CN102039408A - Method for preparing bioactive ceramic coating on surface of porous titanium - Google Patents

Method for preparing bioactive ceramic coating on surface of porous titanium Download PDF

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Publication number
CN102039408A
CN102039408A CN2010105962264A CN201010596226A CN102039408A CN 102039408 A CN102039408 A CN 102039408A CN 2010105962264 A CN2010105962264 A CN 2010105962264A CN 201010596226 A CN201010596226 A CN 201010596226A CN 102039408 A CN102039408 A CN 102039408A
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titanium
porous
diameter
arc oxidation
differential arc
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CN2010105962264A
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魏大庆
成夙
周玉
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention discloses a method for preparing a bioactive ceramic coating on a surface of porous titanium. The method provided by the invention is characterized in that titanium and titanium alloy materials are applied to the replacement of hard tissues such as joints, teeth and bones, and the like of the human body. The method comprises the following steps: carrying out substrate pretreatment: polishing and cleaning the surface of a titanium bead; carrying out vacuum sintering pretreatment: putting the titanium bead into a mould, then putting the mould into a vacuum sintering furnace at a vacuum degree of 10 to 3Pa, heating the titanium bead for 2 hours at a constant temperature of 1,450 DEG C, cooling the titanium bead along with the furnace to room temperature, and then taking out the titanium bead from the furnace, so that the titanium bead is formed into a naturally-lapped porous shape, namely, forming porous titanium; carrying out micro-arc oxidation treatment: putting the porous titanium into a stainless steel cell body containing alkaline electrolyte, wherein the porous titanium is taken as a positive electrode, and the stainless steel cell body is taken as a negative electrode; controlling the liquor in the cell at a temperature of less than 50 DEG C by a cooling system; and controlling micro-arc oxidation electric parameters by a bipolar pulse power, and forming a micro-arc oxidation coating on the surface of the porous titanium through the disruptive discharge of the surface of the porous titanium, wherein the thickness of the coating is 3 to 10mm. The method provided by the invention is used for preparing a bioactive ceramic coating on the surface of porous titanium.

Description

The method of porous Ti biologically active ceramic coating
Technical field:
The present invention relates to a kind ofly will generate loose structure behind the titanium pearl vacuum high-temperature sintering,, be specifically related to a kind of method of porous Ti biologically active ceramic coating then in the method for its surface preparation oxide ceramic coating.
Background technology:
The titanium or titanium alloy material has high mechanical properties, high tenacity and good anti-fatigue performance as important bio-medical material, is widely used in the replacement of the sclerous tissues such as joint, tooth, bone of human body.In order further to improve combining between titanium and alloy implant thereof and the bone tissue, the researcher constantly explores and thinks deeply, be that the research of porous material begins to receive publicity wherein for the titanium matrix, loose structure is owing to can provide the space for growing into of bone tissue, help combining between embedded material and the bone tissue, so porous material has sizable application potential at biomedical aspect.
Summary of the invention:
The purpose of this invention is to provide a kind of energy-and time-economizing, oxide coating and matrix that original position is formed match, more than the film substrate bond strength Gao Keda 30Mpa, are applicable to the POROUS TITANIUM surface product of the biologically active ceramic coating of different aperture, shape and size.
Above-mentioned purpose realizes by following technical scheme:
A kind of method of porous Ti biologically active ceramic coating, this method have three steps:
One: do the matrix pre-treatment with polishing of titanium bead surface and cleaning;
Two: do vacuum-sintering and handle that to insert vacuum after packing into the titanium pearl in the mould be 10 -3In the vacuum sintering furnace of Pa, heating is 2 hours under 1450 ℃ of constant temperature, with the stove air cooling, takes out behind the cool to room temperature then, and the titanium pearl forms the porous shape of nature overlap joint, is POROUS TITANIUM;
Three: do the differential arc oxidation processing POROUS TITANIUM is placed the stainless steel trough body that contains alkaline electrolyte, do anode with POROUS TITANIUM, stainless steel trough body is a negative electrode; By cooling system control flume liquid temp, control temperature＜50 in the oxidizing process oC; Adopt the bipolar pulse power supply, by the control to the differential arc oxidation electrical quantity, lean on the disruptive discharge on POROUS TITANIUM surface to make the POROUS TITANIUM surface form differential arc oxidation coating, differential arc oxidation coating thickness is at 3～10mm.
