CN115887752A - Preparation method of bone repair implant with super-strong bonding strength composite coating - Google Patents
Preparation method of bone repair implant with super-strong bonding strength composite coating Download PDFInfo
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- CN115887752A CN115887752A CN202211504143.7A CN202211504143A CN115887752A CN 115887752 A CN115887752 A CN 115887752A CN 202211504143 A CN202211504143 A CN 202211504143A CN 115887752 A CN115887752 A CN 115887752A
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- 238000000576 coating method Methods 0.000 title claims abstract description 58
- 239000007943 implant Substances 0.000 title claims abstract description 46
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 210000000988 bone and bone Anatomy 0.000 title claims abstract description 25
- 230000008439 repair process Effects 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 70
- 239000010936 titanium Substances 0.000 claims abstract description 70
- 239000000758 substrate Substances 0.000 claims abstract description 41
- JUWGUJSXVOBPHP-UHFFFAOYSA-B titanium(4+);tetraphosphate Chemical compound [Ti+4].[Ti+4].[Ti+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O JUWGUJSXVOBPHP-UHFFFAOYSA-B 0.000 claims abstract description 37
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 23
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- 238000005498 polishing Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 60
- 238000001035 drying Methods 0.000 claims description 33
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 22
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 22
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 18
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 15
- 239000012498 ultrapure water Substances 0.000 claims description 15
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 9
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 9
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000004519 grease Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims 2
- 238000010883 osseointegration Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 12
- 239000011159 matrix material Substances 0.000 description 10
- 241000282414 Homo sapiens Species 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 102100031475 Osteocalcin Human genes 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
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- 238000008157 ELISA kit Methods 0.000 description 1
- 101001098398 Mus musculus Osteocalcin Proteins 0.000 description 1
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- IZTQOLKUZKXIRV-YRVFCXMDSA-N sincalide Chemical compound C([C@@H](C(=O)N[C@@H](CCSC)C(=O)NCC(=O)N[C@@H](CC=1C2=CC=CC=C2NC=1)C(=O)N[C@@H](CCSC)C(=O)N[C@@H](CC(O)=O)C(=O)N[C@@H](CC=1C=CC=CC=1)C(N)=O)NC(=O)[C@@H](N)CC(O)=O)C1=CC=C(OS(O)(=O)=O)C=C1 IZTQOLKUZKXIRV-YRVFCXMDSA-N 0.000 description 1
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Abstract
The invention relates to a preparation method of a bone repair implant with a composite coating with super-strong bonding strength, belongs to the technical field of nano materials, solves the technical problem of insufficient bonding strength of a substrate and the coating, and comprises the following steps: polishing and cleaning the titanium surface; (2) preparing a titanium phosphate coating on the titanium surface by using a hydrothermal method; (3) And modifying the titanium phosphate coating by using a hydrothermal method, and preparing the titanium phosphate/nano-hydroxyapatite composite coating on the titanium surface. The invention has simple preparation process and low cost, and the prepared implant has excellent mechanical property, good chemical stability, super-strong bonding strength between the composite coating and the implant and has better bioactivity, osseointegration, bone repair property and safety. The invention has good application value in the aspects of preparation, modification and application of the bone repair implant material.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of a bone repair implant with a composite coating layer with super-strong bonding strength.
Background
With the continuous progress of medical technology, the average life of human beings is gradually prolonged, orthopedic diseases are correspondingly gradually increased, and orthopedic repair work is increasingly important in the medical field.
Titanium has the advantages of low elastic modulus, light weight, high strength, stable chemical structure and the like as a common material of the bone repair implant, but titanium cannot form a biological integrated tissue with soft tissues due to biological inertia, so that the bone repair time can be greatly prolonged, and the risk of infection of an implanted part can be increased.
