CN113750288B - Ceramic particle reinforced Ti-Ta-based bone implantation composite material and preparation method thereof - Google Patents
Ceramic particle reinforced Ti-Ta-based bone implantation composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a ceramic particle reinforced Ti-Ta based bone implantation composite material and a preparation method thereof, wherein the method comprises the following steps: mixing dimolybdenum carbide or titanium diboride with titanium powder, tantalum powder and nickel carbonyl powder, preparing slurry with a dispersant and a grinding ball, mixing, separating the grinding ball, drying the slurry, and performing compression molding; sintering under vacuum condition, firstly heating the furnace temperature from room temperature to 600 ℃ at the speed of 10 ℃/min, then preserving heat for 30min, then heating to 1250-1300 ℃ at the speed of 10 ℃/min, preserving heat for 60min, and finally cooling to room temperature at the speed of-20 ℃/min; keeping the temperature at 850-940 ℃ in a closed high-pressure device, keeping the pressure at 90-140 MPa by inert gas, cooling to 265 ℃ along with the furnace, and discharging; the temperature is preserved at 900-1200 ℃, water quenching is carried out, the temperature is preserved at 450-700 ℃, and then air cooling is carried out. The uniformity, corrosion resistance and material strength of elements in the composite material are all improved.
Description
Technical Field
The invention relates to a bone implantation composite material, in particular to a ceramic particle reinforced Ti-Ta based bone implantation composite material and a preparation method thereof.
Background
The titanium alloy material for bone implantation mainly comprises alpha type and beta type, wherein the alpha type is Ti-6AL-4V alloy, the beta type is Ti-5AL-2.5Fe and Ti-6AL-7Nb alloy, the alpha type and the beta type are applied to bone implantation, but V and Al elements contained in the alloy are harmful to human bodies, V is used as a beta phase and is a stable alloy element, the cost is high, the cytotoxicity is high, and the Al element easily causes senile dementia after being existed in the human bodies for a long time. From the medical application point of view, the most important criteria for bone implant alloys are not only the non-toxicity, corrosion resistance and cost of the alloy elements. Therefore, it is important to develop a titanium alloy free from harmful elements such as Al.
Among the bone-implanted titanium alloys without harmful elements such as V and Al, ti-Ta alloy is one of the most promising alloys. The excellent biocompatibility and corrosion resistance of pure titanium and pure tantalum have been widely accepted by many medical researchers, and compared to pure Ta, ti-Ta alloys are lighter and cheaper, and are superior materials to replace Ta. Among the currently used bone implant materials, the Ti — Ta alloy has the lowest young's modulus and strength comparable to that of the cobalt-based alloy.
In the powder metallurgy of Ti-Ta alloys, sintering the mixed Ti and Ta powders does not fully guarantee the homogeneity of the alloy despite the high sintering temperatures used (from 1200 to 1500 ℃). Therefore, ti-Ta powder is not fully diffused in the sintering process, so that Ti-rich and Ta-rich areas in the alloy are alternately distributed, and the problem of uneven element distribution can be effectively solved by utilizing an initial mechanical alloying method and then sintering at a temperature lower than the melting point of titanium. In the process of preparing the titanium alloy by powder metallurgy, the porosity (the porosity is 5-20%) can be controlled by adjusting powder components and sintering parameters, so that the Ti-Ta alloy with low elastic modulus is obtained, and is suitable for bone implant, but the strength and the fatigue resistance of the alloy surface are reduced, and even harmful substances in the chemical treatment process remain in pores, so that the problem of obtaining the Ti-Ta alloy with proper pores, high bending strength and good corrosion resistance is a great problem.
Disclosure of Invention
The invention aims to provide a ceramic particle reinforced Ti-Ta based bone implantation composite material and a preparation method thereof.
