CN101591759B - Method for preparing hydroxylapatite coating by microplasma spraying - Google Patents
Method for preparing hydroxylapatite coating by microplasma spraying Download PDFInfo
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Abstract
The invention discloses a method for preparing a hydroxylapatite coating by microplasma spraying, which belongs to the field of implant processing and preparation in biomedical material engineering. The method adopts microplasma spraying equipment to spray dried hydroxylapatite powder onto a matrix of a biomedical implant metal material with the surface subjected to sand blasting treatment, thereby obtaining the hydroxylapatite coating with controllable crystallinity and good biological stability. The preparation of the coating by the method has simple process, and the hydroxylapatite powder has high deposition efficiency. The method can be used for depositing the hydroxylapatite coating on the surfaces of inert implant metal materials such as stainless steel, cobalt-based alloy, titanium and titanium alloy to make the surfaces of biologically inert metal matrixes biologically activated to prepare medical implant devices such as dental roots, artificial joints and the like.
Description
Technical field
The invention belongs to the biological and medicinal implant material preparing technical field, be specifically related to adopt a kind of microplasma spraying method hydroxyapatite coating layer.
Background technology
Nearly 10 for many years, the growth rate of market of global bio-medical material and goods remains on about 20%-25% always, as the highest hi tech and new material of a class technical value added, estimate in following 10 years-15 years, the medical apparatus industry that comprises bio-medical material will reach the pharmaceutical products market scale, the market requirement is big, and development potentiality is big and profit is big, becomes the mainstay industry of 21 century world economy.
(hydroxyapatite HA) is a kind of biological active ceramic material of being used widely to hydroxyapatite.Its feature is: do not produce fibrous tissue when combining at the interface with green bone, their surface can with physiological environment generation selection chemical reaction, implant can be protected in formed interface.With tissue reach key and, to nontoxic, harmless, the no carcinogenesis of animal body, biocompatibility is splendid.Hydroxyapatite is as artificial dental root, artificial bone, and the novel material of prevention of dental caries agent has obtained to use on clinical medicine.With nature person's bone, people's tooth (enamel and ivory) relatively, simple HA sintered compact compressive strength, tensile strength and Young's modulus are bigger, yet dynamic or static bending intensity is very low, fracture toughness property only is the 1/70-1/40 of titanium alloy, fatigue resistance is poor in physiological environment, and the Wei Boolean coefficient only is 12.Therefore hydroxyl apatite bioceramic only limits to the not position of load.K.de.Groot in 1986 and J.F.Kay utilize plasma spraying technology successfully to deposit hydroxyapatite coating layer at biomaterial surface respectively, and China also carried out research in this field from 1988, have used with clinical.This method has overcome the fragility of hydroxyapatite bioactive pottery and the biologically inert problem of metallic substance, repairs embedded material but become a kind of bearing hard tissue.At present, hydroxyapatite coating layer is mainly used in artificial dental root, articular bone handle, Steel Plate For Fixation Of Fracture and artificial bone etc.
Yet also there are some problems in atmospheric plasma spraying technology in application.At first, the temperature of the ion flame of traditional atmospheric plasma thermospray stream is between 2000-20000K, and arc center top temperature can reach 32000K, and spraying back HA powder can take place to change mutually, can comprise crystalline state HA in the coating, calcium phosphate crystal and amorphous HA.This be because, HA can lose hydroxyl between 1200-1400 ℃, 1300 ℃ of left and right sides hydroxyls all disappear, and generate oxygen calcium phosphate.Along with temperature raises, powder further decomposes.Therefore, the plasma spraying of extreme temperatures easily makes HA decompose, and dissolving too early easily takes place behind the implantable bioartificial body peel off, and can not play the effect of inducing the osseous tissue growth, and the work-ing life of material is short.The second, traditional air plasma spraying consumed power is between 40-200kW, and the useful energy that is actually used in the powder heating only accounts for the 10-20% of total power, and the sedimentation effect of powder is low, has only 20-50%, and powder using efficiency is low.And when preparation HA coating, need adopt expensive highly purified HA powder as raw material, caused huge waste.
Comparatively speaking, adopt the decline flame stream of bundle plasma spraying of the outer powder feeding of lower powered external detachable anodic to be laminar flow, power is 1-2kW, and the speed of plasma arc is low.Can reduce the thermolysis of crossing of powder, effectively improve the degree of crystallinity of coating; And the anodic diameter is very little, and the powder using efficiency height has reduced the waste of powder.Be fit to spraying HA coating, the surface modified coat of preparation bio-medical implant.
Summary of the invention
The object of the present invention is to provide a kind of method that adopts microplasma spraying to prepare hydroxyapatite coating layer.Use the hydroxyapatite coating layer of method preparation provided by the invention, have good biologically stable and biological activity when having the good mechanical performance, coating degree of crystallinity is controlled, and the powder using efficiency height has been saved the energy.
Provided by the present inventionly a kind ofly prepare the method for hydroxyapatite coating layer, may further comprise the steps with microplasma spraying:
Particle diameter after employing microplasma spraying equipment will be dried is that the hydroxyapatite powder of 28-53 μ m sprays to the surface through on the metal material embedded matrix of sandblasting bio-medical, spraying parameter is: flame stream power is 1-2kW, and working current is 35-60A; Gun pendulum speed is 150-3900mm/s, spray distance 70-100mm; Work gas is that helium is argon-mixed, and the volume ratio of helium and argon gas is 1: 1, working air current amount 1.0-1.2L/min; Protection gas is the argon-mixed or argon gas of helium, protection airshed 0.4-0.5L/min; Powder feeding gas is the argon-mixed or argon gas of helium, powder feeding gas flow 4-5L/min; Powder feeding rate 0.05-0.50g/min.