The method of described porous Ti biologically active ceramic coating, the pulse voltage of described differential arc oxidation is 200～600V, frequency 400～the 800Hz of described differential arc oxidation, the dutycycle 4～20% of described differential arc oxidation, the solution temperature 0～50 of described differential arc oxidation oC.
The method of described porous Ti biologically active ceramic coating, the composition of described alkaline electrolyte comprise that disodium ethylene diamine tetraacetate EDTA-2Na concentration is that 15 grams per liters, NaOH NaOH concentration are 20 grams per liters, sodium metasilicate Na 2SiO 39H 2O concentration is 14.2 grams per liters, calcium acetate Ca (CH 3COO) 2H 2O concentration 8.8 grams per liters, deionized water are as solvent; Or disodium ethylene diamine tetraacetate EDTA--2Na concentration is that 15 grams per liters, NaOH NaOH concentration are 15 grams per liters, calcium dihydrogen phosphate Ca (H 2PO 4) 2H 2O concentration is 6.3 grams per liters and calcium acetate Ca (CH 3COO) 2H 2O concentration is 13.2 grams per liters, is solvent dilution to a liter with the deionized water.
The method of described porous Ti biologically active ceramic coating, described differential arc oxidation is introduced the method for micro-silicon Si, phosphorus P, the described porous Ti biologically active of calcium Ca. ceramic coating in preparing coating, described POROUS TITANIUM is made the titanium pearl mixture that the raw material that adopted are of a size of the titanium pearl of diameter 100 or diameter 200 or diameter 300 or diameter 400 or diameter 500 or diameter 600mm or diameter 100, diameter 200, diameter 300, diameter 400, diameter 500, diameter 600mm.
Beneficial effect:
The POROUS TITANIUM of the different aperture of the present invention's preparation, and at the oxidation ceramic layer of its surface preparation one deck biologically active, can strengthen the binding ability of implant and bone tissue then, and can improve the biologically active of implant surfaces, having avoided the long-term shortcoming of in the body fluid environment, being on active service and causing metallic surface corrosion and metal ion to enter injected organism tissue and injected organism tissue is gone bad.
2. the coating after the present invention handles embodiment 8 is carried out energy disperse spectroscopy EDS spectroscopy detection, the existence of sodium Na, silicon Si, calcium Ca trace active element is arranged in the coating, silicon Si, calcium Ca element is the indispensable element in the bioactivity glass, by differential arc oxidation method with silicon Si, calcium Ca element is incorporated in the ceramic coating simultaneously and still belongs to the first time, and can make the coating material of titanium dioxide can have the performance of part biological activity glass.Simulated body fluid soaks, soaking to observe at coating surface with ESEM and X-ray energy spectrometer XRD later in 3 days promptly has hydroxyapatite to form, can see the hydroxyapatite that the surface forms when reaching once all above naked eyes, later observation increases hydroxyapatite formation quantity with soak time and also increases, and apatite formation quantity reaches capacity more than one month.Show in actual applications, can significantly improve the biologically active of Ti material by the inventive method arc oxide covering.
Coating after the present invention handles embodiment 9 is carried out energy disperse spectroscopy EDS spectroscopy detection, and the existence of sodium Na, phosphorus P, calcium Ca trace active element is arranged in the coating.The necessary element that P, Ca element hydroxyapatite form, the introducing of these two kinds of elements can remedy the coating surface shortcoming of Ca, P scarcity in vivo, is unfavorable for the formation of hydroxyapatite.The present invention is soaked at simulated body fluid by the coating of the specific embodiment 4 preparations, soaking to observe at coating surface with ESEM and X-ray energy spectrometer XRD later in 3 days promptly has hydroxyapatite to form, can see the hydroxyapatite that the surface forms when reaching once all above naked eyes, later observation increases hydroxyapatite formation quantity with soak time and also increases, and apatite formation quantity reaches capacity more than one month.Show in actual applications, can significantly improve the biologically active of titanium Ti material by the inventive method arc oxide covering.