In order to achieve the above objects, the present invention provides a method for preparing a ceramic particle reinforced Ti-Ta based bone implant composite, the method comprising: the mass ratio is 84-88: 8:4 to 8: 1-5 parts of dimolybdenum carbide or titanium diboride, titanium powder, tantalum powder and nickel carbonyl powder are uniformly mixed, and the mixed powder, a dispersing agent and a grinding ball are mixed according to the mass ratio of 1:1:1, preparing slurry, mixing at the temperature of-5 to-2 ℃, separating the slurry from grinding balls after finishing, drying the slurry, and performing compression molding at the pressure of 180 to 240MPa; at 10 -3 ～10 -2 Sintering under the Pa vacuum degree, firstly heating the furnace temperature from room temperature to 600 ℃ at the heating rate of 10 ℃/min, then preserving the heat for 30min, then heating to 1250-1300 ℃ at the heating rate of 10 ℃/min, preserving the heat for 60min, and finally cooling to the room temperature at the speed of-20 ℃/min; putting the sintered material in a closed high-pressure device, keeping the temperature at 850-940 ℃, keeping the pressure at 90-140 MPa by inert gas, keeping for 2h, cooling to 265 ℃ along with the furnace, and discharging; then the material is subjected to heat preservation at 900-1200 ℃ for 40min, then water quenching is carried out, then heat preservation is carried out at 450-700 ℃ for 5h, and then air cooling is carried out, thus obtaining the ceramic particle reinforced Ti-Ta based bone implantation composite material.
Preferably, the pressure maintaining time is 5min when the material is pressed and formed under the pressure of 180-240 MPa.
Preferably, the dimolybdenum carbide or titanium diboride is mixed with titanium powder, tantalum powder and nickel carbonyl powder in an ultrasonic mode, and the ultrasonic frequency is 35Hz.
Preferably, the dispersant is octadecanoic acid.
Preferably, the grinding balls are zirconia balls.
Preferably, the mixing time is 24 hours at-5 to-2 ℃.
Preferably, the temperature at which the slurry is dried is 72 ℃.
The invention also aims to provide a ceramic particle reinforced Ti-Ta based bone implant composite material prepared by the method.
The ceramic particle reinforced Ti-Ta based bone implantation composite material and the preparation method thereof have the following advantages:
the ceramic particle reinforced Ti-Ta based bone implantation composite material is prepared by mixing ceramic particles Mo 2 C or TiB 2 The Ti-Ta alloy is used as reinforcing particles and added into the Ti-Ta alloy, so that the uniformity, the corrosion resistance and the material strength of elements in the composite material are improved. Wherein Mo is added 2 The C particles are distributed in the matrix material in a criss-cross mode, so that the crack expansion in the material can be effectively hindered, and the bending strength of the material can be favorably improved. Added Mo 2 The wetting property between the C particles and the matrix is strong, the swelling phenomenon of the material can be eliminated, and the uniformity of particle distribution is improved. Ta and Mo are beneficial to alloy to generate a passivation layer, and the corrosion resistance of the material is also improved.
Drawings
FIG. 1 is a schematic diagram of sintering temperatures for various embodiments of the present invention.
Fig. 2 is the EDS element distribution test results of the composite material of example 1 of the present invention.
Fig. 3 is the EDS elemental distribution test results for the composite of example 4 of the invention.
FIG. 4 is a polarization impedance for various embodiments of the present invention.
FIG. 5 is a graph of the flexural strength of composite materials prepared in various examples of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
A ceramic particle reinforced Ti-Ta based bone implantation composite material is prepared by the following steps:
(1) Titanium powder (average particle size of 35 microns) with the purity of 95%, tantalum powder (average particle size of 10 microns), nickel carbonyl powder (average particle size of 10 microns) and molybdenum carbide (average particle size of 6 microns) are mixed together to prepare mixed powder, the mass of the mixed powder is 84g, 8g, 4g and 1g respectively, the mixed powder is subjected to ultrasonic treatment by an ultrasonic cleaning machine and is convenient to mix uniformly, the treatment frequency is 35Hz, and the treatment time is 43min. Octadecanoic acid and zirconia balls are respectively used as a dispersing agent and grinding balls, and the mixed powder, the octadecanoic acid and the grinding balls are prepared into slurry according to the mass ratio of 1.
(2) And (2) putting the slurry prepared in the step (1) into a three-dimensional rotary mixer for mixing for 24 hours at the mixing temperature of-2 ℃. And after the powder mixing is finished, pouring the slurry out, separating the slurry from the grinding balls, placing the slurry in a drying oven at 72 ℃ for baking for 24 hours to remove the octadecanoic acid dispersing agent in the slurry, and carrying out press forming on the dried powder under the pressure of 180MPa for 5 minutes.
