A precision ring material for X-ray imaging of medical devices and a preparation method thereof

Abstract

The present application relates to the technical field of medical devices, and in particular to a precision ring material for X-ray development of medical devices and a preparation method thereof, the preparation method comprising the following steps: treating a platinum or platinum alloy pipe material by using a medium-frequency vacuum melting combined with a rapid cooling and solidification technology to obtain a pipe blank; performing a homogenization heat treatment on the obtained pipe blank; performing a drawing process on the pipe blank after the homogenization heat treatment to obtain a micro pipe material; cutting the micro pipe material into a ring material with a target length; and performing a polishing treatment on the ring material, cleaning and drying to obtain a precision ring material. The preparation method has strong adaptability and is suitable for the processing and preparation process of various platinum and platinum alloy precision ring materials, and can be used to prepare various small-specification ring materials. The prepared precision ring material has good surface smoothness and uniform wall thickness.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of medical devices, in particular to a precision ring material for X-ray imaging of medical devices and a preparation method thereof. BACKGROUND

[0002] With the development of domestic medical device technology and the acceleration of China's population aging, China has ushered in the rapid development of medical device manufacturing industry, especially the rapid increase in market demand for various catheters, stents, and balloon products. The period from 2019 to 2030 is known as the golden decade of China's medical device industry. Today, there are 4 million patients in China who need to undergo cardiovascular surgery, so China is the world's largest potential market for cardiovascular treatment devices. In 2018, the market size of heart and large blood vessel interventional devices in China was about 50 billion yuan. Medical interventional X-ray imaging materials are essential key materials for all interventional medical devices.

[0003] Medical device X-ray imaging platinum and platinum alloy precision ring material is mainly used for interventional minimally invasive treatment imaging materials, which is a key material for determining whether the interventional device accurately reaches the patient's lesion or the required position during the operation. For example, in the treatment of congenital structural heart disease, coronary heart disease, arrhythmia, aneurysm, and vascular dissection, the delivery sheath tube, balloon catheter, microcatheter, and electrophysiological catheter all need to have X-ray non-penetrating imaging materials at the front end of the catheter. Therefore, platinum-iridium rings are the most widely used material among all catheter imaging materials, with usage ranging from a few to several dozen for each catheter.

[0004] As a key imaging material, medical device X-ray imaging platinum and platinum alloy precision ring material has a huge domestic demand. Currently, only a few large medical device companies in the United States and Japan have mastered the industrialization technology of cardiovascular interventional medical devices and key biological materials. China almost entirely relies on imports for the manufacture of key biological materials for interventional devices, which is a major problem restricting the localization of China's interventional medical devices. Therefore, the independent research and development and industrialization of medical device X-ray imaging platinum and platinum alloy precision ring material is crucial for breaking the import dependence and ensuring the production of medical devices. How to prepare medical device X-ray imaging precision ring material with good surface finish and uniform wall thickness to meet the requirements of X-ray imaging is an important issue that needs to be addressed in the industry. SUMMARY

[0005] The application provides a precision ring material for X-ray imaging of medical devices and a preparation method thereof.

[0006] According to a first aspect of the application, the application provides a precision ring material for X-ray imaging of medical devices, wherein the composition of the precision ring material comprises platinum or platinum alloy; the surface roughness Ra of the precision ring material is less than or equal to 0.20 microns; and the wall thickness precision of the precision ring material is ±0.002 mm to ±0.005 mm.

[0007] In the above scheme, the composition of the precision ring material for X-ray imaging of medical devices comprises platinum or platinum alloy, which has excellent X-ray imaging function. The surface roughness Ra of the precision ring material is less than or equal to 0.20 microns, the smoothness is good, the wall thickness precision is ±0.002 mm to ±0.005 mm, the wall thickness is uniform, and the precision ring material can be well combined with the inner tube of the plastic material catheter, and is not easy to cause damage to each other.

[0008] Further, the platinum alloy is a binary or multi-component alloy composed of Pt and one or more of W, Ir, Ni, Rh and Pd.

[0009] In the above scheme, the platinum alloy is a binary or multi-component alloy composed of Pt and one or more of W, Ir, Ni, Rh and Pd, which can better improve the imaging function of the precision ring material.

[0010] According to a second aspect of the application, the application further provides a preparation method of the above-mentioned precision ring material, which comprises the following steps:

[0011] treating the platinum or platinum alloy pipe material by using the intermediate frequency vacuum melting combined with the rapid cooling and solidification technology to obtain a pipe blank;

[0012] uniformly heat treating the obtained pipe blank;

[0013] performing a drawing process on the pipe blank after the uniform heat treatment to obtain a micro pipe material;

[0014] cutting the micro pipe material into a ring material with a target length;

[0015] performing a polishing treatment on the ring material, cleaning and drying to obtain the precision ring material.

