WO2012024849A1 - Medical magnesium alloy biodegradability in vitro dynamic simulation test device - Google Patents

Medical magnesium alloy biodegradability in vitro dynamic simulation test device Download PDF

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Publication number
WO2012024849A1
WO2012024849A1 PCT/CN2010/076992 CN2010076992W WO2012024849A1 WO 2012024849 A1 WO2012024849 A1 WO 2012024849A1 CN 2010076992 W CN2010076992 W CN 2010076992W WO 2012024849 A1 WO2012024849 A1 WO 2012024849A1
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Prior art keywords
tank
test
liquid storage
storage tank
liquid
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PCT/CN2010/076992
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French (fr)
Chinese (zh)
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张永君
刘通
何柳
王治平
耿利红
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华南理工大学
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Publication of WO2012024849A1 publication Critical patent/WO2012024849A1/en

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00Investigating resistance of materials to the weather, to corrosion, or to light
    • G01N17/002Test chambers

Definitions

  • the invention belongs to the field of material performance testing technology and equipment, and relates to a device for dynamic simulation test evaluation of material corrosion degradation performance in a fluid medium, and is particularly suitable for biomedical materials/ In vitro dynamic simulation test of biodegradability of instruments such as medical magnesium alloys and medical device products.
  • LED technology has become increasingly mature. It has many advantages such as high luminous flux, long life, high reliability, energy saving, etc. It is the most potential light source to replace the existing illumination source.
  • the existing LED lamps a plurality of power LEDs are generally used in one fixture, so the heat dissipation of the LEDs becomes an important factor affecting the use state and life of the LED lamps.
  • the existing LED lamps generally adopt a closed structure, and the heat of the light source and the driving power source cannot be dissipated in a timely and effective manner.
  • some lamps are also designed with a special heat dissipation structure, the structure is usually complicated and the heat dissipation effect is not good.
  • the LED light source is generally disposed directly toward the ground, and the light emitted by the LED is uneven, which is irritating to the human eye, which seriously affects the lighting effect of the LED lamp, and is prone to cause visual fatigue in long-term viewing. Even the vision is declining.
  • magnesium alloys are expected to become ideal biomedical metal new materials for coronary artery because of their resources, price and performance, especially biodegradation-absorption, biocompatibility and mechanical compatibility.
  • Design and manufacture of highly value-added medical device products such as stents, tissue engineering scaffolds, bone nails, bone plates, bone meshes, and artificial bones.
  • the problem of too fast biodegradation has always restricted the biomedical use of magnesium alloys. Therefore, it is of great significance to study the biodegradation behavior of magnesium alloys and to develop magnesium alloy biodegradation control technologies (including new alloy development, surface modification, etc.).
  • the evaluation of magnesium alloy biodegradability is one of the core tasks.
  • the object of the present invention is to provide a dynamic simulation test capable of simulating the relative degradation state of the medium/material under the service state, and conveniently, quickly and accurately evaluating the degradation degradation property of the medium and the corrosion degradation behavior of the material, in view of the deficiencies of the prior art and equipment. device.
  • an in vitro dynamic simulation test device for biodegradation performance of medical magnesium alloy including a thermostatic bath, a liquid storage tank, a circulation pump, a flow meter, a test chamber, an upper sample carrier, and a pipette And a return pipe, wherein the liquid suction pipe and the return pipe are respectively placed in the liquid storage tank, the liquid storage tank is placed in the constant temperature tank, the flow meter and the test chamber are respectively vertically fixed, and the upper sample loader is suspended by the top cover of the test cabin In the test chamber; the pipette is located between the nozzle outside the reservoir tank and the inlet of the circulation pump, the outlet of the circulation pump and the inlet of the flow meter, the outlet of the flow meter and the inlet of the test chamber, and the test chamber
  • the outlet pipe and the return pipe are respectively connected by water pipes between the nozzles outside the liquid storage tank, and constitute a liquid medium circulation passage.
  • the liquid storage tank is a closed rectangular body container, and the partition is divided into left and right two independent tank bodies, wherein the right tank volume is 2.1 times of the volume of the left tank; the top of the liquid storage tank tank is provided with a supply port and a filter.
  • the supply port has a matching sealing plug
  • the liquid suction port is located at the top of the left tank of the liquid storage tank and is adjacent to the left side and the front side of the liquid storage tank
  • the return port is located at the liquid storage tank
  • the right tank top is adjacent to the right side and the front side of the liquid storage tank
  • the liquid suction port and the return port are respectively a passage of the liquid suction pipe and the return pipe through the top of the tank, and the pipe is sealed with the port;
  • the left side surface and the right side surface of the liquid storage tank respectively have a liquid discharge port, and the liquid discharge port is close to the bottom and rear sides of the liquid storage tank
  • the internally threaded pipe is seamlessly nested in the overflow hole and the drain port, and the internally threaded pipe has a matching threaded pipe plug.
  • the test cabin is composed of a five-part inlet duct, a trumpet-like progressive expansion, a cylindrical main compartment, a hatch cover and an exit hatch, wherein the intake duct and the main cabin are respectively located at two ends of the progressive expansion cabin and three A total of the central axis, the outboard tube is located on the side of the main cabin and is more than 21mm from the end of the main hatch; the hatch cover is threadedly connected to the main hatch, wherein the main hatch is externally threaded, and the hatch cover is circumferentially and the main hatch is externally threaded.
  • the geometric center of the roof cap is provided with a circular mounting hole for internal positioning of the upper-loading sampler with a circular test hole around the loading hole
  • the sample hole and the test hole are both through holes, and the test hole has a matching sealing plug
  • the inlet pipe and the outlet pipe are hollow bamboo pipes with uniform inner diameter, and the inner diameter of the outfitting pipe is 2.1 of the inner diameter of the inlet pipe.
  • the progressive expansion and the main cabin are hollow structures, and the inlet duct and the progressive expansion cabin, the exit cabin and the main cabin are directly connected; a circular porous steady flow plate is provided between the main cabin and the progressive expansion cabin.
  • the outer wall of the main compartment is marked with a height scale and a cylinder inner diameter, respectively, and the bulkhead bulkhead is transparent.
  • the upper loader consists of a positioning shaft, three loading heads and the same number of connecting bridges as the loading head, wherein one end of the connecting bridge is connected to the lower end of the positioning shaft, and the other end is connected to the upper end of the loading head.
  • the upper end of the positioning shaft and the lower end of the loading head are free ends, and there is a one-to-one correspondence between the loading head and the connecting bridge;
  • the positioning axis and the loading head are both cylindrical;
  • the axes are parallel to each other;
  • the connecting bridges are straight rods of the same size, and the connecting bridges are spatially evenly distributed with the axis of the positioning shaft as a reference line;
  • the dimensions of the loading heads are the same, and the free ends are provided with mounting samples
  • the external thread; the free end of the positioning shaft is a screw matching the circular center hole of the geometrical center of the roof cover;
  • the upper sample carrier is suspended downward in the main compartment of the test
  • the pipette and the return pipe are both hard water pipes, and the height of the pipe ends in the liquid storage tank is 3.5-14 mm from the inner side of the bottom of the liquid storage tank.
  • the invention Compared with the prior art and equipment, the invention has the advantages of compact structure, good controllability, convenient use and strong versatility.
  • the dynamic simulation test of the corrosion degradation performance of the material/device using the present invention can achieve the following outstanding effects:
  • the above-mentioned structural design of the liquid storage tank can ensure that the test medium has a sufficient residence time in the liquid storage tank during the circulation, which is beneficial to the temperature control of the constant temperature tank, and is convenient for accurately studying the temperature change to the medium. And the impact of material properties.
  • test chamber ensures that the flow of the test medium in the test chamber is smooth and controllable.
  • the invention and utilization of the upper loader realizes the loading of the test sample from the upper end of the sample with hard material, which solves the problem encountered by the traditional "suspended" sample loading method.
  • the structural design of the sample carrier can be carried out by one or three or more. It can realize the one-time loading and subsequent research and test of multiple samples, and achieve the purpose of obtaining multiple sets of data through one test, which can greatly reduce the workload and significantly improve the research and development efficiency. To ensure the controllability of the sample/medium relative motion parameters and the parallelism of the test conditions.
  • the device can easily realize the controlled flow of liquid medium in the test chamber, and can easily, quickly and accurately measure the relative movement speed of the material/medium and the surface area ratio, medium temperature, pH value and composition.
  • the effects of erosion and material corrosion degradability are of great value for revealing the corrosion behavior of materials, developing new materials/new instruments and their degradation control, and are of great significance for improving R&D efficiency, R&D quality and reducing R&D costs.
