CN111524774A - Large-caliber diamond side window miniature X-ray tube and packaging method - Google Patents
Large-caliber diamond side window miniature X-ray tube and packaging method Download PDFInfo
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- CN111524774A CN111524774A CN202010638014.1A CN202010638014A CN111524774A CN 111524774 A CN111524774 A CN 111524774A CN 202010638014 A CN202010638014 A CN 202010638014A CN 111524774 A CN111524774 A CN 111524774A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J35/00—X-ray tubes
- H01J35/02—Details
- H01J35/16—Vessels; Containers; Shields associated therewith
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/24—Manufacture or joining of vessels, leading-in conductors or bases
- H01J9/26—Sealing together parts of vessels
Abstract
The invention discloses a large-caliber diamond side window miniature X-ray tube and a packaging method, wherein a base of the large-caliber diamond side window miniature X-ray tube adopts a nickel-copper alloy base, a window body is made of diamond, the window body is welded with the nickel-copper alloy base through welding flux, and the welding flux is a mixture of diamond micro powder, oxygen-free copper-based alloy particles and Monel 67 alloy particles which are burnt to a high-temperature molten state. In the packaging method, the solder is mainly burnt to a high-temperature molten state, and the window and the nickel-copper alloy base are welded and sealed under the conditions of 600-700 ℃. The invention can greatly improve the peak-to-total ratio of the primary spectrum, the mechanical strength of the diamond window is high, the X-ray exit window is larger, and the excitation efficiency of primary X-rays can be improved. The invention effectively expands the application field of the diamond functional material and greatly improves the performance of the existing side window type X-ray tube.
Description
Technical Field
The invention relates to an X-ray tube and a packaging method thereof, in particular to a diamond side window miniature X-ray tube with a large caliber and a packaging method thereof.
Background
At present, the X-ray inspection equipment used in China is basically monopolized by foreign products, and the market of the side-window type micro X-ray tube, which is the most important element, is occupied by foreign companies such as Shimadzu, Oxford, PhoeniX, KeveX and the like. In recent years, although domestic X-ray tube production enterprises are beginning to rise, market share and cost performance are very different compared with foreign companies.
The side window type miniature X-ray tube is mainly used for the energy dispersion X fluorescence field analysis of elements, and has the advantages of light weight, simple structure, convenient operation and long measuring range, and the theoretically measurable range is as follows: Na-U, and the like. The window body of the side window type miniature X-ray tube needs to maintain the vacuum degree in the tube, shield low-energy beta rays and low-energy X rays and meet the technical requirement of ensuring the transmittance of high-energy characteristic X rays.
The existing miniature side window type X-ray tube mostly uses beryllium, aluminum alloy, glass and the like as window materials. Beryllium can ensure certain transparency to X-rays and cannot effectively shield the characteristic X-rays of the metal material in the tube; beryllium and its compounds are all extremely toxic and slightly lethal; and the mechanical strength is not high, so that the method is difficult to be applied to manufacturing a large-diameter X-ray tube. The aluminum alloy window has better ductility and mechanical strength, but primary rays emitted by the anode target can excite characteristic X rays of a window material when passing through the aluminum alloy window, and can interfere with quantitative analysis of the same elements in a subsequent sample to be detected; the glass window light pipe has the simplest structure, and the inherent defects are as follows: the characteristic X-rays of metal materials such as an anode target, a base and the like in the ray tube cannot be effectively shielded, and the collimation of the X-rays is difficult to realize.
Disclosure of Invention
The invention aims to solve the problems, effectively improve the passing rate of high-energy rays in an X-ray primary spectrum, reduce the passing rate of low-energy rays and improve the size of a window body, thereby increasing the caliber of the diamond side window miniature X-ray tube with large caliber and the packaging method.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a diamond side window miniature X-ray tube with large caliber comprises a vacuum envelope, a cathode, an anode and an X-ray transmission assembly;
the vacuum envelope comprises a cylindrical tube body arranged horizontally and an emergent tube positioned on the side wall of the cylindrical tube body, wherein the central axis of the emergent tube is vertical to the central axis of the tube body, and the emergent tube and the tube body are integrally formed and are both made of glass;
the X-ray transmission assembly comprises a base connected with the emergent tube, and a window body is arranged on the base;
the base adopts the nickel-copper alloy base, the window body material is the diamond, the window body passes through solder and nickel-copper alloy base welding, the solder is the mixture burning of diamond miropowder, oxygen-free copper base alloy granule and Monel 67 alloy granule to high temperature molten state.