[0016] In the above scheme, the preparation method of the precision ring material is highly adaptable and suitable for the machining and preparation process of various platinum and platinum alloy precision ring materials. In the preparation method, the intermediate frequency vacuum melting is combined with the rapid cooling and solidification technology, which is more uniform in shape and organization than the traditional process pipe blank, which is beneficial to the subsequent surface control and processing of the micro tube; the pipe material is obtained by isothermal drawing process, which greatly improves the pipe drawing stability and surface quality, avoids the problems of drawing fracture, uneven wall thickness and surface damage caused by work hardening and the like; after being prepared into a ring material, the ultrasonic vibration polishing method is innovatively used to solve the problem of difficult polishing of the inner and outer surfaces of the small ring material, and further improve the surface finish of the ring material.

[0017] Further, the drawing process adopts an isothermal drawing method; the drawing temperature of the isothermal drawing method is 200-600°C, and the drawing speed is 2-5 m / min.

[0018] Alternatively, the drawing temperature of the isothermal drawing method can be 200°C, 250°C, 300°C, 350°C, 400°C, 450°C, 500°C, 550°C or 600°C, and the drawing speed can be 2 m / min, 2.5 m / min, 3 m / min, 3.5 m / min, 4 m / min, 4.5 m / min or 5 m / min.

[0019] Understandably, by limiting the drawing process to an isothermal drawing method, problems such as uneven wall thickness and cracking caused by work hardening and uneven deformation can be avoided. Further limiting the drawing temperature and drawing speed of the isothermal drawing method can greatly improve the pipe drawing stability and surface quality, and better avoid problems such as drawing fracture, uneven wall thickness and surface damage caused by work hardening and the like.

[0020] Further, the length of the micro tube is >1 m, the diameter is 0.15-5 mm, the wall thickness is 0.02-1 mm, and the wall thickness accuracy is ±0.002-±0.005 mm.

[0021] Understandably, by limiting the length of the micro tube within a reasonable range, it is beneficial to the formation of a reasonable size of the ring material. By limiting the diameter and wall thickness of the micro tube and the wall thickness accuracy, the micro tube size is reasonable and the wall thickness is uniform, so that the precision ring material prepared subsequently can be well combined with the inner tube of the plastic material conduit, and damage to each other is not easy.

[0022] Further, the isothermal drawing mode adopts a floating core drawing device for drawing; the floating core drawing device is composed of a drawing core, a drawing outer mold, a heating system and a temperature control system, the drawing outer mold is provided with an accommodating cavity for accommodating the pipe blank, and the heating system and the temperature control system are installed in the drawing outer mold; during drawing, the pipe blank is accommodated in the accommodating cavity, the drawing core is inserted into the pipe blank along the inner wall of the pipe blank, the heating system heats the drawing outer mold, and the temperature control system monitors the temperature of the drawing outer mold.

[0023] Understandably, the isothermal drawing mode adopts a floating core drawing device for drawing, which is very beneficial to improving the drawing productivity, the product yield and the pipe inner surface quality. During drawing, the core is in a free state and is stabilized in the deformation zone by its special shape to realize the reducing of the diameter and wall thickness of the small-diameter stainless steel precision pipe. Further, the floating core drawing device is composed of a drawing core, a drawing outer mold, a heating system and a temperature control system, the drawing outer mold is provided with an accommodating cavity for accommodating the pipe blank, and the heating system and the temperature control system are installed in the drawing outer mold; during drawing, the pipe blank is accommodated in the accommodating cavity, the drawing core is inserted into the pipe blank along the inner wall of the pipe blank, the heating system heats the drawing outer mold, and the temperature control system monitors the temperature of the drawing outer mold, the temperature control system feeds back the temperature change of the drawing outer mold to the heating system to make the heating system heat the drawing outer mold to stabilize the drawing outer mold in a certain temperature value, so as to improve the drawing efficiency.

[0024] Further, the drawing core and the drawing outer mold are made of zirconia ceramic material.

[0025] Understandably, the conventional floating core is made of hard alloy, and the drawing core and the drawing outer mold of the floating core drawing device of the present application are innovatively made of zirconia ceramic material which has stable mechanical properties at high temperature and slow heat dissipation rate, so that the wall thickness error caused by the deformation and oxidation of the mold during hot drawing can be avoided, and the drawing productivity, the product yield and the pipe inner surface quality are improved.

[0026] Further, the heating system adopts an electric heating rod for heating.