  • the device is not only suitable for simulating physiological environment in vivo such as dynamic blood/tissue fluid, etc. for biomedical metal materials such as magnesium alloys, titanium alloys, and degradable biomedical polymer materials such as PLLA, SR-PLLA, etc. and their medical device products. Degradation, and is applicable to the dynamic simulation of interaction between conventional engineering materials and military materials and aggressive media such as seawater and accelerated testing of related properties.
  • Figure 1 is a schematic view of the overall structure of the present invention.
  • FIG. 2 is a schematic front view showing the structure of the liquid storage tank of the present invention.
  • Fig. 3 is a schematic top plan view of the liquid storage tank of the present invention.
  • Figure 4 is a schematic side view showing the structure of the separator in the liquid storage tank of the present invention.
  • Figure 5 is a schematic view showing the structure of the test chamber of the present invention.
  • Figure 6 is a schematic view showing the structure of the hatch cover of the test cabin of the present invention.
  • Fig. 7 is a schematic front view showing the structure of the upper loader of the present invention.
  • FIG. 8 is a schematic top plan view of the upper position loader of the present invention.
  • the present invention comprises a constant temperature tank 1, a liquid storage tank 2, a circulation pump 3, a flow meter 4, a test chamber 5, an upper sample holder 6, a pipette 7 and a return pipe 8.
  • the liquid suction pipe 7 and the return pipe 8 are respectively placed in the liquid storage tank 2, so that the liquid medium enters and exits the liquid storage tank 2 during the test.
  • the liquid storage tank 2 is placed in the constant temperature tank 1, which facilitates the adjustment of the temperature of the liquid in the liquid storage tank 2 by the constant temperature tank 1, thereby ensuring that the temperature of the fluid acting in the test chamber 5 with the sample is within a preset range.
  • the flow meter 4 and the test chamber 5 are vertically fixed to the bracket, respectively, to facilitate regulation of the fluid flow rate and its stability.
  • the upper loader 6 is suspended in the test chamber 5 via the hatch cover 20 of the test chamber 5, and the test sample is loaded with the hard material from the upper end of the sample, thereby solving the traditional "suspended" sample loading method. Puzzle.
  • the pipette 7 is located between the nozzle outside the tank of the liquid storage tank 2 and the inlet of the circulation pump 3, the outlet of the circulation pump 3 and the inlet of the flow meter 4, the outlet of the flow meter 4 and the inlet tube 9 of the test chamber 5.
  • the outlet tube 10 of the test chamber 5 and the outlet tube 8 are respectively connected between the nozzles outside the tank of the liquid storage tank 2 through a water pipe to form a liquid medium circulation passage, and the test medium stored in the liquid storage tank 2 is in the circulation pump. 3
  • the power provided is circulated in the piping system centered on the test chamber 5.
  • the liquid storage tank 2 is a closed rectangular parallelepiped container, which is divided into left and right two independent tanks by the partition plate 11, wherein the right tank volume is 2.1 times or more of the volume of the left tank.
  • the top of the liquid storage tank 2 is provided with a supply port 12, a vent hole 13 with a filter, and a liquid suction port 14 and a return port 15, wherein the supply port 12 is provided with a matching sealing silicone plug.
  • the supply port 12 is for adding a test medium to the liquid storage tank 2, and the opening of the vent hole 13 facilitates the external discharge of the liquid storage tank 2 and maintains the stability of the air pressure in the liquid storage tank 2.
  • the liquid suction port 14 is located at the top of the left tank of the liquid storage tank 2 and is adjacent to the left side surface and the front side surface of the liquid storage tank 2
  • the return flow port 15 is located at the top of the right tank top of the liquid storage tank 2 and is adjacent to the right side of the liquid storage tank 2.
  • the front and front sides, the liquid suction port 14 and the return port 15 are respectively a passage of the pipette 7 and the return pipe 8 through the top of the tank, and the pipe is sealedly connected to the port.
  • Three overflow holes 16 are provided at different heights of the partition 11, and the overflow holes 16 are close to the rear side of the liquid storage tank 2.
  • the above design of the liquid suction port 14, the return port 15 and the partition plate 11 can ensure that the test medium has a sufficient residence time in the liquid storage tank 2 during the cycle, which is favorable for the temperature control of the constant temperature tank 1 and facilitates accurate study of temperature changes. Impact on media and material properties.
  • the left side surface and the right side surface of the liquid storage tank 2 are respectively provided with a liquid discharge port 17 which is close to the bottom of the tank and the rear side of the liquid storage tank 2, so as to facilitate the discharge of the residual liquid in the liquid storage tank 2 after the test is completed. Subsequent cleaning of the liquid storage tank 2.
  • the inner hole pipe is seamlessly nested in the overflow hole 16 and the liquid discharge port 17, and the inner threaded pipe has a matching threaded pipe plug, so that the opening and closing of the opening can be flexibly controlled according to actual conditions.
  • the pipette 7 and the return pipe 8 are hard water pipes to ensure a stable outlet position.
  • the pipette 7 and the return pipe 8 are respectively inserted into the tank through the liquid suction port 14 and the return port 15, and the pipe is sealed and connected with the port, and the pipe end of the tank is 3.5-14 mm away from the inner side of the tank bottom to reduce the test medium. The disturbance effect produced when the liquid storage tank 2 is discharged.
  • the test chamber 5 is composed of an inlet duct 9, a flared progressive expansion tank 18, a cylindrical main compartment 19, a hatch cover 20 and an exit duct 10, wherein the inlet duct 9 and the main compartment 19 are respectively located at both ends of the progressive expansion tank 18 and the three have a central axis.
  • the main compartment 19 has an inner diameter of 70 mm and a length of 490 mm.
  • the outlet duct 10 is located on the side of the main compartment 19 and 28 mm from the end face of the main hatch.
  • the hatch cover 20 is threadedly connected to the main hatch to facilitate frequent loading and unloading of the sample.
  • the inlet pipe 9 and the outlet pipe 10 are hollow bamboo pipes of uniform inner diameter, which facilitate the fastening connection of the external hose to the test chamber 5 and ensure the airtightness of the joint.
  • the inlet tube 9 has an inner diameter of 7.0 mm and the outlet tube 10 has an inner diameter of 15.4 mm.
  • the inner diameter ratio of the inlet tube 9 and the outlet tube 10 ensures that the test medium enters and exits the test chamber 5 at different flow rates. Balance to maintain the stability of the liquid level.
  • the progressive expansion tank 18 and the main cabin 19 are hollow structures, and the inlet duct 9 and the flare bay 18 cabin, the outlet duct 10 and the main cabin 19 cabin are directly in communication.
  • a circular porous flow plate 23 is provided between the main chamber 19 and the flared tank 18, and has an inner diameter of 33 mm.
  • the special structural design of the test chamber ensures that the flow of the test medium in the test chamber is smooth and controllable.
  • the outer wall of the main compartment 19 is marked with a height scale and a cylinder inner diameter to facilitate the adjustment of the liquid level and the sample installation position and the measurement of the medium flow rate.
  • the main compartment 19 scale area bulkhead is transparent, which is convenient for tracking the corrosion degradation process of the sample in the test chamber 5.
  • the geometric center of the hatch cover 20 is provided with a circular loading hole 21 having an internal diameter of 6.3 mm.
  • a circular test hole 22 is provided around the sample loading hole 21, and both the sample hole 21 and the test hole 22 are through holes, and the test hole 22 has a matching sealing plug.
  • the presence of the sample loading hole 21 and the matching of the upper sample holder 6 greatly facilitate the mounting and fixing of the sample.
  • the design of the test hole 22 provides convenience for real-time inspection/monitoring of physical and chemical parameters such as medium temperature, pH value and composition in the test chamber 5.
  • the upper loader 6 is composed of a positioning shaft 24, three loading heads 25 and three connecting bridges 26, wherein one end of the connecting bridge 26 is connected to the lower end of the positioning shaft 24, and the other end is connected.
  • the upper end of the positioning shaft 24 and the lower end of the loading head 25 are free ends, and the loading head 25 and the connecting bridge 26 have a one-to-one correspondence.
  • the positioning shaft 24 and the loading head 25 are both cylindrical.
  • the axis of the loading head 25 is parallel to the axis of the positioning shaft 24.
  • the connecting bridges 26 are straight rods of the same size, and the connecting bridges 26 are spatially evenly distributed with the axis of the positioning shaft 24 as a reference line.
  • the above-mentioned structural design of the upper sample loading device 6 can be used for one-time loading and subsequent research and testing of multiple samples, and achieves the purpose of obtaining multiple sets of data through one test, thereby greatly reducing the workload and significantly improving the research and development. At the same time of efficiency, the controllability of the relative motion parameters of the sample/medium and the parallelism of the test conditions are ensured.
