CN113319283B - Air flow mill pretreatment and micro hydrogen assisted sintering method for titanium coating - Google Patents
Air flow mill pretreatment and micro hydrogen assisted sintering method for titanium coating Download PDFInfo
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Abstract
The invention discloses an air-flow grinding pretreatment and micro-hydrogen assisted sintering method of a titanium coating, and relates to an air-flow grinding treatment and micro-hydrogen assisted sintering synergistic processing method for improving the bonding strength of titanium particles and a matrix. Comprises two steps: firstly, placing powder particles to be treated into fluidized bed type air flow grinding equipment, then introducing 4N high-purity argon, then introducing 4N high-purity hydrogen to 0.105-0.110 MPa, starting a high-pressure pump to enable gas to generate internal circulation movement, carrying out air flow grinding for 10-120 minutes at the speed of 300-500 m/s in a fluidized bed, and screening titanium powder particles with proper granularity as powder particles for coating for standby after the air flow grinding is finished; secondly, placing titanium powder particles meeting the technical requirements of the implant on the surface of the implant after cleaning, transferring the treated implant into a vacuum furnace, opening a high vacuum system, heating to the sintering temperature of 1000-1400 ℃, preserving heat at the sintering temperature, cooling to room temperature, taking out the implant with the sintered titanium bead coating, cleaning and packaging.
Description
Technical Field
The invention discloses an air flow grinding pretreatment and micro hydrogen assisted sintering method of a titanium coating, relates to an air flow grinding treatment and micro hydrogen assisted sintering cooperative processing method for improving the bonding strength of titanium particles and a matrix, and belongs to the field of powder metallurgy materials and biological materials. Is suitable for improving the performance of implants such as orthopaedics, dentistry and the like, in particular to improving the bonding strength of a porous titanium coating on the surface of the implant and a titanium alloy matrix.
Background
Implant coating technology has evolved over the years to gradually mature. Taking an artificial joint as an example, the mature processes at present mainly comprise an air plasma spraying process, a vacuum sintering process and an electrochemical process, and the coating material mainly comprises titanium, hydroxyapatite (hereinafter referred to as HA) and a composite of the titanium and the hydroxyapatite. The current primary bio-coating technology for bio-artificial joints employs vacuum sintering of titanium coating and plasma spraying of HA on the titanium coating, which HAs been widely used in bio-artificial joints, such as SUMMIT total hip prosthesis and PFC total knee prosthesis of DEPUY company in usa, NExgen total knee prosthesis of ZIMMER company in usa, PROFIX total knee prosthesis of SMITH-NEPHEW company and MAXIN total knee prosthesis of biuret company, due to its excellent bone ingrowth clinical effect and low cost.
The product needs to form a titanium coating on the surface of the titanium alloy matrix through vacuum sintering, the bonding strength of the titanium coating and the titanium alloy matrix determines whether the workpiece can enter a subsequent process, and on the premise of ensuring that the titanium coating has proper porosity, the titanium coating and the titanium alloy matrix need to have enough bonding strength, which is the premise of ensuring the safety of the implant, the bone bonding strength and the bone ingrowth effect. However, the connection strength between the titanium coating prepared by adopting the conventional sintering process and the titanium alloy matrix is often low under the condition of ensuring the porosity, so that the reliability of the coating is reduced. The powder adopted for vacuum sintering the titanium coating mainly comprises spherical titanium powder and irregular titanium powder, and the problem of lower connection strength of the coating and a matrix is particularly prominent when the irregular titanium powder is adopted. Thus, subsequent analysis and experimentation is primarily around the case when irregular titanium powder is selected for the coating, and the invention to solve the problem is obviously equally applicable to spherical titanium powder.
Disclosure of Invention
The invention aims to overcome the defects, provides an air-flow grinding pretreatment and micro-hydrogen assisted sintering method for a titanium coating, and provides an air-flow grinding treatment and micro-hydrogen assisted sintering cooperative processing method for improving the bonding strength of titanium particles and a matrix.