Preferably, the method comprises the following steps: the diameter ratio of the window body diameter to the pipe body is 0.69-0.90, and the window body thickness is 2mm-3 mm.
Preferably, the method comprises the following steps: the diameter of the diamond micro powder is phi less than or equal to 0.5 mu m, and the oxygen-free copper-based alloy particles are Sn53Cu47The Monel 67 alloy particles are Ni67Cu28Fe2.5Mn1.5。
Preferably, the method comprises the following steps: and the nickel-copper alloy base is provided with a protective cover which is matched with the nickel-copper alloy base and is in threaded connection with the nickel-copper alloy base, and the protective cover is used for protecting the window body.
A packaging method of a diamond side window miniature X-ray tube with a large caliber comprises the following steps:
(1) inserting the nickel-copper alloy base into the emergent tube, and sealing the emergent tube with sealing glass powder at a sealing temperature of 450 ℃;
(2) transferring the whole in the step (1) to 133.322 × 10-6-133.322×10-7And burning the solder to a high-temperature molten state in a vacuum environment of Pa, and welding and sealing the window body and the nickel-copper alloy base at the temperature of 600-700 ℃, wherein the solder is a mixture of diamond micro powder, oxygen-free copper-based alloy particles and Monel 67 alloy particles.
Preferably, the method comprises the following steps: the diameter of the diamond micro powder is phi less than or equal to 0.5 mu m, and the oxygen-free copper-based alloy particles are Sn53Cu47The Monel 67 alloy particles are Ni67Cu28Fe2.5Mn1.5。
The basic structure and the working principle of the side window type X-ray tube are as follows: the X-ray tube comprises an anode and a cathode, a window is arranged at one side of the X-ray tube corresponding to the anode, and a window body is arranged in the window. The cathode generally comprises a cathode filament, a cathode cover and an electron focusing system, wherein an X-ray tube emits electrons through the cathode filament, the electrons are emitted from a cathode tungsten filament, the electrons form an electron beam through the electron focusing system and emit to an anode target of an anode, the anode target is bombarded by the electron beam, and the electron beam interacts with a target material to generate characteristic X rays and penetrates out through a window body.
The invention improves the material of the window body, selects the monocrystal diamond with the thickness of 2mm-3mm as the material of the window body, and can increase the inner diameter of the emergent tube on the premise of ensuring the strength based on the material of the window body, thereby increasing the diameter of the window body. In addition, the packaging process and the welding flux during packaging are also improved, and the window body and the nickel-copper alloy base can be more firmly bonded together based on the packaging method, so that the vacuum environment in the X-ray tube can be better endured, and the leakage is not easy to occur.
Compared with the prior art, the invention has the advantages that: the interference of low-energy rays in the primary spectrum can be greatly filtered, the background of a characteristic peak area of an element to be detected is reduced, the influence on the transmittance of high-energy exciting rays is small, the peak total ratio of the primary spectrum is greatly improved, the mechanical strength of the diamond window is high, the X-ray exit window is larger, and the exciting efficiency of the primary X-ray can be improved. The invention effectively expands the application field of the diamond functional material and greatly improves the performance of the existing side window type X-ray tube. The method is embodied by the following specific points:
(1) diamond is selected as a window material, and compared with a side window type miniature X-ray tube of a window made of traditional aluminum-magnesium alloy, glass and the like, the diamond window has a better filtering effect on characteristic X rays and low-energy electrons of metal materials such as an anode target, a substrate and the like; the transparency of the window is higher, and the transmittance of high-energy components in the primary spectrum of the X-ray tube is better; the peak total ratio of the original spectrum is improved to the maximum extent.
(2) The diamond window body has high mechanical strength, so that the diameter ratio of the window body to the tube body can reach 0.69-0.90, the X-ray exit window is larger, the X-ray irradiation area is increased, and the performance of the side window type X-ray tube equipment is improved.
