CN116479291A - Novel Al-W composite X-ray prevention material and preparation process thereof - Google Patents
Novel Al-W composite X-ray prevention material and preparation process thereof Download PDFInfo
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Abstract
The invention relates to the technical field of C22C21/00, in particular to a novel Al-W composite X-ray prevention material and a preparation process thereof, wherein the novel Al-W composite X-ray prevention material at least comprises aluminum powder and tungsten powder, the addition amount of the tungsten powder is 5-70wt%, the structure is uniform, the comprehensive mechanical property is excellent, and the novel Al-W composite X-ray prevention material can replace a cast aluminum shell of a bulb tube of a traditional CT machine X-ray generation device to carry out X-ray shielding by using an inner wall lead pasting process.
Description
Technical Field
The invention relates to the technical field of C22C21/00, in particular to a novel Al-W composite X-ray prevention material and a preparation process thereof.
Background
The cast aluminum shell of the bulb tube of the traditional CT machine X-ray generating device uses an inner wall lead pasting process to conduct X-ray shielding, but due to severe conditions of vacuum requirement, non-conduction of oil medium and the like required by the bulb tube, the traditional lead pasting process is easy to bring about degumming, sealing effect is affected, slag is dropped or particles fall into oil to cause high-voltage electric breakdown, and finally the service life of the bulb tube is reduced, so that the bulb tube shell adopts an Al-W composite material to replace the traditional lead pasting process, namely, the requirement of shielding X-rays is met, and meanwhile, the subsequent problem caused by lead pasting is avoided.
However, the problems faced by al—w composites are: tungsten has a melting point of 3422 ℃ and a density of 19.35g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Aluminum has a melting point of 660℃and a density of 2.7g/cm 3 The melting point and density of the two materials are very different, but the plasticity of the composite material is poor due to the dispersion and dispersion of the reinforcing phase in the matrix, for example, chinese patent application No. 104878342A discloses a preparation method and a device for a tungsten powder reinforced aluminum matrix composite material, and by adopting a specific device, tungsten powder is sprayed on the surface of aluminum or aluminum alloy micro-droplets formed by atomization, so that the tungsten powder is dispersed and adhered on the surface of the aluminum or aluminum alloy micro-droplets, and then sprayed and deposited on a substrate together, and the tungsten powder reinforced aluminum matrix composite material is obtained after solidification.
Therefore, developing an Al-W composite material with excellent comprehensive performance and a preparation process thereof is remarkable in attention, and has important economic value and social benefit for solving the service life problem of a product caused by the lead bonding process of a cast aluminum shell of a bulb tube of an X-ray generating device of a CT machine.
Disclosure of Invention
In order to solve the defects, the invention provides a novel Al-W composite X-ray prevention material, which is prepared from at least aluminum powder and tungsten powder, wherein the addition amount of the tungsten powder is 5-70 wt%.
As a preferable technical scheme, the novel Al-W composite X-ray prevention material also comprises an auxiliary composite material; the auxiliary composite material is at least one of metal, nonmetal and alloy; preferably, the auxiliary composite material at least comprises at least one of silicon element, copper element, magnesium element, iron element, zinc element, titanium element and manganese element.
Preferably, the auxiliary composite material is a combination of aluminum-silicon alloy, aluminum-copper alloy and magnesium powder. Preferably, the auxiliary composite material is 15-40% of the aluminum powder by mass, and the mass ratio of the aluminum-silicon alloy to the aluminum-copper alloy to the magnesium powder is (10-20): (1-2): (1-2).
Preferably, the grain size of the aluminum-silicon alloy, aluminum-copper alloy and magnesium powder is 5-30 mu m.
Based on the system, the auxiliary composite material is introduced by compounding according to the mass ratio of (10-20): (1-2): the combination of the aluminum-silicon alloy, the aluminum-copper alloy and the magnesium powder in the (1-2) is especially used for controlling the mass of the auxiliary composite material to be 15-40% of that of aluminum powder, so that the powder mixed by the aluminum powder in the system and the auxiliary composite material forms a liquid system at a lower temperature, the dispersion of tungsten powder in the liquid system is facilitated, the energy loss is reduced, the composite defect is avoided, and the compactness of the composite material is improved by controlling the particle size of the aluminum-silicon alloy, the aluminum-copper alloy and the magnesium powder, so that the tensile strength of a product is improved.