[0027] Understandably, the electric heating rod has small volume, large power, fast heat response, high temperature control precision and high comprehensive thermal efficiency.

[0028] Further, the temperature control system adopts a temperature sensor and a temperature control system for control, and the temperature control precision is ±5℃.

[0029] It can be understood that the temperature sensor can sensitively perceive the temperature of the drawing outer mold, and the temperature control system can control the temperature according to the temperature perception of the temperature sensor, so that the temperature is controlled within an accuracy of ±5℃, so as to better realize isothermal drawing.

[0030] Further, in the pipe drawing process, the pipe inlet and outlet of the movable core drawing device are both protected by blowing inert gas.

[0031] Optionally, the inert gas can be argon, nitrogen, etc. It can be understood that by blowing inert gas at the pipe inlet and outlet of the movable core drawing device, the drawing productivity, yield and pipe inner surface quality can be improved.

[0032] Further, when the outer diameter of the pipe blank is >5mm, the drawing core with a surface finish Ra≤0.16μm is used, and when the outer diameter of the pipe blank is ≤5mm, the drawing core with a surface finish Ra≤0.08μm is used.

[0033] It can be understood that according to the outer diameter of the pipe blank, the drawing core with different surface finish specifications is selected adaptively to improve the drawing efficiency.

[0034] Further, the polishing treatment adopts ultrasonic vibration polishing, specifically, the cut ring material is soaked in an ultrasonic cleaning machine containing diamond polishing liquid for ultrasonic vibration;

[0035] The ultrasonic vibration time is 60min-180min, the temperature is 60℃-80℃, and the vibration frequency is 20kHz-80kHz.

[0036] The diamond polishing liquid includes, by weight percentage, 2%-5% diamond powder, 0.5%-1% water-soluble suspending agent, 0.5%-2% fatty alcohol polyoxyethylene ether dispersant, 0.2%-0.5% polyoxypropylene glycol ether defoaming agent, and the rest is ultrapure water; the particle size of the diamond powder is 0.1μm-2μm.

[0037] Optionally, the ultrasonic vibration time can be 60min, 70min, 80min, 90min, 100min, 110min, 120min, 130min, 140min, 150min, 160min, 170min or 180min, etc., the temperature can be 60℃, 65℃, 70℃, 75℃ or 80℃, etc., and the vibration frequency can be 20kHz, 30kHz, 40kHz, 50kHz, 60kHz, 70kHz or 80kHz, etc.

[0038] It can be understood that the ultrasonic vibration polishing method after the preparation of the ring material solves the problem of difficult polishing of the inner and outer surfaces of the small ring material, and further improves the surface smoothness of the ring material. By limiting the time, temperature and frequency of ultrasonic vibration in a reasonable range, the surface smoothness of the ring material can be further improved. By selecting a specific component of the diamond polishing liquid, the surface smoothness of the ring material can be further improved.

[0039] Further, in the ultrasonic vibration process, the ring material is limited in the ultrasonic cleaning machine by using a supporting device.

[0040] It can be understood that in the ultrasonic vibration process, the ring material is limited in the ultrasonic cleaning machine by using a supporting device, which can avoid the friction between the ring material and the equipment or the friction between the ring materials during the ultrasonic cleaning process, thereby preventing the surface smoothness from being reduced.

[0041] Further, the supporting device comprises a grid-shaped base, a supporting column and a limiting component, the supporting column is connected to the grid-shaped base, and the limiting component is arranged in the grid-shaped base; in the ultrasonic vibration process, the grid-shaped base is stably arranged in the ultrasonic cleaning machine by the supporting column, the ring material is inserted into the grid-shaped base, and the ring material is stably arranged by the limiting component.

[0042] Optionally, the grid-shaped base can be made of plastic material; the limiting component can be a limiting column, a limiting plate or the like. In some possible designs, the limiting component is detachably arranged in the grid-shaped base; further, the detachable manner can be clamping, hanging or the like.

[0043] It can be understood that the supporting device for placing the ring material used in the ultrasonic vibration cleaning process comprises a grid-shaped base, a supporting column and a limiting component, the limiting component is used to limit the movement of the ring material during the polishing process to prevent abrasion, and ensures the consistency of the ultrasonic polishing direction; the supporting device comprises the grid-shaped base, which avoids the obstruction of ultrasonic transmission and ensures the effect of ultrasonic polishing; the size of the supporting device and the spacing of the limiting component are determined by the actual size of the ring material.

[0044] Further, the temperature of the homogenization heat treatment is 800-1500 DEG C, and the time is 120-240 min.

