the alkali metal bifurcated pipe, and continuously starting the molecular pump;
(2) heating the test tube 15 filled with the potassium metal by using flame at 500 ℃ to melt the potassium metal, and automatically dropping the potassium metal into the bottom of the test tube 15; further heating the alkali metal test tube 15 by using a flame at 800 ℃ to boil and vaporize the potassium metal, and allowing the alkali metal gas to flow upwards into the purification tube 14; condensing in an alkali metal purification tube 14, refluxing to an alkali metal test tube 15, and in the repeated vaporization, cooling and falling processes of the potassium metal, vaporizing and pumping out the light volatile impurities by a molecular pump of a gas filling station, wherein the light volatile impurities can be detected by a residual gas analyzer until the residual gas analyzer can only detect hydrogen, water and nitrogen; the impurities which are not easy to volatilize will be attached to the inner wall of the glass tube.
(3) The same operation as in step (2) was carried out for another alkali metal tube 15 containing rubidium metal.
Subpackaging and recovering alkali metals:
(1) after purifying the alkali metal, closing a molecular pump valve, and isolating the molecular pump;
(2) using a flame with the temperature of 1000 ℃ to thermally drive potassium in the potassium metal test tube 15 to the two alkali metal ampoules 141, so that the amount of the potassium metal contained in the two alkali metal ampoules 141 is about 1/2; then, the two potassium metal ampoules 141 are respectively fused, sealed and removed by using a sharp flame with the temperature of 1500 ℃, wherein a tubular opening at the top end of each potassium metal ampoule 141 forms a sharp synapse 2411 after removal, as shown in fig. 3;
(3) the same procedure as in step (2) was carried out for another alkali metal furcation tube containing rubidium metal.
Example 2: preparation of glass air chamber
Early preparation:
(1) firstly, preparing 4 Pyrex glass tubes with different sizes and numbers, and 1 glass tube with the fifth size: the outer diameter is 15mm, the wall thickness is 2mm, and the length is 25 cm; 1 sixth size glass tube: the outer diameter is 12mm, the wall thickness is 2mm, and the length is 30 cm; 1 glass tube of seventh size: the outer diameter is 12mm, the wall thickness is 2mm, and the length is 50 cm; 1 eighth size glass tube: the outer diameter is 12mm, the wall thickness is 2mm, and the length is 75 cm; one Pyrex glass-stainless steel VCR straight-through adapter, wherein the outer diameter of the Pyrex glass end is 15mm, the wall thickness is 2mm, and the inner diameter of the stainless steel VCR end is 1/2 inches;
(2) cleaning the glass tubes and the straight-through adapters with the four sizes by using a Citranox cleaning agent for 5 to 6 times, then rinsing with deionized water until foams are completely removed, and then rinsing with ethanol for 5 to 6 times; fusing the glass tube of the fifth size from the middle by using flame at 1200 ℃ to prepare two alkali metal ampoule test tubes 25 with equal length; fusing the glass tube with the sixth size from the middle by using flame at 1200 ℃ to prepare two free falling body tubes 26 with equal length, and sealing one end opening of each free falling body tube 26, wherein the length of each free falling body tube 26 is 10-15 cm; fusing and not sealing a seventh-size glass tube from the middle by using flame at 1200 ℃ to obtain two glass tubes with equal length, softening and bending one end of each glass tube by using flame at 1200 ℃ to obtain two second alkali metal glass tubes, wherein each second alkali metal glass tube comprises an alkali metal storage tube 23 and an alkali metal purification tube 24, the bent part is the alkali metal storage tube 23, the alkali metal storage tube 23 is provided with a concave part 231, the non-bent part is the alkali metal purification tube 24, and the length of the alkali metal purification tube 24 is 13-18 cm; a glass tube of eighth size is used as the main glass duct 2;
a magnetic metal hammer 262 is placed in the free falling body pipe 26 and is fixed by the magnet 261 in an adsorption manner; and the glass tubes of the aforementioned four sizes are sintered to form a glass line set as shown in fig. 4, the set comprising: a main glass conduit 2 and two sets of alkali metal bifurcated pipes; the main glass pipeline 2 is a glass pipeline with two open ends, and a connector 27 for connecting a glass air chamber is arranged in the middle of the main glass pipeline; of the two ends of the opening, a first end 21 is used for communicating with a gas filling station, and a second end 22 is communicated with an alkali metal bifurcated pipe; the two sets of alkali metal bifurcated pipes are independent respectively and comprise an alkali metal ampoule test tube 25, an alkali metal purification tube 24 and an alkali metal storage tube 23 which are communicated in sequence, and a free falling pipe 26 arranged at the joint of the alkali metal purification tube 24 and the alkali metal ampoule test tube 25; the alkali metal storage tube 23 of each set of alkali metal bifurcated tube is independently communicated with the main glass pipeline 2; when the main glass pipeline 