(3) Firing the pressed green body in a vacuum sintering furnace at 10 deg.C to reduce the adverse effects of harmful components such as nitrogen, oxygen and water in the atmosphere on the workpiece -2 And sintering under Pa vacuum degree, wherein the sintering temperature is shown in figure 1, the furnace temperature is firstly increased from 25 ℃ to 600 ℃ at the heating rate of 10 ℃/min and then is kept for 30min, then is increased to 1250 ℃ at the heating rate of 10 ℃/min and is kept for 60min, and finally is reduced to 25 ℃ at the room temperature at the speed of-20 ℃/min.
(4) And (4) putting the material prepared in the step (3) into a closed high-pressure device, keeping the temperature at 850 ℃, keeping the pressure at 90MPa through inert gas, keeping for 2 hours, cooling to 265 ℃ along with the furnace, and discharging.
(5) And (3) putting the material prepared in the step (4) into a furnace at 900 ℃ for heat preservation for 40min, then carrying out water quenching, then carrying out heat preservation at 450 ℃ for 5h, and then carrying out air cooling to obtain the ceramic particle reinforced Ti-Ta based bone implantation composite material.
Example 2
A ceramic particle reinforced Ti-Ta based bone implant composite prepared substantially as in example 1, except that:
in the step (1), the mass of the titanium powder, the mass of the tantalum powder, the mass of the nickel carbonyl powder and the mass of the molybdenum carbide are respectively 86g, 8g, 6g and 3g;
in the step (2), the mixing temperature of the slurry is-3 ℃; the pressure for pressing and forming the dried powder is 210MPa, and the pressure maintaining time is 5min;
in step (3), at 10 -3 Sintering under Pa vacuum degree at the sintering temperature shown in figure 1Heating the furnace temperature from 25 deg.C to 600 deg.C at a heating rate of 10 deg.C/min, maintaining for 30min, heating to 1275 deg.C at a heating rate of 10 deg.C/min, maintaining for 60min, and cooling to 25 deg.C at a cooling rate of-20 deg.C/min;
in the step (4), the temperature is maintained at 900 ℃, and the pressure is maintained at 120MPa;
in the step (5), the material is put into 1100 ℃ for heat preservation for 40min, then water quenching is carried out, then heat preservation is carried out for 5h at 600 ℃, and then air cooling is carried out.
Example 3
A ceramic particle reinforced Ti-Ta based bone implant composite prepared substantially as in example 1, except that:
in the step (1), the mass of the titanium powder, the mass of the tantalum powder, the mass of the nickel carbonyl powder and the mass of the molybdenum carbide are respectively 88g, 8g and 5g;
in the step (2), the mixing temperature of the slurry is-5 ℃; the pressure for press forming the dried powder is 240MPa;
in step (3), at 10 -3 Sintering under Pa vacuum degree, wherein the sintering temperature is shown in figure 1, the furnace temperature is firstly increased from room temperature 25 ℃ to 600 ℃ at a heating rate of 10 ℃/min and then is preserved for 30min, then the furnace temperature is increased to 1300 ℃ at a heating rate of 10 ℃/min and preserved for 60min, and finally the furnace temperature is reduced to room temperature 25 ℃ at a heating rate of-20 ℃/min;
in the step (4), keeping the temperature at 940 ℃ and the pressure at 140MPa;
in the step (5), the material is subjected to heat preservation at 1200 ℃ and then water quenching, and then is subjected to heat preservation at 700 ℃ and then air cooling.
Example 4
A ceramic particle reinforced Ti-Ta based bone implant composite prepared substantially as in example 1, except that: titanium diboride (average particle size 10 μm) was substituted for dimolybdenum carbide.
Example 5
A ceramic particle reinforced Ti-Ta based bone implant composite prepared substantially as in example 2, except that: titanium diboride (average particle size 10 μm) was substituted for dimolybdenum carbide.
Example 6
A ceramic particle reinforced Ti-Ta based bone implant composite prepared substantially as in example 3, except that: titanium diboride (average particle size 10 μm) was substituted for dimolybdenum carbide.
Uniformity test of elemental distribution for example 1 and example 4
EDS element distribution tests are carried out on the samples prepared in the example 1 and the example 4, and the test results are shown in a figure 2 and a figure 3, wherein in the example 1, C is converted from molybdenum carbide and is distributed in the material in a fine particle shape, other elements are uniformly distributed, and the structure has no obvious pores; in example 4, B is converted from titanium diboride, and the elements are uniformly distributed without obvious pores in the structure.
