CN114247893B - Application of metal powder in field of medical materials - Google Patents

Application of metal powder in field of medical materials Download PDF

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Publication number
CN114247893B
CN114247893B CN202210169867.4A CN202210169867A CN114247893B CN 114247893 B CN114247893 B CN 114247893B CN 202210169867 A CN202210169867 A CN 202210169867A CN 114247893 B CN114247893 B CN 114247893B
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powder
metal
spraying
metal powder
field
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CN114247893A (en
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王荣浩
程波
宰红艳
余文静
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Affiliated Hospital of Southwest Medical University
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Affiliated Hospital of Southwest Medical University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02—Inorganic materials
    • A61L27/04—Metals or alloys
    • A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/28—Materials for coating prostheses
    • A61L27/30—Inorganic materials
    • A61L27/306—Other specific inorganic materials not covered by A61L27/303 - A61L27/32
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C16/00—Alloys based on zirconium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/06—Metallic material
    • C23C4/08—Metallic material containing only metal elements
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/134—Plasma spraying

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Plasma & Fusion (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Dermatology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Transplantation (AREA)
  • Epidemiology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention relates to a method for producing metal powder and the use thereof. In order to improve the corrosion resistance of the medical magnesium alloy material, the ZrTiFeAlY composite coating is formed on the surface of the medical magnesium alloy material by a thermal spraying process. Researches show that the ZrTiFeAlY composite coating can obviously improve the corrosion resistance of the medical magnesium alloy, wherein the rare earth element Y is beneficial to improving the biocompatibility of the composite material, but the corrosion resistance of the composite material is reduced due to excessive rare earth elements. In addition, compared with the traditional method of directly mixing metal element powder for thermal spraying, the thermal spraying powder raw material prepared by the atomization powder preparation method is more favorable for improving the comprehensive performance of the composite coating.