(3) Under the condition of 600 plus 700 ℃, the mixture of the diamond micro powder, the oxygen-free copper-based alloy particles and the Monel 67 alloy particles is combusted to a high-temperature molten state to serve as a welding flux to weld and seal the diamond window body and the nickel-copper alloy base, so that the diamond window body and the nickel-copper alloy base can be welded more stably and have stronger pressure resistance, a higher-pressure vacuum environment is borne, the background can be reduced, and the excitation efficiency is improved.
(4) The invention effectively expands the application field of the diamond functional material and greatly improves the performance of the existing side window type X-ray tube.
Drawings
FIG. 1 is a cross-sectional view of the present invention;
FIG. 2 is an exploded view of the window and nickel-copper base portion;
FIG. 3 is a graph showing the peak-to-total ratio of an X-ray tube made of a three-material window;
FIG. 4 is a projection ratio contrast diagram of an X-ray tube made of a three-material window;
FIG. 5 shows the results of performance tests on the product of the present invention;
FIG. 6 shows the performance test results of an X-ray tube with a glass window;
FIG. 7 shows the performance test results of an X-ray tube with a window made of alloy.
In the figure: 1. a pipe body; 2. an exit tube; 3. a window body; 4. a nickel-copper alloy base; 5. cold fingers; 6. a positioner; 7. an anode target base; 8. an anode target; 9. a seal ring; 10. a pin; 11. an electron gun; 12. a protective cover.
Detailed Description
The invention will be further explained with reference to the drawings.
Example 1: referring to fig. 1 and 2, a diamond side window miniature X-ray tube with a large caliber comprises a vacuum envelope, a cathode, an anode and an X-ray transmission assembly;
the vacuum envelope comprises a cylindrical tube body 1 arranged horizontally and an emergent tube 2 positioned on the side wall of the cylindrical tube body, wherein the central axis of the emergent tube 2 is vertical to the central axis of the tube body 1, and the emergent tube and the tube body are integrally formed and are both made of glass;
the X-ray transmission assembly comprises a base connected with the emergent tube 2, and a window 3 is arranged on the base;
the base adopts nickel-copper alloy base 4, window 3 material is the diamond, and window 3 passes through the solder and welds with nickel-copper alloy base 4, the solder is the mixture burning of diamond miropowder, oxygen-free copper base alloy granule and Monel 67 alloy granule to high temperature molten state.
In this embodiment, the diameter ratio of the window 3 to the pipe body 1 is 0.69-0.90, and the thickness of the window 3 is 2mm-3 mm.
The diameter of the diamond micro powder is phi less than or equal to 0.5 mu m, and the oxygen-free copper-based alloy particles are Sn53Cu47The Monel 67 alloy particles are Ni67Cu28Fe2.5Mn1.5。
The nickel-copper alloy base 4 is provided with a protective cover 12 which is matched with the nickel-copper alloy base and is in threaded connection with the nickel-copper alloy base, and the protective cover 12 is used for protecting the window 3.
A packaging method of a diamond side window miniature X-ray tube with a large caliber comprises the following steps:
(1) the nickel-copper alloy base 4 is inserted into the emergent tube 2, and is sealed with the emergent tube 2 by adopting sealing glass powder at the sealing temperature of 450 ℃;
(2) transferring the whole in the step (1) to 133.322 × 10-6-133.322×10-7And (2) burning the solder to a high-temperature molten state in a vacuum environment of Pa, and welding and sealing the window 3 and the nickel-copper alloy base 4 at the temperature of 600-700 ℃, wherein the solder is a mixture of diamond micro powder, oxygen-free copper-based alloy particles and Monel 67 alloy particles.