  • the loading head 25 has a diameter of 2.8 mm, and the free end thereof is provided with an external thread for mounting the sample. The threaded connection between the loading sample and the sample sample ensures that the loading of the sample is firm and reliable, and at the same time The pose of the sample is controlled.
  • the free end of the positioning shaft 24 is a screw that mates with the geometric center circular loading hole 21 of the roof cap 20, and can be provided with a fastening and sealing nut.
  • the invention and application of the upper loader 6 realizes loading the test sample with the hard material from the upper end thereof, and solves the problem encountered by the traditional "suspended" sample loading method.
  • a pre-configured test medium such as Hank's simulated body fluid is injected through the supply port 12 of the tank top of the liquid storage tank 2
  • the liquid storage tank 2 The liquid storage tank 2; the power switch of the constant temperature tank 1 is turned on, the temperature is preset, the test medium is heated and the temperature is constant; the sample processed with the sample loading hole matched with the sample loading head 25 is subjected to metallographic grinding, washing and drying.
  • Pre-treatment such as micro-arc/anodizing, bionic passivation, etc., and then screwing it into the loading head 25 of the upper-loading sampler 6; the loading head 25 is facing downward, and the positioning shaft 24 of the upper-loading sampler 6 is screwed into the test.
  • the loading hole 21 of the geometric center of the hatch cover 20 of the tank 5; screwing the hatch cover 20 to the main hatch of the test chamber 5; opening the circulation pump 3, and adjusting the medium flow/flow rate to the medium by the flow meter 4 Set the flow rate to stabilize the circulation in the pipeline system; after a certain period of time, close the circulation pump 3, unscrew the top cover 20, remove the upper sample carrier 6, and take the sample on the sample 25; then follow the known method.
  • cleaning, drying, weighing and surface / Surface analysis testing to obtain a material corrosion degradation rich and comprehensive information, such as the mass change, degradation phase composition, microstructure elements and the like.

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Abstract

A medical magnesium alloy biodegradability in vitro dynamic simulation test device includes a thermostatic bath (1), a liquid storage tank (2), a circulation pump (3), a flow meter (4), a test cabin (5), an upper sample loader (6), a liquid absorbing tube (7) and a backflow tube (8). The liquid absorbing tube (7) and the backflow tube (8) are arranged in the liquid storage tank (2), respectively. The liquid storage tank (2) is arranged in the thermostatic bath (1). The flow meter (4) and the test cabin (5) are vertically arranged, respectively. The upper sample loader (6) pierces the top cover (20) and is hung in the test cabin (5). The test device has water tubes respectively arranged between inlets of the liquid absorbing tube (7) and the circulation pump (3), between an outlet of the circulation pump (3) and an inlet of the flow meter (4), and between an outlet of the flow meter (4) and the cabin inlet tube (9) of the test cabin (5). The water tubes are further arranged between the cabin outlet tube (10) of the test cabin (5) and the backflow tube (8) for connection to compose a liquid medium circulation path. The device provides a compact structure, convenient use and strong commonality, and provides fast and accurately test and evaluation of the influence of the flow speed, the component, the temperature and the PH value of a medium on the medium corrodibility and the material degradation.

Description

医用镁合金生物降解性能体外动态模拟测试设备  In vitro dynamic simulation test equipment for biodegradation performance of medical magnesium alloy
技术领域Technical field
本发明属于材料性能测试技术和设备领域,涉及一种在流体介质中对材料腐蚀降解性能进行动态模拟测试评价的设备,特别适用于生物医用材料 / 器械如医用镁合金及其医疗器械产品生物降解性能的体外动态模拟测试。 The invention belongs to the field of material performance testing technology and equipment, and relates to a device for dynamic simulation test evaluation of material corrosion degradation performance in a fluid medium, and is particularly suitable for biomedical materials/ In vitro dynamic simulation test of biodegradability of instruments such as medical magnesium alloys and medical device products.
背景技术Background technique
随着发光二极管技术的发展,大功率LED技术已日趋成熟,其具有光通量高、寿命长、可靠性高、节能等多项优点,是替代现有照明光源的最潜在光源。现有的LED灯具,一般是将多个功率型LED集中在一个灯具上使用,因此LED的散热成为影响LED灯具使用状态及寿命的一个重要因素。但是,现有的LED灯具普遍采用封闭式的结构,光源及驱动电源的热量不能及时有效地散发,虽然有的灯具也设计专门的散热结构,但是通常结构复杂,散热效果不佳。另外,现有大功率LED灯具中,LED光源一般是直接朝向地面设置的,LED射出来的光不均匀,对人眼刺激较大,严重影响LED灯具的照明效果,长期观看,容易引起视觉疲劳甚至视力下降。With the development of LED technology, high-power LED technology has become increasingly mature. It has many advantages such as high luminous flux, long life, high reliability, energy saving, etc. It is the most potential light source to replace the existing illumination source. In the existing LED lamps, a plurality of power LEDs are generally used in one fixture, so the heat dissipation of the LEDs becomes an important factor affecting the use state and life of the LED lamps. However, the existing LED lamps generally adopt a closed structure, and the heat of the light source and the driving power source cannot be dissipated in a timely and effective manner. Although some lamps are also designed with a special heat dissipation structure, the structure is usually complicated and the heat dissipation effect is not good. In addition, in the existing high-power LED lamps, the LED light source is generally disposed directly toward the ground, and the light emitted by the LED is uneven, which is irritating to the human eye, which seriously affects the lighting effect of the LED lamp, and is prone to cause visual fatigue in long-term viewing. Even the vision is declining.
服役于液态环境中的材料,如植入人体内的医疗器械、海水中的舰艇船舶等,与介质间的相对运动对其腐蚀降解行为有着十分重要的影响。研究表明,这种相对运动不仅可以改变材料/器械的腐蚀降解速度,而且可以改变其腐蚀降解类型及其机制。因此,模拟实际服役状况尤其是环境介质与材料/器械间的相对运动,对于揭示介质降解侵蚀性及材料/器械腐蚀降解行为真实规律、开发新材料/新器械及其降解控制技术等具有重要意义。Materials that are used in a liquid environment, such as medical devices implanted in the human body, ship ships in seawater, etc., and the relative motion between the media have a very important influence on the corrosion degradation behavior. Studies have shown that this relative motion can not only change the corrosion degradation rate of materials/devices, but also change the type of corrosion degradation and its mechanism. Therefore, simulating the actual service conditions, especially the relative motion between the environmental medium and the material/device, is of great significance for revealing the degradation of the medium and the true law of material/device corrosion degradation, developing new materials/new instruments and their degradation control technologies. .
以生物医用金属材料为例,镁合金以其资源、价格和性能尤其是生物降解-吸收性、生物相容性和力学相容性优势,有望成为理想的生物医用金属新材料,用于冠脉支架、组织工程支架、骨钉、骨板、骨网以及人工骨等附加值极高的医疗器械产品的设计、制造。但是,生物降解过快的问题却一直制约着镁合金的生物医用。因此,研究镁合金生物降解行为规律、开发镁合金生物降解控制技术(包括新合金开发、表面改性等)具有重要意义。在生物医用镁技术的研发进程中,镁合金生物降解性能的测评是核心任务之一。现有动态模拟试验设备或以满足普通工业用材如铁基材料的性能测试为设计原则,未考虑生物材料测试条件要求的特殊性,如封闭、无菌、恒温等;或以常规生物医用金属材料如不锈钢、钛合金等的性能测试为出发点,未考虑镁合金的特殊性——生物降解性及阴极降解产物在水基介质中的难溶性。因此,现有动态模拟试验设备应用于镁合金生物降解性能的研究存在诸多缺憾。受此限制,镁合金生物降解性能的现有测评仍以经典的全浸腐蚀试验法为主。这种方法虽简单易行,却存在如下主要弊端:1)忽略了材料/介质除对流以外的相对运动对材料腐蚀降解行为的重要影响。而镁合金指日可待的生物医用,尤其是作为冠脉支架等使用时,不可避免会受到流动的人体体液如血液、组织液等的剪切作用;2)作为1)的直接后果,相关结果与体内植入试验结果相去甚远,难以准确预测材料/器械的体内生物降解性能,导致其临床参考价值大打折扣,从而失去了体外研究应有的意义。因此,设计、开发适应镁合金生物降解特性的动态模拟试验设备,已成为生物医用镁技术研发工作的当务之急。 Taking biomedical metal materials as an example, magnesium alloys are expected to become ideal biomedical metal new materials for coronary artery because of their resources, price and performance, especially biodegradation-absorption, biocompatibility and mechanical compatibility. Design and manufacture of highly value-added medical device products such as stents, tissue engineering scaffolds, bone nails, bone plates, bone meshes, and artificial bones. However, the problem of too fast biodegradation has always restricted the biomedical use of magnesium alloys. Therefore, it is of great significance to study the biodegradation behavior of magnesium alloys and to develop magnesium alloy biodegradation control technologies (including new alloy development, surface modification, etc.). In the research and development of biomedical magnesium technology, the evaluation of magnesium alloy biodegradability is one of the core tasks. Existing dynamic simulation test equipment or performance test to meet the performance test of common industrial materials such as iron-based materials, does not consider the specific requirements of biological material test conditions, such as closed, sterile, constant temperature, etc.; or conventional biomedical metal materials The performance test of stainless steel, titanium alloy, etc. is the starting point, and the particularity of magnesium alloy - biodegradability and poor solubility of cathode degradation products in water - based media are not considered. Therefore, there are many shortcomings in the application of existing dynamic simulation test equipment to the biodegradability of magnesium alloys. Due to this limitation, the existing evaluation of the biodegradability of magnesium alloys is still dominated by the classical full immersion corrosion test. Although this method is simple and easy, it has the following main drawbacks: 1) It ignores the important influence of the relative motion of the material/medium except convection on the corrosion degradation behavior of the material. Magnesium alloys are just around the corner for biomedical applications, especially when used as coronary stents, etc., which are inevitably subject to shearing by flowing human body fluids such as blood and tissue fluids; 2) as a direct consequence of 1), related results and in vivo planting The results of the test are far from the same, and it is difficult to accurately predict the in vivo biodegradability of the material/device, which leads to a great compromise in its clinical reference value, thus losing the significance of in vitro research. Therefore, the design and development of dynamic simulation test equipment adapted to the biodegradation characteristics of magnesium alloys has become an urgent task in the research and development of biomedical magnesium technology.
