CN113385676A - Planetary ball milling pretreatment method for titanium powder particles of vacuum sintering porous titanium coating - Google Patents

Planetary ball milling pretreatment method for titanium powder particles of vacuum sintering porous titanium coating Download PDF

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CN113385676A
CN113385676A CN202110625102.2A CN202110625102A CN113385676A CN 113385676 A CN113385676 A CN 113385676A CN 202110625102 A CN202110625102 A CN 202110625102A CN 113385676 A CN113385676 A CN 113385676A
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titanium
ball milling
coating
powder particles
planetary ball
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孙晓华
陈敏
王应静
牛永良
尹琳洁
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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
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • A61L27/06—Titanium or titanium alloys
    • 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
    • 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
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/56—Porous materials, e.g. foams or sponges
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1017—Multiple heating or additional steps
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/11—Making porous workpieces or articles
    • 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
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
    • 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
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/002—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of porous nature
    • B22F7/004—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of porous nature comprising at least one non-porous part
    • 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
    • A61L2420/00—Materials or methods for coatings medical devices
    • A61L2420/02—Methods for coating medical devices
    • 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
    • A61L2430/00—Materials or treatment for tissue regeneration
    • A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
    • 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
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

Abstract

The invention discloses a planetary ball milling pretreatment method for titanium powder particles of a vacuum sintering porous titanium coating, and relates to a planetary ball milling pretreatment method for powder particles for improving the bonding strength of a vacuum sintering titanium alloy particle coating and a matrix. Is suitable for improving the performance of implants in orthopedics, dentistry and the like. A titanium powder particle planetary ball milling pretreatment method for vacuum sintering of a porous titanium coating is characterized in that titanium hydride particles accounting for 1-3% of the mass percentage are added into titanium powder particles, the particle size of the titanium hydride particles is smaller than 150 micrometers, then stainless steel balls are selected, the ball-material ratio is 1:2, 4N high-purity argon gas is filled for protection after pre-vacuumizing, ball milling is carried out for 1-20 hours in planetary ball milling equipment with the maximum movement speed of a ball milling tank being 1.5 m/s to 9 m/s, titanium powder particles with proper particle size are screened as powder particles for coating after ball milling is finished, and then a vacuum sintering process is adopted to obtain an open type porous titanium coating on the surface of implants such as orthopedics and dentistry.

