CN115475278B - Degradable zinc-cerium alloy bone grafting bed device for back of vertebral body - Google Patents
Degradable zinc-cerium alloy bone grafting bed device for back of vertebral body Download PDFInfo
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- CN115475278B CN115475278B CN202210933903.XA CN202210933903A CN115475278B CN 115475278 B CN115475278 B CN 115475278B CN 202210933903 A CN202210933903 A CN 202210933903A CN 115475278 B CN115475278 B CN 115475278B
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- 210000000988 bone and bone Anatomy 0.000 title claims abstract description 80
- UFNRFBFHJJPDNF-UHFFFAOYSA-N [Zn].[Ce] Chemical compound [Zn].[Ce] UFNRFBFHJJPDNF-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 229910000636 Ce alloy Inorganic materials 0.000 title claims abstract description 65
- 239000000843 powder Substances 0.000 claims abstract description 56
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 19
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 16
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 11
- 239000011701 zinc Substances 0.000 claims abstract description 11
- 239000010935 stainless steel Substances 0.000 claims abstract description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- 238000005488 sandblasting Methods 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 31
- 239000002245 particle Substances 0.000 claims description 22
- 230000008569 process Effects 0.000 claims description 22
- 238000004140 cleaning Methods 0.000 claims description 20
- 238000000498 ball milling Methods 0.000 claims description 13
- 229910052593 corundum Inorganic materials 0.000 claims description 12
- 239000010431 corundum Substances 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 12
- 239000004576 sand Substances 0.000 claims description 12
- 238000004381 surface treatment Methods 0.000 claims description 12
- 238000005507 spraying Methods 0.000 claims description 11
- 239000010410 layer Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000005422 blasting Methods 0.000 claims description 8
- 239000006187 pill Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 229910001297 Zn alloy Inorganic materials 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003082 abrasive agent Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- 238000009499 grossing Methods 0.000 claims description 3
- 239000002356 single layer Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 238000000713 high-energy ball milling Methods 0.000 claims description 2
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 13
- 208000035143 Bacterial infection Diseases 0.000 abstract description 4
- 206010061218 Inflammation Diseases 0.000 abstract description 4
- 208000022362 bacterial infectious disease Diseases 0.000 abstract description 4
- 230000004054 inflammatory process Effects 0.000 abstract description 4
- 229910001069 Ti alloy Inorganic materials 0.000 abstract description 3
- 238000006479 redox reaction Methods 0.000 abstract description 3
- 230000008439 repair process Effects 0.000 abstract description 3
- 241000894006 Bacteria Species 0.000 abstract description 2
- 229910000531 Co alloy Inorganic materials 0.000 abstract description 2
- QMTNJXLAAQEFPY-UHFFFAOYSA-N [Zn].[Fe].[Ce] Chemical compound [Zn].[Fe].[Ce] QMTNJXLAAQEFPY-UHFFFAOYSA-N 0.000 abstract description 2
- 230000015556 catabolic process Effects 0.000 abstract description 2
- -1 cerium ions Chemical class 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 239000007943 implant Substances 0.000 abstract 2
- 230000000694 effects Effects 0.000 abstract 1
- 238000001727 in vivo Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 15
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- 208000027418 Wounds and injury Diseases 0.000 description 5
- 239000000956 alloy Substances 0.000 description 5
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- 230000001580 bacterial effect Effects 0.000 description 4
- 230000006837 decompression Effects 0.000 description 4
- 210000001951 dura mater Anatomy 0.000 description 4
- 230000005764 inhibitory process Effects 0.000 description 4
- 238000002684 laminectomy Methods 0.000 description 4
- 239000007857 degradation product Substances 0.000 description 3
- 125000001475 halogen functional group Chemical group 0.000 description 3
- 230000009471 action Effects 0.000 description 2
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- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 238000002513 implantation Methods 0.000 description 2
- 210000000944 nerve tissue Anatomy 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
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- 208000012287 Prolapse Diseases 0.000 description 1
- 206010040026 Sensory disturbance Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 230000002146 bilateral effect Effects 0.000 description 1
- 210000000845 cartilage Anatomy 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000011038 discontinuous diafiltration by volume reduction Methods 0.000 description 1
- 239000007902 hard capsule Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 206010025005 lumbar spinal stenosis Diseases 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000011164 ossification Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 210000000278 spinal cord Anatomy 0.000 description 1