In this embodiment: the diameter of the diamond micro powder is phi less than or equal to 0.5 mu m, and the oxygen-free copper-based alloy particles are Sn53Cu47The Monel 67 alloy particles are Ni67Cu28Fe2.5Mn1.5。
Example 2: referring to fig. 1 to 2, this embodiment shows a specific structure of a diamond side window miniature X-ray tube with a large caliber. As shown in fig. 1, the device comprises a tube body 1, an exit tube 2, a window 3, a nickel-copper alloy base 4, a cold finger 5, a positioner 6, an anode target base 7, an anode target 8, a sealing ring 9, a pin 10, an electron gun 11 and a protective cover 12. The cathode and the anode in the tube body 1 and the connection mode are as follows:
anode: the anode target 8 is connected with an anode target base 7, the anode target base 7 is connected with the cold finger 5, and the anode target 8, the anode target base 7 and the cold finger 5 are fixed at one end of the tube body 1 by a positioner 6;
cathode: the pin 10 is connected with an electron gun 11 containing a collimator and fixed at the other end of the tube body 1;
a cold finger 5: the anode target 8 is welded on the positioner 6 and is led out by the cold finger 5 to realize heat conduction.
Nickel-copper alloy base 4: in this embodiment, a specific structure of the nickel-copper alloy base 4 is provided, as shown in fig. 2, the nickel-copper alloy base 4 is a solid of revolution with a T-shaped cross section, and includes a large end and a small end, the small end is inserted into the exit tube 2 from top to bottom and is fixedly connected with the exit tube 2, a sealing ring is disposed between the small end and the exit tube 2, the large end is located at the top of the exit tube 2, a counter bore is disposed at the top of the nickel-copper alloy base 4, and a through hole with a diameter smaller than that of the counter bore is disposed from the bottom of the counter bore to the bottom of the nickel-copper alloy base 4. A window 3 of diamond material is mounted in the counterbore.
When the nickel-copper alloy base 4 is arranged at the position of the emergent tube 2, a sealing ring can be sleeved between the nickel-copper alloy base and the emergent tube for ensuring better sealing. Of course, the specific structure of the nickel-copper alloy base 4 is not limited to this embodiment, as long as it can be connected to the exit tube 2 in a matching manner and the window 3 can be installed.
Example 3: on the basis of the examples 1 and 2, the solder is further described, wherein the solder is a mixture of diamond micropowder, oxygen-free copper-based alloy particles and Monel 67 alloy particles, the diameter of the diamond micropowder is phi less than or equal to 0.5 mu m, and the oxygen-free copper-based alloy particles are Sn53Cu47The Monel 67 alloy particles are Ni67Cu28Fe2.5Mn1.5And the remaining 1% is impurities.
The solder comprises the following three components in percentage by mass: diamond: 20-27; oxygen-free copper-based alloy particles: 56-65; monel 67 alloy particles: 15-17.
The following mass ratios are specifically adopted:
table 1: mass ratio of each component of solder
Multiple experiments show that the mass ratio can realize the tight welding of the diamond window 3 and the base, and the 133.322 × 10 is ensured-6-133.322×10-7Pa vacuum degree.
Example 4: referring to fig. 3-7, in order to better illustrate the effect of the product of the present invention, we use the product of the present invention, a side window miniature X-ray tube with a window 3 made of glass, and a side window miniature X-ray tube with a window 3 made of aluminum-magnesium alloy for comparison, and the test conditions are all rated high voltage at 50 keV. The three types of parameters of the X-ray tube are shown in Table 2:
in this embodiment, the anode target material is Ag, but not limited to Ag. Due to the structure and the packaging process, the diameter ratio of the window 3 to the pipe body 1 can be increased, and the window 3 can be larger.
Aiming at the three ray tubes in table 2, the performance of the three ray tubes is tested, and particularly, the performances can be seen in fig. 3 and 4, and fig. 3 is a peak-to-total ratio comparison diagram of the X ray tube made of a window 3 made of three materials; the peak to total ratio can be calculated by the following formula:
wherein the content of the first and second substances,A feature(s) In order to characterize the counting rate of the X-rays,A total in order to be the full-spectrum counting rate,A bg the count rate of the low energy region rays.
As can be seen in fig. 3, the "peak to total" ratio of diamond window 3 can gradually increase as the thickness of window 3 increases, while the "peak to total" ratios of the other two gradually decrease as the thickness of window 3 increases. This is because low energy radiation is absorbed by the diamond window 3, while the characteristic X-ray energy, which is much higher than the absorption limit of the diamond material, is not absorbed and can pass through the window 3, ensuring a higher transmission. Not only can the background of the low energy region be reduced, but also the transmittance of the high energy region ray can be improved, and the peak total ratio can be improved. The peak to total ratio of the product of the invention is highest.
