CN101250682B - Injection type plasma spraying device for producing hydroxyapatite bioactivity coating - Google Patents
Injection type plasma spraying device for producing hydroxyapatite bioactivity coating Download PDFInfo
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- CN101250682B CN101250682B CN2008100450671A CN200810045067A CN101250682B CN 101250682 B CN101250682 B CN 101250682B CN 2008100450671 A CN2008100450671 A CN 2008100450671A CN 200810045067 A CN200810045067 A CN 200810045067A CN 101250682 B CN101250682 B CN 101250682B
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Abstract
The invention relates to a suspending liquid injection type plasma spraying device which prepares hydroxyapatite bioactive coating and comprises a plasma ejection gun and also comprises a spraying raw material suspending liquid storage container, a suspending liquid transmission system and a suspending liquid injection system, wherein the suspending liquid storage container is a pressure tank or a container which is provided with the high energy ultrasonic oscillation function, the transmission system comprises a power transmitting device and a transmitting tube which is matched with the power transmitting device, a duct with small diameter in the injection system is installed on a holder which is connected with the plasma ejection gun through a regulating component, compressed air in the pressure tank in the power transmitting device or an electronic peristaltic pump injects the suspending liquid into the duct with the small diameter through the transmitting tube, the duct with the small diameter injects the suspending liquid to a high temperature region on the center of plasma flame directly and radially in a leaner type jet-flow mode, the hydroxyapatite bioactive coating with even structure is generated on the surface of a metal base, and the device of the invention is simple in structure and easy in operation, and saves the raw materials.
Description
Technical field
The present invention relates to a kind of injection type plasma spraying device for preparing hydroxyapatite bioactive coating, be particularly related to a kind of suspension injection type plasma spraying new device for preparing hydroxyapatite bioactive coating, belong to bio-medical material engineering apparatus field.
Background technology
Hydroxyapatite have with tissue bone and tooth in similar chemical constitution and the crystalline structure of main mine material, be the main inorganic composition of skeleton tissue.The hydroxyapatite superior bioactive can combine it with skeleton tissue formation chemical combination key simultaneously, has good osteoconductive; And new bone growth had certain inducing action, be the biological active materials of a quasi-representative.Yet simple hydroxyapatite mechanical property is relatively poor, its bending strength and fracture toughness property index all are lower than the human body dense bone, be difficult to use at organism carrying position, has the biological implantation material that deposition one deck hydroxyapatite coating layer obtains having good over-all properties on the medical metal material matrix of biologically inert, make its intensity with base metal and toughness, also have the good biological activity and the biocompatibility of hydroxyapatite.
At present, the technology of preparation hydroxyapatite coating layer is a lot, mainly contains plasma spraying, ion beam sputtering, electrophoretic deposition, sol-gel processing, bionical solution growth method etc.In the equipment that these preparation methods use, the preparation hydroxyapatite bioactive coating uses plasma spraying equipment usually.Because plasma spraying technology, the employing plasma arc is a thermal source, all with metal or non-metal solid powder as raw material, behind fusion or semi-melting state, high-velocity jet is on treated metal substrate surface and form top coat through the high-temperature plasma flame heating for used powder stock.The process of using existing pressed powder plasma spray apparatus to prepare hydroxyapatite bioactive coating generally is, the pressed powder spraying raw material is placed the feeder of this device, various ways such as that feeder has is funneling, spiral, oscillatory type, tipping bucket type, powder stock in the feeder is sent to the other powder jet of plasma gun through piping under the effect of pressure, be directly injected to the plasma flame from powder jet then.The required powder stock of powder plasma spraying generally will synthesize through wet chemistry method, ageing, spraying drying, powder granulation nodularization, calcining, pulverize, ball milling, a series of loaded down with trivial details process procedures such as sub-sieve, the execution cycle need be gone through 4-7 days time usually, this has not only increased cost, has also reduced production efficiency.In addition, the conventional powder plasma spray apparatus also exists the uneven problem of coating structure that makes.For solving the problem that exists in the existing pressed powder plasma spray apparatus, this purpose of the present invention just.
Summary of the invention
Purpose of the present invention then is at existing defective in the described existing plasma spray apparatus, is intended to propose a kind of plasma gun that comprises, metal base and substrate anchor thereof; Further comprise spraying raw material suspension storage vessel, suspension transfer system, the suspension injection type plasma spraying new device of the preparation hydroxyapatite bioactive coating of suspension injected system.Described device by the transmission power set in the transfer system with its transmission medium of being connected of being complementary suspension directly is sent to small diameter catheter in the injected system; Small diameter catheter is directly radially injected the high-temperature area at plasma flame center with suspension with the linear pattern mode of jet again, at metal substrate surface generating structure uniform hydroxylapatite bioactive coating; Apparatus of the present invention are simple in structure, easy handling, and economize in raw materials.
For realizing above-mentioned purpose of the present invention, the technical scheme that the present invention's employing is made of following technical measures realizes.
The present invention prepares the suspension injection type plasma spraying device of hydroxyapatite bioactive coating, comprises plasma gun, metal base and substrate anchor thereof; It is characterized in that also comprising plasma spraying stock suspension storage vessel, suspension transfer system, suspension injected system; Wherein said suspension transfer system comprise transmit power set with its transmission medium that is complementary and is connected, transmission medium one end is communicated with the transmission power set, the other end is communicated with injected system; One small diameter catheter is set in the described injected system, and small diameter catheter is installed on plasma gun by adjustment means and is complementary on the permanent seat that is connected; Suspension in the storage vessel is transported to small diameter catheter in the injected system by transmitting power set and transmission medium, small diameter catheter is directly radially injected the high-temperature area at plasma flame center with the linear pattern mode of jet, at metal substrate surface generating structure uniform hydroxylapatite bioactive coating.