The present invention significantly improves the surface bioactive of POROUS TITANIUM, has expanded the range of application of POROUS TITANIUM as optimal bone substitute.
Description of drawings:
Accompanying drawing 1 is the structural representation of titanium bead surface among the present invention.
Accompanying drawing 2 is structural representations of vacuum-sintering POROUS TITANIUM among the present invention.
Accompanying drawing 3 is structural representations of POROUS TITANIUM surface by micro-arc oxidation coating in the accompanying drawing 1.
The specific embodiment:
Embodiment 1:
A kind of method of porous Ti biologically active ceramic coating, this method have three steps:
One: do the matrix pre-treatment with polishing of titanium bead surface and cleaning;
Two: do vacuum-sintering and handle that to insert vacuum after packing into the titanium pearl in the mould be 10 -3In the vacuum sintering furnace of Pa, heating is 2 hours under 1450 ℃ of constant temperature, with the stove air cooling, takes out behind the cool to room temperature then, and the titanium pearl forms the porous shape of nature overlap joint, is POROUS TITANIUM;
Three: do the differential arc oxidation processing POROUS TITANIUM is placed the stainless steel trough body that contains alkaline electrolyte, do anode with POROUS TITANIUM, stainless steel trough body is a negative electrode; By cooling system control flume liquid temp, control temperature＜50 in the oxidizing process oC; Adopt the bipolar pulse power supply, by the control to the differential arc oxidation electrical quantity, lean on the disruptive discharge on POROUS TITANIUM surface to make the POROUS TITANIUM surface form differential arc oxidation coating, differential arc oxidation coating thickness is at 3～10mm.
Embodiment 2:
The method of embodiment 1 described porous Ti biologically active ceramic coating, the pulse voltage of described differential arc oxidation is 200～600V, frequency 400～the 800Hz of described differential arc oxidation, the dutycycle 4～20% of described differential arc oxidation, the solution temperature 0～50 of described differential arc oxidation oC.
Embodiment 3:
The method of embodiment 1 or 2 described porous Ti biologically active ceramic coatings, the proportioning of described alkaline electrolyte comprise that disodium ethylene diamine tetraacetate EDTA-2Na concentration is that 15 grams per liters, NaOH NaOH concentration are 20 grams per liters, sodium metasilicate Na 2SiO 39H 2O concentration is 14.2 grams per liters, calcium acetate Ca (CH 3COO) 2H 2O concentration 8.8 grams per liters, deionized water are solvent dilution to a liter.
Embodiment 3:
The method of embodiment 1 or 2 described porous Ti biologically active ceramic coatings, described differential arc oxidation is introduced micro-silicon Si, phosphorus P, calcium Ca. in the preparation coating, the ceramic of compact layer that is obtained contains useful silicon Si, calcium Ca, the phosphorus P trace element of body bone tissue growth, the generation of inducing hydroxyapatite in simulated body fluid that can success helps to improve implant binding ability with bone tissue of POROUS TITANIUM matrix alternative.
Described POROUS TITANIUM is made the titanium pearl mixture that the raw material that adopted are of a size of the titanium pearl of diameter 100 or diameter 200 or diameter 300 or diameter 400 or diameter 500 or diameter 600mm or diameter 100, diameter 200, diameter 300, diameter 400, diameter 500, diameter 600mm.
Embodiment 4:
The method of above-mentioned porous Ti biologically active ceramic coating adopts alkaline electrolyte, and as anode, stainless steel is as negative electrode with the POROUS TITANIUM of the different porosities of vacuum high-temperature sintering.Energy in the oxidizing process is provided by adjustable high voltagehigh frequency bipolar pulse power supply, and pulse parameter is voltage 200 ~ 600V, frequency 400 ~ 800Hz, dutycycle 4 ~ 10%.When applied voltage surpasses when placing the critical voltage of electrolyte POROUS TITANIUM surface insulating film, the spark discharge that piece surface produces is with the oxidation of POROUS TITANIUM matrix and form fine and close TiO 2Oxide coating by the composition of control electrolyte, can make the oxidizing process of the helpful trace element of live body by material be introduced in the oxide layer surface and go, and follow-uply can successfully induce the hydroxyapatite deposition by immersing in the simulated body fluid on the oxide layer surface.The TiO of this technology preparation 2Ceramic layer has excellent corrosion-resistant, rub resistance and biologically active, greatly expand POROUS TITANIUM as the range of application in the human body hard tissue alternative, thereby the present invention has important economy and using value.
