CN111270240B - Two-step polishing method of magnesium alloy intravascular stent and polishing solution thereof - Google Patents
Two-step polishing method of magnesium alloy intravascular stent and polishing solution thereof Download PDFInfo
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- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
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- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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Abstract
The invention provides a two-step polishing method of a magnesium alloy intravascular stent, which comprises the following steps: putting the magnesium alloy stent into a mixed solution of ethanol, acetone and petroleum ether for ultrasonic degreasing and oil removal; placing the degreased blood vessel stent into pickling solution for pickling treatment; thirdly, performing multiple times of electrochemical polishing treatment by adopting electrochemical polishing liquid; fourthly, chemical polishing treatment is carried out by adopting chemical polishing solution; and fifthly, drying after cleaning, and placing in a centrifuge tube for sealing and storing by a vacuum bag. The invention also provides the electrochemical polishing solution and the chemical polishing solution used. The invention has the following technical effects: 1. the polishing solution does not contain toxic chromic anhydride and has little pollution to the environment. 2. The process is simple, no complex pretreatment is needed, the electrochemical polishing process is mild, and various parameters are easy to control. 3. The polished bracket has smooth and bright inner and outer surfaces and uniform size.
Description
Technical Field
The invention relates to a two-step polishing method of a magnesium alloy intravascular stent and polishing solution thereof. The two-step polishing method provided by the invention is to perform electrochemical polishing on the blood vessel stent after acid cleaning and then perform chemical polishing. The invention aims to solve the problem that the inner surface and the outer surface of a magnesium alloy bracket are difficult to be polished in a mirror surface mode.
Background
The magnesium alloy is a high-performance light structural material taking magnesium as a raw material, and has the advantages of small density, high strength, good rigidity and good machinability. Most importantly, the magnesium alloy has good biocompatibility and is degradable in a human body, so that the magnesium alloy is an ideal blood vessel stent material and becomes a research hotspot of the stent material.
Burrs exist in the vascular stent after the magnesium alloy thin-wall microtubule is cut by laser, and if the vascular stent is directly implanted into a human body without treatment, platelet adhesion is caused, so that thrombus and intimal hyperplasia are formed. Therefore, a polishing process is required for the surface of the stent. Magnesium metal has strong activity, the reaction speed is difficult to control in the polishing process, the flatness and the brightness are poor, and the mirror polishing effect is difficult to achieve. The magnesium alloy polishing solution in the prior art mainly refers to electrochemical polishing solutions of other metals, and has the problems of poor polishing quality, serious pitting corrosion and the like. Among them, there is a technique related to an electrochemically polished portion in preparation of a magnesium alloy Electron Back Scattering Diffraction (EBSD) sample. However, the EBSD sample has low requirements on the overall polishing effect, only a small flat and smooth part on the sample needs to be found, and the polishing of the heart stent needs to achieve the overall flatness and smoothness. Therefore, the conventional method mainly refers to industrial magnesium alloy electrochemical polishing solution, but the polishing quality requirement of industrial products is far lower than that of vascular stents, and the conventional method cannot be used for polishing magnesium alloy stents.
At present, the polishing technology related to the magnesium alloy stent mainly comprises the following steps:
for example, chromic anhydride with high toxicity exists in the components of the polishing solution disclosed in the invention patent (patent application No. 201510127404.1) named as 'treatment solution and treatment method of magnesium alloy stent' and the invention patent (patent application No. 200810020030.3) named as 'processing and preparation method of biodegradable magnesium alloy vascular stent body', and the polishing solution is easy to pollute the environment.
For example, in the polishing process disclosed in the invention patent (patent application No. 201510503835.3) entitled "electrolytic polishing solution for magnesium alloy medical cardiac stents and surface polishing process thereof", the stent is firstly ground and polished by sand paper and then ground and polished by diamond polishing paste, and the process is complicated. In addition, the heart stent is very small, so that the polishing difficulty is high on the basis, and the stent is easy to deform and scrap. Also, the polishing process disclosed in the invention patent (patent application No. 201810076786.3) entitled "surface polishing Process and Assist mechanism for magnesium alloy intravascular stents" also mechanically polishes the stent.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a magnesium alloy intravascular stent polishing method and polishing solution thereof. The invention integrates the leveling effect of electrochemical polishing and the brightening effect of chemical polishing, so that the magnesium alloy polishing is easy to control and has good surface quality.