In the technique scheme, described suspension storage vessel or in Plasma Spraying Process Using, in real time particle in the suspension being carried out the container of dispersive band high-energy ultrasound oscillation functions; Or be pressure-pot.
In the technique scheme, transmit power set in the described suspension transfer system or be electronic peristaltic pump; Or for importing compressed-air actuated pressure-pot; Electronic peristaltic pump is connected with the suspension injected system by the container of transmission medium with band high-energy ultrasound oscillation functions; Pressure-pot also is connected with the suspension injected system by transmission medium.
In the technique scheme, the transmission medium that connects electronic peristaltic pump or connection pressure-pot in the described suspension transfer system is a pressure piping;
In the technique scheme, the pressure piping that described electronic peristaltic pump is connected with injected system is provided with check valve that makes suspension arrive injected system smoothly and the under meter of doing indication; Or also being provided with check valve on pressure-pot and the pressure piping that injected system is connected, flow is taken into account the valve that may command opens and closes.
In the technique scheme, the transfer rate that described transmission power set electronic peristaltic pump uses is 10-100ml/min.
In the technique scheme, the gas of input is pressurized air in the described transmission power set pressure-pot, and the pressure in the pressure-pot is 0.15-0.6Mpa.
In the technique scheme, the internal diameter of described small diameter catheter is the 50-300 micron.
In the technique scheme, the be complementary permanent seat that is connected of described and plasma gun size can be regulated the relative angle of permanent seat and plasma gun by the rotating mechanism that nut screw constitutes.
In the technique scheme, described suspension injection type plasma spraying device, it is characterized in that installing on the described permanent seat horizontal adjustment support, regulating support is connected with the adjusting slider coupling that threaded hole is opened at the center, regulating sleeve pipe is connected with adjusting slider by threaded hole, small diameter catheter is installed on the catheter holder of regulating the sleeve pipe below, move horizontally adjusting slider and can regulate the distance of small diameter catheter and plasma spray muzzle, the rotary regulating sleeve pipe can be regulated small diameter catheter and plasma flame distance.
Suspension storage vessel of the present invention is meant the used special container of hydroxyapatite suspension that has prepared, because in order to obtain higher deposition efficiency, prepared suspension need have higher concentration, make its viscosity often higher like this, therefore hydroxyapatite content is bigger in the unit volume, simultaneously because the interaction between individual particles, the macrobead that is agglomerated into " cluster " shape easily stops up plasma nozzle, so the container of the band ultrasonic wave high energy of one of suspension storage vessel that the present invention adopts concussion disperses suspension particle, in the process of spraying, carry out real-time high-energy ultrasound concussion whole spraying process is carried out smoothly.
Suspension transfer system of the present invention has comprised transmission power set and corresponding transmission medium, wherein transmitting power set adopts electronic peristaltic pump or adopts input pressurized air in the pressure-pot to realize transmission to suspension, use the pressure piping that mates mutually with the transmission power set as corresponding transmission medium, suspension is directly sent into small diameter catheter in the injected system, whole spraying process is carried out smoothly.
Utilize this device to prepare the method for hydroxyapatite bioactive coating, comprise following processing step:
(1) preparation of hydroxyapatite suspension
Press calcium phosphorus mol ratio 1.67, the configuration volumetric molar concentration is that calcium nitrate aqueous solution and the volumetric molar concentration of 0.5-2.5mol/L is the ammonium dibasic phosphate aqueous solution of 0.5-3mol/L; Under constantly stirring, the ammonium dibasic phosphate aqueous solution of configuration is added drop-wise in the calcium nitrate aqueous solution with 5-15ml/min speed and reacts, and then the ammoniacal liquor of percentage concentration 10%-30% is added drop-wise in the reaction solution with 1-10ml/min speed, the control reacting liquid pH value is 9-12, keep temperature of reaction at 30-90 ℃, treat complete reaction after, left standstill 5-15 minute, ageing 24-48 hour again, it was standby promptly to make hydroxyapatite suspension;
(2) transmission of hydroxyapatite suspension
A) or with the hydroxyapatite suspension for preparing place a pressure-pot, pressurized air is fed in the pressure-pot, making pressure wherein is malleation, utilize this malleation as transmitting power, with hydroxyapatite suspension by being sent in the suspension injected system with the pressure-pot dispatch tube that is connected that is complementary;
B) or the hydroxyapatite suspension for preparing is placed the container of a band high-energy ultrasound oscillation functions, utilize electronic peristaltic pump as transmitting power set, with hydroxyapatite suspension by being sent in the suspension injected system with the electronic peristaltic pump dispatch tube that is connected that is complementary;
(3) injection of hydroxyapatite suspension
Adopt small diameter catheter the hydroxyapatite suspension for preparing directly radially to be injected the high-temperature area at plasma flame center in linear pattern effusive mode;
(4) generation of hydroxyapatite bioactive coating
With hydroxyapatite suspension is the plasma spraying raw material, makes base material with the bio-medical metal; By the preparation of step (1) to suspension, step (2) is to the injection to suspension of the transmission of suspension and step (3); The high-temperature plasma flame generation heat exchange that suspension and plasma gun eject, pass through evaporation of liquid in the suspension subsequently, particulate fragmentation, fusion and deposition are directly at bio-medical metal substrate surface generating structure uniform hydroxylapatite bioactive coating.
In the such scheme, described metal base is a biomedical titanium, or biological medical titanium alloy, or biological medical stainless steel, or the bio-medical cobalt base alloy.
The present invention compared with prior art has following useful technique effect:
1, suspension injection type plasma spraying device of the present invention, the preparation technology of used suspension raw material is simple, and easy handling does not need the loaded down with trivial details preparation technology through the used pressed powder raw material of conventional powder plasma spray apparatus.