Embodiment 5:
The method of described porous Ti biologically active ceramic coating:
Step 1: the titanium pearl is handled: choose the different pure titanium pearl of particle diameter, cleaning, oil removing;
Step 2: vacuum-sintering: the titanium pearl is packed in the mould, and putting into vacuum is＜10 -3In the vacuum sintering furnace of Pa, 1450 ℃ of heated at constant temperature 2h with the stove air cooling, take out behind the cool to room temperature then, and the titanium pearl forms the porous shape of nature overlap joint, is POROUS TITANIUM 2;
Step 3: differential arc oxidation: POROUS TITANIUM is placed the stainless steel trough body that contains alkaline electrolyte, do anode with POROUS TITANIUM, stainless steel trough body is a negative electrode; Pass through cooling system control flume liquid temp＜50 in the oxidizing process oC; Adopt the bipolar pulse power supply, by the control to the differential arc oxidation electrical quantity, lean on the disruptive discharge on POROUS TITANIUM surface to make POROUS TITANIUM surface 2 form differential arc oxidation coatings 3, differential arc oxidation coating 3 THICKNESS CONTROL are at 3～10mm.
Embodiment 6:
The method of the described porous Ti biologically active of above embodiment ceramic coating, present embodiment with implement that 3 differences are that the titanium bead that is adopted in step 1 and the step 2 directly is respectively 100,200,300,400 ~ 600mm one or more be mixed and clean and sintering.
Embodiment 7:
The method of the described porous Ti biologically active of above embodiment ceramic coating, present embodiment and embodiment 5 differences are that the energy of the differential arc oxidation process in the step 3 is provided by adjustable high voltagehigh frequency bipolar pulse power supply, and pulse voltage is 200～600V, frequency 400～800Hz, dutycycle 4～20%, solution temperature 0～50oC.In above-mentioned selected differential arc oxidation electrical quantity, differential arc oxidation 5-20 minute, the thickness of coating can reach 3 ~ 10 microns.Other step is identical with the specific embodiment 1.
Embodiment 8:
The method of the described porous Ti biologically active of above embodiment ceramic coating, present embodiment carries out differential arc oxidation with the embodiment 5 different step 3 that are to POROUS TITANIUM 2, and its step is as follows: POROUS TITANIUM is placed contain EDTA-2Na, NaOH, Na 2SiO 39H 2O and Ca (CH 3COO) 2H 2O(concentration is decided to be 15 grams per liters, 20 grams per liters, 14.2 grams per liters and 8.8 grams per liters respectively) be that solvent is mixed with in the stainless steel trough body of electrolyte with the deionized water, the adjusting power source voltage is that 500V, dutycycle are 8%, frequency is that 600Hz, oxidization time are 5min, make the POROUS TITANIUM surface form differential arc oxidation coating 3, thickness is 3 ~ 10mm.
Embodiment 9:
The method of the described porous Ti biologically active of above embodiment ceramic coating, present embodiment and embodiment 7 different are that mixture kind and quantity that step 3 adds are different, and admixture is EDTA--2Na, NaOH, Ca (H 2PO 4) 2H 2O and Ca (CH 3COO) 2H 2O concentration is that solvent is mixed with in the stainless steel trough body of electrolyte with the deionized water for (concentration is decided to be 15 grams per liters, 15 grams per liters, 6.3 grams per liters and 13.2 grams per liters respectively), the adjusting power source voltage is that 400V, dutycycle are 8%, frequency is that 600Hz, oxidization time are 5min, make the POROUS TITANIUM surface form differential arc oxidation coating 3, thickness is 3 ~ 10mm.

