CN107779812A - A kind of method of modifying on medical titanium alloy surface - Google Patents

A kind of method of modifying on medical titanium alloy surface Download PDF

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Publication number
CN107779812A
CN107779812A CN201710979757.3A CN201710979757A CN107779812A CN 107779812 A CN107779812 A CN 107779812A CN 201710979757 A CN201710979757 A CN 201710979757A CN 107779812 A CN107779812 A CN 107779812A
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CN
China
Prior art keywords
titanium alloy
medical titanium
alloy surface
modifying
hno
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CN201710979757.3A
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Chinese (zh)
Inventor
许成
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Jhy Titanium Industry Co Ltd
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Jhy Titanium Industry Co Ltd
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Priority to CN201710979757.3A priority Critical patent/CN107779812A/en
Publication of CN107779812A publication Critical patent/CN107779812A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C10/00Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
    • C23C10/34Embedding in a powder mixture, i.e. pack cementation
    • C23C10/36Embedding in a powder mixture, i.e. pack cementation only one element being diffused
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/28Materials for coating prostheses
    • A61L27/30Inorganic materials
    • A61L27/306Other specific inorganic materials not covered by A61L27/303 - A61L27/32

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Dermatology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (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)
  • Materials For Medical Uses (AREA)

Abstract

The invention discloses a kind of medical titanium alloy surface modifying method, this method is:Silica flour is coated by activation process, on medical titanium alloy surface, Atmosphere controlling heat-treatment finally gives the medical titanium alloy with titanium silicon coating.Medical titanium alloy made from this method has good corrosion resistance and biocompatibility, can be firmly combined with titanium implantation instrument surface.Processing is modified to medical titanium alloy surface using this method, technique is simpler, and process produces without waste residue and liquid, more environmentally-friendly.