The air flow mill pretreatment and micro hydrogen assisted sintering method of the titanium coating is realized by adopting the following technical scheme:
the air flow mill pretreatment and micro hydrogen assisted sintering method of the titanium coating comprises two steps:
firstly, powder particles to be treated are placed into fluidized bed type air flow mill equipment, then 4N high-purity argon is introduced to enable the oxygen content of atmosphere in the air flow mill equipment to be lower than 2000ppm, the air pressure in the air flow mill is kept to be 0.101MPa, then 4N high-purity hydrogen is introduced to be 0.105-0.110 MPa, a high-pressure pump is opened to enable the gas to generate internal circulation movement, the air flow in the fluidized bed is subjected to air flow mill for 10-120 minutes at the speed of 300-500 m/s, and after the air flow mill is finished, titanium powder particles with proper granularity are screened to be used as powder particles for coating for standby.
Secondly, titanium powder particles meeting the technical requirements of the implant are adopted to be placed on the surface of the implant after the implant is cleaned, and the titanium alloy is implantedPlacing titanium powder particles with average thickness of 600-800 mu m on the surface of the object, transferring the treated implant into a vacuum furnace, and vacuumizing to 10 -2 And (3) heating and sintering the mixture above Pa, wherein the sintering schedule is as follows: heating from room temperature to 500-600 ℃ at a speed of 1-30 ℃/min, then cooling to 320-380 ℃, closing the high vacuum system, starting only a mechanical pump, introducing micro-flow hydrogen to keep the pressure in the furnace at 30-60 Pa, preserving heat for 30-80 min, opening the high vacuum system, and vacuumizing to be less than 5 x 10 -2 And (3) heating to the sintering temperature of 1000-1400 ℃ at the speed of 15-30 ℃/min, preserving the temperature at the sintering temperature for 0.5-10 hours, cooling 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.
The particle size of the pretreated titanium powder is 50-250 micrometers (mu m).
After the air flow grinding treatment and the micro hydrogen treatment are cooperatively adopted, the bonding strength of the titanium alloy particle coating and the matrix is further and effectively improved: if any treatment is not performed, the bonding strength is 40-55 MPa; performing jet milling treatment independently, and improving the bonding strength to 65-80 MPa; the trace hydrogen treatment is carried out independently, and the bonding strength is improved to 68-78 MPa; after the air flow grinding treatment and the micro hydrogen treatment are cooperatively adopted, the bonding strength between the titanium alloy particle coating and the substrate can be improved to 100-115 MPa. On one hand, the coating maintains a good space structure of the high-vacuum sintered titanium coating, and on the other hand, the bonding strength of the titanium coating on the surface of the implant and the titanium alloy matrix is greatly improved through cooperative treatment, so that the reliability and safety of the implant are improved. And the process cost is lower.
The invention has the beneficial effects and advantages that:
the purpose of making the porous titanium coating on the surface of the implant is to allow the new bone tissue to grow into the pores of the porous titanium bead coating, so that the implant and the bone tissue are fixed together. This way of achieving implant fixation using bone ingrowth into the porous surface is called biosensing. As bone tissue grows into the pores, the interfacial area between the bone and the implant is greatly increased, along with the mechanical engagement between the bone and the porous surface, the shear strength of the implant and bone interface is also greatly increased. However, in the process of sintering the porous titanium coating in vacuum, 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, resulting in insufficient reliability of the coating. The powder adopted for vacuum sintering the titanium coating mainly comprises spherical titanium powder and irregular titanium powder, and the problem of lower connection strength of the coating and a matrix is particularly prominent when the irregular titanium powder is adopted.