2 is horizontally placed, the alkali metal storage pipe 23 of the alkali metal bifurcated pipe and the main glass pipeline 2 are in the same horizontal plane, and the concave part 231 of the alkali metal storage pipe 23 is used for storing alkali metal; the alkali metal purification tube 24 is designed to be inclined downwards, one end of the alkali metal purification tube 24 is communicated with the alkali metal storage tube 23, and the other end is communicated with the alkali metal ampoule test tube 25; the alkali metal ampoule test tube 25 is provided with an opening on the side wall of the glass tube wall near the joint with the alkali metal purification tube 24, and the opening is connected with the free falling body tube 26, so that the free falling body tube 26 is vertical or nearly vertical;
(3) after the completion of the sintering of the glass pipe apparatus shown in fig. 4, annealing each sintering point using a flame at a temperature of 500 ℃; rinsing the fired glass pipeline with deionized water for 5-6 times, and then rinsing the glass pipeline with ethanol to remove residual deionized water; connecting and sealing the main glass pipeline 2 with a gas filling station by a Pyrex glass-stainless steel VCR through adapter;
filling alkali metal:
(1) after the preliminary preparation was completed, the glass line set was charged with 0.3barg of high purity nitrogen at 99.999% purity, maintaining a gage pressure reading of 0.3barg, and allowing N to pass through2Continuously punching, namely taking one ampoule 241 packaged with metal potassium and metal rubidium obtained in example 1, respectively putting the ampoules into two alkali metal ampoule test tubes 25, preheating an open port of the ampoule test tube 25 in which the metal potassium ampoule 241 is placed by using flame at 550 ℃, softening and sealing the ampoule test tube by using flame at 1200 ℃, and then annealing a seal by using 500 flame; preheating an open port of an ampoule test tube 25 placed with a rubidium metal ampoule 241 by using flame at 550 ℃, softening and sealing the open port by using flame at 1200 ℃, quickly closing a pressure reducing valve of a nitrogen bottle before sealing to prevent the opening of the test tube from being burst by gas before solidification, and then annealing a seal by using flame at 550 ℃;
(2) uniformly winding the gas filling station and the glass pipeline at all positions by using a heating belt, keeping the temperature of 200 ℃ constant for heating, starting a molecular pump of the gas filling station to discharge gas in the pipeline system and impurities released from the inner surface of the pipeline due to heating at the same time until the vacuum degree of the pipeline system reaches 10-9mbar level, hydrogen content up to 10-8The Torr level and the moisture content reach 10-9The Torr level.
Unsealing the alkali metal ampoule:
(1) removing the heating belt coated on the alkali metal ampoule test tube 25, the free falling body tube 26, the alkali metal purifying tube 24 and the alkali metal storage tube 23; as shown in fig. 5, the position of the alkali metal ampoule 241 is adjusted to ensure that the tip synapse 2411 and the ridge 2412 of the ampoule are directly under the magnetic metal hammer 262, the magnetic metal hammer 262 is fixed on the top end of the free fall tube 26 by using the magnet 261, the magnet 261 is removed, and the magnetic metal hammer 262 falls freely to break the alkali metal ampoule 241; then the magnet 261 is reused to pull the magnetic metal hammer 262 to a high place, and the magnet 261 is used to fix the magnetic metal hammer 262; and filling inert gas into the glass pipeline system, sealing and cutting the free falling body tube 26, sealing an opening of the alkali metal ampoule test tube 25 connected with the free falling body tube 26, and thus finishing the clean unsealing of the alkali metal and the recovery of the magnetic metal hammer 262.
Purification of alkali metals:
(1) after the alkali metal ampoule 241 is unsealed, pumping out residual nitrogen in the glass pipeline device;
(2) heating an ampoule test tube 25 filled with potassium metal by using flame at 800 ℃, so that the potassium metal is melted and vaporized, flows upwards into an alkali metal purification tube 24, is condensed in the purification tube 24, and flows back into the ampoule test tube 25, and during repeated vaporization, cooling and falling processes of the potassium metal, light volatile impurities are vaporized and are pumped out by a molecular pump of a gas filling station and can be detected by a residual gas analyzer until the residual gas analyzer can only detect hydrogen, water and nitrogen, and the impurities which are difficult to volatilize are attached to the inner wall of a glass tube; the potassium in a potassium metal ampoule test tube 25 is thermally driven to an alkali metal storage tube 23 by using flame at 1000 ℃, then, the other parts except the alkali metal storage tube 23 in the alkali metal bifurcated tube are melted and removed by using sharp flame at 1500 ℃, the alkali metal storage tube 23 is sealed, and then, the seal is annealed by using flame at 550 ℃;
(3) the same procedure as in step (2) was carried out for another alkali metal ampoule tube 25 containing rubidium metal.