The technical scheme of the invention is as follows:
a two-step polishing method of a magnesium alloy intravascular stent comprises the following steps:
putting the magnesium alloy stent into a mixed solution of ethanol, acetone and petroleum ether for ultrasonic degreasing and oil removal;
placing the degreased blood vessel stent into pickling solution for pickling treatment;
thirdly, performing multiple times of electrochemical polishing treatment by adopting electrochemical polishing liquid;
fourthly, chemical polishing treatment is carried out by adopting chemical polishing solution;
and fifthly, drying after cleaning, and placing in a centrifuge tube for sealing and storing by a vacuum bag.
Preferably, the first and second electrodes are formed of a metal,
the volume ratio of the ethanol, the acetone and the petroleum ether in the step (i) is 1-5: 1-5.
The pickling solution in the step (II) comprises the following components: 50-200 ml/L of nitric acid, 50-200 g/L of ammonium bifluoride and the balance of deionized water.
The electrochemical polishing conditions in the third step are as follows: the temperature is-5-15 ℃, the voltage is 12-20V, the time is 80-120 s/time, and the clamping part is changed and turned upside down each time.
In the step IV, the chemical polishing temperature is 0-15 ℃ and the time is 40-60 s.
An electrochemical polishing solution for a magnesium alloy intravascular stent comprises the following components: 100-300 ml/L of inorganic acid, 100-300 ml/L of organic acid, 0-20 g/L of urea and polyhydric alcohol as a solvent.
The inorganic acid is one or two of nitric acid and phosphoric acid, the organic acid is one or two of acetic acid and lactic acid, and the polyalcohol is one or more of ethanol, ethylene glycol and glycerol.
A chemical polishing solution for a magnesium alloy intravascular stent comprises the following components: 5-100 ml/L of inorganic acid and polyhydric alcohol as a solvent.
The inorganic acid is one or two of nitric acid and sulfuric acid, and the polyalcohol is one or more of ethanol, ethylene glycol and glycerol.
The magnesium alloy intravascular stent material is Mg-Zn series, Mg-Mn series, Mg-Al series or Mg-RE series.
More preferably still, the first and second liquid crystal compositions are,
in the step I, the volume ratio of the acetone to the ethanol to the petroleum ether is 1: 1-2: 1-3.
In the step (II), the pickling solution comprises the following components: 100-150 ml/L of nitric acid, 50-100 g/L of ammonium bifluoride and the balance of deionized water.
In the third step, the electrochemical polishing conditions are as follows: the temperature is 0-10 ℃, the voltage is 12-20V, the time is 80-120 s/time, and the clamping part is changed and turned upside down each time.
In the step IV, the chemical polishing temperature is 0-10 ℃ and the time is 40-60 s.
In the electrochemical polishing solution, the content of inorganic acid is 220-260 ml/L, the content of organic acid is 200-300 ml/L, and the content of urea is 8-16 g/L.
The chemical polishing solution contains 50-80 ml/L of inorganic acid.
The technical concept of the invention breaks through the conventional technical means. Conventionally, metal is polished better than chemical polishing, so the conventional experience is to perform chemical rough polishing and then electrochemical fine polishing. If the chemical polishing is performed after the electrochemical polishing, the polishing effect is rather deteriorated. However, the conventional technical means cannot solve the problem due to the strong activity of magnesium. Therefore, the invention provides a polishing solution composition and a corresponding polishing method, namely phosphoric acid-acetic acid electrochemical polishing is firstly carried out to level the surface, and then chemical polishing is carried out to improve the surface brightness.
The invention also has the following technical effects:
1. the polishing solution does not contain toxic chromic anhydride and has little pollution to the environment.
2. The process is simple, no complex pretreatment is needed, the electrochemical polishing process is mild, and various parameters are easy to control.
3. The polished bracket has smooth and bright inner and outer surfaces and uniform size.
Drawings
FIG. 1 is a process flow diagram of the polishing method of the magnesium alloy stent of the present invention.
FIG. 2 is a photomicrograph of the surface of the stent obtained in example 1 of the present invention.
FIG. 3 is a photomicrograph of the surface of the stent obtained in example 2 of the present invention.