[0045] Optionally, the temperature of the homogenization heat treatment can be 800 DEG C, 900 DEG C, 1000 DEG C, 1100 DEG C, 1200 DEG C, 1300 DEG C, 1400 DEG C or 1500 DEG C, etc., and the time can be 120 min, 130 min, 140 min, 150 min, 160 min, 170 min, 180 min, 190 min, 200 min, 210 min, 220 min, 230 min or 240 min, etc.

[0046] It can be understood that by limiting the temperature and time of the homogenization heat treatment within a reasonable range, the efficiency of the heat treatment can be improved.

[0047] Further, the homogenization heat treatment atmosphere is vacuum heat treatment.

[0048] It can be understood that vacuum heat treatment refers to the whole or part of the heat treatment process being carried out in a vacuum state, and the heat treatment quality is greatly improved. Compared with conventional heat treatment, vacuum heat treatment can realize non-oxidation, non-decarburization and non-carburization, can remove phosphorus scraps on the surface of the ring material, and has the effects of degreasing and degassing, thereby achieving the effect of surface brightening and purification.

[0049] Further, the melting temperature of the intermediate frequency vacuum melting combined with the rapid cooling and solidification technology is 1500 DEG C to 3500 DEG C, and a downward drawing device is used for directional solidification.

[0050] Optionally, the melting temperature of the intermediate frequency vacuum melting combined with the rapid cooling and solidification technology can be 1500 DEG C, 1800 DEG C, 2000 DEG C, 2300 DEG C, 2500 DEG C, 2800 DEG C, 3000 DEG C, 3250 DEG C or 3500 DEG C, etc.

[0051] It can be understood that by limiting the melting temperature of the intermediate frequency vacuum melting combined with the rapid cooling and solidification technology within a reasonable range, and by limiting the use of a downward drawing device for directional solidification, the efficiency of the melting can be improved, and the shape and organization of the obtained pipe blank are more uniform, which is more conducive to the subsequent surface control and processing of the micro tube.

[0052] The preparation method of the precision ring material for X-ray development of medical devices provided by the application has strong adaptability and is suitable for the processing and preparation process of various platinum and platinum alloy precision ring materials. In the preparation method, the melting adopts intermediate frequency vacuum melting combined with rapid cooling and solidification technology, which is more uniform in pipe blank shape and organization compared with traditional processes, and is conducive to the subsequent surface control and processing of the micro tube. The pipe material is obtained by using a special drawing process, which greatly improves the pipe drawing stability and surface quality, avoids problems such as drawing fracture, uneven wall thickness and surface damage caused by work hardening, etc. After being prepared into a ring material, the ultrasonic vibration polishing method is innovatively used to solve the problem of difficult polishing of the inner and outer surfaces of small ring materials, and further improve the surface finish of the ring material. BRIEF DESCRIPTION OF DRAWINGS

[0053] In order to more clearly illustrate the technical solutions of the present application or the prior art, the drawings required to be used in the following embodiments or prior art description will be briefly introduced. Obviously, the drawings in the following description are some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor on the basis of these drawings.

[0054] Figure 1 is a structural schematic view of the movable core drawing device used in the embodiment of the present application at a first angle;

[0055] Figure 2 is a structural schematic view of the movable core drawing device used in the embodiment of the present application at a second angle;

[0056] Figure 3 is a structural schematic view of the support device used in the embodiment of the present application at a first angle;

[0057] Figure 4 is a structural schematic view of the support device used in the embodiment of the present application at a second angle.

[0058] Reference signs:

[0059] 1: drawing core; 2: drawing outer mold; 3: electric heating rod; 4: temperature sensor; 5: pipe blank; 6: grid matrix; 61: bottom surface; 62: side surface; 7: support column; 8: limiting assembly; 81: first limiting piece; 82: second limiting piece; 9: ring material. DETAILED DESCRIPTION

[0060] In order to make the purpose, technical solutions and advantages of the present application more clear, the technical solutions in the present application will be clearly and completely described below in combination with the drawings in the present application. Obviously, the described embodiments are some embodiments of the present application, but not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor belong to the protection scope of the present application.

[0061] Embodiment 1

[0062] The embodiment provides a preparation method of a precision ring material for X-ray development of medical instruments, and specifically includes the following steps:

[0063] (1) According to the ingredient ratio of Pt content 90% and Ir content 10%, a continuous casting melting directional solidification melting mode is adopted, the melting temperature is 2600℃, a downward device is used for directional solidification, a PtIr10 alloy pipe blank with uniform structure and good processing performance is obtained, the pipe blank diameter is 20mm, the wall thickness is 2mm, and the length is 1000mm.