Preparing a glass air chamber:
and after the purification of alkali metal is finished, communicating the glass gas chamber with the main glass pipeline 2, respectively thermally driving metal potassium and metal rubidium into the glass gas chamber by using 1000 ℃ flame, filling helium tri-gas into the glass gas chamber by using a gas filling station, and packaging the glass gas chamber to finish the preparation of the helium tri-neutron polarized glass gas chamber.
The present invention has been described in terms of specific examples, which are provided to aid understanding of the invention and are not intended to be limiting. Numerous simple deductions, modifications or substitutions may also be made by those skilled in the art in light of the present teachings.
Claims (10)
1. A glass tubing apparatus for use in the production of a polarized helium triple glass gas cell, comprising: the device comprises a main glass pipeline and alkali metal bifurcated pipes corresponding to the number of alkali metals;
the main glass pipeline is a glass pipeline with openings at two ends, one end of each of the two ends of each opening is connected with the gas filling station, the other end of each opening is connected with the alkali metal bifurcated pipe, and an opening connected with the glass gas chamber is further arranged in the middle of the main glass pipeline;
when the alkali metal bifurcated tubes are multiple sets, each set of alkali metal bifurcated tube is independent and comprises an alkali metal storage tube, an alkali metal purification tube, an alkali metal ampoule test tube and a free falling tube arranged at the joint of the alkali metal purification tube and the alkali metal ampoule test tube, wherein the alkali metal storage tube, the alkali metal purification tube and the alkali metal ampoule test tube are sequentially connected; the alkali metal storage tube of each alkali metal bifurcated tube is independently communicated with the main glass pipeline;
when the main glass pipeline is horizontally placed, the alkali metal storage pipe and the main glass pipeline are on the same horizontal plane, and the alkali metal storage pipe is provided with a concave part for storing alkali metal; the alkali metal purification pipe is obliquely arranged; an opening is formed in the side wall, close to the glass tube wall at the joint of the alkali metal ampoule test tube and the alkali metal purification tube, of the alkali metal ampoule test tube, and the opening is connected with the free falling body tube, so that the free falling body tube is vertical or nearly vertical; the free falling body pipe is a closed pipe and is communicated with the alkali metal ampoule test tube through the opening, and a magnetic metal hammer capable of moving freely is placed in the free falling body pipe.
2. The glass tubing set according to claim 1, wherein the magnetic metal hammer is enclosed within a glass capsule, the glass capsule enclosing the magnetic metal hammer being freely movable within the free-fall tube.
3. The glass tubing set according to claim 1, comprising: the length of the free falling pipe is 10-15 cm; the length of the alkali metal purification pipe is 13-18 cm.
4. The glass tubing set according to claim 1, wherein said alkali metal furcation tubes are provided in two sets for housing potassium metal and rubidium metal, respectively.
5. A method of making a polarized helium tri-glass gas cell, comprising encapsulating an alkali metal and helium tri-gas into said glass gas cell using the glass tubing set of any of claims 1-4.