The present invention has following beneficial effect:
The powder using efficiency of method provided by the present invention is between 70-90%, and the bonding strength between coating and matrix can reach 35.6MPa, and is controlled between the degree of crystallinity 65-85%, biological activity is good, good stability can not come off in simulated body fluid in long-time immersion, can be used as the coating of artificial growth body.
The invention will be further described below in conjunction with embodiment.
Embodiment
Employed hydroxyapatite powder is the commercial goods among the subordinate embodiment.The hydroxyapatite powder particle diameter is 28-53 μ m, the spraying before in stoving oven 120 ℃ the oven dry 3h.Body material is the biological medical titanium alloy through sandblasting.
Embodiment 1: adopt the microplasma spraying system that the hydroxyapatite powder is sprayed on the matrix, spraying parameter is: work gas is the argon helium gas mixture, the volume ratio of helium and argon gas is 1: 1, working air current amount 1.0L/min, protection gas is industrial straight argon, protection airshed 0.5L/min, powder feeding gas is industrial straight argon, powder feeding gas flow 4L/min, powder feeding rate 0.05g/min, working current 40A, gun pendulum speed 150mm/min, stepping 2mm, spraying number of times 3 times, spray distance 80mm, obtaining coat-thickness is 50 μ m; Powder using efficiency 90%, degree of crystallinity are 85%.
Embodiment 2: adopt the microplasma spraying system that the hydroxyapatite powder is sprayed on the matrix, spraying parameter is: work gas is the argon helium gas mixture, the volume ratio of helium and argon gas is 1: 1, working air current amount 1.1L/min, protection gas is the argon helium gas mixture, protection airshed 0.4L/min, powder feeding gas is the argon helium gas mixture, powder feeding gas flow 5L/min, powder feeding rate 0.10g/min, working current 35A, gun pendulum speed 600mm/min, stepping 3mm, spraying number of times 2 times, spray distance 70mm, obtaining coat-thickness is 20 μ m; Powder using efficiency 74%, degree of crystallinity are 79%.
Embodiment 3: adopt the microplasma spraying system that the hydroxyapatite powder is sprayed on the matrix, spraying parameter is: work gas is the argon helium gas mixture, the volume ratio of helium and argon gas is 1: 1, working air current amount 1.2L/min, protection gas is the argon helium gas mixture, protection airshed 0.4L/min, powder feeding gas is the argon helium gas mixture, powder feeding gas flow 5L/min, powder feeding rate 0.50g/min, working current 60A, gun pendulum speed 3900mm/min, stepping 2mm, spraying number of times 3 times, spray distance 100mm, obtaining coat-thickness is 100 μ m; Powder using efficiency 70%, degree of crystallinity are 65%.
Embodiment 4: adopt the air plasma spraying system that the hydroxyapatite powder is sprayed on the matrix, spraying parameter is: work gas is industrial straight argon, working air current amount 41L/min; Auxiliary gas is helium, substreams amount 8L/min; Protection gas is industrial straight argon, protection airshed 8L/min; Powder feeding rate 18g/min, electric current 600A, gun pendulum speed 500mm/min, stepping 4mm, spraying number of times 3 times, spray distance 100mm, obtaining coat-thickness is 100 μ m; Powder using efficiency 43%, degree of crystallinity are 52%.
As can be seen from the above embodiments, compare with traditional air plasma spraying method, the microplasma spraying method prepares the powder using efficiency height of hydroxyapatite coating layer, can save cost.The coating degree of crystallinity height of preparation does not need aftertreatment, and biologically stable is good.
Claims (1)
1. one kind prepares the method for hydroxyapatite coating layer with microplasma spraying, it is characterized in that, may further comprise the steps:
Particle diameter after employing microplasma spraying equipment will be dried is that the hydroxyapatite powder of 28-53 μ m sprays on the matrix, and spraying parameter is: working current is 35-60A; Gun pendulum speed is 150-3900mm/min, spray distance 70-100mm; Work gas is that helium is argon-mixed, and the volume ratio of helium and argon gas is 1: 1, working air current amount 1.0-1.2L/min; Protection gas is the argon-mixed or argon gas of helium, protection airshed 0.4-0.5L/min; Powder feeding gas is the argon-mixed or argon gas of helium, powder feeding gas flow 4-5L/min; Powder feeding rate 0.05-0.50g/min.
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| CN101591759B true CN101591759B (en) | 2011-05-25 |
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| CN105018924B (en) * | 2014-11-14 | 2017-12-26 | 中国兵器工业第五二研究所 | A kind of preparation method of titanium alloy substrate hydroxyapatite coating on surface |
| WO2019112001A1 (en) * | 2017-12-08 | 2019-06-13 | 富田製薬株式会社 | Plasma spray material |
| CN112176272B (en) * | 2020-09-09 | 2022-03-01 | 西南科技大学 | Method for preparing hydroxyapatite coating by plasma spraying |
| CN116590715A (en) * | 2023-07-12 | 2023-08-15 | 德州正瑞健康科技有限公司 | Method and equipment for pickling surface of plant |
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| CN101186999A (en) * | 2007-12-07 | 2008-05-28 | 华北电力大学 | Method for preparing ceramic-metal composite material cladding layer |
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| CN101186999A (en) * | 2007-12-07 | 2008-05-28 | 华北电力大学 | Method for preparing ceramic-metal composite material cladding layer |
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| 赵秋颖，等.微束等离子喷涂制备羟基磷灰石涂层.《焊接学报》.2008,第29卷(第3期),第137页. * |
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