[0064] (2) Homogenization heat treatment of the pipe blank, heat treatment temperature 1100℃, time 150min;

[0065] (3) Isothermal drawing of the pipe blank after homogenization heat treatment using a floating core drawing device, isothermal drawing temperature 400℃, drawing speed 2m / min, and argon partial blowing protection should be provided at the pipe inlet and outlet during drawing.

[0066] Specifically, as shown in Figure 1 and Figure 2 , the floating core drawing device is composed of a drawing core 1, a drawing outer mold 2, a heating system, and a temperature control system. The drawing core 1 and the drawing outer mold 2 are both made of zirconia ceramic material. The heating system uses an electric heating rod 3 for heating, and the temperature control system uses a temperature sensor 4 and a temperature control system for control. The temperature control precision is ±5℃. The drawing outer mold 2 is provided with a containing cavity for accommodating the pipe blank. The heating system and the temperature control system are installed in the drawing outer mold 2. During drawing, the pipe blank 5 is accommodated in the containing cavity, the drawing core 1 is inserted into the pipe blank 5 along the inner wall of the pipe blank 5, the heating system heats the drawing outer mold 2, and the temperature control system monitors the temperature of the drawing outer mold 2.

[0067] The surface glossiness requirement of the floating core drawing device is that when the outer diameter of the pipe blank is >5mm, the surface finish Ra of the drawing core is ≤0.16μm, and when the outer diameter of the pipe blank is ≤5mm, the surface finish Ra of the drawing core is 0.05μm. After drawing, a micro-tube material with a length of 3m, a diameter of 0.02mm, and a wall thickness of 0.02mm is obtained.

[0068] (4) The micro-tube material is cut into a ring material with a length of 2mm using a femtosecond or picosecond laser.

[0069] (5) The cut platinum alloy ring material is polished by ultrasonic vibration polishing. The main method is to immerse the cut ring material in an ultrasonic cleaning machine containing diamond polishing liquid for ultrasonic vibration. The ultrasonic vibration time is 180min, the temperature is 80℃, and the ultrasonic vibration frequency is 40kHz. The composition of the diamond polishing liquid is as follows: diamond powder with a particle size of 0.1μm 2%, water-based suspending agent 1%, dispersing agent fatty alcohol polyoxyethylene ether 2%, defoaming agent polyoxypropylene glycol ether 0.2%, and the rest is ultrapure water.

[0070] Specifically, during the ultrasonic vibration process, a support device is used to limit the ring material in the ultrasonic cleaning machine, and the support device is placed in the cleaning tank of the ultrasonic cleaning machine. As shown in Figure 3 and Figure 4 ​As shown, the support device comprises a grid base 6, a support column 7 connected to the grid base 6, and a limiting assembly 8 arranged in the grid base 6; the grid base 6 is a groove structure surrounded by a bottom surface 61 and a side surface 62, and a plurality of limiting assemblies 8 are arranged in the grid base 6 at intervals to separate and stably position a plurality of ring materials 9 in the grid base 6. The limiting assembly 8 comprises two first limiting members 81 and two second limiting members 82, the first limiting members 81 are fixedly or detachably installed in the grid base 6, the second limiting members 82 are detachably installed in the grid base 6, and the first limiting members 81 and the second limiting members 82 can be independently support rods. When the ring material 9 is installed, first, the two first limiting members 81 are installed in the grid base 6, then the ring material 9 is placed on the first limiting members 81, and then the two second limiting members 82 are installed in the grid base 6 to position the ring material 9 between the first limiting members 81 and the second limiting members 82.

[0071] After polishing, the PtIr10 alloy ring material with an inner and outer surface roughness Ra=0.12 μm and a wall thickness accuracy of ±0.002 mm is obtained.

[0072] Embodiment 2

[0073] The embodiment provides a preparation method of a precision ring material for X-ray imaging of a medical instrument, and specifically comprises the following steps:

[0074] (1) According to the ingredient ratio of 92% of Pt content and 8% of W content, a continuous casting melting directional solidification melting mode is adopted, the melting temperature is 3500°C, the directional solidification is performed by using a downward drawing device, a PtW8 alloy pipe blank with uniform structure and good processing performance is obtained, the pipe blank diameter is 5mm, and the pipe blank length is 2m.

[0075] (2) The pipe blank is subjected to homogenization heat treatment, the heat treatment temperature is 1000°C, and the time is 240 min.