- 210000000273 spinal nerve root Anatomy 0.000 description 1
- 208000005198 spinal stenosis Diseases 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
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- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
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- A—HUMAN NECESSITIES
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- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/54—Biologically active materials, e.g. therapeutic substances
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/09—Mixtures of metallic powders
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/60—Treatment of workpieces or articles after build-up
- B22F10/66—Treatment of workpieces or articles after build-up by mechanical means
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y80/00—Products made by additive manufacturing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
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- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/38—Materials or treatment for tissue regeneration for reconstruction of the spine, vertebrae or intervertebral discs
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- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention relates to a degradable zinc-cerium alloy bone grafting bed device for the rear of a vertebral body, wherein the degradable zinc-cerium alloy bone grafting bed device comprises a net-shaped main body structure and fixing wings on two sides of the net-shaped main body, the degradable zinc-cerium alloy bone grafting bed device is formed by melting degradable zinc-cerium alloy powder through a laser powder bed, and the iron-zinc-cerium alloy powder comprises 1-3wt% of cerium and 97-99wt% of zinc. The implant of the degradable zinc-cerium alloy bone grafting bed device can be naturally degraded in vivo, can disappear from the body after the repair effect is finished, avoids the defect that the implants such as the traditional titanium alloy, cobalt alloy, stainless steel and the like are required to be taken out by secondary operation, and has good antibacterial performance. During service, the cerium ions released by degradation can kill bacteria through oxidation-reduction reaction, thereby avoiding inflammatory reaction caused by bacterial infection.
Description
Technical Field
The invention relates to the technical field of medical materials, in particular to a degradable zinc-cerium alloy bone grafting bed device for the back of a vertebral body.
Background
The prolapse of lumbar intervertebral disc is characterized in that after various parts of lumbar intervertebral disc (nucleus pulposus, annulus fibrosus and cartilage plate) are degenerated to different degrees, the annulus fibrosus is broken under the action of external factors, the nucleus pulposus protrudes from the broken part to cause the shrinkage and volume reduction of various radial lines of vertebral canal and side crypt, and the hard capsule, spinal cord or nerve root are pressed to cause injury, so that the waist and leg are finally caused to generate a series of clinical symptoms such as pain, acid swelling, sensory disturbance and the like, which is one of the common clinical lumbar diseases. To effectively eliminate the disease, a surgical approach of laminectomy, decompression, is commonly used. Due to the complex physiological structure of spinal column, after the laminectomy, the vertebral canal decompression operation is performed, the intervertebral disc is resected through the outside of the dura mater or the inside of the dura mater, so that the lumbar vertebrae are combined. However, the lumbar vertebra is unstable after combination, and complications such as lumbar spinal stenosis and the like are caused, so that spinal fusion operation is needed.
Spinal fusion procedures typically employ an inter-transverse process bone graft fusion outside the spinal column for bone defect repair. Because the spine after laminectomy has no post-column support, the transverse process bone graft cannot be fully embedded and compacted, so that the bone graft blocks fall into the vertebral canal to cause new hard compression of nerve tissues, meanwhile, the transverse process bone graft cannot provide effective mechanical support, and the postoperative internal fixation fracture loosening and the nerve tissues are likely to be stressed and damaged again, so that the postoperative rehabilitation failure is finally caused. Therefore, the effective and biomechanical bone grafting fusion is important after laminectomy and spinal canal decompression. While achieving reliable bone fusion often requires good bone grafting conditions: firstly, the bone grafting bed can provide enough volume and mechanical strength support, so that the bone grafting is fully embedded and compacted, and the effective stability of the vertebra is achieved; secondly, the bone grafting bed and the dura mater sac keep enough gaps to prevent the dura mater sac from adhering with surrounding tissues; thirdly, the bone grafting bed has good biocompatibility, does not generate toxicity to surrounding tissues, and can fully play the roles of bone induction, bone conduction and bone formation of the transplanted bone.