As a preferable technical scheme, the addition amount of the tungsten powder is 40-60 wt%.
As a preferable technical scheme, the particle size of the tungsten powder is 1-40 mu m; preferably, the particle size of the tungsten powder is 20-30 mu m.
As a preferable technical scheme, the aluminum powder comprises high-particle-diameter aluminum powder with particle diameter of 20-30 μm and low-particle-diameter aluminum powder with particle diameter of 1-10 μm; preferably, the mass ratio of the Gao Lijing aluminum powder to the low-particle-size aluminum powder is 1: (1-3).
Based on the system, the addition amount of the tungsten powder is controlled to be 30-50 wt%, so that the provided composite material has both enhanced tensile strength and excellent X-ray shielding effect. The inventor finds that in the actual research and development process, the tungsten powder with small particle size is adopted as the raw material to prepare the composite material at first, but the mechanical property of the prepared composite material is reduced, and the analysis reasons of the inventor are as follows: in the sintering process of the tungsten powder with smaller particle size, the activity of the tungsten powder is higher, the dispersion uniformity degree of the tungsten powder in an aluminum-based liquid system is greatly reduced, the density of the composite material is reduced, and the structure has larger aggregate structure defects, so that the tungsten powder with the particle size of 20-30 mu m is used as a preparation raw material, on the basis, the inventor controls the combination of the introduced aluminum powder with the high particle size of 20-30 mu m and the aluminum powder with the low particle size of 1-10 mu m, and particularly controls the mass ratio of Gao Lijing aluminum powder to the aluminum powder with the low particle size of 1: (1-3) effectively improving the density of the composite material after sintering, effectively making up the defect of relatively low density of the composite material caused by sintering at a lower temperature and sintering at a higher temperature, and ensuring the overall mechanical property and excellent X-ray shielding effect of the composite material.
The invention further provides a preparation process of the novel Al-W composite X-ray prevention material, which at least comprises the steps of powder preparation, mixing, hydraulic pressure, sintering, quenching and aging.
As a preferable technical scheme, the powder preparation specifically comprises: weighing the raw materials according to the formula amount.
As a preferable technical scheme, the mixing materials specifically include: adding the raw materials weighed according to the formula amount into a three-dimensional mixer, controlling the rotating speed to be 10-20r/min, and mixing for 3-5h to obtain mixed powder.
As a preferable technical solution, the hydraulic pressure specifically includes: and (3) carrying out hydraulic pressure on the mixed powder for 30-120min under 20-100MPa to obtain the hydraulic mixture.
As a preferable technical scheme, the sintering specifically comprises: and heating by adopting a programmed temperature, and preserving the temperature of the hydraulic mixture at 550-700 ℃ for 90-180min to obtain the sintered material. Preferably, the sintering temperature is 570-590 ℃; the heat preservation time is 120-180min.
Preferably, the temperature programming conditions are specifically as follows: heating from 20-30deg.C to 200-300deg.C, maintaining for 60min, heating to 400-500deg.C, maintaining for 60min, and heating to 550-700 deg.C for three times.
Preferably, the time for the primary temperature rise, the secondary temperature rise and the tertiary temperature rise is 60min, 60min and 90min respectively.
Based on the system, the hydraulic mixture after hydraulic mixing is kept at the temperature of 570-590 ℃ for 120-180min, and particularly, the temperature programming is adopted to balance the tensile strength and toughness of the composite material, so that the reduction of the density of the composite material caused by shorter heat preservation time and the reduction of the toughness of the composite material caused by the generation of hard and brittle phase aluminum tungsten compounds in the composite material caused by high-temperature sintering are avoided.
As a preferable technical scheme, the quenching specifically comprises: cooling the sintering material to 480-550 ℃, preserving heat for 90-240min, and quenching to obtain the quenching material.