[0076] (3) The pipe blank after the homogenization heat treatment is subjected to isothermal drawing by using a floating core drawing device, the isothermal drawing temperature is 600°C, the drawing speed is 5m / min, and nitrogen gas partial blowing protection should be provided at the pipe inlet and the pipe outlet in the drawing process; the floating core drawing device is the same as that in embodiment 1. The surface glossiness requirement of the floating core drawing device is that when the pipe blank diameter is greater than 5mm, the drawing core surface finish Ra=0.12 μm, and when the pipe blank diameter is less than or equal to 5mm, the drawing core surface finish Ra=0.02 μm. After drawing, a micro pipe material with a length of 2m, a diameter of 0.05mm and a wall thickness of 0.05mm is obtained.

[0077] (4) A femtosecond or picosecond laser is used to cut the capillary into a ring material with a length of 2mm to 10mm. ​

[0078] (5) The cut platinum alloy ring material is polished by ultrasonic vibration polishing. The main method is to immerse the cut ring material in an ultrasonic cleaning machine containing diamond polishing liquid for ultrasonic vibration. The ultrasonic vibration time is 120 min, the temperature is 60°C, and the ultrasonic vibration frequency is 60 kHz. The composition of the diamond polishing liquid is as follows: 3% of diamond powder with a particle size of 0.15 μm, 1% of water-soluble suspending agent, 0.5% of dispersant fatty alcohol polyoxyethylene ether, 0.5% of defoaming agent polyoxypropylene glycol ether, and the rest is ultrapure water.

[0079] Specifically, during the ultrasonic vibration process, the ring material is limited in the ultrasonic cleaning machine by using a support device, wherein the structure of the support device is the same as that of Embodiment 1.

[0080] After polishing, the PtW8 alloy ring material with an inner and outer surface roughness Ra = 0.18 μm and a wall thickness accuracy of ± 0.002 mm is obtained.

[0081] Embodiment 3

[0082] The embodiment provides a preparation method of a precision ring material for X-ray imaging of medical devices, which specifically comprises the following steps:

[0083] (1) According to the component ratio of 85% of Pt content and 15% of Rh content, a continuous casting melting directional solidification melting method is adopted, the melting temperature is 2200°C, the directional solidification is performed by using a downward drawing device, a platinum and platinum alloy pipe blank with uniform structure and good processing performance is obtained, the pipe blank diameter is 5mm, and the pipe blank length is 1m.

[0084] (2) The pipe blank is subjected to homogenization heat treatment, the heat treatment temperature is 1000°C, and the time is 220 min.

[0085] (3) The pipe blank after homogenization heat treatment is subjected to isothermal drawing by using a floating core drawing device, the isothermal drawing temperature is 500°C, the drawing speed is 3 m / min, and the nitrogen gas local blowing protection should be provided at the pipe inlet and outlet during the drawing process; the floating core drawing device is the same as that of Embodiment 1. The surface glossiness requirement of the floating core drawing device is that when the pipe blank diameter is greater than 5 mm, the surface finish Ra of the drawing core is 0.1 μm, and when the pipe blank diameter is less than or equal to 5 mm, the surface finish Ra of the drawing core is 0.03 μm. After drawing, the micro-pipe material with a length of 1 m, a diameter of 1 mm and a wall thickness of 1 mm is obtained.

[0086] (4) The capillary tube is cut into a ring material with a length of 10 mm by using a femtosecond or picosecond laser.

[0087] ​(5) The cut PtRh15 ring material is polished by ultrasonic vibration polishing. The main method is to immerse the cut ring material in an ultrasonic cleaning machine containing diamond polishing liquid for ultrasonic vibration. The ultrasonic vibration time is 80 min, the temperature is 70°C, and the ultrasonic vibration frequency is 80 kHz. The composition ratio of the diamond polishing liquid is as follows: 3% of diamond powder with a particle size of 0.15 μm, 0.8% of water-soluble suspending agent, 1% of fatty alcohol polyoxyethylene ether dispersant, 0.3% of polyoxypropylene glycol ether defoaming agent, and the rest is ultrapure water.

[0088] Specifically, in the ultrasonic vibration process, the ring material is limited in the ultrasonic cleaning machine by using a support device, wherein the structure of the support device is the same as that of Embodiment 1.

[0089] After polishing, the PtRh15 alloy ring material with an inner and outer surface roughness Ra = 0.2 μm and a wall thickness accuracy of ± 0.005 mm is obtained.

[0090] Comparative Example 1

[0091] The present comparative example provides a preparation method of a ring material for X-ray imaging of medical devices, which specifically comprises the following steps:

[0092] (1) According to the component ratio of Pt content 90% and Ir content 10%, a PtIr10 alloy pipe blank with uniform structure and good processability is obtained by adopting continuous casting melting directional solidification melting method, the melting temperature is 2600°C, and the directional solidification is carried out by using a downward device. The pipe blank diameter is 5 mm.

[0093] (2) The pipe blank is subjected to homogenization heat treatment, the heat treatment temperature is 1100°C, and the time is 150 min.