发明内容Summary of the invention
本发明的目的就是针对现有技术及设备之不足,提供一种能够模拟服役状态下介质/材料间相对运动状态,方便、快捷、准确地评价介质降解侵蚀性和材料腐蚀降解行为的动态模拟测试设备。The object of the present invention is to provide a dynamic simulation test capable of simulating the relative degradation state of the medium/material under the service state, and conveniently, quickly and accurately evaluating the degradation degradation property of the medium and the corrosion degradation behavior of the material, in view of the deficiencies of the prior art and equipment. device.
本发明的上述目的通过以下技术方案实现:一种医用镁合金生物降解性能体外动态模拟测试设备,包括恒温槽、储液罐、循环泵、流量计、测试舱、上位载样器、吸液管和回流管,其中吸液管和回流管分别置于储液罐中,储液罐置于恒温槽中,流量计和测试舱分别竖直固定,上位载样器经测试舱之舱顶盖悬挂于测试舱内;吸液管位于储液罐罐外的管口与循环泵之入口间、循环泵之出口与流量计之入口间、流量计之出口与测试舱之进舱管间、测试舱之出舱管与回流管位于储液罐罐外的管口间分别通过水管相连,构成液态介质循环通路。The above object of the present invention is achieved by the following technical solutions: an in vitro dynamic simulation test device for biodegradation performance of medical magnesium alloy, including a thermostatic bath, a liquid storage tank, a circulation pump, a flow meter, a test chamber, an upper sample carrier, and a pipette And a return pipe, wherein the liquid suction pipe and the return pipe are respectively placed in the liquid storage tank, the liquid storage tank is placed in the constant temperature tank, the flow meter and the test chamber are respectively vertically fixed, and the upper sample loader is suspended by the top cover of the test cabin In the test chamber; the pipette is located between the nozzle outside the reservoir tank and the inlet of the circulation pump, the outlet of the circulation pump and the inlet of the flow meter, the outlet of the flow meter and the inlet of the test chamber, and the test chamber The outlet pipe and the return pipe are respectively connected by water pipes between the nozzles outside the liquid storage tank, and constitute a liquid medium circulation passage.
所述储液罐为封闭方体容器,由隔板分成左、右两个独立罐体,其中右罐容积为左罐容积的2.1倍以上;储液罐罐顶设有补给口、带滤器的通气孔、吸液口和回流口,其中补给口带匹配的密封塞,吸液口位于储液罐之左罐罐顶并靠近储液罐之左侧面和前侧面,回流口位于储液罐之右罐罐顶并靠近储液罐之右侧面和前侧面,吸液口和回流口分别是吸液管和回流管通过罐顶的通道,管与口之间密封连接;在隔板的不同高度间隔设有溢流孔,溢流孔靠近储液罐之后侧面;储液罐之左侧面和右侧面分别开有排液口,排液口靠近储液罐之罐底和后侧面;溢流孔和排液口内均无缝嵌套内螺纹管,内螺纹管带匹配的螺纹管塞。The liquid storage tank is a closed rectangular body container, and the partition is divided into left and right two independent tank bodies, wherein the right tank volume is 2.1 times of the volume of the left tank; the top of the liquid storage tank tank is provided with a supply port and a filter. a vent, a suction port and a return port, wherein the supply port has a matching sealing plug, the liquid suction port is located at the top of the left tank of the liquid storage tank and is adjacent to the left side and the front side of the liquid storage tank, and the return port is located at the liquid storage tank The right tank top is adjacent to the right side and the front side of the liquid storage tank, and the liquid suction port and the return port are respectively a passage of the liquid suction pipe and the return pipe through the top of the tank, and the pipe is sealed with the port; There are overflow holes at different height intervals, and the overflow holes are close to the rear side of the liquid storage tank; the left side surface and the right side surface of the liquid storage tank respectively have a liquid discharge port, and the liquid discharge port is close to the bottom and rear sides of the liquid storage tank The internally threaded pipe is seamlessly nested in the overflow hole and the drain port, and the internally threaded pipe has a matching threaded pipe plug.
所述测试舱由进舱管、喇叭状渐扩舱、圆筒状主舱、舱顶盖和出舱管五部分构成,其中进舱管和主舱分别位于渐扩舱的两端且三者共中轴线,出舱管位于主舱侧面且距主舱口端面21mm以上;舱顶盖与主舱口通过螺纹连接,其中主舱口带外螺纹,舱顶盖盖周带与主舱口外螺纹匹配的内螺纹,盖顶内衬密封垫圈;舱顶盖几何中心设有带内螺纹的用于对上位载样器进行定位的圆形装样孔,在装样孔周围设有圆形测试孔,装样孔和测试孔均为通孔,且测试孔带匹配的密封塞;进舱管和出舱管均为内径均匀的中空竹节管,且出舱管内径为进舱管内径的2.1倍以上;渐扩舱和主舱为中空结构,且进舱管与渐扩舱舱室、出舱管与主舱舱室分别直接相通;主舱与渐扩舱之间设有圆形多孔稳流板;主舱外壁分别标有高度刻度和圆筒内径,且刻度区舱壁透明。The test cabin is composed of a five-part inlet duct, a trumpet-like progressive expansion, a cylindrical main compartment, a hatch cover and an exit hatch, wherein the intake duct and the main cabin are respectively located at two ends of the progressive expansion cabin and three A total of the central axis, the outboard tube is located on the side of the main cabin and is more than 21mm from the end of the main hatch; the hatch cover is threadedly connected to the main hatch, wherein the main hatch is externally threaded, and the hatch cover is circumferentially and the main hatch is externally threaded. Matching internal thread, cap-lined gasket; the geometric center of the roof cap is provided with a circular mounting hole for internal positioning of the upper-loading sampler with a circular test hole around the loading hole The sample hole and the test hole are both through holes, and the test hole has a matching sealing plug; the inlet pipe and the outlet pipe are hollow bamboo pipes with uniform inner diameter, and the inner diameter of the outfitting pipe is 2.1 of the inner diameter of the inlet pipe. More than double; the progressive expansion and the main cabin are hollow structures, and the inlet duct and the progressive expansion cabin, the exit cabin and the main cabin are directly connected; a circular porous steady flow plate is provided between the main cabin and the progressive expansion cabin. The outer wall of the main compartment is marked with a height scale and a cylinder inner diameter, respectively, and the bulkhead bulkhead is transparent.