2, suspension injection type plasma spraying device of the present invention, adopt small diameter catheter in its injected system, make suspension form high speed minor diameter liquid stream, this liquid stream directly injects the plasma flame high-temperature area, utilize the turbulent flow of plasma gas, flame formation, carry out original position refinement, dispersion to injecting suspension, and obtain good thinning effect, thereby make the structural uniformity of hydroxyapatite bioactive coating of spraying good.
3, suspension injection type plasma spraying device of the present invention, adopt small diameter catheter in its injected system, because it is very little to inject suspension liquid flow diameter, can directly accurately inject plasma flame height of center temperature area, guarantee that further spraying raw material all injects, this has not only improved the sedimentation effect of injection efficiency, the coating of spraying raw material, has also improved production efficiency, and has saved spraying raw material.
4, suspension injection type plasma spraying device of the present invention, adopt small diameter catheter in its injected system, because it is very little to inject suspension liquid flow diameter, all spraying raw material drops all can enter plasma flame height of center temperature area, thereby all drops all have similar heat exchanging process, thereby fundamentally guarantee to obtain the homogeneity of hydroxyapatite bioactive coating structure.
5, suspension injection type plasma spraying device of the present invention, the storage vessel of used suspension, transfer system, injected system all is in the isolated tightness system, thereby has realized the pollution-free transmission of spraying raw material, guarantees the quality of coating.
6, suspension injection type plasma spraying device of the present invention, can be in when operation by the distance of adjustment means and plasma flame and plasma gun, adjusting aspect the angle to realize the structure of change hydroxyapatite bioactive coating, has bigger commercial application prospect, while method is simple, processing ease, the efficient height.
7, suspension injection type plasma spraying device of the present invention is simple in structure, easy handling, and cost is low.
8, suspension injection type plasma spraying device of the present invention, if used spraying raw material has kept nanostructure to a great extent when adopting nano suspending liquid, can improve the performance of coating.
Description of drawings
Transmitting power set in Fig. 1 suspension injection type plasma spraying device of the present invention transfer system is the example structure synoptic diagram of electronic peristaltic pump;
Transmitting power set in Fig. 2 suspension injection type plasma spraying device of the present invention transfer system is the example structure synoptic diagram of pressure-pot;
Fig. 3 is the right TV structure synoptic diagram of suspension injected system among Fig. 1 and Fig. 2;
Fig. 4 is the main TV structure synoptic diagram of suspension injected system among Fig. 1 and Fig. 2.
Each code name implication among the figure: 1 electronic peristaltic pump, 2 pressure pipings, 3 hydroxyapatite suspension, the container of 4 band high-energy ultrasound oscillation functions, 5 plasma flames, 6 substrate anchors, 7 substrates, 8 plasma gunes, 9 injected systems, 10 check valves, 11 under meters, 12 valves, 13 tensimeters, 14 pressure-pots, 15 regulate sleeve pipe, 16 adjusting sliders, 17 regulate support, 18 catheter holders, 19 small diameter catheter, 20 nuts, 21 screws, 22 permanent seats.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing and with specific embodiment, but it only is used to illustrate concrete embodiments more of the present invention, and should not be construed as the qualification to protection domain of the present invention.
Among Fig. 1, the suspension storage vessel is the container 4 of band high-energy ultrasound oscillation functions, a joint that transmits power set electronic peristaltic pump 1 in the transfer system is connected by the interior spraying raw material hydroxyapatite suspension 3 of transmission medium pressure piping 2 and band high-energy ultrasound oscillation functions container, make in spraying process, high-energy ultrasound oscillator in the suspension storage vessel disperses suspension particle in real time, whole spraying process is carried out smoothly, the pressure piping 2 of another joint of electronic peristaltic pump by under meter 11 and check valve 10 are housed connected with the small diameter catheter 19 in the injected system 9, and small diameter catheter is installed in plasma gun 8 by adjustment means and is complementary on the permanent seat 22 that is connected.Realized the adjusting of small diameter catheter and plasma gun angle with respect to the rotation of plasma gun 8 by permanent seat.Make the direct effective diameter of suspension that injects small diameter catheter to the high-temperature area that is injected into plasma flame, suspension and high-temperature plasma flame generation heat exchange, and the evaporation of suspension liquid, a series of processes such as particulate fragmentation, fusion, deposition deposit to metal substrate surface generating structure uniform hydroxylapatite bioactive coating at last.
Among Fig. 2, the suspension storage vessel is a pressure-pot 14, transmitting power set in the transfer system then is the compressed-air actuated pressure-pot of input, valve 12 on the pressure-pot and tensimeter 13 are used for regulating and control the pressurized air by pressure piping 2 input pressure jars, hydroxyapatite suspension 3 in one end of transmission medium pressure piping 2 and the pressure-pot is connected, valve 12 is housed on the pressure piping, small diameter catheter 19 in the other end of under meter 11 and check valve 10 and the injected system 9 is connected, and small diameter catheter is installed in plasma gun 8 by adjustment means and is complementary on the permanent seat 22 that is connected.Realized the adjusting of small diameter catheter and plasma gun angle aspect with respect to the rotation of plasma gun 8 by permanent seat 22.Make the direct effective diameter of suspension that injects small diameter catheter to the high-temperature area that is injected into plasma flame, suspension and high-temperature plasma flame generation heat exchange, and the evaporation of suspension liquid, a series of processes such as particulate fragmentation, fusion, deposition deposit to metal substrate surface generating structure uniform hydroxylapatite bioactive coating at last.