Hydroxyapatite (HA) is a main inorganic component of human bone tissues, can participate in vivo metabolism, and HAs stimulation and induction effects on bone repair, so the HA is commonly used for endowing a titanium implant with bioactivity, namely the HA is used as a coating to cover the surface of a titanium substrate, so that the HA helps the implant to be biologically integrated with surrounding bones and soft tissues while maintaining the excellent mechanical properties of the titanium implant, and the bone repair is promoted. Research shows that the titanium phosphate coating has great influence on the proliferation, adhesion, differentiation and other behaviors of cells, and further influences the osseointegration of the implant and the biomechanical stability of the implant. However, due to the low bonding strength of the coating to the substrate, mechanical loading, etc., the bond between the coating and the substrate is prone to early rupture, which prevents successful implantation of the implant into the human body. Therefore, the increase of the bonding strength of the substrate and the coating can greatly prolong the service life of the implant and has better application value in clinical aspect.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a preparation method of a bone repair implant with a composite coating with super-strong bonding strength, namely, a titanium phosphate/nano-hydroxyapatite composite coating with super-strong bonding strength is prepared on the surface of a bone repair implant matrix.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
a preparation method of a bone repair implant with a super-strong bonding strength composite coating comprises the following steps:
s1, cleaning a titanium substrate: polishing the surface of the titanium substrate, then ultrasonically cleaning the titanium substrate in a mixed solution of ethanol and distilled water for 10 minutes to remove stains and grease on the surface of the titanium substrate, and drying the titanium substrate at room temperature for later use;
s2, preparing a titanium phosphate coating on the surface of the titanium substrate:
firstly, weighing hydrogen peroxide and concentrated phosphoric acid according to the same volume ratio, adding the hydrogen peroxide and the concentrated phosphoric acid into a reaction kettle, and uniformly stirring;
then, putting the titanium substrate prepared in the step S1 into a reaction kettle, heating the reaction kettle to 110-130 ℃, preserving heat for 6-24 h, and then terminating the reaction;
finally, after the temperature in the reaction kettle is cooled to room temperature, taking out the product from the reaction kettle, washing the product for at least 2 times by using ultrapure water, and then placing the product in a drying oven for drying at the drying temperature of 50 ℃ for 24 hours to prepare the titanium implant covered with the titanium phosphate coating;
s3, preparing a titanium phosphate/nano-hydroxyapatite composite coating on the surface of the titanium substrate:
first, the molar ratio of 2:1, weighing anhydrous calcium chloride and hexamethylenetetramine, adding the anhydrous calcium chloride and the hexamethylenetetramine into a reaction kettle, adding ultrapure water, and uniformly stirring, wherein the concentration of the anhydrous calcium chloride solution is 6-11 wt%, and the concentration of the hexamethylenetetramine composite solution is 5-10 wt%;
then, putting the titanium implant covered with the titanium phosphate coating prepared in the step S2 into a reaction kettle, heating the reaction kettle to 110-130 ℃, preserving heat for 6-12 h, and then stopping the reaction;
and finally, after the temperature in the reaction kettle is cooled to room temperature, taking out the product from the reaction kettle, washing the product for at least 2 times by using ultrapure water, and then placing the product in a drying oven for drying at the drying temperature of 50 ℃ for 24 hours to obtain the titanium implant covered with the titanium phosphate/nano-hydroxyapatite composite coating.
Further, in the step S1, the concentration of hydrogen peroxide is 6wt% -11wt%, and the concentration of concentrated phosphoric acid is 6wt% -11wt%.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention utilizes a two-step hydrothermal method to prepare the titanium phosphate/nano-hydroxyapatite composite coating bone repair implant with super-strong bonding strength, maintains the advantages of low elastic modulus, light weight, high strength, stable chemical structure and the like of titanium, and simultaneously utilizes the hydroxyapatite and the titanium phosphate coating to modify the titanium, so that the coating has super-strong bonding strength with a substrate, improves the biocompatibility and osseointegration of the titanium implant, and also has certain bone repair capability and good biological safety, thereby having practical value in the application of the titanium implant in organisms.