Description

Application of metal powder in field of medical materials
Technical Field
The invention relates to the field of metal powder manufacturing, in particular to a manufacturing method and application of metal powder.
Background
Currently, metal implant materials widely used in clinical applications include stainless steel, cobalt-chromium alloys, titanium alloys, and magnesium alloys. The magnesium alloy has good mechanical compatibility, high specific strength and specific stiffness, the density is close to that of natural bones, the elastic modulus is 41-45GPa and is more close to that of human bones, the stress shielding effect can be effectively relieved, the growth and healing of the bones are promoted, and the occurrence of secondary fracture is prevented.
However, the standard electrode potential of magnesium is very low, is susceptible to corrosion, and has a P-B value of 0.8, and does not allow the formation of an effective protective oxide film, particularly Cl in body fluids-Can accelerate the corrosion of the magnesium alloy, has serious corrosion before the body is not healed due to higher degradation rate, and reduces the corrosion of the implanted materialThe mechanical property and stability of the material can cause the material to lose efficacy. In view of the above, how to improve the corrosion resistance of the medical magnesium alloy is a problem to be solved urgently.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a manufacturing method of metal powder, and the metal powder is sprayed on the surface of the medical magnesium alloy through a thermal spraying process so as to improve the corrosion resistance of the medical magnesium alloy.
A method of manufacturing a metal powder, comprising the steps of:
accurately weighing zirconium powder, titanium powder, iron powder, aluminum powder and yttrium powder according to the weight ratio, putting the weighed materials into a smelting furnace, and smelting at 1900-2000 ℃;
introducing the obtained metal melt into a preheated tundish;
enabling the metal melt to flow out of a nozzle of a tundish, and obtaining a metal powder material by an atomization powder making method under the protection of high-pressure inert gas;
the powder material with a particle size of 50 to 150 μm is obtained by sieving.
Preferably, the weight ratio of the zirconium powder, the titanium powder, the iron powder, the aluminum powder and the yttrium powder is 60: 10: 5-20.
Furthermore, the invention also provides application of the metal powder, wherein the metal powder is prepared by the preparation method, and the ZrTiFeAlY composite coating is formed by spraying the metal powder on the surface of the medical material by adopting a thermal spraying process.
Preferably, the medical material is medical magnesium alloy.
Preferably, the thermal spray process is plasma spray.
Preferably, the plasma spraying process conditions are as follows: the spraying voltage is 60-80V, the spraying current is 350-400A, the spraying distance is 50-60mm, and the powder feeding speed is 30-35 r/min.
Preferably, the plasma spraying process conditions are as follows: the spraying voltage is 80V, the spraying current is 400A, the spraying distance is 50mm, and the powder feeding speed is 30 r/min.
In order to improve the corrosion resistance of the medical magnesium alloy material, the ZrTiFeAlY composite coating is formed on the surface of the medical magnesium alloy material by a thermal spraying process. Researches show that the ZrTiFeAlY composite coating can obviously improve the corrosion resistance of the medical magnesium alloy, wherein the rare earth element Y is beneficial to improving the biocompatibility of the composite material, but the corrosion resistance of the composite material is reduced due to excessive rare earth elements. In addition, compared with the traditional method of directly mixing metal element powder for thermal spraying, the thermal spraying powder raw material prepared by the atomization powder preparation method is more favorable for improving the comprehensive performance of the composite coating.
Detailed Description
The technical effects of the present invention are demonstrated below by specific examples, but the embodiments of the present invention are not limited thereto.
Example 1
Accurately weighing zirconium powder, titanium powder, iron powder, aluminum powder and yttrium powder according to the weight ratio of 60: 10: 5, putting the weighed materials into a smelting furnace, and smelting at 1900 ℃; introducing the obtained metal melt into a preheated tundish; enabling the metal melt to flow out of a nozzle of a tundish, and obtaining a metal powder material by an atomization powder making method under the protection of high-pressure inert gas; finally, the powder material with the particle size of 50-150 μm is obtained by sieving.
Example 2
Accurately weighing zirconium powder, titanium powder, iron powder, aluminum powder and yttrium powder according to the weight ratio of 60: 10: 8, putting the weighed materials into a smelting furnace, and smelting at 1900 ℃; introducing the obtained metal melt into a preheated tundish; enabling the metal melt to flow out of a nozzle of a tundish, and obtaining a metal powder material by an atomization powder making method under the protection of high-pressure inert gas; finally, the powder material with the particle size of 50-150 μm is obtained by sieving.
Example 3
Accurately weighing zirconium powder, titanium powder, iron powder, aluminum powder and yttrium powder according to the weight ratio of 60: 10, putting into a smelting furnace, and smelting at 1900 ℃; introducing the obtained metal melt into a preheated tundish; enabling the metal melt to flow out of a nozzle of a tundish, and obtaining a metal powder material by an atomization powder making method under the protection of high-pressure inert gas; finally, the powder material with the particle size of 50-150 μm is obtained by sieving.
Example 4
Accurately weighing zirconium powder, titanium powder, iron powder, aluminum powder and yttrium powder according to the weight ratio of 60: 10: 13, putting the weighed materials into a smelting furnace, and smelting at 1900 ℃; introducing the obtained metal melt into a preheated tundish; enabling the metal melt to flow out of a nozzle of a tundish, and obtaining a metal powder material by an atomization powder making method under the protection of high-pressure inert gas; finally, the powder material with the particle size of 50-150 μm is obtained by sieving.
Example 5
Accurately weighing zirconium powder, titanium powder, iron powder, aluminum powder and yttrium powder according to the weight ratio of 60: 10: 16, putting the weighed materials into a smelting furnace, and smelting at 1900 ℃; introducing the obtained metal melt into a preheated tundish; enabling the metal melt to flow out of a nozzle of a tundish, and obtaining a metal powder material by an atomization powder making method under the protection of high-pressure inert gas; finally, the powder material with the particle size of 50-150 μm is obtained by sieving.
Example 6
Accurately weighing zirconium powder, titanium powder, iron powder, aluminum powder and yttrium powder according to the weight ratio of 60: 10: 20, putting into a smelting furnace, and smelting at 1900 ℃; introducing the obtained metal melt into a preheated tundish; enabling the metal melt to flow out of a nozzle of a tundish, and obtaining a metal powder material by an atomization powder making method under the protection of high-pressure inert gas; finally, the powder material with the particle size of 50-150 μm is obtained by sieving.
Comparative example 1
Accurately weighing zirconium powder, titanium powder, iron powder, aluminum powder and yttrium powder according to the weight ratio of 60: 10: 13, putting the weighed materials into a smelting furnace, and smelting at 1900 ℃; introducing the obtained metal melt into a preheated tundish; and (3) enabling the molten metal to flow out from a nozzle of the tundish, and obtaining the metal powder material by an atomization powder making method under the protection of high-pressure inert gas.
Comparative example 2
Accurately weighing zirconium powder, titanium powder, iron powder and aluminum powder according to the weight ratio of 60: 10, putting into a smelting furnace, and smelting at 1900 ℃; introducing the obtained metal melt into a preheated tundish; enabling the metal melt to flow out of a nozzle of a tundish, and obtaining a metal powder material by an atomization powder making method under the protection of high-pressure inert gas; finally, the powder material with the particle size of 50-150 μm is obtained by sieving.
Comparative example 3
Accurately weighing zirconium powder, titanium powder, iron powder, aluminum powder and yttrium powder according to the weight ratio of 60: 10: 30, putting the weighed materials into a smelting furnace, and smelting at 1900 ℃; introducing the obtained metal melt into a preheated tundish; enabling the metal melt to flow out of a nozzle of a tundish, and obtaining a metal powder material by an atomization powder making method under the protection of high-pressure inert gas; finally, the powder material with the particle size of 50-150 μm is obtained by sieving.
Next, the metal powder materials in examples 1 to 6 and comparative examples 1 to 3 were sprayed on the surface of the medical magnesium alloy by a plasma spraying process to form a composite coating, and the specific method was: the method comprises the steps of putting a medical magnesium alloy substrate into plasma spraying equipment, preheating the equipment after a power supply is turned on, starting spraying after preheating is finished, wherein the spraying voltage is 80V, the spraying current is 400A, the spraying distance is 50mm, the powder feeding rate is 30r/min, and forming a ZrTiFeAlY composite coating on the surface of the medical magnesium alloy after plasma spraying is finished.
The corrosion resistance and biocompatibility of each of the above samples were evaluated as follows.
The hemocompatibility of each sample was evaluated by a hemolysis test, which is based on the following principle: the sample is directly contacted with blood, and the amount of hemoglobin released after rupture of erythrocyte membrane is measured to detect the degree of hemolysis in vitro of each sample. The absorption wavelength of hemoglobin is 545nm, and its concentration can be detected by a spectrophotometer. The specific operation steps are as follows:
(1) blood is collected from the heart of a healthy rabbit by 100mL, and 2% potassium oxalate by 5mL is added to prepare fresh anticoagulation blood. And taking 40mL of anticoagulation blood, and adding 50mL of 0.9% sodium chloride injection for dilution.
(2) Taking 3 silicified test tubes, loading a test sample and 10mL of sodium chloride injection into one test tube, taking a blank of one test tube as a negative control group, adding 10mL of sodium chloride normal saline, and taking a blank of the other test tube as a positive control group, and respectively adding 10mL of distilled water.
(3) All the test tubes are kept constant in a water bath at 37 ℃ for 30min, 5mL of anticoagulated rabbit blood is added respectively, and the temperature is kept at 37 ℃ for 60 min.
(4) The supernatant of the test tube was taken and the absorbance was measured at 545 nm. Three replicates of each sample were run and averaged.
The hemolysis rate is calculated as follows:
hemolysis ratio (%) = (sample average absorbance-absorbance in negative group)/(absorbance in positive group-absorbance in negative group) × 100
The corrosion resistance of each sample was evaluated by measuring the self-corrosion current density in Simulated Body Fluid (SBF), and five parallel tests were performed for each set of experiments, and the average value was taken.
The experimental results of the samples are shown in table 1, and the medical magnesium alloy without any treatment is used as a blank control group.
TABLE 1 self-etching Current Density and hemolysis ratio of each sample
Numbering Percent of hemolysis% Self-corrosion current density mA/cm2
Example 1 4.5 0.0127
Example 2 3.3 0.0204
Example 3 3.9 0.0215
Example 4 2.5 0.0217
Example 5 1.0 0.0315
Example 6 1.4 0.0526
Comparative example 1 3.1 0.0656
Comparative example 2 7.7 0.0263
Comparative example 3 1.9 0.1760
Blank control group 4.7 0.3290
As can be seen from Table 1, the incorporation of a suitable amount of yttrium, a rare earth element, into the composite coating is beneficial to improve the biocompatibility, but excessive amounts of yttrium (as in comparative example 3) can lead to a reduction in the corrosion resistance of the composite coating. And the screening process of the metal alloy powder is beneficial to improving the comprehensive performance of the composite coating.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.