At present, the bone grafting bed is mainly made of non-degradable stainless steel, titanium alloy or cobalt alloy and other materials, however, the bone grafting bed prepared from the non-degradable materials is implanted into a body to be used as a foreign body for a long time, and the bone grafting bed is taken out through a secondary operation after service completion, so that secondary injury is caused to a patient. More importantly, local vicinity of the bone graft bed may cause inflammatory reaction due to bacterial infection, resulting in failure of bone repair. Therefore, a bone grafting bed device which can be naturally degraded after implantation, has no toxicity of degradation products and has good antibacterial effect is sought, and the bone grafting bed device becomes a problem which needs to be solved after the vertebral canal decompression operation.
Disclosure of Invention
It is an object of the present invention to address at least the above problems and/or disadvantages and to provide at least the advantages described below.
The degradable zinc-cerium alloy bone grafting bed device for the rear of the vertebral body is characterized by comprising a net-shaped main body structure and fixing wings on two sides of the net-shaped main body, wherein degradable zinc-cerium alloy powder is formed by melting a laser powder bed, and the iron-zinc-cerium alloy powder comprises 1-3wt% of cerium and 97-99wt% of zinc.
The preparation method of the degradable zinc-cerium alloy bone grafting bed device for the back of the vertebral body comprises the following steps:
step one, constructing a three-dimensional bone grafting bed model through 3D modeling;
step two, mixing zinc-cerium powder by a high-energy ball milling process to obtain degradable zinc-cerium alloy powder;
and thirdly, selecting a sintering process by laser, and printing and sintering the degradable cerium-zinc alloy bone grafting bed device according to the built three-dimensional bone grafting bed model.
Preferably, the zinc-cerium alloy in the second step is prepared by: weighing 1-3 parts of cerium powder and 97-99 parts of zinc powder by mass, taking stainless steel grinding balls as grinding bodies, uniformly mixing in an argon atmosphere by a planetary ball mill, wherein the ball milling speed is 150rpm/min, and the ball milling time is 2-3 hours, so as to obtain the degradable zinc-cerium alloy powder.
Preferably, the method comprises the steps of setting the rest time for 30min of each continuous ball milling, then reversing the high-energy ball mill for 30min, and taking out the zinc-cerium alloy powder in a vacuum glove box after the ball milling is completed and the tank body of the ball milling tank is completely cooled.
Preferably, the ball-to-material ratio between the stainless steel grinding balls and the zinc-cerium premixed powder is 10:1.
preferably, the particle size of the zinc powder is 17-45 μm, and the purity is 99.9%; the particle size of the cerium powder is 1-5 mu m, and the purity is 99.9%; the purity of the argon gas was 99.999%.
Preferably, the laser selects a sintering process: the zinc-cerium alloy powder is paved in a laser powder bed melting and forming system, and is printed and sintered into a degradable cerium/zinc alloy bone grafting bed device layer by layer according to the built three-dimensional model, wherein an alternate scanning strategy is adopted, namely, the scanning direction is rotated by 90 degrees compared with the previous layer; the laser scanning power is 45-55W, the scanning speed is 270-320 mm/s, and the single-layer powder thickness is 40-60 mu m.