Corrosion resistance testing of examples 1-6
The corrosion resistance of the material is tested by adopting a dynamic potential polarization experimental method, the test specification refers to ASTM G59-97, the electrolyte is 0.5mol/L sulfuric acid aqueous solution, the auxiliary electrode is platinum, ag/AgCl is a reference electrode, and the area of a corrosion test sample is 0.8cm 2 。
The polarization resistance of each example is shown in FIG. 4, where the polarization resistance is the greatest and the corrosion resistance is the best in example 3, followed by example 6, surface Mo 2 C and TiB 2 The addition of (2) is beneficial to improving the corrosion resistance of the composite material.
Flexural Strength testing of examples 1-6
The bending strength test adopts a three-point bending strength experimental method for measurement, the measurement specification refers to ASTM B528-2016, the loading rate is 2mm/min, the width, the height and the length of a tested sample are respectively 5.5mm, 6mm and 200mm, and the span of two supporting points below the test sample is 25.4mm.
The bending strength calculation formula is as follows:
TRS＝(3×P×L)/(2×T 2 ×W)
where P is the measured breaking load (N) of the material, L is the span (mm) of the two fulcrums below the specimen, T is the height (mm) of the specimen, and W is the width (mm) of the specimen.
As shown in FIG. 5, for the bending strength of the composite materials prepared in the respective examples, it can be seen that in examples 1, 2 and 3Mo 2 The content of C particles is increased in sequence, the bending strength is also increased, and Mo is shown 2 The addition of the C particles can effectively prevent the crack from expanding, thereby improving the bending strength of the material. TiB in example 4, example 5 and example 6 2 The particle content increases in turn when TiB 2 The particles are enlarged to a certain degree, and the bending strength of the material is improved.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.
Claims (8)
1. A method for preparing a ceramic particle reinforced Ti-Ta based bone implant composite, the method comprising:
mixing the components in a mass ratio of 84-88: 8:4 to 8:1 to 5 portions of molybdenum carbide or titanium diboride, titanium powder, tantalum powder and nickel carbonyl powder are evenly mixed, and the mixed powder, a dispersant and a grinding ball are mixed according to the mass ratio of 1:1:1, preparing slurry, mixing at-5 to-2 ℃, separating the slurry from grinding balls after finishing, drying the slurry, and performing compression molding under 180 to 240MPa;
at 10 -3 ～10 -2 Sintering under Pa vacuum degree, firstly heating the furnace temperature from room temperature to 600 ℃ at a heating rate of 10 ℃/min, then preserving the temperature for 30min, then heating to 1250-1300 ℃ at a heating rate of 10 ℃/min, preserving the temperature for 60min, and finally cooling to the room temperature at a speed of-20 ℃/min;
putting the sintered material in a closed high-pressure device, keeping the temperature at 850-940 ℃, keeping the pressure at 90-140 MPa by inert gas, keeping for 2h, cooling to 265 ℃ along with the furnace, and discharging; then the material is subjected to heat preservation at 900-1200 ℃ for 40min, then water quenching is carried out, then heat preservation is carried out at 450-700 ℃ for 5h, and then air cooling is carried out, thus obtaining the ceramic particle reinforced Ti-Ta based bone implantation composite material.
2. The method of claim 1, wherein the pressure maintaining time is 5min when the composite material is formed by compression under 180 to 240 MPa.
3. The method for preparing a ceramic particle reinforced Ti-Ta based bone implant composite material according to claim 1, wherein the dimolybdenum carbide or titanium diboride is mixed with titanium powder, tantalum powder and nickel carbonyl powder in an ultrasonic manner, and the ultrasonic frequency is 35Hz.
4. The method of claim 1, wherein the dispersant is octadecanoic acid.
5. The method of claim 1, wherein the grinding balls are zirconia balls.
6. The method for preparing a ceramic particle reinforced Ti-Ta based bone implant composite according to claim 1, wherein the mixing time at-5 to-2 ℃ is 24 hours.
7. The method for preparing a ceramic particle reinforced Ti-Ta based bone implant composite according to claim 1, wherein the temperature of drying the slurry is 72 ℃.
8. A ceramic particle reinforced Ti-Ta based bone implant composite prepared by the method of any one of claims 1 to 7.
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