Aiming at the defects, the invention provides an air flow grinding treatment and micro-hydrogen assisted sintering cooperative processing method for improving the bonding strength of titanium particles and a matrix. The method comprises the following two steps: firstly, powder particles to be treated are placed into fluidized bed type air flow mill equipment, then 4N high-purity argon is introduced to enable the oxygen content of atmosphere in the air flow mill equipment to be lower than 2000ppm, the air pressure in the air flow mill is kept to be 0.101MPa, then 4N high-purity hydrogen is introduced to be 0.105-0.110 MPa, a high-pressure pump is opened to enable the gas to generate internal circulation movement, the air flow in the fluidized bed is subjected to air flow mill for 10-120 minutes at the speed of 300-500 m/s, and after the air flow mill is finished, titanium powder particles with proper granularity are screened to be used as powder particles for coating for standby. Secondly, titanium powder particles meeting the technical requirements of the implant are adopted on the surface of the implant after cleaning and cleaning, the implant after being treated is placed on the surface of the implant, the implant after being treated is moved into a vacuum furnace, and the vacuum is pumped to 10 -2 And (3) heating and sintering the mixture above Pa, wherein the sintering schedule is as follows: heating from room temperature to 500-600 ℃ at a speed of 1-30 ℃/min, then cooling to 320-380 ℃, at the moment, turning off a high vacuum system, only starting a mechanical pump, introducing micro-flow hydrogen to keep the pressure in the furnace at 30-60 Pa, preserving heat for 30-80 min, opening the high vacuum system, heating to a sintering temperature of 1000-1400 ℃ at a speed of 15-30 ℃/min, preserving heat for 0.5-10 hours at the sintering temperature, cooling from the sintering temperature to room temperature at a speed of 1-10 ℃/min, taking out the implant with the sintered titanium bead coating, cleaning with distilled water and medical alcohol, and packaging. On one hand, the coating maintains a good space structure of the high-vacuum sintered titanium coating, on the other hand, the bonding strength of the titanium coating on the surface of the implant and a titanium alloy matrix is greatly improved through cooperative treatment, no hydride exists in a final finished product, and the product is goodThe biological performance test requirements of cytotoxicity test, sensitization test, intradermal reaction test, acute systemic toxicity (vein route), genetic toxicity test (Ames) and the like are met.
According to the air flow grinding treatment and micro hydrogen assisted sintering cooperative processing method for improving the bonding strength of the vacuum sintering titanium alloy particle coating and the matrix, the bonding performance of the titanium alloy coating and the matrix is effectively improved, the reliability and the safety of the implant are improved, and the process cost is low.
Detailed Description
The air-flow grinding treatment and micro-hydrogen assisted sintering method of the titanium powder particle coating comprise two steps:
firstly, powder particles to be treated are placed into fluidized bed type air flow mill equipment, then 4N high-purity argon is introduced to enable the oxygen content of atmosphere in the air flow mill equipment to be lower than 2000ppm, the air pressure in the air flow mill is kept to be 0.101MPa, then 4N high-purity hydrogen is introduced to be 0.105-0.110 MPa, a high-pressure pump is opened to enable the gas to generate internal circulation movement, the air flow in the fluidized bed is subjected to air flow mill for 10-120 minutes at the speed of 300-500 m/s, and after the air flow mill is finished, titanium powder particles with proper granularity are screened to be used as powder particles for coating for standby.
The particle size of the pretreated titanium powder is 50-250 micrometers (mu m).
Secondly, placing titanium powder particles meeting the technical requirements of the implant on the surface of the implant after cleaning, placing titanium powder particles with average thickness of 800 mu m on the surface of the titanium alloy implant, transferring the treated implant into a vacuum furnace, and vacuumizing to 10 DEG -2 And (3) heating and sintering the mixture above Pa, wherein the sintering schedule is as follows: heating from room temperature to 500-600 ℃ at a speed of 1-30 ℃/min, then cooling to 320-380 ℃, closing the high vacuum system, starting only a mechanical pump, introducing micro-flow hydrogen to keep the pressure in the furnace at 30-60 Pa, preserving heat for 30-80 min, opening the high vacuum system, and vacuumizing to be less than 5 x 10 -2 Pa, heating to a sintering temperature of 1000-1400 ℃ at a speed of 15-30 ℃/min, preserving heat at the sintering temperature for 0.5-10 hours, cooling from the sintering temperature to room temperature at a speed of 1-10 ℃/min, and taking out the sintered materialThe implant with titanium bead coating is cleaned with distilled water and medical alcohol, and packaged.