Claims (4)

1. the method for a porous Ti biologically active ceramic coating, it is characterized in that: this method has three steps:
One: do the matrix pre-treatment with polishing of titanium bead surface and cleaning;
Two: do vacuum-sintering and handle that to insert vacuum after packing into the titanium pearl in the mould be 10 -3In the vacuum sintering furnace of Pa, heating is 2 hours under 1450 ℃ of constant temperature, with the stove air cooling, takes out behind the cool to room temperature then, and the titanium pearl forms the porous shape of nature overlap joint, is POROUS TITANIUM;
Three: do the differential arc oxidation processing POROUS TITANIUM is placed the stainless steel trough body that contains alkaline electrolyte, do anode with POROUS TITANIUM, stainless steel trough body is a negative electrode; By cooling system control flume liquid temp, control temperature＜50 in the oxidizing process oC; Adopt the bipolar pulse power supply, by the control to the differential arc oxidation electrical quantity, lean on the disruptive discharge on POROUS TITANIUM surface to make the POROUS TITANIUM surface form differential arc oxidation coating, differential arc oxidation coating thickness is at 3～10mm.
2. the method for porous Ti biologically active ceramic coating according to claim 1, it is characterized in that: the pulse voltage of described differential arc oxidation is 200～600V, frequency 400～the 800Hz of described differential arc oxidation, the dutycycle 4～20% of described differential arc oxidation, the solution temperature 0～50 of described differential arc oxidation oC.
3.. the method for porous Ti biologically active ceramic coating according to claim 1 and 2 is characterized in that: the composition of described alkaline electrolyte comprises that disodium ethylene diamine tetraacetate EDTA-2Na concentration is that 15 grams per liters, NaOH NaOH concentration are 20 grams per liters, sodium metasilicate Na2SiO 39H 2O concentration is 14.2 grams per liters, calcium acetate Ca (CH 3COO) 2H 2O concentration 8.8 grams per liters, deionized water are as solvent; Or disodium ethylene diamine tetraacetate EDTA--2Na concentration is that 15 grams per liters, NaOH NaOH concentration are 15 grams per liters, calcium dihydrogen phosphate Ca (H 2PO 4) 2H 2O concentration is 6.3 grams per liters and calcium acetate Ca (CH 3COO) 2H 2O concentration is 13.2 grams per liters, is solvent with the deionized water.
4.. the method for porous Ti biologically active ceramic coating according to claim 1 and 2 is characterized in that: described differential arc oxidation is introduced micro-silicon Si, phosphorus P, calcium Ca in the preparation coating; Described POROUS TITANIUM is made the titanium pearl mixture that the raw material that adopted are of a size of the titanium pearl of diameter 100 or diameter 200 or diameter 300 or diameter 400 or diameter 500 or diameter 600mm or diameter 100, diameter 200, diameter 300, diameter 400, diameter 500, diameter 600mm.
CN2010105962264A 2010-12-20 2010-12-20 Method for preparing bioactive ceramic coating on surface of porous titanium Pending CN102039408A (en)

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CN102526800A (en) * 2012-01-05 2012-07-04 哈尔滨工业大学 Method for uploading cefazolin sodium medicine film on micro-arc oxidation titanium implant
CN102560597A (en) * 2012-01-05 2012-07-11 哈尔滨工业大学 Method for preparing high bioactivity titanium dioxide coating containing nano-crystalline grains
CN102560599A (en) * 2012-02-09 2012-07-11 常州大学 Preparation method for in-situ growth of oxide film on titanium alloy surface
CN103147111A (en) * 2013-03-25 2013-06-12 邹智群 Pure-titanium micro-arc oxidation coating and application thereof
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CN103320840A (en) * 2013-07-09 2013-09-25 昆明冶金研究院 Titanium alloy anodic oxidation alkaline electrolyte and preparation technique of color film layer
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CN110528048A (en) * 2019-08-30 2019-12-03 广东省新材料研究所 A kind of titanium alloy implant Bio-surface active coating and preparation method thereof
CN111330071A (en) * 2020-02-25 2020-06-26 北京爱康宜诚医疗器材有限公司 Antibacterial three-dimensional porous bone implant material

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