所述上位载样器由一个定位轴、三个以上载样头以及与载样头相同数量的衔接桥组成,其中衔接桥的一端与定位轴的下端相连,另一端与载样头的上端相连,定位轴的上端和载样头的下端均为自由端,载样头与衔接桥之间为一一对应关系;定位轴与载样头均为圆柱体;载样头的轴线与定位轴的轴线相互平行;衔接桥均为尺寸相同的直杆,且衔接桥以定位轴的轴线为基准线在空间上均匀分布;载样头的尺寸均相同,且其自由端均设有用于安装试样的外螺纹;定位轴之自由端为与舱顶盖几何中心圆形装样孔匹配的螺杆;上位载样器载样头朝下经装样孔悬挂于测试舱之主舱内。The upper loader consists of a positioning shaft, three loading heads and the same number of connecting bridges as the loading head, wherein one end of the connecting bridge is connected to the lower end of the positioning shaft, and the other end is connected to the upper end of the loading head. The upper end of the positioning shaft and the lower end of the loading head are free ends, and there is a one-to-one correspondence between the loading head and the connecting bridge; the positioning axis and the loading head are both cylindrical; the axis of the loading head and the positioning axis The axes are parallel to each other; the connecting bridges are straight rods of the same size, and the connecting bridges are spatially evenly distributed with the axis of the positioning shaft as a reference line; the dimensions of the loading heads are the same, and the free ends are provided with mounting samples The external thread; the free end of the positioning shaft is a screw matching the circular center hole of the geometrical center of the roof cover; the upper sample carrier is suspended downward in the main compartment of the test chamber through the sample hole.
所述吸液管和回流管均为硬质水管,两者在储液罐内的管口端距储液罐罐底内侧面的高度为3.5-14mm。The pipette and the return pipe are both hard water pipes, and the height of the pipe ends in the liquid storage tank is 3.5-14 mm from the inner side of the bottom of the liquid storage tank.
与现有技术及设备相比,本发明具有结构紧凑、可控性好、使用方便、通用性强等优点。利用本发明进行材料/器械腐蚀降解性能的动态模拟测试,可取得如下突出效果: Compared with the prior art and equipment, the invention has the advantages of compact structure, good controllability, convenient use and strong versatility. The dynamic simulation test of the corrosion degradation performance of the material/device using the present invention can achieve the following outstanding effects:
1)恒温槽的利用,储液罐的上述结构设计,可确保测试介质在循环期间在储液罐内有充裕的停留时间,有利于恒温槽对其温度的调控,便于精确研究温度变化对介质及材料性能的影响。1) The use of the constant temperature tank, the above-mentioned structural design of the liquid storage tank can ensure that the test medium has a sufficient residence time in the liquid storage tank during the circulation, which is beneficial to the temperature control of the constant temperature tank, and is convenient for accurately studying the temperature change to the medium. And the impact of material properties.
2)测试舱的上述结构设计,可确保测试介质在测试舱内的流动平稳、可控。2) The above structural design of the test chamber ensures that the flow of the test medium in the test chamber is smooth and controllable.
3)上位载样器的发明和利用,实现了对试验样品以硬质材料从样品上端进行装载,解决了传统“悬吊式”载样法遇到的难题。载样器一拖三或以上的结构设计,可实现对多个样品的一次性装载及后续研究测试,达到通过一次试验获取多组数据的目的,在大幅降低工作量、显著提高研发效率的同时,确保试样/介质相对运动参数的可控性以及测试条件的平行性。3) The invention and utilization of the upper loader realizes the loading of the test sample from the upper end of the sample with hard material, which solves the problem encountered by the traditional "suspended" sample loading method. The structural design of the sample carrier can be carried out by one or three or more. It can realize the one-time loading and subsequent research and test of multiple samples, and achieve the purpose of obtaining multiple sets of data through one test, which can greatly reduce the workload and significantly improve the research and development efficiency. To ensure the controllability of the sample/medium relative motion parameters and the parallelism of the test conditions.
4)利用该设备易于实现液态介质在测试舱内的受控流动,可方便、快捷、准确地测评材料/介质间相对运动速度及面容比、介质温度、pH值和组分等重要参数对介质侵蚀性及材料腐蚀降解性的影响,对揭示材料腐蚀降解行为规律、开发新材料/新器械及其降解控制等应用技术具有重要价值,对提高研发效率和研发质量、降低研发成本具有重要意义。4) The device can easily realize the controlled flow of liquid medium in the test chamber, and can easily, quickly and accurately measure the relative movement speed of the material/medium and the surface area ratio, medium temperature, pH value and composition. The effects of erosion and material corrosion degradability are of great value for revealing the corrosion behavior of materials, developing new materials/new instruments and their degradation control, and are of great significance for improving R&D efficiency, R&D quality and reducing R&D costs.
5)该设备不仅适用于模拟体内生理环境如动态血液/组织液等对生物医用金属材料如镁合金、钛合金等以及可降解生物医用高分子材料如PLLA、SR-PLLA等及其医疗器械产品的降解作用,而且适用于常规工程材料以及军工材料等与诸如海水之类的侵蚀性介质间相互作用的动态模拟及相关性能的加速测试。5) The device is not only suitable for simulating physiological environment in vivo such as dynamic blood/tissue fluid, etc. for biomedical metal materials such as magnesium alloys, titanium alloys, and degradable biomedical polymer materials such as PLLA, SR-PLLA, etc. and their medical device products. Degradation, and is applicable to the dynamic simulation of interaction between conventional engineering materials and military materials and aggressive media such as seawater and accelerated testing of related properties.
附图说明DRAWINGS
图1为本发明整体结构示意图。Figure 1 is a schematic view of the overall structure of the present invention.
图2为本发明之储液罐主视结构示意图。2 is a schematic front view showing the structure of the liquid storage tank of the present invention.
图3为本发明之储液罐俯视结构示意图。Fig. 3 is a schematic top plan view of the liquid storage tank of the present invention.
图4为本发明之储液罐中隔板侧视结构示意图。Figure 4 is a schematic side view showing the structure of the separator in the liquid storage tank of the present invention.
图5为本发明之测试舱结构示意图。Figure 5 is a schematic view showing the structure of the test chamber of the present invention.
图6为本发明之测试舱的舱顶盖结构示意图。Figure 6 is a schematic view showing the structure of the hatch cover of the test cabin of the present invention.
图7为本发明之上位载样器主视结构示意图。Fig. 7 is a schematic front view showing the structure of the upper loader of the present invention.
图8为本发明之上位载样器俯视结构示意图。FIG. 8 is a schematic top plan view of the upper position loader of the present invention.
图中:1—恒温槽,2—储液罐,3—循环泵,4—流量计,5—测试舱,6—上位载样器,7—吸液管,8—回流管,9—进舱管,10—出舱管,11—隔板,12—补给口,13—通气孔,14—吸液口,15—回流口,16—溢流孔,17—排液口,18—渐扩舱,19—主舱,20—舱顶盖,21—装样孔,22—测试孔,23—多孔稳流板,24—定位轴,25—载样头,26—衔接桥。In the picture: 1 - constant temperature tank, 2 - liquid storage tank, 3 - circulation pump, 4 - flow meter, 5 - test chamber, 6 - upper load sampler, 7 - pipette, 8 - return pipe, 9 - feed Cabin, 10 - outboard, 11 - partition, 12 - supply, 13 - vent, 14 - suction, 15 - return, 16 - overflow, 17 - drain, 18 - Expansion, 19-main cabin, 20-cap top cover, 21-packing hole, 22-test hole, 23-porous steady flow plate, 24-positioning shaft, 25-loading head, 26-connecting bridge.
具体实施方式detailed description
下面结合附图对本发明的具体实施作进一步说明,但本发明的保护范围和实施不限于此。The specific implementation of the present invention will be further described below with reference to the accompanying drawings, but the scope and implementation of the present invention are not limited thereto.
如图1所示,本发明由恒温槽1、储液罐2、循环泵3、流量计4、测试舱5、上位载样器6、吸液管7和回流管8组成。其中吸液管7和回流管8分别置于储液罐2中,便于测试时液态介质进、出储液罐2。储液罐2置于恒温槽1中,有利于恒温槽1对储液罐2中液体温度的调控,从而确保测试舱5内与试样作用的流体的温度处于预设范围。流量计4和测试舱5分别垂直固定于支架上,便于对流体流速及其平稳性等进行调控。上位载样器6经测试舱5之舱顶盖20悬挂于测试舱5内,实现了对试验样品以硬质材料从样品上端进行装载,从而解决了传统“悬吊式”载样法遇到的难题。吸液管7位于储液罐2罐外的管口与循环泵3之入口间、循环泵3之出口与流量计4之入口间、流量计4之出口与测试舱5之进舱管9间、测试舱5之出舱管10与回流管8位于储液罐2罐外的管口间分别通过水管相连,构成液态介质循环通路,便于存贮于储液罐2中的测试介质在循环泵3提供的动力下在以测试舱5为中心的管路系统中循环流动。As shown in Fig. 1, the present invention comprises a constant temperature tank 1, a liquid storage tank 2, a circulation pump 3, a flow meter 4, a test chamber 5, an upper sample holder 6, a pipette 7 and a return pipe 8. The liquid suction pipe 7 and the return pipe 8 are respectively placed in the liquid storage tank 2, so that the liquid medium enters and exits the liquid storage tank 2 during the test. The liquid storage tank 2 is placed in the constant temperature tank 1, which facilitates the adjustment of the temperature of the liquid in the liquid storage tank 2 by the constant temperature tank 1, thereby ensuring that the temperature of the fluid acting in the test chamber 5 with the sample is within a preset range. The flow meter 4 and the test chamber 5 are vertically fixed to the bracket, respectively, to facilitate regulation of the fluid flow rate and its stability. The upper loader 6 is suspended in the test chamber 5 via the hatch cover 20 of the test chamber 5, and the test sample is loaded with the hard material from the upper end of the sample, thereby solving the traditional "suspended" sample loading method. Puzzle. The pipette 7 is located between the nozzle outside the tank of the liquid storage tank 2 and the inlet of the circulation pump 3, the outlet of the circulation pump 3 and the inlet of the flow meter 4, the outlet of the flow meter 4 and the inlet tube 9 of the test chamber 5. The outlet tube 10 of the test chamber 5 and the outlet tube 8 are respectively connected between the nozzles outside the tank of the liquid storage tank 2 through a water pipe to form a liquid medium circulation passage, and the test medium stored in the liquid storage tank 2 is in the circulation pump. 3 The power provided is circulated in the piping system centered on the test chamber 5.