After the air flow grinding treatment and the micro hydrogen treatment are cooperatively adopted, the bonding strength of the titanium alloy particle coating and the matrix is further and effectively improved: if any treatment is not performed, the bonding strength is 40-55 MPa; performing jet milling treatment independently, and improving the bonding strength to 65-80 MPa; the trace hydrogen treatment is carried out independently, and the bonding strength is improved to 68-78 MPa; after the air flow grinding treatment and the micro hydrogen treatment are adopted cooperatively, the bonding strength can be improved to 100-115 MPa. On one hand, the coating maintains a good space structure of the high-vacuum sintered titanium coating, and on the other hand, the bonding strength of the titanium coating on the surface of the implant and the titanium alloy matrix is greatly improved through cooperative treatment, so that the reliability and safety of the implant are improved. And the process cost is lower.
The invention will be further illustrated with reference to the following examples:
comparative example 1:
screening titanium powder particles with proper granularity by using a standard sieve to be used as powder for coating, placing titanium particles with average thickness of 800 mu m on the surface of a titanium alloy implant, transferring the treated implant into a vacuum furnace, and vacuumizing to 10 -2 And (5) heating and sintering the mixture. The sintering system is as follows: the temperature is raised from room temperature to 1400 ℃ at a speed of 5 ℃/min, the temperature is kept at the sintering temperature for 0.5 hours, the temperature is lowered from the sintering temperature to room temperature at a speed of 1 ℃/min, and the implant with the sintered titanium bead coating and the furnace-following strength test sample are taken out. Cleaning with distilled water, medical alcohol, etc., and packaging. The test specimens were tested for tensile strength of the titanium particle coating according to ASTM F1147 or EN 582 standards, with a tensile strength of 48 MPa.
Comparative example 2:
placing titanium powder particles to be treated into fluidized bed type air flow mill equipment, then introducing 4N high-purity argon gas to ensure that the oxygen content of the atmosphere in the air flow mill equipment is lower than 2000ppm, keeping the air pressure in the air flow mill to be 0.101MPa, then introducing 4N high-purity hydrogen gas to be 0.108MPa, opening a high-pressure pump to ensure that the gas generates internal circulation movement, grinding the air flow in the fluidized bed for 55 minutes at the speed of 400 m/s, and screening after the air flow grinding is finishedTitanium powder particles of a suitable particle size are used as powder particles for coating. Placing titanium particles with average thickness of 800 mu m on the surface of a titanium alloy implant, transferring the treated implant into a vacuum furnace, and vacuumizing to 10 DEG C -2 And (5) heating and sintering the mixture. The sintering system is as follows: the temperature is raised from room temperature to 1400 ℃ at a speed of 5 ℃/min, the temperature is kept at the sintering temperature for 0.5 hours, the temperature is lowered from the sintering temperature to room temperature at a speed of 1 ℃/min, and the implant with the sintered titanium bead coating and the furnace-following strength test sample are taken out. Cleaning with distilled water, medical alcohol, etc., and packaging. The test specimens were tested for tensile strength of the titanium particle coating according to ASTM F1147 or EN 582 standards, with a tensile strength of 71 MPa.
Comparative example 3:
screening titanium powder particles with proper granularity by using a standard sieve to be used as powder for coating, placing titanium particles with average thickness of 800 mu m on the surface of a titanium alloy implant, transferring the treated implant into a vacuum furnace, and vacuumizing to 10 -2 And (5) heating and sintering the mixture. The sintering system is as follows: heating from room temperature to 550 ℃ at a speed of 15 ℃/min, then cooling to 350 ℃, at the moment, turning off a high vacuum system, starting a mechanical pump only, introducing micro-flowing hydrogen to keep the pressure in the furnace at 45 Pa, preserving heat for 50 min, turning on the high vacuum system, heating to a sintering temperature of 1200 ℃ at a speed of 22 ℃/min, preserving heat for 5 hours at the sintering temperature, cooling from the sintering temperature to the room temperature at a speed of 5 ℃/min, and taking out the implant with the sintered titanium bead coating and the furnace-following strength test sample. Cleaning with distilled water, medical alcohol, etc., and packaging. The test specimens were tested for tensile strength of the titanium particle coating according to ASTM F1147 or EN 582 standards, with a tensile strength of 72 MPa.