FIG. 4 shows the transmittance of three products, and it can be seen from FIG. 4 that the transmittance of the product of the present invention is much higher than that of the other two products. The product of the invention can effectively improve the passing rate of high-energy rays in the primary spectrum of the X-ray.
As can be seen from FIG. 3 and FIG. 4, the product of the present invention can increase the passing rate of high-energy rays in the primary spectrum of X-rays, i.e. increase the transmittance; the passing rate of low-energy rays can be effectively reduced, namely, the peak total ratio is improved; thereby improving the performance of the device.
Fig. 5 to 7 show the results of performance tests of the three products of example 4, and it can be seen that the K-system characteristic X-ray of the diamond window X-ray tube Ag (the counting rate is improved by about 1 times compared with the glass window X-ray tube and by about 1.3 times compared with the alloy window X-ray tube) is obtained under the condition of the same window 3 thickness of 2.0 mm.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. A diamond side window miniature X-ray tube with large caliber comprises a vacuum envelope, a cathode, an anode and an X-ray transmission assembly;
the vacuum envelope comprises a cylindrical tube body arranged horizontally and an emergent tube positioned on the side wall of the cylindrical tube body, wherein the central axis of the emergent tube is vertical to the central axis of the tube body, and the emergent tube and the tube body are integrally formed and are both made of glass;
the X-ray transmission assembly comprises a base connected with the emergent tube, and a window body is arranged on the base;
the method is characterized in that: the base adopts the nickel-copper alloy base, the window body material is the diamond, the window body passes through solder and nickel-copper alloy base welding, the solder is the mixture burning of diamond miropowder, oxygen-free copper base alloy granule and Monel 67 alloy granule to high temperature molten state.
2. A large diameter diamond side window miniature X-ray tube as claimed in claim 1 wherein: the diameter ratio of the window body diameter to the pipe body is 0.69-0.90, and the window body thickness is 2mm-3 mm.
3. A large diameter diamond side window miniature X-ray tube as claimed in claim 1 wherein: the diameter of the diamond micro powder is phi less than or equal to 0.5 mu m, and the oxygen-free copper-based alloy particles are Sn53Cu47The Monel 67 alloy particles are Ni67Cu28Fe2.5Mn1.5。
4. A large diameter diamond side window miniature X-ray tube as claimed in claim 1 wherein: and the nickel-copper alloy base is provided with a protective cover which is matched with the nickel-copper alloy base and is in threaded connection with the nickel-copper alloy base, and the protective cover is used for protecting the window body.
5. The method for encapsulating the diamond side window miniature X-ray tube with the large caliber as claimed in claim 1, wherein: the method comprises the following steps:
(1) inserting the nickel-copper alloy base into the emergent tube, and sealing the emergent tube with sealing glass powder at a sealing temperature of 450 ℃;
(2) transferring the whole in the step (1) to 133.322 × 10-6-133.322×10-7Burning the solder to a high-temperature molten state in a vacuum environment of Pa, and performing heat treatment at 600-700 deg.C
And under the condition, welding and sealing the window body and the nickel-copper alloy base, wherein the welding flux is a mixture of diamond micro powder, oxygen-free copper-based alloy particles and Monel 67 alloy particles.
6. The method for encapsulating the diamond side window miniature X-ray tube with the large caliber as claimed in claim 5, wherein: the diameter of the diamond micro powder is phi less than or equal to 0.5 mu m, and the oxygen-free copper-based alloy particles are Sn53Cu47The Monel 67 alloy particles are Ni67Cu28Fe2.5Mn1.5。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114063140A (en) * | 2021-11-16 | 2022-02-18 | 郑州工程技术学院 | Preparation method of diamond neutron detector for eliminating polarization effect |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114063140A (en) * | 2021-11-16 | 2022-02-18 | 郑州工程技术学院 | Preparation method of diamond neutron detector for eliminating polarization effect |
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