Among Fig. 3, the size of permanent seat 22 by nut 20 screws 21 and plasma gun 8 is complementary and is connected and fixed in the described injected system 9, and permanent seat is regulated by the rotating mechanism that supporting nut 20 screws 21 constitute, one horizontal adjustment support 17 is installed on the permanent seat, regulate support and be connected, and adjusting slider 16 can regulated support 17 upper edge horizontal throws slips with adjusting slider 16 couplings that the center has threaded hole; In the centre hole of adjusting slider, insert one and can in axial direction regulate the adjusting sleeve pipe 15 of the distance of small diameter catheter and plasma flame, adjusting slider passes through the connecting thread axial adjustment with the adjusting sleeve pipe, installs and fixes the catheter holder 18 of small diameter catheter 19 below the adjusting sleeve pipe.Move on adjusting support 17 by along continuous straight runs adjusting slider 16, and the distance of regulating small diameter catheter and plasma spray muzzle has realized the adjusting of small diameter catheter and plasma gun angle aspect with respect to the rotation of plasma gun 8 by permanent seat 22.Make the direct effective diameter of suspension that injects small diameter catheter to the high-temperature area that is injected into plasma flame, deposit to metal substrate surface generating structure uniform hydroxylapatite bioactive coating at last.
Among Fig. 4, the rotating mechanism that constitutes by nut 20 screws 21 and adjusting support 17 in the described injected system 9, the angle that can regulate small diameter catheter and flame; Adjusting slider 16 can be adjusted the distance of small diameter catheter and plasma gun; Regulate the distance that sleeve pipe 15 can be regulated small diameter catheter and flame; Permanent seat 22 can be regulated the angle that suspension injects plasma flame; Make the direct effective diameter of suspension that injects small diameter catheter to the high-temperature area that is injected into plasma flame, deposit to metal substrate surface generating structure uniform hydroxylapatite bioactive coating at last.
Embodiment 1
This example connects each assembly of equipment used by the structural arrangement of Fig. 1, use B702 type electronic peristaltic pump 1 (Tianjin association reaches great achievement Electronics Co., Ltd.) to make the transmission power set of suspension 3, the plasma spraying equipment operating voltage is 50 volts, working current is 450 peaces, small diameter catheter 19 internal diameters are 50um, titanium metal substrate 7 and plasma gun 8 spacing 10cm are regulated small diameter catheter by adjustment means suspension are horizontal injected plasma flame 5.
At first prepare spraying raw material hydroxyapatite suspension, according to calcium phosphorus mol ratio 1.67, the configuration volumetric molar concentration is that calcium nitrate aqueous solution and the volumetric molar concentration of 1.6mol/L is the ammonium dibasic phosphate aqueous solution of 2.5mol/L; Under constantly stirring, with the above-mentioned ammonium dibasic phosphate aqueous solution that configures and percentage concentration 30% ammoniacal liquor, be added drop-wise in the calcium nitrate aqueous solution that configures with the speed of 5ml/min and react, and the pH value of maintenance reaction solution is 10, temperature of reaction is 40 ℃, treat complete reaction after, left standstill 5 minutes, ageing is 24 hours again, and it is standby promptly to make spraying raw material hydroxyapatite suspension.
Place the container 4 of band high-energy ultrasound oscillation functions to shake the hydroxyapatite suspension for preparing,, avoid its reunion to realize the homodisperse of suspension particle.Show under the speed of 10ml/min under meter 11, suspension is sent to injected system 9 by the pressure piping 2 that is equipped with check valve 10, small diameter catheter from injected system is with the height of center temperature area of the direct effective diameter of linear pattern mode of jet to the injection plasma flame again, a series of complicated change procedures such as the evaporation of suspension by high-temperature plasma flame, fusion, deposition are at titanium metal substrate surface generating structure uniform hydroxylapatite bioactive coating.
This example connects each assembly of equipment used by the structural arrangement of Fig. 1, use B702 type electronic peristaltic pump 1 (Tianjin association reaches great achievement Electronics Co., Ltd.) to make the transmission power set of suspension 3, this moment, the plasma spraying equipment operating voltage was 60 volts, working current is 450 peaces, small diameter catheter 19 internal diameters are 75um, titanium metal substrate 7 and plasma gun 8 spacing 10cm, small diameter catheter is horizontal injected plasma flame 5 with suspension.
At first prepare hydroxyapatite suspension, according to calcium phosphorus mol ratio 1.67, the configuration volumetric molar concentration is that calcium nitrate aqueous solution and the volumetric molar concentration of 1.6mol/L is the ammonium dibasic phosphate aqueous solution of 2.5mol/L; Under constantly stirring, with volumetric molar concentration is that the ammonium dibasic phosphate aqueous solution of 2.5mol/L and percentage concentration are 30% ammoniacal liquor, be added drop-wise in the calcium nitrate aqueous solution that volumetric molar concentration is 2.5mol/L with the speed of 5ml/min and react, and the pH value of maintenance reaction solution is 10, temperature of reaction is 40 ℃, treat complete reaction after, left standstill 5 minutes, last ageing 24 hours, it is standby promptly to make suspension.
Place the container 4 of band high-energy ultrasound oscillation functions to shake the hydroxyapatite suspension for preparing,, avoid its reunion to realize the homodisperse of suspension particle.Show under the speed of 20ml/min under meter 11, suspension is sent to injected system 9 by the pressure piping 2 that is equipped with check valve 10, to the height of center temperature area that injects plasma flame, a series of processes such as the evaporation of suspension by plasma flame, fusion, deposition form hydroxyapatite coating layer on the titanium metal substrate surface to small diameter catheter from injected system with the direct effective diameter of linear pattern mode of jet again.