Example 1:
putting titanium powder particles to be treated into fluidized bed type air flow mill equipment, then introducing 4N high-purity argon gas to ensure that the oxygen content of the atmosphere in the air flow mill equipment is lower than 2000ppm, keeping the air pressure in the air flow mill to be 0.101MPa, then introducing 4N high-purity hydrogen gas to be 0.108MPa, opening a high-pressure pump to ensure that the gas generates internal circulation motion, grinding the air flow in the fluidized bed for 55 minutes at the speed of 400 m/s, and screening titanium powder particles with proper granularity as powder particles for coating after the air flow mill is finished for standby.
Placing titanium powder particles with average thickness of 600 μm on the surface of titanium alloy implant, transferring the treated implant into vacuum furnace, and vacuumizing to 10% -2 And (5) heating and sintering the mixture. The sintering system is as follows: heating from room temperature to 550 ℃ at a speed of 15 ℃/min, then cooling to 350 ℃, closing the high vacuum system, starting only a mechanical pump, introducing micro-flowing hydrogen to keep the pressure in the furnace at 45 Pa, preserving heat for 50 min, opening the high vacuum system, and vacuumizing to be less than 5 x 10 -2 Pa, heating to a sintering temperature of 1200 ℃ at a speed of 22 ℃/min, preserving heat at the sintering temperature for 5 hours, cooling to room temperature from the sintering temperature at a speed of 5 ℃/min, and taking out the implant with the sintered titanium bead coating and the furnace-following strength test sample. Cleaning with distilled water, medical alcohol, etc., and packaging. The test specimens were tested for tensile strength of the titanium particle coating according to ASTM F1147 or EN 582 standards, with a tensile strength of 110MPa.
Example 2:
putting titanium powder particles to be treated into fluidized bed type air flow mill equipment, then introducing 4N high-purity argon gas to ensure that the oxygen content of the atmosphere in the air flow mill equipment is lower than 2000ppm, keeping the air pressure in the air flow mill to be 0.101MPa, then introducing 4N high-purity hydrogen gas to be 0.105MPa, opening a high-pressure pump to ensure that the gas generates internal circulation motion, grinding the air flow in the fluidized bed for 120 minutes at the speed of 300 m/s, and screening titanium powder particles with proper granularity as powder particles for coating after the air flow mill is finished for standby.
Placing titanium powder particles with average thickness of 1000 μm on the surface of titanium alloy implant, transferring the treated implant into vacuum furnace, and vacuumizing to 10% -2 And (5) heating and sintering the mixture. The sintering system is as follows: heating from room temperature to 500 ℃ at a speed of 1 ℃/min, then cooling to 320 ℃, closing the high vacuum system, starting only a mechanical pump, introducing micro-flowing hydrogen to keep the pressure in the furnace at 30 Pa, preserving heat for 30 minutes, opening the high vacuum system, and vacuumizing to be less than 5 x 10 -2 Pa, heating to 1000 ℃ at 15 ℃/min, maintaining the temperature at the sintering temperature for 0.5 hour, and cooling from the sintering temperature to room temperature at 1 ℃/minThe sintered titanium bead coated implant and the green strength test specimen were removed. Cleaning with distilled water, medical alcohol, etc., and packaging. The test specimens were tested for tensile strength of the titanium particle coating according to ASTM F1147 or EN 582 standards, with a tensile strength of 100MPa.
Example 3:
putting titanium powder particles to be treated into fluidized bed type air flow mill equipment, then introducing 4N high-purity argon gas to ensure that the oxygen content of the atmosphere in the air flow mill equipment is lower than 2000ppm, keeping the air pressure in the air flow mill to be 0.101MPa, then introducing 4N high-purity hydrogen gas to be 0.110MPa, opening a high-pressure pump to ensure that the gas generates internal circulation motion, grinding the air flow in the fluidized bed for 10 minutes at the speed of 500 m/s, and screening titanium powder particles with proper granularity as powder particles for coating after the air flow mill is finished for standby.