Description

A kind of method of modifying on medical titanium alloy surface
Technical field
The invention belongs to biomaterial processing technique field, is related to a kind of method of modifying on medical titanium alloy surface.
Background technology
Titanium material obtains a wide range of applications with its excellent combination property in medical embedded instrument field, as synthetism is produced Product, backbone correcting internal fixation system, tooth implant, joint prosthesis, heart valve prosthesis, Interventional angiocarpy bracket etc..But For titanium metal material due to its inertia reason, itself does not possess bioactivity, strong as that can not be formed between implant and bone tissue Strong chemical synostosis, there can be loose phenomenon after long-term use of;In addition in implantation process, implant may be brought into week The bacterium in collarette border, so as to trigger the postoperative infections such as osteomyelitis.To improve the interface fusion between implant and bone tissue, and change The biocidal property of kind implant, surface is carried out to titanium and titanium alloy and is modified as one of current study hotspot of implantation material.
The domestic surface treatment to orthopaedics titanium implantation instrument can not yet meet clinical practice requirement, wear resistance and corrosion resistance well Can poor, product technology stability and poor repeatability, skin covering of the surface colour fading, poor biocompatibility be all common problem.
The content of the invention
It is an object of the invention to provide a kind of method of modifying on medical titanium alloy surface, it is resistance to solve existing medical titanium alloy The problem of corrosion is poor, poor biocompatibility.
The technical solution adopted in the present invention is a kind of method of modifying on medical titanium alloy surface, specifically according to following step It is rapid to implement:
Step 1, medical titanium alloy surface is cleaned, remove surface impurity;
Step 2, step 1 is handled after medical titanium alloy HF, HNO3Mixed liquor activation process 15-20 minutes;
Step 3, silica flour is coated to step 2 gained medical titanium alloy surface;
Step 4, Atmosphere controlling heat-treatment is carried out to step 3 gained medical titanium alloy, so that medical titanium alloy Surface Creation Titanium silicon coating;
Step 5, polishing processing is carried out to step 4 gained medical titanium alloy, so that coating surface is smooth.
The features of the present invention also resides in:
Cleaning is to use H in step 12O2Aqueous cleaning, scavenging period are 35-40 minutes;
In the mixed liquor that activation process uses in step 2, HF, HNO3Volume ratio be HF:HNO3=2:15, activation process Time is 10 minutes, and HF mass concentrations are 55%-70%, HNO3Mass concentration is 25%-35%;
Silica flour coating layer thickness is 300-450 μm in step 3;
Atmosphere in step 4 is circulation nitrogen oxygen mixed gas, the volume ratio of nitrogen and oxygen wherein in nitrogen oxygen mixed gas Respectively:Nitrogen 50-60%, oxygen 40-50%, treatment temperature are 1100-1200 DEG C, and processing time is 3-4 hours.
Processing is modified to medical titanium alloy the beneficial effects of the invention are as follows the method using the present invention, can be in medical titanium Alloy surface forms thicker, even compact, is well combined, chemically stable thin film of titanium oxide modified layer, meanwhile, this method is not Waste liquid, waste residue are produced, cost is relatively low, and low-carbon environment-friendly, wear and corrosion behavior significantly improves, and has good bio-compatible Property.
Embodiment
With reference to embodiment, the present invention is described in detail.
A kind of method of modifying on medical titanium alloy surface of the present invention, specifically implements according to following steps:
Step 1, to medical titanium alloy surface H2O2Aqueous cleaning, remove surface impurity;
Step 2, step 1 is handled after medical titanium alloy with volume ratio be HF:HNO3=2:At 15 mixed liquor activation Manage 15-20 minutes;
Step 3, silica flour is coated to step 2 gained medical titanium alloy surface;
Step 4, Atmosphere controlling heat-treatment is carried out to step 3 gained medical titanium alloy, so that medical titanium alloy Surface Creation Titanium silicon coating;
Step 5, polishing processing is carried out to step 4 gained medical titanium alloy, so that coating surface is smooth.
Embodiment 1
One piece of titanium alloy bone plate is chosen, is handled as follows:1st, titanium alloy bone plate is used into H2O2Aqueous cleaning 35-40 minutes, remove surface impurity;2nd, the titanium alloy bone plate volume ratio HF after cleaning:HNO3=2:15 mixed liquor is lived Change processing 10 minutes, wherein HF mass percentage concentration is 55%, HNO3Mass percentage concentration be 25%;3rd, in activation process Titanium alloy synthetism plate surface 300 μm of silica flour of coating afterwards;4th, the titanium alloy bone plate for having coated silica flour is put into controlled atmosphere to add Hot stove carries out surface modification treatment, and atmosphere is circulation nitrogen oxygen mixed gas, and the volume ratio of wherein nitrogen and oxygen is:Nitrogen 50%, oxygen 50%, treatment temperature is 1100 DEG C, and processing time is 3 hours, at this moment forms one on the surface of titanium alloy bone plate Layer titanium silicon coating;Titanium alloy bone plate after processing is subjected to polishing processing, obtain surfacing, uniform and smooth, corrosion resistance is high, The titanium alloy bone plate of good biocompatibility.
Embodiment 2
A tooth implant is chosen, is handled as follows:1st, tooth implant is used into H2O2Aqueous cleaning 35-40 minutes, Remove surface impurity;2nd, the tooth implant volume ratio HF after cleaning:HNO3=2:15 mixed liquor activation process 10 minutes, its Middle HF mass percentage concentration is 60%, HNO3Mass percentage concentration be 30%;3rd, the Dental implantion body surface after activation process Face coats 380 μm of silica flour;4th, coated tooth implant is put into controlled atmosphere heating furnace and carries out surface modification treatment, atmosphere is Nitrogen oxygen mixed gas are circulated, the volume ratio of wherein nitrogen and oxygen is:Nitrogen 55%, oxygen 45%, treatment temperature are 1150 DEG C, Processing time is 3.5 hours, and the surface of tooth implant can form one layer of titanium silicon coating;Tooth implant after processing is polished Processing, obtains surfacing, uniform and smooth, corrosion resistance is high, the tooth implant of good biocompatibility.
Embodiment 3
A bone nail is chosen, is handled as follows:1st, bone nail is used into H2O2Aqueous cleaning 35-40 minutes, remove Surface impurity;2nd, the bone nail volume ratio HF after cleaning:HNO3=2:15 mixed liquor activation process 10 minutes, wherein HF's Mass percentage concentration is 70%, HNO3Mass percentage concentration be 35%;3rd, the bone nail surface coating silicon after activation process 450 μm of powder;4th, coated bone nail is put into controlled atmosphere heating furnace and carries out surface modification treatment, atmosphere is that cyclic nitrogen oxygen mixes Gas is closed, the volume ratio of wherein nitrogen and oxygen is:Nitrogen 60%, oxygen 40%, treatment temperature are 1200 DEG C, and processing time is 4 hours, the surface of bone nail can form one layer of titanium silicon coating;Bone nail after processing is subjected to polishing processing, surface is obtained and puts down It is whole, uniform and smooth, corrosion resistance is high, the bone nail of good biocompatibility.