Preferably, the convex surface of the mesh main body and the outer surface of the fixing wing of the degradable zinc-cerium alloy bone grafting bed device are frosted surfaces, the concave surface of the mesh main body and the inner surface of the fixing wing are smooth surfaces, and the surface treatment steps of the degradable zinc-cerium alloy bone grafting bed device are as follows:
firstly, carrying out primary surface treatment on the whole bone grafting bed device by utilizing a sand blasting process, wherein corundum sand with the powder particle size of 80 meshes is adopted as abrasive for sand blasting, the sand blasting distance is 10cm, the sand blasting pressure is 0.6-0.8 MPa, the spraying time is 1-1.5 min, and the coverage rate is more than 100%;
secondly, smoothing the concave surface of the net-shaped main body and the inner surface of the fixed wing of the bone grafting bed device by using a shot blasting process, wherein the shot blasting adopts glass shots with powder particle diameters of 180-220 meshes as abrasive materials, the sand blasting distance is 10-15 cm, the sand blasting pressure is 0.5-0.8 MPa, the spraying time is 2-3 min, and the coverage rate is more than 100%;
step three, the convex surface of the net-shaped main body of the bone grafting bed device and the outer surface of the fixed wing are frosted by utilizing a sand blasting process, corundum sand with the powder particle size of 24-80 meshes and glass pill mixed abrasive with the powder particle size of 180-220 meshes are adopted for sand blasting, wherein the proportion of the corundum sand to the glass pills is 4:1, the sand blasting distance is 10-15 cm, the sand blasting pressure is 3.0MPa, the spraying time is 0.5-1 min, and the coverage rate is more than 100%;
step four, cleaning the bone grafting bed device obtained in the step three: and (3) under the assistance of an ultrasonic cleaner, cleaning for 2-3 times by using acetone, cleaning for 3-4 times by using absolute ethyl alcohol, wherein the cleaning time is about 10min each time, and drying by using nitrogen after cleaning.
The invention provides a degradable zinc-cerium alloy bone grafting bed device, which has the following action principle:
the bone grafting bed device is prepared by using zinc-cerium alloy materials. As a biomedical metal material, the metal zinc has natural degradability, the degradation products are nontoxic and can be absorbed by human bodies, meanwhile, the metal zinc has good biocompatibility and can not cause secondary injury to the human bodies, and the alloy element rare earth cerium can generate good antibacterial effect through oxidation-reduction reaction. The bone grafting bed device prepared from the zinc-cerium alloy material has good biocompatibility, can be naturally degraded in a human body after being implanted into the human body, can not cause secondary injury to the human body, and has good antibacterial effect, and can avoid inflammatory reaction caused by bacterial infection.
Compared with the prior art, the preparation method of the degradable zinc-cerium alloy bone grafting bed device has the following advantages:
(1) Compared with devices made of non-degradable alloys such as titanium alloy, stainless steel and the like, the device made of the degradable zinc-cerium alloy material can be naturally degraded, and degradation products are nontoxic and can be absorbed by a human body, so that secondary operation injury caused after the non-degradable bone grafting bed device is implanted is avoided.
(2) The degradable zinc-cerium alloy bone grafting bed device has good antibacterial performance. During service, the cerium ions released by degradation can kill bacteria through oxidation-reduction reaction, thereby avoiding inflammatory reaction caused by bacterial infection.
(3) The degradable zinc-cerium alloy bone implantation bed device is structurally designed, and the net-shaped main body of the device adopts a smooth concave surface to be contacted with the dural sac, so that the device can be prevented from being adhered to the device, and the convex surface of the net-shaped main body adopts a frosted structure, so that the device is convenient to combine with transplanted bone, and forms an integrated structure.
Description of the drawings:
FIG. 1 is a chart showing the antibacterial property test in example 1, wherein chart a is a chart showing a halo method bacteriostasis zone, chart b is a chart showing comparison of the width of the bacteriostasis zone in chart a, chart c is a chart showing a test of bacterial inhibition rate, and chart d is a chart showing comparison of the results of bacterial inhibition rate in chart c;
fig. 2 is a view showing a bone grafting bed device according to the present invention.
The specific embodiment is as follows:
in order that the invention may be readily understood, a more complete description of the invention will be rendered by reference to the appended drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The following describes in more detail the embodiments of the present invention in terms of several specific examples.