This example connects each assembly of equipment used by the structural arrangement of Fig. 1, use B702 type electronic peristaltic pump 1 (Tianjin association reaches great achievement Electronics Co., Ltd.) to make the transmission power set of suspension 3, this moment, the plasma spraying equipment operating voltage was 50 volts, working current is 450 peaces, small diameter catheter 19 internal diameters are 100um, titanium metal substrate 7 and plasma gun 8 spacing 10cm, small diameter catheter is horizontal injected plasma flame 5 with suspension.
At first prepare hydroxyapatite suspension, according to calcium phosphorus mol ratio 1.67, the configuration volumetric molar concentration is that calcium nitrate aqueous solution and the volumetric molar concentration of 1.6mol/L is the ammonium dibasic phosphate aqueous solution of 2.5mol/L; Under constantly stirring, with volumetric molar concentration is that the ammonium dibasic phosphate aqueous solution of 2.5mol/L and percentage concentration are 30% ammoniacal liquor, be added drop-wise in the calcium nitrate aqueous solution that volumetric molar concentration is 2.5mol/L with the speed of 5ml/min and react, and the pH value of maintenance reaction solution is 10, temperature of reaction is 40 ℃, treat complete reaction after, left standstill 5 minutes, last ageing 24 hours, it is standby promptly to make suspension.
Place the container 4 of band high-energy ultrasound oscillation functions to shake the hydroxyapatite suspension for preparing,, avoid its reunion to realize the homodisperse of suspension particle.Show under the speed of 30ml/min under meter 11, suspension is sent to injected system 9 by the pressure piping 2 that is equipped with check valve 10, to the height of center temperature area that injects plasma flame, processes such as the evaporation of suspension by plasma flame, fusion, deposition form the hydroxyapatite bioactive coating of even structure to small diameter catheter from injected system on the titanium metal substrate surface with the direct effective diameter of linear pattern mode of jet again.
This example connects each assembly of equipment used by the structural arrangement of Fig. 1, use B702 type electronic peristaltic pump 1 (Tianjin association reaches great achievement Electronics Co., Ltd.) to make the transmission power set of suspension 3, this moment, the plasma spraying equipment operating voltage was 40 volts, working current is 500 peaces, small diameter catheter 19 internal diameters are 50um, stainless steel metal substrate 7 and plasma gun 8 spacing 15cm, small diameter catheter is with the vertical from top to bottom injected plasma flame 5 of suspension.
At first prepare hydroxyapatite suspension, according to calcium phosphorus mol ratio 1.67, the configuration volumetric molar concentration is that calcium nitrate aqueous solution and the volumetric molar concentration of 1.6mol/L is the ammonium dibasic phosphate aqueous solution of 2.5mol/L; 15% calcium nitrate aqueous solution volume of ethanol amine is joined in the calcium nitrate aqueous solution, after fully stirring, place 60 ℃ of waters bath with thermostatic control; 15% ammonium dibasic phosphate aqueous solution volume of ethanol amine is joined in the ammonium dibasic phosphate aqueous solution, after fully stirring, place 60 ℃ of waters bath with thermostatic control; Remain on 60 ℃ in temperature of reaction, and constantly stir down, the ammonium dibasic phosphate aqueous solution that added thanomin is added drop-wise to the calcium nitrate aqueous solution that has added thanomin according to the speed of 14ml/min reacts, after treating complete reaction, left standstill 15 minutes, ageing 48 hours, it is standby promptly to make suspension.
Place the container 4 of band high-energy ultrasound oscillation functions to shake the hydroxyapatite suspension for preparing,, avoid its reunion to realize the homodisperse of suspension particle.Show under the speed of 10ml/min under meter 11, suspension is sent to injected system 9 by the pressure piping 2 that is equipped with check valve 10, to the height of center temperature area that injects plasma flame, processes such as the evaporation of suspension by plasma flame, fusion, deposition form the hydroxyapatite bioactive coating of even structure to small diameter catheter from injected system at the stainless steel metal substrate surface with the direct effective diameter of linear pattern mode of jet again.
This example connects each assembly of equipment used by the structural arrangement of Fig. 1, use B702 type electronic peristaltic pump 1 (Tianjin association reaches great achievement Electronics Co., Ltd.) to make the transmission power set of suspension 3, this moment, the plasma spraying equipment operating voltage was 40 volts, working current is 500 peaces, small diameter catheter 19 internal diameters are 75um, stainless steel metal substrate 7 and plasma gun 8 spacing 15cm, small diameter catheter is with the vertical from top to bottom injected plasma flame 5 of suspension.
At first prepare hydroxyapatite suspension, according to calcium phosphorus mol ratio 1.67, the configuration volumetric molar concentration is that calcium nitrate aqueous solution and the volumetric molar concentration of 1.6mol/L is the ammonium dibasic phosphate aqueous solution of 2.5mol/L; 15% calcium nitrate aqueous solution volume of ethanol amine is joined in the calcium nitrate aqueous solution, after fully stirring, place 60 ℃ of waters bath with thermostatic control; 15% ammonium dibasic phosphate aqueous solution volume of ethanol amine is joined in the ammonium dibasic phosphate aqueous solution, after fully stirring, place 60 ℃ of waters bath with thermostatic control; Remain on 60 ℃ in temperature of reaction, and constantly stir down, the ammonium dibasic phosphate aqueous solution that added thanomin is added drop-wise to the calcium nitrate aqueous solution that has added thanomin according to the speed of 15ml/min reacts, after treating complete reaction, left standstill 15 minutes, ageing 48 hours, it is standby promptly to make suspension.