As a preferable technical scheme, the aging specifically includes: and (3) placing the quenching material in a drying oven at 150-200 ℃ for aging for 8-10 hours to obtain the novel Al-W composite X-ray prevention material.
The beneficial effects are that:
(1) The invention provides a simple and efficient novel Al-W composite X-ray prevention material which has uniform tissue and excellent comprehensive mechanical property, and can replace a cast aluminum shell of a bulb tube of a traditional CT machine X-ray generation device to shield X-rays by using an inner wall lead-sticking process.
(2) Based on the system, the auxiliary composite material is introduced by compounding according to the mass ratio of (10-20): (1-2): the combination of the aluminum-silicon alloy, the aluminum-copper alloy and the magnesium powder in the (1-2) is especially used for controlling the mass of the auxiliary composite material to be 15-40% of that of aluminum powder, so that the powder mixed by the aluminum powder in the system and the auxiliary composite material forms a liquid system at a lower temperature, the dispersion of tungsten powder in the liquid system is facilitated, the energy loss is reduced, the composite defect is avoided, and the compactness of the composite material is improved by controlling the particle size of the aluminum-silicon alloy, the aluminum-copper alloy and the magnesium powder, so that the tensile strength of a product is improved.
(3) Based on the system, the addition amount of the tungsten powder is controlled to be 40-60 wt%, so that the provided composite material has both enhanced tensile strength and excellent X-ray shielding effect.
(4) The inventor controls the introduced aluminum powder to be the combination of high-grain-diameter aluminum powder with the grain diameter of 20-30 mu m and low-grain-diameter aluminum powder with the grain diameter of 1-10 mu m, and particularly controls the mass ratio of the Gao Lijing aluminum powder to the low-grain-diameter aluminum powder to be 1: (1-3) effectively improving the density of the composite material after sintering, effectively making up the defect of relatively low density of the composite material caused by sintering at a lower temperature and sintering at a higher temperature, and ensuring the overall mechanical property and excellent X-ray shielding effect of the composite material.
(5) Based on the system, the hydraulic mixture after hydraulic mixing is kept at the temperature of 570-590 ℃ for 120-180min, and particularly, the temperature programming is adopted to balance the tensile strength and toughness of the composite material, so that the reduction of the density of the composite material caused by shorter heat preservation time and the reduction of the toughness of the composite material caused by the generation of hard and brittle phase aluminum tungsten compounds in the composite material caused by high-temperature sintering are avoided.
Drawings
Fig. 1 is a gold phase diagram of the novel Al-W composite X-ray protection material provided in example 4 at 1000 times and 100 times, wherein 1000 times corresponds to fig. 1 (a) and 100 times corresponds to fig. 1 (b).
FIG. 2 shows the structure of example 1 at 500 times and 2000 times, respectively, wherein 500 times corresponds to FIG. 2 (a) and 2000 times corresponds to FIG. 2 (b).
Detailed Description
Example 1
In one aspect, embodiment 1 of the present invention provides a novel Al-W composite X-ray preventing material, wherein the preparation raw materials include 43.8wt% of aluminum powder, 40wt% of tungsten powder and 16.2wt% of auxiliary composite material.
The auxiliary composite material is a combination of aluminum-silicon alloy, aluminum-copper alloy and magnesium powder. The mass ratio of the aluminum-silicon alloy to the aluminum-copper alloy to the magnesium powder is 15:1:1.
the grain size of the aluminum-silicon alloy is 28 mu m, the grain size of the aluminum-copper alloy is 10 mu m, and the grain size of the magnesium powder is 10 mu m.
The particle size of the tungsten powder is 30 mu m.
The aluminum powder comprises high-particle-size aluminum powder with the particle size of 28 mu m and low-particle-size aluminum powder with the particle size of 10 mu m; the mass ratio of the Gao Lijing aluminum powder to the low-particle-size aluminum powder is 1:2.
the embodiment 1 of the invention provides a preparation process of a novel Al-W composite X-ray prevention material, which comprises the steps of powder mixing, material mixing, hydraulic pressure, sintering, quenching and aging.
The powder preparation specifically comprises the following steps: weighing the raw materials according to the formula amount.