Description

Planetary ball milling pretreatment method for titanium powder particles of vacuum sintering porous titanium coating
Technical Field
The invention discloses a planetary ball milling pretreatment method for titanium powder particles of a vacuum sintering porous titanium coating, relates to a planetary ball milling pretreatment method for powder particles for improving the bonding strength of a vacuum sintering titanium alloy particle coating and a matrix, is a preparation method for an open type porous titanium coating, and belongs to the field of powder metallurgy materials and biological materials. Is suitable for improving the performance of implants in orthopaedics, dentistry and the like, in particular to improving the bonding strength of the porous titanium powder particle coating on the surface of the implant and a titanium alloy matrix.
Background
Implant coating technology has matured over the years. Taking an artificial joint as an example, the current mature process mainly comprises an air plasma spraying process, a vacuum sintering process and an electrochemical process, and the coating material mainly comprises titanium, hydroxyapatite (HA for short) and the combination of the titanium and the hydroxyapatite. The current major bio-coating technology for bio-type artificial joints, which uses vacuum sintering of titanium coating and plasma spraying of HA on the titanium coating, HAs found a number of applications in bio-type artificial joints due to its excellent bone ingrowth clinical effect and low cost, such as SUMMIT total hip prosthesis and PFC total knee prosthesis of DEPUY, NEXGEN total knee prosthesis of ZIMMER, PROFIX total knee prosthesis of SMITH-NEPHEW, and MAXIN total knee prosthesis of BIOMET.
The titanium coating is formed on the surface of the titanium alloy substrate through vacuum sintering, the bonding strength of the titanium coating and the titanium alloy substrate determines whether the workpiece can enter a subsequent process, and on the premise that the titanium coating is ensured to have proper porosity, the titanium coating and the titanium alloy substrate need to have enough connection strength, which is the premise that the safety of an implant, the bone bonding strength and the bone growth effect are guaranteed. However, the connection strength between the titanium coating prepared by the conventional sintering process and the titanium alloy substrate is often low under the condition of ensuring the porosity, so that the reliability of the coating is reduced. The powder adopted by the vacuum sintering titanium coating mainly comprises spherical titanium powder and irregular titanium powder, and the problem of low connection strength of the coating and the substrate is particularly prominent when the irregular titanium powder is adopted. Therefore, subsequent analysis and experiments mainly focus on the situation when irregular titanium powder is selected for the coating, and the invention for solving the problem is obviously also applicable to spherical titanium powder.
Disclosure of Invention
Aiming at the defects, the invention provides a planetary ball milling pretreatment method for titanium powder particles of a vacuum sintering porous titanium coating, which comprises the steps of adding titanium hydride accounting for 1-3% of the mass of the powder into the titanium powder particles, carrying out ball milling for 1-20 hours in planetary ball milling equipment with the maximum movement speed of a ball milling tank being 1.5-9 m/s, screening titanium powder particles with proper particle sizes after ball milling is finished to serve as coating powder, and then obtaining the open type porous titanium coating on the surface of implants such as orthopedics and dentistry by adopting a vacuum sintering process. The coating keeps a good space structure of a high vacuum sintering titanium coating, and greatly improves the bonding strength of the titanium coating on the surface of the implant and a titanium alloy matrix through ball milling pretreatment of adding titanium hydride, thereby improving the reliability and safety of the implant. And the process has low cost.
The planetary ball milling pretreatment method for titanium powder particles of the vacuum sintering porous titanium coating is realized by adopting the following technical scheme:
a planetary ball milling pretreatment method for titanium powder particles of a vacuum sintering porous titanium coating comprises the steps of adding 1-3% by mass of titanium hydride particles into the titanium powder particles, wherein the particle size of the titanium hydride particles is smaller than 150 micrometers, then selecting stainless steel balls with the ball-material ratio of 1:2, pre-vacuumizing, then flushing 4N high-purity argon gas for protection, carrying out ball milling for 1-20 hours in planetary ball milling equipment with the maximum motion speed of a ball milling tank of 1.5-9 m/s, and screening the titanium powder particles with proper particle size as coating powder particles for later use after finishing ball milling. And then a vacuum sintering process is adopted to obtain the open porous titanium coating on the surface of the implant of orthopedics, dentistry and the like.
The stainless steel ball is selected from stainless steel balls with the diameter of 6-10 mm.
The particle size of the pretreated titanium powder particles is 50-250 micrometers.
The vacuum sintering process of vacuum sintering porous titanium coating includes pre-treating the surface of cleaned implant, setting titanium powder grains in the required thickness of 600-1000 microns on the surface of the implant, setting titanium grains in the average thickness of 600-1000 microns on the surface of the titanium alloy implant, transferring the treated implant into a vacuum furnace, and vacuum pumping to 10 deg.c-2Heating and sintering above Pa, wherein the sintering system is as follows: heating from room temperature to 1000 ℃ and 1400 ℃ at the speed of 1-30 ℃/min, preserving the heat at the sintering temperature for 0.5-10 hours, cooling from the sintering temperature to room temperature at the speed of 1-10 ℃/min, taking out the implant with the sintered titanium bead coating, cleaning by using distilled water and medical alcohol, and packaging. After planetary ball milling pretreatment, titanium is sintered in vacuumThe bonding strength of the alloy particle coating and the matrix is effectively improved, and the bonding strength is improved from 40-55MPa without ball milling pretreatment to 60-80 MPa.
The invention has the advantages that:
the porous titanium coating is made on the surface of the implant, so that new bone tissues grow into pores of the porous titanium bead coating, and the implant and the bone tissues are fixed together. This manner of implant fixation by bone growth into porous surfaces is called biological fixation. Due to the fact that bone tissues grow into the pores, the area of the interface between the bone and the implant is greatly increased, and due to the mechanical embedding effect between the bone and the porous surface, the shearing strength of the interface between the implant and the bone is also greatly increased. However, in the process of vacuum sintering of the porous titanium coating, it is found that the connection strength between the titanium coating prepared by the conventional sintering process and the titanium alloy substrate is often low under the condition of ensuring the porosity, so that the reliability of the coating is insufficient. The powder adopted by the vacuum sintering titanium coating mainly comprises atomized spherical titanium powder and irregular titanium powder, and the problem of low connection strength of the coating and the substrate is particularly prominent when the irregular titanium powder is adopted.
Aiming at the problems, the invention adopts a powder planetary ball milling pretreatment method of a porous titanium vacuum sintering coating, titanium hydride particles accounting for 1-3% of the mass percent are added into the titanium powder particles, the granularity of the titanium hydride particles is less than 150 micrometers, then stainless steel balls with the diameter of 6-10 millimeters are selected, the ball-material ratio is 1:2, 4N high-purity argon gas is injected for protection after pre-vacuumizing, the ball milling is carried out for 1-20 hours in planetary ball milling equipment with the maximum movement speed of a ball milling tank being 1.5-9 m/s, titanium powder particles with proper granularity are screened as powder particles for the coating after the ball milling is finished, and then the vacuum sintering process is adopted to obtain the open type porous titanium coating on the surfaces of implants such as orthopedics, dentistry and the like. The coating keeps a good space structure of a high vacuum sintering titanium coating, on the other hand, the ball milling pretreatment by adding titanium hydride greatly improves the bonding strength of the titanium coating on the surface of the implant and a titanium alloy matrix, titanium hydride does not exist in a final finished product, the titanium coating and the titanium alloy matrix are completely converted into titanium and hydrogen, the hydrogen is completely decomposed and discharged in the vacuum sintering process, and the product meets all requirements of biological performance detection such as cytotoxicity test, sensitization test, intradermal reaction test, acute systemic toxicity (venous approach), genetic toxicity test (Ames) and the like.
The planetary ball milling pretreatment method for titanium powder particles of the vacuum sintering porous titanium coating effectively improves the bonding performance of the titanium alloy coating and the matrix, improves the reliability and safety of the implant, and has lower process cost.
Detailed Description
A planetary ball milling pretreatment method for titanium powder particles of a vacuum sintering porous titanium coating is adopted, titanium hydride particles accounting for 1-3% of the mass percentage are added into the titanium powder particles, the particle size of the titanium hydride particles is smaller than 150 micrometers, then stainless steel balls are selected, the ball-material ratio is 1:2, the titanium powder particles are pre-vacuumized, then 4N high-purity argon gas is injected for protection, the titanium powder particles are ball-milled for 1-20 hours in planetary ball-milling equipment with the maximum movement speed of a ball-milling tank being 1.5 m/s to 9 m/s, the titanium powder particles with proper particle size are screened as powder particles for the coating after the ball-milling is finished, and then the vacuum sintering process is adopted to obtain the open porous titanium coating on the surfaces of implants such as orthopedics and dentistry.
The stainless steel ball is selected from stainless steel balls with the diameter of 6-10 mm.
The particle size of the pretreated titanium powder particles is 50-250 micrometers.
The vacuum sintering process of vacuum sintering porous titanium coating includes pre-treating the surface of cleaned implant, setting titanium powder grains in the required thickness of 600-1000 microns on the surface of the implant, setting titanium grains in the average thickness of 600-1000 microns on the surface of the titanium alloy implant, transferring the treated implant into a vacuum furnace, and vacuum pumping to 10 deg.c-2Heating and sintering above Pa, wherein the sintering system is as follows: heating from room temperature to 1000 ℃ and 1400 ℃ at the speed of 1-30 ℃/min, preserving the heat at the sintering temperature for 0.5-10 hours, cooling from the sintering temperature to room temperature at the speed of 1-10 ℃/min, taking out the implant with the sintered titanium bead coating, cleaning by using distilled water and medical alcohol, and packaging. After planetary ball milling pretreatment, the titanium alloy is sintered in vacuumThe bonding strength of the particle coating and the matrix is effectively improved, and the bonding strength is improved from 40-55MPa without ball milling pretreatment to 60-80 MPa.
The invention will be further illustrated with reference to the following examples:
comparative example:
screening titanium powder particles with proper particle size by using a standard sieve to serve as coating powder, placing titanium particles with the average thickness of 800 mu m on the surface of a titanium alloy implant, transferring the treated implant into a vacuum furnace, vacuumizing to more than 10-2 Pa, and heating and sintering. The sintering system is as follows: heating from room temperature to 1400 ℃ at the speed of 5 ℃/min, preserving the heat at the sintering temperature for 0.5 hour, then cooling from the sintering temperature to room temperature at the speed of 1 ℃/min, and taking out the implant with the sintered titanium bead coating and the furnace strength test sample. Cleaning with distilled water and medical alcohol, and packaging. The tensile strength of the titanium granule coating of the strength test specimen was measured according to the ASTM F1147 or EN 582 standard, and the tensile strength was 48 MPa.
Example 1:
weighing 1 kg of titanium powder particles, adding 10 g (1%) of 150-micron fine titanium hydride particles, loading the titanium powder particles into a ball milling tank of planetary ball milling equipment, selecting stainless steel balls with the diameter of 6-10 mm, adding the steel balls according to the ball-to-material ratio of 1:2, pre-vacuumizing, then flushing 4N high-purity argon gas for protection, setting the movement speed of the ball milling tank to be 5 m/s, ball milling for 15 hours, screening titanium powder particles with proper particle size by using a standard sieve after the ball milling is finished to be used as coating powder, placing titanium particles with the average thickness of 800 mu m on the surface of a titanium alloy implant, transferring the treated implant into a vacuum furnace, vacuumizing to 10 mu m, and performing vacuum pumping-2Heating and sintering above Pa. The sintering system is as follows: heating from room temperature to 1400 ℃ at the speed of 5 ℃/min, preserving the heat at the sintering temperature for 0.5 hour, then cooling from the sintering temperature to room temperature at the speed of 1 ℃/min, and taking out the implant with the sintered titanium bead coating and the furnace strength test sample. Cleaning with distilled water and medical alcohol, and packaging. The tensile strength of the titanium granule coating of the strength test specimen was measured according to ASTM F1147 or EN 582 standard, and the tensile strength was 80 MPa. The particle size of the pretreated titanium powder particles is 50-250 micrometers.
Example 2:
weighing 1 kg of titanium powder particles, adding 30 g (3%) of 150-micron fine titanium hydride particles, loading the titanium powder particles into a ball milling tank of planetary ball milling equipment, selecting stainless steel balls with the diameter of 6 mm, adding the steel balls according to the ball-to-material ratio of 1:2, pre-vacuumizing, then flushing 4N high-purity argon gas for protection, setting the moving speed of the ball milling tank to be 9 m/s, carrying out ball milling for 1 hour, screening the titanium powder particles with proper particle size by using a standard sieve after the ball milling is finished to be used as coating powder, placing the titanium particles with the average thickness of 1000 mu m on the surface of a titanium alloy implant, transferring the treated implant into a vacuum furnace, vacuumizing to 10 mu m, and carrying out vacuum pumping-2Heating and sintering above Pa. The sintering system is as follows: heating from room temperature to 1300 ℃ at the speed of 1 ℃/min, preserving the heat for 5 hours at the sintering temperature, then cooling from the sintering temperature to the room temperature at the speed of 5 ℃/min, and taking out the implant with the sintered titanium bead coating and the furnace strength test sample. Cleaning with distilled water and medical alcohol, and packaging. The tensile strength of the titanium granule coating of the strength test specimen was measured according to ASTM F1147 or EN 582 standard, and the tensile strength was 75 MPa. The particle size of the pretreated titanium powder particles is 50-250 micrometers.
Example 3:
weighing 1 kg of titanium powder particles, adding 15 g (1.5%) of 150-micron fine titanium hydride particles, loading the titanium powder particles into a ball milling tank of a planetary ball milling device, selecting stainless steel balls with the diameter of 10 mm, adding the steel balls according to the ball-to-material ratio of 1:2, pre-vacuumizing, then flushing 4N high-purity argon gas for protection, setting the movement speed of the ball milling tank to be 1.5 m/s, ball milling for 20 hours, screening titanium powder particles with proper particle size by using a standard sieve after ball milling is finished to be used as coating powder, placing the titanium particles with the average thickness of 600 mu m on the surface of a titanium alloy implant, transferring the treated implant into a vacuum furnace, vacuumizing to 10 mu m, and performing vacuum pumping-2Heating and sintering above Pa. The sintering system is as follows: heating from room temperature to 1000 ℃ at the speed of 30 ℃/min, preserving the heat for 5 hours at the sintering temperature, then cooling from the sintering temperature to room temperature at the speed of 10 ℃/min, and taking out the implant with the sintered titanium bead coating and the furnace strength test sample. Cleaning with distilled water and medical alcohol, and packaging. Strength measurement according to ASTM F1147 or EN 582 StandardThe tensile strength of the titanium particle coating of the test sample was 60 MPa. The particle size of the pretreated titanium powder particles is 50-250 micrometers.
The biological performance of the treated implant was tested, and the test items included cytotoxicity test, sensitization test, intradermal reaction test, acute systemic toxicity (intravenous route), and genotoxicity test (Ames). The detection criteria according to are:
1) GB/T16886.5-2003 medical devices biology evaluation fifth part: in vitro cytotoxicity test;
2) the tenth part of the biological evaluation of GB/T16886.10-2005 medical devices: stimulation and delayed type hypersensitivity tests;
3) GB/T16886.11-1997 eleventh part of the Biol evaluation of medical devices: systemic toxicity test;
4) GB/T16886.3-1997 medical devices biology evaluation third part: genotoxicity, carcinogenicity, and reproductive toxicity tests;
5) the pharmacopoeia of the people's republic of China 2005 edition appendix XID pyrogen test.
The detection result shows that the treated implant meets the five standard requirements.
The invention relates to a preparation method for obtaining a high-bonding-strength, bioactive and open type porous non-spherical titanium powder particle coating on the surface of an implant. The implant is suitable for biological fixation type implants in orthopedics, dentistry and the like, and can improve the bone ingrowth effect of the implants, improve the bone combination strength and improve the reliability of the implants. The method is to carry out planetary ball milling pretreatment on the pre-sintered titanium powder particles. Adding 150-micron fine titanium hydride accounting for 1-3% of the powder by mass into titanium powder particles, carrying out ball milling for 1-20 hours in a planetary ball milling device with a ball milling tank with the maximum movement speed of 1.5-9 m/s, and screening the titanium powder particles with proper particle size as coating powder particles for later use after the ball milling is finished. Placing titanium powder particles which meet the technical requirements of the implant on the surface of the cleaned implant, transferring the treated implant into a vacuum furnace, and vacuumizing to 10 DEG C-2Heating and sintering above Pa, wherein the sintering system is as follows: at a speed of 1-30 ℃/minAnd (3) heating from room temperature to sintering temperature of 1000-1400 ℃, preserving heat at the sintering temperature for 0-10 hours, cooling from the sintering temperature to room temperature at the speed of 1-10 ℃/min, taking out the implant with the sintered titanium bead coating, cleaning with distilled water and medical alcohol, and packaging. After planetary ball milling pretreatment is adopted, the bonding strength of the vacuum sintering titanium alloy particle coating and the matrix is effectively improved, and the bonding strength is improved from 40-55MPa of which the ball milling pretreatment is not carried out to 60-80 MPa.