如图2、图3和图4所示,储液罐2为封闭的长方体容器,由隔板11分成左、右两个独立罐体,其中右罐容积为左罐容积的2.1倍以上。储液罐2罐顶设有补给口12、带滤器的通气孔13以及吸液口14和回流口15,其中补给口12带匹配的密封用硅胶塞。补给口12用于向储液罐2中添加测试介质,通气孔13的开设便于储液罐2向外排气以及维持储液罐2中气压的稳定。吸液口14位于储液罐2之左罐罐顶并靠近储液罐2之左侧面和前侧面,回流口15位于储液罐2之右罐罐顶并靠近储液罐2之右侧面和前侧面,吸液口14和回流口15分别是吸液管7和回流管8通过罐顶的通道,管与口之间密封连接。在隔板11的不同高度设有三个溢流孔16,溢流孔16靠近储液罐2之后侧面。吸液口14、回流口15以及隔板11的上述设计可确保测试介质在循环期间在储液罐2内有充裕的停留时间,有利于恒温槽1对其温度的调控,便于精确研究温度变化对介质及材料性能的影响。储液罐2之左侧面和右侧面分别设有排液口17,排液口17靠近储液罐2之罐底和后侧面,便于测试结束后储液罐2内残液的排放及对储液罐2的后续清洗。溢流孔16和排液口17内均无缝嵌套内螺纹管,内螺纹管带匹配的螺纹管塞,便于根据实际情况灵活控制孔口的开与关。吸液管7和回流管8为硬质水管,可确保其出口位置稳定。吸液管7和回流管8分别经吸液口14和回流口15插入罐内,管与口之间密封连接,其罐内管口端距罐底内侧面3.5-14mm,以降低测试介质进、出储液罐2时产生的扰动效应。As shown in FIG. 2, FIG. 3 and FIG. 4, the liquid storage tank 2 is a closed rectangular parallelepiped container, which is divided into left and right two independent tanks by the partition plate 11, wherein the right tank volume is 2.1 times or more of the volume of the left tank. The top of the liquid storage tank 2 is provided with a supply port 12, a vent hole 13 with a filter, and a liquid suction port 14 and a return port 15, wherein the supply port 12 is provided with a matching sealing silicone plug. The supply port 12 is for adding a test medium to the liquid storage tank 2, and the opening of the vent hole 13 facilitates the external discharge of the liquid storage tank 2 and maintains the stability of the air pressure in the liquid storage tank 2. The liquid suction port 14 is located at the top of the left tank of the liquid storage tank 2 and is adjacent to the left side surface and the front side surface of the liquid storage tank 2, and the return flow port 15 is located at the top of the right tank top of the liquid storage tank 2 and is adjacent to the right side of the liquid storage tank 2. The front and front sides, the liquid suction port 14 and the return port 15 are respectively a passage of the pipette 7 and the return pipe 8 through the top of the tank, and the pipe is sealedly connected to the port. Three overflow holes 16 are provided at different heights of the partition 11, and the overflow holes 16 are close to the rear side of the liquid storage tank 2. The above design of the liquid suction port 14, the return port 15 and the partition plate 11 can ensure that the test medium has a sufficient residence time in the liquid storage tank 2 during the cycle, which is favorable for the temperature control of the constant temperature tank 1 and facilitates accurate study of temperature changes. Impact on media and material properties. The left side surface and the right side surface of the liquid storage tank 2 are respectively provided with a liquid discharge port 17 which is close to the bottom of the tank and the rear side of the liquid storage tank 2, so as to facilitate the discharge of the residual liquid in the liquid storage tank 2 after the test is completed. Subsequent cleaning of the liquid storage tank 2. The inner hole pipe is seamlessly nested in the overflow hole 16 and the liquid discharge port 17, and the inner threaded pipe has a matching threaded pipe plug, so that the opening and closing of the opening can be flexibly controlled according to actual conditions. The pipette 7 and the return pipe 8 are hard water pipes to ensure a stable outlet position. The pipette 7 and the return pipe 8 are respectively inserted into the tank through the liquid suction port 14 and the return port 15, and the pipe is sealed and connected with the port, and the pipe end of the tank is 3.5-14 mm away from the inner side of the tank bottom to reduce the test medium. The disturbance effect produced when the liquid storage tank 2 is discharged.
如图5所示,测试舱5由进舱管9、喇叭状渐扩舱18、圆筒状主舱19、舱顶盖20和出舱管10五部分构成,其中进舱管9和主舱19分别位于渐扩舱18的两端且三者共中轴线,主舱19内径为70mm,长度为490mm。出舱管10位于主舱19侧面且距主舱口端面28mm。舱顶盖20与主舱口通过螺纹连接,方便试样的频繁装卸。其中主舱口带外螺纹,舱顶盖20盖周带与主舱口外螺纹匹配的内螺纹,舱顶盖20盖顶内衬密封垫圈,可确保舱顶盖20与测试舱5之间的气密性要求,防止因漏气导致流体外泄、液位波动等系列问题。进舱管9和出舱管10均为内径均匀的中空竹节管,便于外接软管与测试舱5的紧固连接以及确保连接处的气密性。进舱管9的内径为7.0mm,出舱管10的内径为15.4mm,进舱管9和出舱管10的内径比例设计可确保测试介质在不同流速下在测试舱5内的进、出平衡,从而维持其中液位的稳定。渐扩舱18和主舱19为中空结构,且进舱管9与渐扩舱18舱室、出舱管10与主舱19舱室分别直接相通。主舱19与渐扩舱18之间设有圆形多孔稳流板23,其内径为33mm。测试舱上述特殊的结构设计,可确保测试介质在测试舱内的流动平稳、可控。主舱19外壁分别标有高度刻度和圆筒内径,便于液位及试样安装位置的调整以及介质流速的测算。主舱19刻度区舱壁透明,便于跟踪测试舱5内试样的腐蚀降解过程。As shown in Fig. 5, the test chamber 5 is composed of an inlet duct 9, a flared progressive expansion tank 18, a cylindrical main compartment 19, a hatch cover 20 and an exit duct 10, wherein the inlet duct 9 and the main compartment 19 are respectively located at both ends of the progressive expansion tank 18 and the three have a central axis. The main compartment 19 has an inner diameter of 70 mm and a length of 490 mm. The outlet duct 10 is located on the side of the main compartment 19 and 28 mm from the end face of the main hatch. The hatch cover 20 is threadedly connected to the main hatch to facilitate frequent loading and unloading of the sample. Wherein the main hatch is externally threaded, the hatch cover 20 is covered with an internal thread matching the external thread of the main hatch, and the hatch cover 20 is covered with a lining gasket to ensure the air between the hatch cover 20 and the test chamber 5. The tightness requirement is to prevent series of problems such as fluid leakage and liquid level fluctuation caused by air leakage. The inlet pipe 9 and the outlet pipe 10 are hollow bamboo pipes of uniform inner diameter, which facilitate the fastening connection of the external hose to the test chamber 5 and ensure the airtightness of the joint. The inlet tube 9 has an inner diameter of 7.0 mm and the outlet tube 10 has an inner diameter of 15.4 mm. The inner diameter ratio of the inlet tube 9 and the outlet tube 10 ensures that the test medium enters and exits the test chamber 5 at different flow rates. Balance to maintain the stability of the liquid level. The progressive expansion tank 18 and the main cabin 19 are hollow structures, and the inlet duct 9 and the flare bay 18 cabin, the outlet duct 10 and the main cabin 19 cabin are directly in communication. A circular porous flow plate 23 is provided between the main chamber 19 and the flared tank 18, and has an inner diameter of 33 mm. The special structural design of the test chamber ensures that the flow of the test medium in the test chamber is smooth and controllable. The outer wall of the main compartment 19 is marked with a height scale and a cylinder inner diameter to facilitate the adjustment of the liquid level and the sample installation position and the measurement of the medium flow rate. The main compartment 19 scale area bulkhead is transparent, which is convenient for tracking the corrosion degradation process of the sample in the test chamber 5.