The mixing materials specifically comprise: and adding the raw materials weighed according to the formula amount into a three-dimensional mixer, controlling the rotating speed to be 15/min, and mixing for 4 hours to obtain mixed powder.
The hydraulic pressure is specifically as follows: and (5) carrying out hydraulic pressure on the mixed powder for 90min under 30Pa to obtain a hydraulic mixture.
The sintering is specifically as follows: and (3) heating by adopting a programmed temperature, and preserving the temperature of the hydraulic mixture at 590 ℃ for 180min to obtain the sintered material.
The temperature programming conditions are specifically as follows: the temperature is raised to 250 ℃ from 25 ℃ once, the temperature is raised to 450 ℃ twice after the heat preservation is carried out for 60min, and the temperature is raised to 590 ℃ three times after the heat preservation is carried out for 60 min.
The time for the primary temperature rise, the secondary temperature rise and the tertiary temperature rise is respectively 60min, 60min and 90min.
The quenching specifically comprises the following steps: and cooling the sintering material to 500 ℃, preserving heat for 180min, and quenching to obtain the quenching material.
The aging is specifically as follows: and (3) placing the quenching material in a drying oven at 175 ℃ for aging for 9 hours to obtain the novel Al-W composite X-ray prevention material.
Example 2
The embodiment 2 of the invention provides a novel Al-W composite X-ray prevention material and a preparation method thereof, and the specific implementation mode is the same as the embodiment 1, and the specific implementation mode is that the sintering is as follows: and (3) heating by adopting a programmed temperature, and preserving the temperature of the hydraulic mixture at 590 ℃ for 120min to obtain the sintered material.
Example 3
The embodiment 2 of the invention provides a novel Al-W composite X-ray prevention material and a preparation method thereof, and the specific implementation mode is the same as the embodiment 1, and the specific implementation mode is that the sintering is as follows: and (3) heating by adopting a programmed temperature, and preserving the temperature of the hydraulic mixture at 590 ℃ for 90min to obtain the sintered material.
Example 4
The embodiment 4 of the invention provides a novel Al-W composite X-ray prevention material and a preparation method thereof, and the specific implementation mode is the same as the embodiment 1, wherein the preparation raw materials comprise 28.5wt% of aluminum powder, 60wt% of tungsten powder and 11.5wt% of auxiliary composite material.
Example 5
The embodiment 5 of the invention provides a novel Al-W composite X-ray prevention material and a preparation method thereof, and the specific implementation mode is the same as the embodiment 1, and is different in that the preparation raw materials comprise 28.5wt% of aluminum powder, 60wt% of tungsten powder and 11.5wt% of auxiliary composite material, and the sintering is specifically as follows: and (3) heating by adopting a programmed temperature, and preserving the temperature of the hydraulic mixture at 590 ℃ for 120min to obtain the sintered material.
Example 6
The embodiment 6 of the invention provides a novel Al-W composite X-ray prevention material and a preparation method thereof, and the specific implementation mode is the same as the embodiment 1, and is different in that the preparation raw materials comprise 28.5wt% of aluminum powder, 60wt% of tungsten powder and 11.5wt% of auxiliary composite material, and the sintering is specifically as follows: and (3) heating by adopting a programmed temperature, and preserving the temperature of the hydraulic mixture at 590 ℃ for 90min to obtain the sintered material.
Comparative example 1
The comparative example 1 of the present invention provides a novel Al-W composite X-ray preventing material and a preparation process thereof, and a specific embodiment is the same as example 1, in that the sintering is specifically: and (3) heating by adopting a programmed temperature, and preserving the temperature of the hydraulic mixture at 660 ℃ for 180min to obtain the sintered material.
Comparative example 2
The comparative example 2 of the present invention provides a novel Al-W composite X-ray preventing material and a process for preparing the same, and a specific embodiment is the same as example 1, except that the preparation raw materials thereof include 23.1wt% of aluminum powder, 70wt% of tungsten powder and 6.9wt% of auxiliary composite material.