FIG. 4 is a photomicrograph of the surface of a stent obtained in example 3 of the present invention.
Detailed Description
In examples 1, 2 and 3, the self-made magnesium alloy intravascular stent is formed by cutting a metal alloy tube by laser, wherein the tube material is respectively made of commercially available Mg-Zn series, Mg-Mn series and Mg-RE series materials, and the grades are as follows: ZK60, AM50, WE 43. The specific processing mode references are as follows:
in Guxing, a key technical research on design and manufacture of a novel functionalized drug-eluting intravascular stent [ D ]. Jiangsu, university of southeast, 2008.
Example 1
In this embodiment, the two-step polishing method for the magnesium alloy stent includes the following steps:
preparing electrochemical polishing solution: 100ml of phosphoric acid, 10ml of nitric acid, 125ml of acetic acid and 5g of urea are added into a beaker, absolute ethyl alcohol is added to a constant volume of 500ml, and the mixture is stirred uniformly.
Preparing a chemical polishing solution: adding 30ml of nitric acid and 30ml of glycerol into the beaker, and adding absolute ethyl alcohol until the volume is up to 500ml, and uniformly stirring.
Performing degreasing and oil removal: putting the magnesium alloy intravascular stent into a mixed solution of acetone, ethanol and petroleum ether (the volume ratio is 1: 1) for ultrasonic cleaning.
Fourth, pickling treatment: and (3) placing the intravascular stent obtained from the step three into a pickling solution for ultrasonic pickling, wherein the pickling solution comprises 150ml/L nitric acid, 50g/L ammonium bifluoride and the balance of deionized water.
Fifthly, electrochemical polishing: and (3) taking the acid-washed intravascular stent as an anode, putting the intravascular stent into electrochemical polishing solution for electrochemical polishing, wherein the process parameters are 5 ℃, 16.0V of voltage and 90s of time, and polishing for 4 times in total, wherein the stent needs to be rotated by 90 degrees in the same direction after each polishing, and the stent is turned upside down to ensure uniform polishing.
Sixthly, chemically polishing: putting the electrochemical polishing solution into the chemical polishing solution for polishing for 60s at 0 ℃;
saving-in-place: and cleaning with absolute ethyl alcohol, drying, and sealing and storing in a centrifuge tube with a vacuum bag.
Example 2
In this embodiment, the two-step polishing method for the magnesium alloy stent includes the following steps:
preparing electrochemical polishing solution: 130ml of phosphoric acid, 50ml of acetic acid, 50ml of lactic acid and 8g of urea are added into a beaker, absolute ethyl alcohol is added to the volume of 500ml, and the mixture is stirred uniformly.
Preparing a chemical polishing solution: adding 15ml of nitric acid, 10ml of sulfuric acid, 100ml of ethylene glycol and absolute ethyl alcohol into the beaker, fixing the volume to 500ml, and uniformly stirring.
Performing degreasing and oil removal: putting the magnesium alloy intravascular stent into a mixed solution of acetone, ethanol and petroleum ether (the volume ratio is 1: 2) for ultrasonic cleaning.
Fourth, pickling treatment: and (3) placing the intravascular stent obtained from the step three into a pickling solution for ultrasonic pickling, wherein the pickling solution comprises 100ml/L of nitric acid, 80g/L of ammonium bifluoride and the balance of deionized water.
Fifthly, electrochemical polishing: and (3) taking the acid-washed intravascular stent as an anode, putting the intravascular stent into electrochemical polishing solution for electrochemical polishing, wherein the process parameters are 0 ℃, 12.0V of voltage and 120s of time, and polishing for 4 times in total, wherein the stent needs to be rotated by 90 degrees in the same direction after each polishing, and the stent needs to be turned upside down to ensure uniform polishing.
Sixthly, chemically polishing: putting the electrochemical polishing solution into the chemical polishing solution for polishing for 40s at 5 ℃;
saving-in-place: and cleaning with absolute ethyl alcohol, drying, and sealing and storing in a centrifuge tube with a vacuum bag.
Example 3
In this embodiment, the two-step polishing method for the magnesium alloy stent includes the following steps:
preparing electrochemical polishing solution: adding 80ml of phosphoric acid, 50ml of nitric acid, 150ml of acetic acid, 100ml of ethylene glycol, 10ml of glycerol, 4g of urea and absolute ethyl alcohol into a beaker to reach the constant volume of 500ml, and uniformly stirring.