Placing titanium powder particles with average thickness of 800 μm on the surface of titanium alloy implant, transferring the treated implant into vacuum furnace, and vacuumizing to 10% -2 And (5) heating and sintering the mixture. The sintering system is as follows: heating from room temperature to 600 ℃ at a speed of 30 ℃/min, then cooling to 380 ℃, turning off a high vacuum system, starting only a mechanical pump, introducing micro-flowing hydrogen to keep the pressure in the furnace at 60 Pa, preserving heat for 80 minutes, turning on the high vacuum system, and vacuumizing to be less than 5 x 10 -2 Pa, heating to a sintering temperature of 1400 ℃ at a speed of 30 ℃/min, preserving the temperature at the sintering temperature for 10 hours, cooling from the sintering temperature to room temperature at a speed of 10 ℃/min, and taking out the implant with the sintered titanium bead coating and the furnace-following strength test sample. Cleaning with distilled water, medical alcohol, etc., and packaging. The test specimens were tested for tensile strength of the titanium particle coating according to ASTM F1147 or EN 582 standards, with a tensile strength of 115MPa.
The implant treated as described above was subjected to biological performance tests, including "cytotoxicity test, sensitization test, intradermal reaction test, acute systemic toxicity (intravenous route), genotoxicity test (Ames)". The detection standard according to the method is as follows:
1) GB/T16886.5-2003 medical device biological evaluation fifth section: in vitro cytotoxicity assays;
2) GB/T16886.10-2005 medical device biological evaluation tenth part: stimulus and delayed type hypersensitivity tests;
3) GB/T16886.11-1997 medical device biological evaluation eleventh section: systemic toxicity test;
4) GB/T16886.3-1997 medical device biological evaluation third part: genotoxicity, carcinogenicity, and reproductive toxicity tests;
5) The appendix XID pyrogen test of the pharmacopoeia 2005 edition of the people's republic of China.
The test results show that the treated implants all meet the five standard requirements.
The invention relates to a preparation method for obtaining an open porous non-spherical titanium powder particle coating with high bonding strength and bioactivity on the surface of an implant. The implant is suitable for biosolidation type implants such as orthopaedics, dentistry and the like, can improve the bone growth effect of the implant, improve the bone bonding strength and improve the reliability of the implant. The method comprises the following two steps: firstly, powder particles to be treated are placed into fluidized bed type air flow mill equipment, then 4N high-purity argon is introduced to enable the oxygen content of atmosphere in the air flow mill equipment to be lower than 2000ppm, the air pressure in the air flow mill is kept to be 0.101MPa, then 4N high-purity hydrogen is introduced to be 0.105-0.110 MPa, a high-pressure pump is opened to enable the gas to generate internal circulation movement, the air flow in the fluidized bed is subjected to air flow mill for 10-120 minutes at the speed of 300-500 m/s, and after the air flow mill is finished, titanium powder particles with proper granularity are screened to be used as powder particles for coating for standby. Secondly, titanium powder particles meeting the technical requirements of the implant are adopted on the surface of the implant after cleaning and cleaning, the implant after being treated is placed on the surface of the implant, the implant after being treated is moved into a vacuum furnace, and the vacuum is pumped to 10 -2 And (3) heating and sintering the mixture above Pa, wherein the sintering schedule is as follows: heating from room temperature to 500-600 ℃ at a speed of 1-30 ℃/min, then cooling to 320-380 ℃, closing the high vacuum system, starting only a mechanical pump, introducing micro-flow hydrogen to keep the pressure in the furnace at 30-60 Pa, preserving heat for 30-80 min, opening the high vacuum system, and vacuumizing to be less than 5 x 10 -2 Pa, heating to a sintering temperature of 1000-1400 ℃ at a speed of 15-30 ℃/min, preserving heat at the sintering temperature for 0.5-10 hours, and then heating at a speed of 1-10 ℃/minCooling to room temperature from sintering temperature, taking out the implant with sintered titanium bead coating, cleaning with distilled water and medical alcohol, and packaging. After the air flow grinding treatment and the micro hydrogen treatment are cooperatively adopted, the bonding strength of the titanium alloy particle coating and the matrix is further and effectively improved: if any treatment is not performed, the bonding strength is 40-55 MPa; performing jet milling treatment independently, and improving the bonding strength to 65-80 MPa; the trace hydrogen treatment is carried out independently, and the bonding strength is improved to 68-78 MPa; after the air flow grinding treatment and the micro hydrogen treatment are cooperatively adopted, the bonding strength between the titanium alloy particle coating and the substrate can be improved to 100-115 MPa.