Claims (5)

1. a kind of method of modifying on medical titanium alloy surface, it is characterised in that specifically implement according to following steps:
Step 1, medical titanium alloy surface is cleaned, remove surface impurity;
Step 2, step 1 is handled after medical titanium alloy HF, HNO3Mixed liquor activation process 15-20 minutes;
Step 3, silica flour is coated to step 2 gained medical titanium alloy surface;
Step 4, Atmosphere controlling heat-treatment is carried out to step 3 gained medical titanium alloy, so that medical titanium alloy Surface Creation titanium silicon Coating;
Step 5, polishing processing is carried out to step 4 gained medical titanium alloy, so that coating surface is smooth.
2. the method for modifying on a kind of medical titanium alloy surface according to claim 1, it is characterised in that clear in the step 1 Wash is to use H2O2Aqueous cleaning, scavenging period are 35-40 minutes.
3. the method for modifying on a kind of medical titanium alloy surface according to claim 1, it is characterised in that living in the step 2 Change in the mixed liquor that processing uses, HF, HNO3Volume ratio be HF:HNO3=2:15, the activation process time is 10 minutes, HF matter Amount concentration is 55%-70%, HNO3Mass concentration is 25%-35%.
A kind of 4. method of modifying on medical titanium alloy surface according to claim 1, it is characterised in that silicon in the step 3 Powder coating thickness is 300-450 μm.
5. the method for modifying on a kind of medical titanium alloy surface according to claim 1, it is characterised in that in the step 4 Atmosphere is circulation nitrogen oxygen mixed gas, and the volume ratio of nitrogen and oxygen is respectively wherein in nitrogen oxygen mixed gas:Nitrogen 50- 60%th, oxygen 40-50%, treatment temperature are 1100-1200 DEG C, and processing time is 3-4 hours.
CN201710979757.3A 2017-10-19 2017-10-19 A kind of method of modifying on medical titanium alloy surface Pending CN107779812A (en)

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CN107779812A true CN107779812A (en) 2018-03-09

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1995029270A1 (en) * 1994-04-25 1995-11-02 Sturm, Ruger & Company, Inc. Method of treating titanium parts
CN101507836A (en) * 2009-03-23 2009-08-19 戚培毅 Thermal processing method capable of increasing medical titanium implant surface performance
CN102162080A (en) * 2011-03-31 2011-08-24 戚培毅 Medicinal titanium implanting apparatus surface modification layer and preparation method thereof
CN104099609A (en) * 2014-06-26 2014-10-15 华中科技大学 Surface modification method for medical titanium alloy
CN104480464A (en) * 2014-12-25 2015-04-01 安徽工业大学 Method for laser cladding of Ti-Si gradient wear-resistantcoating on Ti alloy surface

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1995029270A1 (en) * 1994-04-25 1995-11-02 Sturm, Ruger & Company, Inc. Method of treating titanium parts
CN101507836A (en) * 2009-03-23 2009-08-19 戚培毅 Thermal processing method capable of increasing medical titanium implant surface performance
CN102162080A (en) * 2011-03-31 2011-08-24 戚培毅 Medicinal titanium implanting apparatus surface modification layer and preparation method thereof
CN104099609A (en) * 2014-06-26 2014-10-15 华中科技大学 Surface modification method for medical titanium alloy
CN104480464A (en) * 2014-12-25 2015-04-01 安徽工业大学 Method for laser cladding of Ti-Si gradient wear-resistantcoating on Ti alloy surface

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Application publication date: 20180309

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