Place the container 4 of band high-energy ultrasound oscillation functions to shake the hydroxyapatite suspension for preparing,, avoid its reunion to realize the homodisperse of suspension particle.Show under the speed of 20ml/min under meter 11, suspension is sent to injected system 9 by the pressure piping 2 that is equipped with check valve 10, to the height of center temperature area that injects plasma flame, processes such as the evaporation of suspension by plasma flame, fusion, deposition form the hydroxyapatite bioactive coating of even structure to small diameter catheter from injected system at the stainless steel metal substrate surface with the direct effective diameter of linear pattern mode of jet again.
Embodiment 6
This example connects each assembly of equipment used by the structural arrangement of Fig. 1, use B702 type electronic peristaltic pump 1 (Tianjin association reaches great achievement Electronics Co., Ltd.) to make the transmission power set of suspension 3, this moment, the plasma spraying equipment operating voltage was 40 volts, working current is 500 peaces, small diameter catheter 19 internal diameters are 100um, stainless steel metal substrate 7 and plasma gun 8 spacing 15cm, small diameter catheter is with the vertical from top to bottom injected plasma flame 5 of suspension.
At first prepare hydroxyapatite suspension, according to calcium phosphorus mol ratio 1.67, the configuration volumetric molar concentration is that calcium nitrate aqueous solution and the volumetric molar concentration of 1.6mol/L is the ammonium dibasic phosphate aqueous solution of 2.5mol/L; 15% calcium nitrate aqueous solution volume of ethanol amine is joined in the calcium nitrate aqueous solution, after fully stirring, place 60 ℃ of waters bath with thermostatic control; 15% ammonium dibasic phosphate aqueous solution volume of ethanol amine is joined in the ammonium dibasic phosphate aqueous solution, after fully stirring, place 60 ℃ of waters bath with thermostatic control; Remain on 60 ℃ in temperature of reaction, and constantly stir down, the ammonium dibasic phosphate aqueous solution that added thanomin is added drop-wise to the calcium nitrate aqueous solution that has added thanomin according to the speed of 15ml/min reacts, after treating complete reaction, left standstill 15 minutes, ageing 48 hours, it is standby promptly to make suspension.
Place the container 4 of band high-energy ultrasound oscillation functions to shake the hydroxyapatite suspension for preparing,, avoid its reunion to realize the homodisperse of suspension particle.Show under the speed of 30ml/min under meter 11, suspension is sent to injected system 9 by the pressure piping 2 that is equipped with check valve 10, to the height of center temperature area that injects plasma flame, processes such as the evaporation of suspension by plasma flame, fusion, deposition form the hydroxyapatite bioactive coating of even structure to small diameter catheter from injected system at the stainless steel metal substrate surface with the direct effective diameter of linear pattern mode of jet again.
Embodiment 7
This example connects each assembly of equipment used by the structural arrangement of Fig. 2, applying pressure jar 14 is made the transmission power set of suspension 3, this moment, the plasma spraying equipment operating voltage was 40 volts, working current is 500 peaces, small diameter catheter 19 internal diameters are 50um, stainless steel metal substrate 7 and plasma gun 8 spacing 15cm, small diameter catheter is horizontal injected plasma flame 5 with suspension.
At first prepare hydroxyapatite suspension, according to calcium phosphorus mol ratio 1.67, the configuration volumetric molar concentration is that calcium nitrate aqueous solution and the volumetric molar concentration of 0.5mol/L is the ammonium dibasic phosphate aqueous solution of 0.5mol/L; Under constantly stirring, the ammonium dibasic phosphate aqueous solution of configuration is added drop-wise in the calcium nitrate aqueous solution with 5ml/min speed and reacts, and then the ammoniacal liquor of percentage concentration 10% is added drop-wise in the reaction solution with 1ml/min speed, the control reacting liquid pH value is 9, keep temperature of reaction at 30 ℃, treat complete reaction after, left standstill 5 minutes, last ageing 24 hours promptly makes hydroxyapatite suspension.
The hydroxyapatite suspension for preparing is placed pressure-pot, under pressure-pot 0.15Mpa malleation drives, suspension is sent to injected system 9 by the pressure piping 2 that is equipped with check valve 10, to the height of center temperature area that injects plasma flame, processes such as the evaporation of suspension by plasma flame, fusion, deposition form the hydroxyapatite bioactive coating of even structure to small diameter catheter from injected system at the stainless steel metal substrate surface with the direct effective diameter of linear pattern mode of jet again.
This example connects each assembly of equipment used by the structural arrangement of Fig. 2, applying pressure jar 14 is made the transmission power set of suspension 3, this moment, the plasma spraying equipment operating voltage was 45 volts, working current is 500 peaces, small diameter catheter 19 diameters are 75um, stainless steel metal substrate 7 and plasma gun 8 spacing 10cm, small diameter catheter is horizontal injected plasma flame 5 with suspension 3.
Preparation hydroxyapatite suspension, according to calcium phosphorus mol ratio 1.67, the configuration volumetric molar concentration is that calcium nitrate aqueous solution and the volumetric molar concentration of 0.5mol/L is the ammonium dibasic phosphate aqueous solution of 0.5mol/L; Under constantly stirring, the ammonium dibasic phosphate aqueous solution of configuration is added drop-wise in the calcium nitrate aqueous solution with 5ml/min speed and reacts, and then the ammoniacal liquor of percentage concentration 10% is added drop-wise in the reaction solution with 1ml/min speed, the control reacting liquid pH value is 9, keep temperature of reaction at 30 ℃, treat complete reaction after, left standstill 5 minutes, last ageing 24 hours promptly makes hydroxyapatite suspension.
The hydroxyapatite suspension for preparing is placed pressure-pot, under pressure-pot 0.25Mpa malleation drives, suspension is sent to injected system 9 by the pressure piping 2 that is equipped with check valve 10, to the height of center temperature area that injects plasma flame, processes such as the evaporation of suspension by plasma flame, fusion, deposition form the hydroxyapatite bioactive coating of even structure to small diameter catheter from injected system at the stainless steel metal substrate surface with the direct effective diameter of linear pattern mode of jet again.