[0094] (3) The pipe blank after homogenization heat treatment is subjected to room temperature drawing by using a floating core drawing device, the drawing rate is 2 m / min, and the floating core drawing device is the same as that of Embodiment 1. The surface glossiness requirement of the floating core drawing device is that when the pipe blank diameter is > 5 mm, the surface finish Ra of the floating core is ≤ 0.16 μm, and when the pipe blank diameter is ≤ 5 mm, the surface finish Ra of the floating core is 0.05 μm; when drawn to , slight bamboo-shaped lines appear in part of the pipe blank area, and the wall thickness starts to deform unevenly.

[0095] Comparative Example 2

[0096] The difference between the present comparative example and Embodiment 1 is that in step (5), the ring material is not limited in the ultrasonic cleaning machine by using a support device.

[0097] A PtIr10 alloy ring material with an inner and outer surface roughness Ra = 0.2 μm and a wall thickness accuracy of ± 0.002 mm is obtained.

[0098] From the experimental results of Examples 1-3, it can be seen that the medical instrument X-ray developing precision ring material prepared by the preparation method of the present application has low surface roughness and uniform wall thickness. By applying the precision ring material of the present application to the X-ray developing process of interventional medical instruments, it is found that the developing profile is clear, the gloss is uniform, and there are no virtual shadows and dark spots.

[0099] From the comparative experimental results of Example 1 and Comparative Example 1, it can be seen that the control of isothermal drawing process conditions in the preparation process of the medical instrument X-ray developing precision ring material is very important, especially the temperature control during isothermal drawing. By reasonably selecting the isothermal drawing process conditions, the pipe drawing stability and surface quality can be greatly improved, and problems such as drawing fracture, uneven wall thickness and surface damage caused by work hardening, etc. can be avoided.

[0100] From the comparative experimental results of Example 1 and Comparative Example 2, it can be seen that the control of ultrasonic vibration polishing conditions in the preparation process of the medical instrument X-ray developing precision ring material is very important. In particular, during the ultrasonic vibration process, the ring material is limited in the ultrasonic cleaning machine using a specific support device, which can effectively prevent the wear caused by the movement of the ring material during polishing and ensure the consistency of the ultrasonic polishing direction, thereby improving the surface finish of the precision ring material.

[0101] Finally, it should be noted that: the above examples are only used to illustrate the technical solutions of the present application, but not to limit it; although the present application has been described in detail with reference to the foregoing examples, those skilled in the art should understand that: it can still modify the technical solutions recorded in the foregoing examples, or make equivalent replacement for part of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims

1. A precision ring member for X-ray visualization of a medical device, characterized by The component of the precision ring material is platinum or platinum alloy; the surface roughness Ra of the precision ring material is ≤0.20μm; and the wall thickness precision of the precision ring material is ±0.005mm. The preparation method of the precision ring material comprises the following steps: The platinum or platinum alloy pipe material is treated by adopting the intermediate frequency vacuum smelting combined with the rapid cooling and solidification technology to obtain a pipe blank; The obtained pipe blank is subjected to homogenization heat treatment; The pipe blank after the homogenization heat treatment is subjected to a drawing process to obtain a micro pipe material; the drawing process adopts an isothermal drawing mode; the drawing temperature of the isothermal drawing mode is 200℃-600℃, and the drawing speed is 2m / min-5m / min; the length of the micro pipe material is >1m, the diameter is 0.15mm-5mm, the wall thickness is 0.02mm-1mm, and the wall thickness precision is ±0.005mm; The micro pipe material is cut into a ring material with a target length; The ring material is subjected to polishing treatment, cleaning and drying to obtain the precision ring material; the polishing treatment adopts ultrasonic vibration polishing, specifically, the cut ring material is soaked in an ultrasonic cleaning machine filled with diamond polishing liquid for ultrasonic vibration; The ultrasonic vibration time is 60min-180min, the temperature is 60℃-80℃, and the vibration frequency is 20kHz-80kHz; in the ultrasonic vibration process, a supporting device is used to limit the precision ring material in the ultrasonic cleaning machine; The components of the diamond polishing liquid are, by weight percentage, 2%-5% of diamond powder, 0.5%-1% of water-soluble suspending agent, 0.5%-2% of fatty alcohol polyoxyethylene ether dispersant, 0.2%-0.5% of polyoxypropylene glycol ether defoaming agent, and the rest is ultrapure water; the particle size of the diamond powder is 0.1μm-2μm.

2. The precision ring material for X-ray visualization of medical devices according to claim 1, characterized in that, The platinum alloy is a binary or multi-alloy composed of Pt and one or more of W, Ir, Ni, Rh and Pd.