Comparative example 3
The invention provides a novel Al-W composite X-ray prevention material and a preparation process thereof, and the specific implementation mode is the same as the embodiment 1, except that 70 weight percent of aluminum powder and 30 weight percent of tungsten powder are adopted.
Comparative example 4
Comparative example 4 of the present invention provides a novel Al-W composite X-ray preventing material and a process for preparing the same, and a specific embodiment is the same as example 1, except that the particle size of the tungsten powder is 5 μm.
Comparative example 5
The comparative example 5 of the present invention provides a novel Al-W composite X-ray preventing material and a process for preparing the same, and a specific embodiment is the same as example 1, except that the aluminum powder is high-grain-size aluminum powder with grain size of 28 μm.
Performance test method
(1) Sintered density: the actual sintered densities of the novel Al-W composite X-ray preventive materials prepared in examples and comparative examples were measured using a solid density tester (high-precision solid densitometer model JHY-20F), and the relative densities were calculated according to the formula (relative density=actual density/theoretical density), and the results are shown in table 1.
(2) Tensile strength: the novel Al-W composite X-ray resistant materials (5 mm thick) prepared in examples and comparative examples were subjected to tensile test with reference to standard GB/T228.1 (first part of tensile test of metallic materials: room temperature test method), and the results are shown in Table 1.
(3) Metallographic analysis: metallographic analysis is carried out on the novel Al-W composite X-ray prevention materials prepared in the example 1 and the example 3, and the result is shown in figure 1.
(4) Section analysis: the fracture of the tensile sample of example 1 was observed under a scanning electron microscope for its morphological characteristics, and the results are shown in fig. 2.
(5) X-ray shielding effect: the X-ray shielding effect of the novel 5mm thick Al-W composite X-ray shielding material prepared in the examples and the comparative examples was tested by using a mobile dr and a flat panel detector and an influence system (fine image 4343A), and the transmitted ray dose results are shown in Table 1.
TABLE 1
Claims (10)
1. The novel Al-W composite X-ray preventing material is characterized in that the preparation raw materials at least comprise aluminum powder and tungsten powder, and the addition amount of the tungsten powder is 5-70 wt%.
2. The novel Al-W composite X-ray protective material of claim 1, further comprising an auxiliary composite material; the auxiliary composite material is at least one of metal, nonmetal and alloy.
3. The novel Al-W composite X-ray protective material according to claim 1, wherein the auxiliary composite material comprises at least one of silicon element, copper element, magnesium element, iron element, zinc element, titanium element, and manganese element.
4. A novel Al-W composite X-ray protection material according to claim 2 or 3, characterized in that the auxiliary composite material is 15-40% of the mass of the aluminium powder.
5. The novel Al-W composite X-ray prevention material according to claim 4, wherein the addition amount of the tungsten powder is 40-60 wt%.
6. The novel Al-W composite X-ray protective material according to claim 4, wherein the particle size of the tungsten powder is 1-40 μm.
7. The novel Al-W composite X-ray preventing material according to claim 6, wherein the aluminum powder comprises high-particle-diameter aluminum powder having a particle diameter of 20 to 30 μm and low-particle-diameter aluminum powder having a particle diameter of 1 to 10 μm.
8. A novel Al-W composite X-ray protection material according to any one of claims 1 to 7, characterized in that it comprises at least the steps of compounding, mixing, hydraulic, sintering, quenching, ageing, said compounding being in particular: weighing the raw materials according to the formula amount.
9. The preparation process of the novel Al-W composite X-ray prevention material according to claim 8, wherein the mixing materials are specifically: adding the raw materials weighed according to the formula amount into a three-dimensional mixer, controlling the rotating speed to be 10-20/min, and mixing for 3-5h to obtain mixed powder; the hydraulic pressure is specifically as follows: and (3) carrying out hydraulic pressure on the mixed powder for 30-120min under 20-100MPa to obtain the hydraulic mixture.
10. The process for preparing the novel Al-W composite X-ray prevention material according to claim 9, wherein the sintering is specifically: and heating by adopting a programmed temperature, and preserving the temperature of the hydraulic mixture at 550-700 ℃ for 90-180min to obtain the sintered material.
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