Claims (5)

1. A planetary ball milling pretreatment method for titanium powder particles of a vacuum sintering porous titanium coating is characterized in that titanium hydride particles accounting for 1-3% of the mass percentage are added into the titanium powder particles, the particle size of the titanium hydride particles is smaller than 150 micrometers, then stainless steel balls are selected, the ball-material ratio is 1:2, 4N high-purity argon gas is filled for protection after pre-vacuumizing, ball milling is carried out for 1-20 hours in planetary ball milling equipment with the maximum motion speed of a ball milling tank being 1.5 m/s to 9 m/s, the titanium powder particles with proper particle size are screened as powder particles for coating after the ball milling is finished, and then the vacuum sintering process is adopted to obtain the open type porous titanium coating on the surface of an orthopedic implant and a dental implant.
2. The planetary ball milling pretreatment method of titanium powder particles for vacuum sintering of porous titanium coating according to claim 1, wherein the vacuum sintering process of vacuum sintering of porous titanium coating comprises placing the pretreated titanium powder particles meeting the technical requirements of the implant on the surface of the cleaned implant, placing the titanium particles with an average thickness of 600-1000 μm on the surface of the titanium alloy implant, transferring the treated implant into a vacuum furnace, and vacuumizing to 10 ≤-2Heating and sintering above Pa, wherein the sintering system is as follows: heating from room temperature to 1000 ℃ and 1400 ℃ at the speed of 1-30 ℃/min, preserving the heat at the sintering temperature for 0.5-10 hours, cooling from the sintering temperature to room temperature at the speed of 1-10 ℃/min, taking out the implant with the sintered titanium bead coating, cleaning by using distilled water and medical alcohol, and packaging.
3. The planetary ball milling pretreatment method of the titanium powder particles of the vacuum sintered porous titanium coating as claimed in claim 2, wherein the bonding strength of the vacuum sintered titanium alloy particle coating and the matrix is improved to 60-80MPa after planetary ball milling pretreatment.
4. The planetary ball milling pretreatment method of titanium powder particles for vacuum sintering porous titanium coating according to claim 1, characterized in that the stainless steel balls are selected from stainless steel balls with diameter of 6-10 mm.
5. The planetary ball milling pretreatment method of the titanium powder particles of the vacuum sintered porous titanium coating as claimed in claim 1, wherein the particle size of the pretreated titanium powder particles is 50-250 μm.
CN202110625102.2A 2021-06-04 2021-06-04 Planetary ball milling pretreatment method for titanium powder particles of vacuum sintering porous titanium coating Withdrawn CN113385676A (en)

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