3. A method for producing a precision ring member for X-ray visualization of a medical instrument, characterized by, The component of the precision ring material is platinum or platinum alloy; the surface roughness Ra of the precision ring material is ≤0.20μm; and the wall thickness precision of the precision ring material is ±0.005mm. The preparation method of the precision ring material comprises the following steps: The platinum or platinum alloy pipe material is treated by adopting the intermediate frequency vacuum smelting combined with the rapid cooling and solidification technology to obtain a pipe blank; The obtained pipe blank is subjected to homogenization heat treatment; The pipe blank after the homogenization heat treatment is subjected to a drawing process to obtain a micro pipe material; the drawing process adopts an isothermal drawing mode; the drawing temperature of the isothermal drawing mode is 200℃-600℃, and the drawing speed is 2m / min-5m / min; the length of the micro pipe material is >1m, the diameter is 0.15mm-5mm, the wall thickness is 0.02mm-1mm, and the wall thickness precision is ±0.005mm; The micro pipe material is cut into a ring material with a target length; The ring material is subjected to polishing treatment, cleaning and drying to obtain the precision ring material; the polishing treatment adopts ultrasonic vibration polishing, specifically, the cut ring material is soaked in an ultrasonic cleaning machine filled with diamond polishing liquid for ultrasonic vibration; The ultrasonic vibration time is 60-180 min, the temperature is 60-80 DEG C, and the vibration frequency is 20-80 kHz; during the ultrasonic vibration, a supporting device is used to limit the precision ring material in the ultrasonic cleaning machine; The diamond polishing liquid comprises, by weight percentage, 2-5% of diamond powder, 0.5-1% of water-soluble suspending agent, 0.5-2% of fatty alcohol polyoxyethylene ether dispersant, 0.2-0.5% of polyoxypropylene glycol ether defoaming agent, and the rest of ultrapure water; the particle size of the diamond powder is 0.1-2 microns.

4. The method of claim 3, wherein the precision ring is made of a material selected from the group consisting of a metal, a ceramic, a glass, a plastic, and a composite material. The isothermal drawing mode adopts a floating core drawing device for drawing; the floating core drawing device is composed of a drawing core, a drawing outer mold, a heating system and a temperature control system; the drawing outer mold is provided with a containing cavity for containing the pipe blank; the heating system and the temperature control system are installed in the drawing outer mold; during drawing, the pipe blank is contained in the containing cavity, the drawing core is inserted into the pipe blank along the inner wall of the pipe blank, the heating system heats the drawing outer mold, and the temperature control system monitors the temperature of the drawing outer mold.

5. The method of claim 4, wherein the precision ring is formed by a process comprising: The drawing core and the drawing outer mold are both made of zirconia ceramic material; the heating system adopts an electric heating rod; and the temperature control system adopts a temperature sensor and a temperature control system for control, with a temperature control accuracy of ±5 DEG C.

6. The method of claim 5, wherein the precision ring is formed by a process comprising: During pipe drawing, the inlet and outlet of the floating core drawing device are both protected by inert gas blowing.

7. The method of claim 6, wherein the precision ring is formed by a process comprising: When the outer diameter of the pipe blank is greater than 5 mm, the drawing core with a surface roughness Ra of 0.16 microns or less is used; when the outer diameter of the pipe blank is less than or equal to 5 mm, the drawing core with a surface roughness Ra of 0.08 microns or less is used.

8. The method of claim 3, wherein the precision ring is made of a material selected from the group consisting of a metal, a ceramic, a glass, a plastic, and a composite material. The supporting device comprises a grid-shaped base, supporting columns and a limiting assembly; the supporting columns are connected to the grid-shaped base, and the limiting assembly is arranged in the grid-shaped base; during ultrasonic vibration, the grid-shaped base is stably arranged in the ultrasonic cleaning machine through the supporting columns, the precision ring material is inserted into the grid-shaped base, and the precision ring material is stably arranged through the limiting assembly.

9. The method of claim 3, wherein the precision ring is made of a material selected from the group consisting of a metal, a ceramic, a glass, a plastic, and a composite material. The temperature of the homogenization heat treatment is 800-1500 DEG C, and the time is 120-240 min; and / or the homogenization heat treatment atmosphere is vacuum heat treatment.

10. The method of claim 3, wherein the precision ring is made of a material selected from the group consisting of a metal, a ceramic, a glass, a plastic, and a composite material. The melting temperature of the medium-frequency vacuum melting combined with the rapid cooling and solidification technology is 1500-3500 DEG C, and the downward drawing equipment is used for directional solidification.

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