Preparing a chemical polishing solution: adding 30ml of nitric acid, 10ml of sulfuric acid, 15ml of glycerol, 150ml of ethylene glycol and absolute ethyl alcohol into the beaker, fixing the volume to 500ml, and uniformly stirring.
Performing degreasing and oil removal: putting the magnesium alloy intravascular stent into a mixed solution of acetone, ethanol and petroleum ether (the volume ratio is 1: 2: 3) for ultrasonic cleaning.
Fourth, pickling treatment: and (3) placing the intravascular stent obtained from the step three into a pickling solution for ultrasonic pickling, wherein the pickling solution comprises 150ml/L nitric acid, 100g/L ammonium bifluoride and the balance of deionized water.
Fifthly, electrochemical polishing: and (3) taking the acid-washed intravascular stent as an anode, putting the intravascular stent into electrochemical polishing solution for electrochemical polishing, wherein the process parameters are 10 ℃, the voltage is 20.0V, the time is 80s, the total polishing time is 4 times, and the stent needs to be rotated by 90 degrees in the same direction after each polishing, and the stent is turned upside down to ensure the uniform polishing.
Sixthly, chemically polishing: putting the electrochemical polishing solution into the chemical polishing solution for polishing for 40s at 10 ℃;
saving-in-place: and cleaning with absolute ethyl alcohol, drying, and sealing and storing in a centrifuge tube with a vacuum bag.
Example 4
And (3) size measurement:
the connecting ribs at the left, middle and right parts of the bracket are randomly selected as measuring objects, the width of the polished ribs is measured by an imager for 3 times, and the results are shown in table 1.
TABLE 1
FIGS. 2, 3 and 4 are micrographs of the stent surface obtained in examples 1, 2 and 3 of the present invention, respectively, as seen from the figure and the table: the polished bracket has the advantages of smooth and bright surface, no obvious pitting pits, round and smooth corners and uniform size.
Claims (3)
1. A two-step polishing method of a magnesium alloy intravascular stent is characterized by comprising the following steps:
putting the magnesium alloy stent into a mixed solution of ethanol, acetone and petroleum ether for ultrasonic degreasing and oil removal;
placing the degreased blood vessel stent into pickling solution for pickling treatment;
thirdly, performing multiple times of electrochemical polishing treatment by adopting electrochemical polishing liquid;
fourthly, chemical polishing treatment is carried out by adopting chemical polishing solution;
drying after cleaning, and placing in a centrifuge tube for sealing and storing by a vacuum bag;
the volume ratio of the ethanol, the acetone and the petroleum ether in the step I is 1-5: 1-5;
the electrochemical polishing solution comprises the following components: 100-300 ml/L of inorganic acid, 100-300 ml/L of organic acid, 0-20 g/L of urea and polyhydric alcohol as a solvent; the inorganic acid is phosphoric acid, or phosphoric acid and nitric acid, the organic acid is one or two of acetic acid and lactic acid, and the polyalcohol is one or more of ethanol, ethylene glycol and glycerol;
the chemical polishing solution comprises the following components: 5-100 ml/L of inorganic acid and polyhydric alcohol as a solvent; the inorganic acid is one or two of nitric acid and sulfuric acid, and the polyalcohol is one or more of ethanol, glycol and glycerol;
the electrochemical polishing conditions in the third step are as follows: the temperature is-5-15 ℃, the voltage is 12-20V, the time is 80-120 s/time, the clamping part is changed every time, and the clamping part is turned upside down;
in the step IV, the chemical polishing temperature is 0-15 ℃ and the time is 40-60 s.
2. The two-step polishing method of magnesium alloy stent as set forth in claim 1, wherein the pickling solution in the step (ii) comprises the following components: 50-200 ml/L of nitric acid, 50-200 g/L of ammonium bifluoride and the balance of deionized water.
3. The two-step polishing method for a magnesium alloy vascular stent as set forth in any one of claims 1 to 2, wherein the magnesium alloy vascular stent material is a Mg-Zn system, a Mg-Mn system, a Mg-Al system or a Mg-RE system.
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