6. The preparation method according to claim 5, comprising the following steps:
filling alkali metal: filling inert gas into the glass pipeline system, and continuously flushing the inert gas out; putting the ampoule packaged with the clean alkali metal into an alkali metal ampoule test tube; preheating an open port of an alkali metal ampoule test tube, softening and sealing the open port, stopping introducing inert gas while sealing the open port of the alkali metal ampoule test tube, and annealing a seal; heating the gas filling station and the glass pipeline at constant temperature, starting a molecular pump of the gas filling station at the same time, and pumping out gas in the glass pipeline system until the glass pipeline system reaches a vacuum state;
unsealing the alkali metal ampoule: after the alkali metal is filled, stopping heating the alkali metal ampoule test tube, the free falling body tube, the alkali metal purifying tube and the alkali metal storage tube; adjusting the position of the alkali metal ampoule; fixing the magnetic metal hammer at the top end of the free falling pipe by using a magnet, removing the magnet, and enabling the magnetic metal hammer to fall freely to break an alkali metal ampoule; then the magnet is reused to pull the magnetic metal hammer to a high place, and the magnet is utilized to fix the magnetic metal hammer; filling inert gas into the glass pipeline system, and finally sealing and cutting off the free falling body pipe;
purification of alkali metals: after the alkali metal ampoule is unsealed, pumping out residual inert gas in the glass pipeline device; continuously starting a molecular pump, heating alkali metal to melt and vaporize the alkali metal, enabling the alkali metal to flow upwards into the alkali metal purification tube, condensing the alkali metal in the alkali metal purification tube, and refluxing the alkali metal to the alkali metal ampoule test tube;
and (3) packaging the glass air chamber: after the purification of the alkali metal is finished, thermally driving the alkali metal to a corresponding alkali metal storage tube, fusing and cutting off the other parts except the alkali metal storage tube in the alkali metal bifurcated tube, sealing the opening of the alkali metal storage tube, and annealing the seal; and communicating the glass gas chamber with the main glass pipeline, thermally driving the alkali metal in the alkali metal storage pipe into the glass gas chamber, filling helium tri-gas into the glass gas chamber by using the gas filling station, and packaging the glass gas chamber to finish the preparation of the polarized helium tri-glass gas chamber.
7. The method according to claim 6, wherein the step of purifying the alkali metal further comprises detecting the gas pumped out by the molecular pump using a gas analyzer, and judging the degree of purification of the alkali metal based on the composition and content of the gas pumped out.
8. The method of claim 6, wherein the alkali metal ampoule comprises a first glass tube, a bump, and a spike;
one end of the first glass pipeline is sealed, and the other end of the first glass pipeline is connected with the bulge part; one end of the bulge part, which is far away from the first glass pipeline, is connected with the spike-shaped synapse; the first glass tube is used for storing alkali metal.
9. The method of claim 8, wherein the ridges are ellipsoidal or spherical.
10. The manufacturing method according to claim 6, wherein in the alkali metal filling step, the vacuum state of the glass tube is: the vacuum degree of the pipeline system reaches 10-9mbar level and H in the pipeline2In an amount of 10-8Torr level, H2The content of O is 10-9The Torr level;
preferably, in the alkali metal charging step, after charging the inert gas, the gas pressure in the glass line apparatus is 0.3barg, and the purity of the inert gas is 99.999%;
preferably, in the step of encapsulating the glass gas chamber, the flame temperature for thermally driving alkali metal to the alkali metal reservoir tube and for thermally driving alkali metal to the glass gas chamber are both 1000 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210343282.XA CN114560624B (en) | 2022-03-31 | 2022-03-31 | Glass pipeline device for preparing polarized helium three-glass air chamber and preparation method of glass air chamber |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115353278A (en) * | 2022-08-03 | 2022-11-18 | 散裂中子源科学中心 | Glass ware chamber and manufacturing process of glass air chamber |
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| JP2004113317A (en) * | 2002-09-25 | 2004-04-15 | Ge Medical Systems Global Technology Co Llc | Noble gas polarizer apparatus and magnetic-resonance imaging apparatus |
| US20120060561A1 (en) * | 2010-09-15 | 2012-03-15 | Fujikura Ltd. | Glass preform manufacturing method |
| CN106896065A (en) * | 2017-01-19 | 2017-06-27 | 合肥工业大学 | A kind of polarization cavity systems and its application method based on hyperpolarized gas |
| CN110972564B (en) * | 2015-09-01 | 2018-02-02 | 中国航天科技集团公司第五研究院第五一〇研究所 | Device and method for filling cascaded alkali metal air chamber |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004113317A (en) * | 2002-09-25 | 2004-04-15 | Ge Medical Systems Global Technology Co Llc | Noble gas polarizer apparatus and magnetic-resonance imaging apparatus |
| US20120060561A1 (en) * | 2010-09-15 | 2012-03-15 | Fujikura Ltd. | Glass preform manufacturing method |
| CN110972564B (en) * | 2015-09-01 | 2018-02-02 | 中国航天科技集团公司第五研究院第五一〇研究所 | Device and method for filling cascaded alkali metal air chamber |
| CN106896065A (en) * | 2017-01-19 | 2017-06-27 | 合肥工业大学 | A kind of polarization cavity systems and its application method based on hyperpolarized gas |
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| CN115353278A (en) * | 2022-08-03 | 2022-11-18 | 散裂中子源科学中心 | Glass ware chamber and manufacturing process of glass air chamber |
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