Claims (5)

1. The application of the metal powder in the field of medical materials is characterized in that a thermal spraying process is selected to spray the metal powder on the surface of the medical materials to form a ZrTiFeAlY composite coating, wherein the manufacturing method of the metal powder comprises the following steps:
accurately weighing zirconium powder, titanium powder, iron powder, aluminum powder and yttrium powder according to the weight ratio, putting the weighed materials into a smelting furnace, and smelting at the temperature of 1900-2000 ℃, wherein the weight ratio of the zirconium powder to the titanium powder to the iron powder to the aluminum powder to the yttrium powder is 60: 10: 5-20;
introducing the obtained metal melt into a preheated tundish;
enabling the metal melt to flow out of a nozzle of a tundish, and obtaining a metal powder material by an atomization powder making method under the protection of high-pressure inert gas;
the powder material with a particle size of 50 to 150 μm is obtained by sieving.
2. Use of the metal powder according to claim 1 in the field of medical materials, wherein the medical material is a medical magnesium alloy.
3. Use of the metal powder according to claim 1 in the field of medical materials, wherein the thermal spraying process is plasma spraying.
4. The use of the metal powder according to claim 3 in the field of medical materials, wherein the plasma spraying process conditions are as follows: the spraying voltage is 60-80V, the spraying current is 350-400A, the spraying distance is 50-60mm, and the powder feeding speed is 30-35 r/min.
5. The use of the metal powder according to claim 4 in the field of medical materials, wherein the plasma spraying process conditions are as follows: the spraying voltage is 80V, the spraying current is 400A, the spraying distance is 50mm, and the powder feeding speed is 30 r/min.
CN202210169867.4A 2022-02-24 2022-02-24 Application of metal powder in field of medical materials Expired - Fee Related CN114247893B (en)

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