2. The invention has simple preparation process and low cost, and the prepared implant has excellent mechanical property, good chemical stability, super-strong bonding strength with the composite coating and better bioactivity, osseointegration, bone repair and safety. Has good application value in the aspects of preparation, modification and application of the bone repair implant material.
Drawings
FIG. 1 is a scanning electron microscope image of a titanium phosphate composite coating;
FIG. 2 is a scanning electron microscope image of the titanium phosphate/nano hydroxyapatite composite coating.
Detailed Description
The invention is described in further detail below with reference to the figures and examples.
Example 1
A preparation method of a bone repair implant with a super-strong bonding strength composite coating comprises the following steps:
s1, cleaning a titanium substrate: processing an industrial pure titanium plate (with the purity of 99.7%) into a substrate blank with the size of 10mm in length, 10mm in width and 0.1 mm in thickness, grinding and flattening the surface of the substrate blank by using 400 grit, 800 grit and 1000 grit silicon carbide paper in sequence, polishing to obtain a titanium matrix, ultrasonically cleaning the titanium matrix in a mixed solution of ethanol and distilled water for 10 minutes, removing stains and grease on the surface of the titanium matrix, drying at room temperature, and reserving for the later step;
s2, preparing a titanium phosphate coating on the surface of the titanium substrate:
firstly, weighing 5mL of hydrogen peroxide (with the concentration of 9 wt%) and 5mL of concentrated phosphoric acid (with the concentration of 8.5 wt%), adding the hydrogen peroxide and the concentrated phosphoric acid into a reaction kettle with the volume of 100mL, and uniformly stirring;
then, putting the titanium substrate prepared in the step S1 into a reaction kettle, heating the reaction kettle to 120 ℃, preserving heat for 24 hours, and then terminating the reaction;
finally, after the temperature in the reaction kettle is cooled to room temperature, taking out the product from the reaction kettle, washing the product for 2 times by using ultrapure water, and then placing the product in an oven for drying at the drying temperature of 50 ℃ for 24 hours to obtain the titanium implant covered with the titanium phosphate coating (shown in figure 1);
s3, preparing a titanium phosphate/nano hydroxyapatite composite coating on the surface of the titanium substrate:
firstly, weighing 1.11g of anhydrous calcium chloride and 0.701g of hexamethylenetetramine, adding into a reaction kettle, adding 10mL of ultrapure water, and uniformly stirring;
then, putting the titanium implant covered with the titanium phosphate coating prepared in the step S2 into a reaction kettle, heating the reaction kettle to 120 ℃, preserving heat for 12 hours and then stopping the reaction;
and finally, after the temperature in the reaction kettle is cooled to room temperature, taking out the product from the reaction kettle, washing the product for at least 2 times by using ultrapure water, and then placing the product in a drying oven for drying at the drying temperature of 50 ℃ for 24 hours to obtain the titanium implant covered with the titanium phosphate/nano hydroxyapatite composite coating (as shown in figure 2).
The titanium implant sample of the titanium phosphate/nano-hydroxyapatite composite coating prepared in the embodiment 1 is sterilized by high-pressure steam and then placed in a 24-pore plate. MC3T3 cells were plated at 2X 10 4 Density of cells/holePlanted on the surface of the sample, 37 o C was incubated in a container containing 5% carbon dioxide. The cells were cultured for 24h, 96h and 168h for proliferation assays and their cell activity was determined using the CCK-8 kit. The result shows that the titanium implant with the titanium phosphate/nano hydroxyapatite coating has good biocompatibility. The content of OCN in the cell culture solution was determined using a mouse osteocalcin ELISA kit. The result shows that the titanium implant with the titanium phosphate/nano hydroxyapatite coating can improve the content of OCN in cells and has good bone repair capability.
The sample was placed in a 40 kHZ ultrasonic washer at a water temperature of 37 deg.C o C power 180W for 20 minutes. The surface of the obtained sample is observed by a scanning electron microscope, and the result shows that the coating has complete appearance and no peeling trace. And (3) bonding the sample with the strong AB adhesive through a bonding test, and stripping the coating by using a universal mechanical testing machine. The results show that the coating has high bonding strength with the substrate and is difficult to fall off.