Embodiment 9
This example connects each assembly of equipment used by the structural arrangement of Fig. 2, applying pressure jar 14 is made the transmission power set of suspension 3, this moment, the plasma spraying equipment operating voltage was 45 volts, working current is 500 peaces, small diameter catheter 19 diameters are 100um, stainless steel metal substrate 7 and plasma gun 8 spacing 10cm, small diameter catheter is horizontal injected plasma flame 5 with suspension.
Preparation hydroxyapatite suspension, according to calcium phosphorus mol ratio 1.67, the configuration volumetric molar concentration is that calcium nitrate aqueous solution and the volumetric molar concentration of 0.5mol/L is the ammonium dibasic phosphate aqueous solution of 0.5mol/L; Under constantly stirring, the ammonium dibasic phosphate aqueous solution of configuration is added drop-wise in the calcium nitrate aqueous solution with 5ml/min speed and reacts, and then the ammoniacal liquor of percentage concentration 10% is added drop-wise in the reaction solution with 1ml/min speed, the control reacting liquid pH value is 9, keep temperature of reaction at 30 ℃, treat complete reaction after, left standstill 5 minutes, last ageing 24 hours promptly makes hydroxyapatite suspension.
The hydroxyapatite suspension for preparing is placed pressure-pot, under pressure-pot 0.3Mpa malleation drives, suspension is sent to injected system 9 by the pressure piping 2 that is equipped with check valve 10, small diameter catheter from injected system is directly radially injected the height of center temperature area of plasma flame with the linear pattern mode of jet again, and processes such as the evaporation of suspension by plasma flame, fusion, deposition form the hydroxyapatite bioactive coating of even structure at the stainless steel metal substrate surface.
This example connects each assembly of equipment used by the structural arrangement of Fig. 2, applying pressure jar 14 is made the transmission power set of suspension 3, this moment, the plasma spraying equipment operating voltage was 50 volts, working current is 400 peaces, small diameter catheter 19 diameters are 50um, titanium metal substrate 7 and plasma gun 8 spacing 20cm, small diameter catheter is with the vertical from top to bottom injected plasma flame 5 of suspension.
Preparation hydroxyapatite suspension, according to calcium phosphorus mol ratio 1.67, the configuration volumetric molar concentration is that calcium nitrate aqueous solution and the volumetric molar concentration of 1.2mol/L is the ammonium dibasic phosphate aqueous solution of 2mol/L; Under constantly stirring, with volumetric molar concentration is that to be 24% ammoniacal liquor with the speed of 10ml/min be added drop-wise in the calcium nitrate aqueous solution that volumetric molar concentration is 1.2mol/L reacts for the ammonium dibasic phosphate aqueous solution of 2mol/L and percentage concentration, and the pH value of maintenance reaction solution is 11, temperature of reaction is 50 ℃, after treating complete reaction, left standstill 10 minutes, last ageing 36 hours promptly makes hydroxyapatite suspension.
The hydroxyapatite suspension for preparing is placed pressure-pot, under pressure-pot 0.4Mpa malleation drives, suspension is sent to injected system 9 by the pressure piping 2 that is equipped with check valve 10, to the height of center temperature area that injects plasma flame, processes such as the evaporation of suspension by plasma flame, fusion, deposition form the hydroxyapatite bioactive coating of even structure to small diameter catheter from injected system on the titanium metal substrate surface with the direct effective diameter of linear pattern mode of jet again.
This example connects each assembly of equipment used by the structural arrangement of Fig. 2, applying pressure jar 14 is made the transmission power set of suspension 3, this moment, the plasma spraying equipment operating voltage was 50 volts, working current is 400 peaces, small diameter catheter 19 diameters are 75um, titanium metal substrate 7 and plasma gun 8 spacing 20cm, small diameter catheter is with the vertical from top to bottom injected plasma flame 5 of suspension.
Preparation hydroxyapatite suspension, according to calcium phosphorus mol ratio 1.67, the configuration volumetric molar concentration is that calcium nitrate aqueous solution and the volumetric molar concentration of 1.2mol/L is the ammonium dibasic phosphate aqueous solution of 2mol/L; Under constantly stirring, with volumetric molar concentration is that to be 24% ammoniacal liquor with the speed of 10ml/min be added drop-wise in the calcium nitrate aqueous solution that volumetric molar concentration is 1.2mol/L reacts for the ammonium dibasic phosphate aqueous solution of 2mol/L and percentage concentration, and the pH value of maintenance reaction solution is 11, temperature of reaction is 50 ℃, after treating complete reaction, left standstill 10 minutes, last ageing 36 hours promptly makes hydroxyapatite suspension.
The hydroxyapatite suspension for preparing is placed pressure-pot, under pressure-pot 0.5Mpa malleation drives, suspension is sent to injected system 9 by the pressure piping 2 that is equipped with check valve 10, to the height of center temperature area that injects plasma flame, processes such as the evaporation of suspension by plasma flame, fusion, deposition form the hydroxyapatite bioactive coating of even structure to small diameter catheter from injected system on the titanium metal substrate surface with the direct effective diameter of linear pattern mode of jet again.
This example connects each assembly of equipment used by the structural arrangement of Fig. 2, make pressure-pot 14 make the transmission power set of suspension 3, this moment, the plasma spraying equipment operating voltage was 50 volts, working current is 400 peaces, small diameter catheter 19 diameters are 100um, titanium metal substrate 7 and plasma gun 8 spacing 20cm, small diameter catheter is with the vertical from top to bottom injected plasma flame 5 of suspension.