如图6所示,舱顶盖20几何中心设有带内螺纹的孔径为6.3mm的圆形装样孔21。在装样孔21周围设有圆形测试孔22,装样孔21和测试孔22均为通孔,且测试孔22带匹配的密封塞。装样孔21的存在以及上位载样器6的配套极大地方便了试样的安装、固定。测试孔22的设计,为测试舱5内介质温度、pH值和组分等理化参数的实时检/监测提供了方便。As shown in Fig. 6, the geometric center of the hatch cover 20 is provided with a circular loading hole 21 having an internal diameter of 6.3 mm. A circular test hole 22 is provided around the sample loading hole 21, and both the sample hole 21 and the test hole 22 are through holes, and the test hole 22 has a matching sealing plug. The presence of the sample loading hole 21 and the matching of the upper sample holder 6 greatly facilitate the mounting and fixing of the sample. The design of the test hole 22 provides convenience for real-time inspection/monitoring of physical and chemical parameters such as medium temperature, pH value and composition in the test chamber 5.
如图7、图8所示,上位载样器6由一个定位轴24、三个载样头25以及三个衔接桥26组成,其中衔接桥26的一端与定位轴24的下端相连,另一端与载样头25的上端相连,定位轴24的上端和载样头25的下端均为自由端,载样头25与衔接桥26之间为一一对应关系。定位轴24与载样头25均为圆柱体。载样头25的轴线与定位轴24的轴线相互平行。衔接桥26均为尺寸相同的直杆,且衔接桥26以定位轴24的轴线为基准线在空间上均匀分布。上位载样器6一拖三或以上的上述结构设计,可实现对多个样品的一次性装载及后续研究测试,达到通过一次试验获取多组数据的目的,在大幅降低工作量、显著提高研发效率的同时,确保试样/介质相对运动参数的可控性以及测试条件的平行性。载样头25直径为2.8mm,且其自由端均设有用于安装试样的外螺纹,载样头与试样样品间的螺纹连接设计,可确保试样的装载牢固、可靠,同时可对试样的位姿进行控制。定位轴24之自由端为与舱顶盖20几何中心圆形装样孔21匹配的螺杆,可带紧固和密封用螺母。上位载样器6的发明和应用,实现了对试验样品以硬质材料从其上端进行装载,解决了传统“悬吊式”载样法遇到的难题。As shown in FIG. 7 and FIG. 8, the upper loader 6 is composed of a positioning shaft 24, three loading heads 25 and three connecting bridges 26, wherein one end of the connecting bridge 26 is connected to the lower end of the positioning shaft 24, and the other end is connected. Connected to the upper end of the loading head 25, the upper end of the positioning shaft 24 and the lower end of the loading head 25 are free ends, and the loading head 25 and the connecting bridge 26 have a one-to-one correspondence. The positioning shaft 24 and the loading head 25 are both cylindrical. The axis of the loading head 25 is parallel to the axis of the positioning shaft 24. The connecting bridges 26 are straight rods of the same size, and the connecting bridges 26 are spatially evenly distributed with the axis of the positioning shaft 24 as a reference line. The above-mentioned structural design of the upper sample loading device 6 can be used for one-time loading and subsequent research and testing of multiple samples, and achieves the purpose of obtaining multiple sets of data through one test, thereby greatly reducing the workload and significantly improving the research and development. At the same time of efficiency, the controllability of the relative motion parameters of the sample/medium and the parallelism of the test conditions are ensured. The loading head 25 has a diameter of 2.8 mm, and the free end thereof is provided with an external thread for mounting the sample. The threaded connection between the loading sample and the sample sample ensures that the loading of the sample is firm and reliable, and at the same time The pose of the sample is controlled. The free end of the positioning shaft 24 is a screw that mates with the geometric center circular loading hole 21 of the roof cap 20, and can be provided with a fastening and sealing nut. The invention and application of the upper loader 6 realizes loading the test sample with the hard material from the upper end thereof, and solves the problem encountered by the traditional "suspended" sample loading method.
实施例Example
下面以利用本发明进行医用镁合金生物降解性能的动态模拟测试为例,详细介绍本发明的用法:将预先配置好的测试介质如Hank’s模拟体液等通过储液罐2罐顶的补给口12注入储液罐2;打开恒温槽1的电源开关,预设温度,加热测试介质并对其进行恒温;将加工有与载样头25匹配的装样孔的试样进行金相打磨、清洗、干燥、微弧/阳极氧化、仿生钝化等前处理,之后将其旋入上位载样器6的载样头25;载样头25朝下,将上位载样器6之定位轴24旋入测试舱5之舱顶盖20几何中心的装样孔21;将舱顶盖20与测试舱5之主舱口进行旋接;打开循环泵3,通过流量计4调整介质流量/流速至介质以预设流速在管路系统稳定循环;特定时段后关闭循环泵3,旋下舱顶盖20,卸下上位载样器6,取下载样头25上的试样;之后按照公知的方法进行后续操作如清洗、干燥、称重以及表面/截面分析测试等,即可获得材料腐蚀降解丰富而全面的信息,如质量变化、降解产物相组成、元素组成及微观形貌等。In the following, the dynamic simulation test of the biodegradation performance of the medical magnesium alloy by the present invention is taken as an example, and the usage of the present invention is described in detail: a pre-configured test medium such as Hank's simulated body fluid is injected through the supply port 12 of the tank top of the liquid storage tank 2 The liquid storage tank 2; the power switch of the constant temperature tank 1 is turned on, the temperature is preset, the test medium is heated and the temperature is constant; the sample processed with the sample loading hole matched with the sample loading head 25 is subjected to metallographic grinding, washing and drying. Pre-treatment such as micro-arc/anodizing, bionic passivation, etc., and then screwing it into the loading head 25 of the upper-loading sampler 6; the loading head 25 is facing downward, and the positioning shaft 24 of the upper-loading sampler 6 is screwed into the test. The loading hole 21 of the geometric center of the hatch cover 20 of the tank 5; screwing the hatch cover 20 to the main hatch of the test chamber 5; opening the circulation pump 3, and adjusting the medium flow/flow rate to the medium by the flow meter 4 Set the flow rate to stabilize the circulation in the pipeline system; after a certain period of time, close the circulation pump 3, unscrew the top cover 20, remove the upper sample carrier 6, and take the sample on the sample 25; then follow the known method. Such as cleaning, drying, weighing and surface / Surface analysis testing, to obtain a material corrosion degradation rich and comprehensive information, such as the mass change, degradation phase composition, microstructure elements and the like.

Claims (1)

1.医用镁合金生物降解性能体外动态模拟测试设备,其特征在于包括恒温槽(1)、储液罐(2)、循环泵(3)、流量计(4)、测试舱(5)、上位载样器(6)、吸液管(7)和回流管(8),其中吸液管(7)和回流管(8)分别置于储液罐(2)中,储液罐(2)置于恒温槽(1)中,流量计(4)和测试舱(5)分别竖直固定,上位载样器(6)经测试舱(5)之舱顶盖(20)悬挂于测试舱(5)内;吸液管(7)位于储液罐(2)罐外的管口与循环泵(3)之入口间、循环泵(3)之出口与流量计(4)之入口间、流量计(4)之出口与测试舱(5)之进舱管(9)间、测试舱(5)之出舱管(10)与回流管(8)位于储液罐(2)罐外的管口间分别通过水管相连,构成液态介质循环通路。1. In vitro dynamic simulation test equipment for biodegradation of medical magnesium alloy, characterized by including thermostatic bath (1), liquid storage tank (2), circulation pump (3), flow meter (4), test chamber (5), upper load sample (6), a pipette (7) and a return pipe (8), wherein the pipette (7) and the return pipe (8) are respectively placed in the liquid storage tank (2), and the liquid storage tank (2) is placed In the constant temperature tank (1), the flow meter (4) and the test chamber (5) are vertically fixed respectively, and the upper sample holder (6) is suspended from the test chamber (5) via the hatch cover (20) of the test chamber (5). Inside; the pipette (7) is located between the nozzle outside the tank (2) and the inlet of the circulation pump (3), the outlet of the circulation pump (3) and the inlet of the flow meter (4), the flow meter ( 4) Between the inlet and test tubes of the test chamber (5), the outlet tube (10) and the return tube (8) of the test chamber (5) are located between the nozzles outside the tank (2) They are connected by water pipes to form a liquid medium circulation path.