Example 2
A preparation method of a bone repair implant with a super-strong bonding strength composite coating comprises the following steps:
s1, cleaning a titanium substrate: processing an industrial pure titanium plate (with the purity of 99.7%) into a substrate blank with the size of 10mm in length, 10mm in width and 0.1 mm in thickness, grinding and flattening the surface of the substrate blank by using 400 grit, 800 grit and 1000 grit silicon carbide paper in sequence, polishing to obtain a titanium matrix, ultrasonically cleaning the titanium matrix in a mixed solution of ethanol and distilled water for 10 minutes, removing stains and grease on the surface of the titanium matrix, drying at room temperature, and reserving for the later step;
s2, preparing a titanium phosphate coating on the surface of the titanium substrate:
firstly, weighing 5mL of hydrogen peroxide (with the concentration of 9 wt%) and 5mL of concentrated phosphoric acid (with the concentration of 8.5 wt%), adding the hydrogen peroxide and the concentrated phosphoric acid into a reaction kettle with the volume of 100mL, and uniformly stirring;
then, putting the titanium substrate prepared in the step S1 into a reaction kettle, heating the reaction kettle to 120 ℃, preserving heat for 24 hours and then terminating the reaction;
finally, after the temperature in the reaction kettle is cooled to room temperature, taking out the product from the reaction kettle, washing the product for 2 times by using ultrapure water, and then placing the product in a drying oven for drying at the drying temperature of 50 ℃ for 24 hours to obtain the titanium implant covered with the titanium phosphate coating;
s3, preparing a titanium phosphate/nano-hydroxyapatite composite coating on the surface of the titanium substrate:
firstly, weighing 1.07g of anhydrous calcium chloride and 0.699g of hexamethylenetetramine, adding into a reaction kettle, adding 10mL of ultrapure water, and uniformly stirring;
then, putting the titanium implant covered with the titanium phosphate coating prepared in the step S2 into a reaction kettle, heating the reaction kettle to 120 ℃, preserving heat for 12 hours and then stopping the reaction;
and finally, after the temperature in the reaction kettle is cooled to room temperature, taking out the product from the reaction kettle, washing the product for at least 2 times by using ultrapure water, and then placing the product in a drying oven for drying at the drying temperature of 50 ℃ for 24 hours to obtain the titanium implant covered with the titanium phosphate/nano-hydroxyapatite composite coating.
Example 3
A preparation method of a bone repair implant with a super-strong bonding strength composite coating comprises the following steps:
s1, cleaning a titanium substrate: processing an industrial pure titanium plate (with the purity of 99.7%) into a substrate blank with the size of 10mm in length, 10mm in width and 0.1 mm in thickness, grinding and flattening the surface of the substrate blank by using 400 grit, 800 grit and 1000 grit silicon carbide paper in sequence, polishing to obtain a titanium matrix, ultrasonically cleaning the titanium matrix in a mixed solution of ethanol and distilled water for 10 minutes, removing stains and grease on the surface of the titanium matrix, drying at room temperature, and reserving for the later step;
s2, preparing a titanium phosphate coating on the surface of the titanium substrate:
firstly, weighing 5mL of hydrogen peroxide (with the concentration of 9 wt%) and 5mL of concentrated phosphoric acid (with the concentration of 8.5 wt%), adding the hydrogen peroxide and the concentrated phosphoric acid into a reaction kettle with the volume of 100mL, and uniformly stirring;
then, putting the titanium substrate prepared in the step S1 into a reaction kettle, heating the reaction kettle to 120 ℃, preserving heat for 24 hours, and then terminating the reaction;
finally, after the temperature in the reaction kettle is cooled to room temperature, taking out the product from the reaction kettle, washing the product for 2 times by using ultrapure water, and then placing the product in a drying oven for drying at 37 ℃ for 48 hours to obtain the titanium implant covered with the titanium phosphate coating;
s3, preparing a titanium phosphate/nano hydroxyapatite composite coating on the surface of the titanium substrate:
firstly, weighing 1.13g of anhydrous calcium chloride and 0.703g of hexamethylenetetramine, adding into a reaction kettle, adding 10mL of ultrapure water, and uniformly stirring;
then, putting the titanium implant covered with the titanium phosphate coating prepared in the step S2 into a reaction kettle, heating the reaction kettle to 120 ℃, preserving heat for 12 hours and then stopping the reaction;
and finally, after the temperature in the reaction kettle is cooled to room temperature, taking out the product from the reaction kettle, washing the product for at least 2 times by using ultrapure water, and then placing the product in a drying oven for drying at the drying temperature of 37 ℃ for 48 hours to obtain the titanium implant covered with the titanium phosphate/nano-hydroxyapatite composite coating.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (2)
1. A preparation method of a bone repair implant with a super-strong bonding strength composite coating is characterized by comprising the following steps:
s1, cleaning a titanium substrate: polishing the surface of the titanium substrate, then ultrasonically cleaning the titanium substrate in a mixed solution of ethanol and distilled water for 10 minutes to remove stains and grease on the surface of the titanium substrate, and drying the titanium substrate at room temperature for later use;
s2, preparing a titanium phosphate coating on the surface of the titanium substrate:
firstly, hydrogen peroxide and concentrated phosphoric acid are weighed according to the same volume ratio and added into a reaction kettle to be uniformly stirred;
then, putting the titanium substrate prepared in the step S1 into a reaction kettle, heating the reaction kettle to 110-130 ℃, preserving heat for 6-24 h, and then terminating the reaction;
finally, after the temperature in the reaction kettle is cooled to room temperature, taking out the product from the reaction kettle, washing the product for at least 2 times by using ultrapure water, and then placing the product in a drying oven for drying at the drying temperature of 50 ℃ for 24 hours to prepare the titanium implant covered with the titanium phosphate coating;
s3, preparing a titanium phosphate/nano-hydroxyapatite composite coating on the surface of the titanium substrate:
first, the molar ratio of 2:1, weighing anhydrous calcium chloride and hexamethylenetetramine, adding the anhydrous calcium chloride and the hexamethylenetetramine into a reaction kettle, adding ultrapure water, and uniformly stirring, wherein the concentration of the anhydrous calcium chloride solution is 6-11 wt%, and the concentration of the hexamethylenetetramine composite solution is 5-10 wt%;
then, putting the titanium implant covered with the titanium phosphate coating prepared in the step S2 into a reaction kettle, heating the reaction kettle to 110-130 ℃, preserving heat for 6-12 h, and then stopping the reaction;
and finally, after the temperature in the reaction kettle is cooled to room temperature, taking out the product from the reaction kettle, washing the product for at least 2 times by using ultrapure water, and then placing the product in a drying oven for drying at the drying temperature of 50 ℃ for 24 hours to obtain the titanium implant covered with the titanium phosphate/nano-hydroxyapatite composite coating.
2. The method for preparing the bone repair implant with the ultra-strong bonding strength composite coating according to claim 1, wherein the method comprises the following steps: in the step S1, the concentration of the hydrogen peroxide is 6wt% -11wt%, and the concentration of the concentrated phosphoric acid is 6wt% -11wt%.
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| CN113652692A (en) * | 2021-08-17 | 2021-11-16 | 河南科技大学 | Preparation method of surface calcification modified titanium-molybdenum-zirconium metastable beta titanium alloy and product thereof |
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| CN113652692A (en) * | 2021-08-17 | 2021-11-16 | 河南科技大学 | Preparation method of surface calcification modified titanium-molybdenum-zirconium metastable beta titanium alloy and product thereof |
Non-Patent Citations (1)
| Title |
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| 黄棣，等: "高结合强度TiP/n-HA复合涂层钛植入体研究", 医用生物力学, vol. 36, 31 August 2021 (2021-08-31), pages 156 * |
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