Claims (2)
1. The air flow mill pretreatment and micro hydrogen assisted sintering method for the titanium coating is characterized by comprising the following two steps:
firstly, placing powder particles to be treated into fluidized bed type air flow mill equipment, then introducing 4N high-purity argon gas to ensure that the oxygen content of the atmosphere in the air flow mill equipment is lower than 2000ppm, keeping the air pressure in the air flow mill to be 0.101MPa, then introducing 4N high-purity hydrogen gas to be 0.105-0.110 MPa, opening a high-pressure pump to ensure that the gas generates internal circulation motion, carrying out air flow mill for 10-120 minutes at the speed of 300-500 m/s in the fluidized bed, and screening titanium powder particles with proper granularity as powder particles for coating for standby after the air flow mill is finished;
secondly, placing titanium powder particles meeting the technical requirements of the implant on the surface of the implant after cleaning, placing titanium powder particles with the average thickness of 600-800 mu m on the surface of the titanium alloy implant, transferring the treated implant into a vacuum furnace, and vacuumizing to 10 -2 And (3) heating and sintering the mixture above Pa, wherein the sintering schedule is as follows: heating from room temperature to 500-600 ℃ at a speed of 1-30 ℃/min, then cooling to 320-380 ℃, closing the high vacuum system, starting only a mechanical pump, introducing a micro-flow hydrogen to keep the pressure in the furnace at 30-60 Pa, preserving heat for 30-80 min, opening the high vacuum system, and vacuumizing to be less than 5 x 10 -2 Pa, heating to a sintering temperature of 1000-1400 ℃ at a speed of 15-30 ℃/min, preserving heat at the sintering temperature for 0.5-10 hours, and then moving from the sintering temperature at a speed of 1-10 ℃/minCooling to room temperature, taking out the implant with sintered titanium bead coating, cleaning with distilled water and medical alcohol, and packaging;
the particle size of the pretreated titanium powder is 50-250 micrometers (mu m).
2. The method for pretreating the titanium coating by air flow grinding and sintering the titanium coating by micro hydrogen assisted method according to claim 1, wherein after the air flow grinding treatment and the micro hydrogen treatment are adopted cooperatively, the bonding strength of the titanium alloy particle coating and the substrate is improved to 100-115 MPa.
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| CN101138649A (en) * | 2007-10-24 | 2008-03-12 | 常州天力生物涂层技术有限公司 | Method for obtaining bioactivity and open type stephanoporate titanium coating from implant surface |
| CN103266319A (en) * | 2013-05-21 | 2013-08-28 | 李建久 | Method for preparing porous titanium coating on surface of titanium alloy |
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| EP3666932A1 (en) * | 2018-12-14 | 2020-06-17 | Nano-implant Sp. z o.o. | Production method of a personalised, biocompatible and bioactive orthopaedic implant |
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| CN101138649A (en) * | 2007-10-24 | 2008-03-12 | 常州天力生物涂层技术有限公司 | Method for obtaining bioactivity and open type stephanoporate titanium coating from implant surface |
| CN103266319A (en) * | 2013-05-21 | 2013-08-28 | 李建久 | Method for preparing porous titanium coating on surface of titanium alloy |
| CN106623952A (en) * | 2016-12-19 | 2017-05-10 | 南京理工大学 | Preparation method of titanium or titanium alloy powder with micro-hydrogenated surface |
| EP3666932A1 (en) * | 2018-12-14 | 2020-06-17 | Nano-implant Sp. z o.o. | Production method of a personalised, biocompatible and bioactive orthopaedic implant |
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