2. 根据权利要求1所述的医用镁合金生物降解性能体外动态模拟测试设备,其特征在于:所述储液罐(2)为封闭方体容器,由隔板(11)分成左、右两个独立罐体,其中右罐容积为左罐容积的2.1倍以上;储液罐(2)罐顶设有补给口(12)、带滤器的通气孔(13)、吸液口(14)和回流口(15),其中补给口(12)带匹配的密封塞,吸液口(14)位于储液罐(2)之左罐罐顶并靠近储液罐(2)之左侧面和前侧面,回流口(15)位于储液罐(2)之右罐罐顶并靠近储液罐(2)之右侧面和前侧面,吸液口(14)和回流口(15)分别是吸液管(7)和回流管(8)通过罐顶的通道,管与口之间密封连接;在隔板(11)的不同高度间隔设有溢流孔(16),溢流孔(16)靠近储液罐(2)之后侧面;储液罐(2)之左侧面和右侧面分别设有排液口(17),排液口(17)靠近储液罐(2)之罐底和后侧面;溢流孔(16)和排液口(17)内均无缝嵌套内螺纹管,内螺纹管带匹配的螺纹管塞。2. The in vitro dynamic simulation test device for biodegradability of medical magnesium alloy according to claim 1, wherein the liquid storage tank (2) is a closed rectangular container, and the partition (11) is divided into left and right independent. The tank body, wherein the right tank volume is more than 2.1 times the volume of the left tank; the tank top (2) tank top is provided with a replenishing port (12), a venting port with a filter (13), a liquid suction port (14) and a return port. (15), wherein the supply port (12) has a matching sealing plug, and the liquid suction port (14) is located at the top of the left tank of the liquid storage tank (2) and adjacent to the left side and the front side of the liquid storage tank (2). The return port (15) is located at the top of the right tank of the liquid storage tank (2) and is adjacent to the right side and the front side of the liquid storage tank (2), and the liquid suction port (14) and the return port (15) are respectively pipettes (7) and the return pipe (8) passes through the passage of the tank top, and the pipe is connected to the port; the overflow hole (16) is arranged at different heights of the partition plate (11), and the overflow hole (16) is close to the storage The rear side of the liquid tank (2); the left side and the right side of the liquid storage tank (2) are respectively provided with a liquid discharge port (17), and the liquid discharge port (17) is close to the liquid storage port (2) and a rear side bottom of the tank; the overflow opening (16) and outlet (17) are nested seamless inner thread, the thread of the threaded tube with matching pipe plug.
3. 根据权利要求1所述的医用镁合金生物降解性能体外动态模拟测试设备,其特征在于:所述测试舱(5)由进舱管(9)、喇叭状渐扩舱(18)、圆筒状主舱(19)、舱顶盖(20)和出舱管(10)五部分构成,其中进舱管(9)和主舱(19)分别位于渐扩舱(18)的两端且三者共中轴线,出舱管(10)位于主舱(19)侧面且距主舱口端面21mm以上;舱顶盖(20)与主舱口通过螺纹连接,其中主舱口带外螺纹,舱顶盖(20)盖周带与主舱口外螺纹匹配的内螺纹,盖顶内衬密封垫圈;舱顶盖(20)几何中心设有带内螺纹的用于对上位载样器(6)进行定位的圆形装样孔(21),在装样孔(21)周围设有圆形测试孔(22),装样孔(21)和测试孔(22)均为通孔,且测试孔(22)带匹配的密封塞;进舱管(9)和出舱管(10)均为内径均匀的中空竹节管,且出舱管(10)内径为进舱管(9)内径的2.1倍以上;渐扩舱(18)和主舱(19)为中空结构,且进舱管(9)与渐扩舱(18)舱室、出舱管(10)与主舱(19)舱室分别直接相通;主舱(19)与渐扩舱(18)之间设有圆形多孔稳流板(23);主舱(19)外壁分别标有高度刻度和圆筒内径,且刻度区舱壁透明。3. The in vitro dynamic simulation test apparatus for biodegradability of medical magnesium alloy according to claim 1, characterized in that the test chamber (5) is composed of an inlet duct (9), a flared progressive expansion chamber (18), and a cylindrical shape. The main compartment (19), the hatch cover (20) and the exit hatch (10) are composed of five parts, wherein the inlet duct (9) and the main cabin (19) are respectively located at two ends of the diverging tank (18) and three The central axis, the outboard tube (10) is located on the side of the main compartment (19) and is more than 21 mm from the end of the main hatch; the hatch cover (20) is threadedly connected to the main hatch, wherein the main hatch is externally threaded, the roof The cover (20) covers an inner thread matching the outer thread of the main hatch, and the top is sealed with a gasket; the geometric center of the top cover (20) is provided with an internal thread for positioning the upper loader (6) The circular loading hole (21) is provided with a circular test hole (22) around the loading hole (21), and the sampling hole (21) and the test hole (22) are both through holes and test holes (22) ) with matching sealing plug; the inlet pipe (9) and the outlet pipe (10) are hollow bamboo pipes with uniform inner diameter, and the inner diameter of the outer casing (10) It is more than 2.1 times the inner diameter of the inlet pipe (9); the progressive expansion (18) and the main compartment (19) are hollow structures, and the inlet pipe (9) and the flared (18) compartment and the outbound pipe (10) ) directly communicating with the main compartment (19); a circular porous flow plate (23) is provided between the main compartment (19) and the progressive expansion chamber (18); the outer wall of the main compartment (19) is marked with a height scale and The inner diameter of the cylinder, and the bulkhead bulkhead is transparent.
4. 根据权利要求1所述的医用镁合金生物降解性能体外动态模拟测试设备,其特征在于:所述上位载样器(6)由一个定位轴(24)、三个以上载样头(25)以及与载样头(25)相同数量的衔接桥(26)组成,其中衔接桥(26)的一端与定位轴(24)的下端相连,另一端与载样头(25)的上端相连,定位轴(24)的上端和载样头(25)的下端均为自由端,载样头(25)与衔接桥(26)之间为一一对应关系;定位轴(24)与载样头(25)均为圆柱体;载样头(25)的轴线与定位轴(24)的轴线相互平行;衔接桥(26)均为尺寸相同的直杆,且衔接桥(26)以定位轴(24)的轴线为基准线在空间上均匀分布;载样头(25)的尺寸均相同,且其自由端均设有用于安装试样的外螺纹;定位轴(24)之自由端为与舱顶盖(20)几何中心圆形装样孔(21)匹配的螺杆;上位载样器(6)载样头(25)朝下经装样孔(21)悬挂于测试舱(5)之主舱(19)内。4. The in vitro dynamic simulation test apparatus for biodegradability of medical magnesium alloy according to claim 1, wherein the upper loader (6) comprises a positioning shaft (24), three loading heads (25), and The same number of connecting bridges (26) as the loading head (25), wherein one end of the connecting bridge (26) is connected to the lower end of the positioning shaft (24), and the other end is connected to the upper end of the loading head (25), the positioning shaft The upper end of (24) and the lower end of the loading head (25) are free ends, and there is a one-to-one correspondence between the loading head (25) and the connecting bridge (26); the positioning shaft (24) and the loading head (25) Both are cylindrical; the axis of the loading head (25) is parallel to the axis of the positioning shaft (24); the connecting bridges (26) are straight rods of the same size, and the connecting bridge (26) is positioned with the axis (24) The axis of the reference line is spatially evenly distributed; the size of the loading head (25) is the same, and the free end is provided with an external thread for mounting the sample; the free end of the positioning shaft (24) is the top cover of the housing (20) Geometric center circular loading hole (21) matching screw; upper load sample (19) (6) the loaded head (25) down through the hole-like means (21) is suspended in a test chamber (5) of the main cabin.
5. 根据权利要求1所述的医用镁合金生物降解性能体外动态模拟测试设备,其特征在于:吸液管(7)和回流管(8)均为硬质水管,两者在储液罐(2)内的管口端距储液罐(2)罐底内侧面的高度为3.5-14mm。5. The in vitro dynamic simulation test device for biodegradability of medical magnesium alloy according to claim 1, wherein the pipette (7) and the return pipe (8) are both hard water pipes, and the two are in the liquid storage tank (2) The inner nozzle end is 3.5-14 mm from the inner side of the tank bottom of the liquid storage tank (2).
PCT/CN2010/076992 2010-08-27 2010-09-16 Medical magnesium alloy biodegradability in vitro dynamic simulation test device WO2012024849A1 (en)

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