Preparation hydroxyapatite suspension, according to calcium phosphorus mol ratio 1.67, the configuration volumetric molar concentration is that calcium nitrate aqueous solution and the volumetric molar concentration of 1.2mol/L is the ammonium dibasic phosphate aqueous solution of 2mol/L; Under constantly stirring, with volumetric molar concentration is that to be 24% ammoniacal liquor with the speed of 10ml/min be added drop-wise in the calcium nitrate aqueous solution that volumetric molar concentration is 1.2mol/L reacts for the ammonium dibasic phosphate aqueous solution of 2mol/L and percentage concentration, and the pH value of maintenance reaction solution is 11, temperature of reaction is 50 ℃, after treating complete reaction, left standstill 10 minutes, last ageing 36 hours promptly makes hydroxyapatite suspension.
The hydroxyapatite suspension for preparing is placed pressure-pot, under pressure-pot 0.6Mpa malleation drives, suspension is sent to injected system 9 by the pressure piping 2 that is equipped with check valve 10, to the height of center temperature area that injects plasma flame, processes such as the evaporation of suspension by plasma flame, fusion, deposition form the hydroxyapatite bioactive coating of even structure to small diameter catheter from injected system on the titanium metal substrate surface with the direct effective diameter of linear pattern mode of jet again.
Claims (10)
1. a suspension injection type plasma spraying device for preparing hydroxyapatite bioactive coating comprises plasma gun (8), metal base (7) and substrate anchor (6) thereof; It is characterized in that also comprising plasma spraying stock suspension storage vessel, suspension transfer system, suspension injected system; Wherein said suspension transfer system comprise transmit power set with its transmission medium that is complementary and is connected, transmission medium one end is communicated with the transmission power set, the other end is communicated with suspension injected system (9); One small diameter catheter (19) is set in the described suspension injected system (9), and small diameter catheter is installed on plasma gun (8) by adjustment means and is complementary on the permanent seat (22) that is connected; Suspension in the storage vessel (3) is transported to small diameter catheter in the suspension injected system by transmitting power set and transmission medium, small diameter catheter is directly radially injected the high-temperature area at plasma flame (5) center with the linear pattern mode of jet, at metal substrate surface generating structure uniform hydroxylapatite bioactive coating.
2. suspension injection type plasma spraying device according to claim 1 is characterized in that the container (4) of described suspension storage vessel for band high-energy ultrasound oscillation functions; Or be pressure-pot (14).
3. suspension injection type plasma spraying device according to claim 1 is characterized in that transmitting in the described suspension transfer system power set or is electronic peristaltic pump (1); Or for importing compressed-air actuated pressure-pot (14); Electronic peristaltic pump is connected with the suspension injected system by the container of transmission medium with band high-energy ultrasound oscillation functions; Pressure-pot also is connected with the suspension injected system by transmission medium.
4. suspension injection type plasma spraying device according to claim 3 is characterized in that the transmission medium that connects electronic peristaltic pump (1) in the described suspension transfer system or connect pressure-pot (14) is pressure piping (2).
5. according to claim 3 or 4 described suspension injection type plasma spraying devices, it is characterized in that on described electronic peristaltic pump (1) and the pressure piping (2) that suspension injected system (9) is connected a check valve (10) and under meter (11) being set; Or a check valve (10) is set, under meter (11) and valve (12) on the pressure piping (2) that is connected with the suspension injected system of pressure-pot (14).
6. suspension injection type plasma spraying device according to claim 3 is characterized in that the transfer rate that described transmission power set electronic peristaltic pump (1) uses is 10-100ml/min.
7. suspension injection type plasma spraying device according to claim 3 is characterized in that the compressed-air actuated pressure of importing in the pressure-pot (14) in the described transmission power set is 0.15-0.6MPa.
8. suspension injection type plasma spraying device according to claim 1, the internal diameter that it is characterized in that described small diameter catheter is the 50-300 micron.
9. suspension injection type plasma spraying device according to claim 1, it is characterized in that the described permanent seat (22) that is complementary and is connected with plasma gun (8) size, the rotating mechanism that can pass through nut (20) screw (21) formation is regulated the relative angle of permanent seat and plasma gun.
10. according to claim 1 or 9 described suspension injection type plasma spraying devices, it is characterized in that installing on the described permanent seat horizontal adjustment support (17), regulating support is connected with adjusting slider (16) coupling that threaded hole is opened at the center, regulate sleeve pipe (15) and be connected with adjusting slider (16) by threaded hole, small diameter catheter (19) is installed on the catheter holder (18) of regulating sleeve pipe (15) below.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100450671A CN101250682B (en) | 2008-03-27 | 2008-03-27 | Injection type plasma spraying device for producing hydroxyapatite bioactivity coating |
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| CN2008100450671A CN101250682B (en) | 2008-03-27 | 2008-03-27 | Injection type plasma spraying device for producing hydroxyapatite bioactivity coating |
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| CN101250682B true CN101250682B (en) | 2011-08-31 |
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| CN101619434B (en) * | 2009-05-12 | 2011-04-13 | 四川大学 | Method for preparing porous hydroxylapatite coating by suspending liquid plasma spraying |
| CN103031508A (en) * | 2011-09-30 | 2013-04-10 | 中国农业机械化科学研究院 | Liquid feedstock plasma spraying device |
| CN102728292B (en) * | 2012-07-11 | 2014-05-07 | 中国计量学院 | Method for completely gasifying grains in frequency-conversion plasma jet flow |
| EP3060693B1 (en) | 2013-10-25 | 2018-06-27 | United Technologies Corporation | Plasma spraying system with adjustable coating medium nozzle |
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