Example 1:
(1) The three-dimensional model of the bone grafting bed device is constructed by utilizing 3D modeling, the bone grafting bed device comprises a net-shaped main body 1 and fixed wings 2 on two sides of the net-shaped main body, wherein the net-shaped main body 1 is provided with a plurality of net-shaped circular holes 3, the fixed wings 2 are provided with a plurality of screw holes 4 which are distributed in bilateral symmetry, and the net-shaped main body part of the device is designed into an arc-shaped net structure and adjusts the angle of a central angle according to the cone curvature of the back of a vertebral body of a patient.
(2) Weighing 0.2g of cerium powder with an electronic balance, wherein the particle size of the cerium powder is 1-5 mu m, weighing 9.8g of zinc powder, and the particle size of the zinc powder is 17-45 mu m, wherein the purity of the zinc powder is 99.9%; the two powders are added into a hard stainless steel ball milling tank, 100g of stainless steel grinding balls with the diameter of 3mm are added, and ball milling is carried out for 2 hours under the protection of 99.999% high-purity argon atmosphere in a planetary ball milling mode at the rotating speed of 150 rpm/min. And taking out the zinc-cerium alloy powder from the vacuum glove box after the tank body is completely cooled.
(3) The zinc-cerium alloy powder is paved in a laser powder bed melting and forming system, and is printed and sintered into a degradable cerium/zinc alloy bone grafting bed device layer by layer according to the built three-dimensional model, wherein an alternate scanning strategy is adopted, namely, the scanning direction is rotated by 90 degrees compared with the previous layer; the laser scanning power is 50W, the scanning speed is 300mm/s, and the thickness of the single-layer powder is 50 mu m.
In example 1, performance characterization was performed for the prepared degradable zinc-cerium alloy bone grafting bed device;
(a) The antibacterial property of the zinc-cerium alloy sample is qualitatively and quantitatively tested, and the zinc-cerium alloy is qualitatively tested by a bacteriostasis ring test method (a halo method), wherein the test result is shown in figure 1, the width of a bacteriostasis ring of the zinc-cerium alloy is larger than that of a zinc metal bacteriostasis ring, and the zinc-cerium alloy has obvious antibacterial capability; the antibacterial property of the zinc-cerium alloy is quantitatively tested, and the bacterial inhibition rate is higher than 80% and is obviously superior to that of zinc metal.
(b) And (3) preparing a tensile test bar by the same laser sintering process as the step (3), and testing the tensile mechanical property of the test bar to obtain the ultimate tensile strength of 247.4MPa, the yield strength of 180.6MPa and the tensile deformation amount of 7.6 percent, wherein the tensile test bar is improved to a certain extent compared with zinc metal.
Example 2:
(1) The remaining parameters were the same as in example 1, so that details were not repeated, except that 0.1g of cerium powder and 9.9g of zinc powder were weighed by an electronic balance.
(a) The mechanical property test shows that the ultimate tensile strength of the zinc-cerium alloy sample is 194.1MPa, the yield strength is 138.5MPa, and the tensile deformation amount is 6%, and the zinc-cerium alloy sample has a certain degree of improvement compared with zinc metal.
Example 3:
the other parameters are the same as those in embodiment 1, and thus will not be described in detail. Except that 0.3g of cerium powder and 9.7g of cerium powder were weighed using an electronic balance.
(a) The mechanical property test shows that the ultimate tensile strength of the zinc-cerium alloy sample is 230.3MPa, the yield strength is 188.2MPa, and the tensile deformation amount is 6.8 percent, and the zinc-cerium alloy sample is improved to a certain extent compared with zinc metal.
Example 4:
the other parameters are the same as those in embodiment 1, and thus will not be described in detail. The method is characterized in that the obtained bone grafting bed device is subjected to surface treatment, and the steps are as follows:
firstly, carrying out primary surface treatment on the whole bone grafting bed device by utilizing a sand blasting process, wherein corundum sand with the powder particle size of 80 meshes is adopted as abrasive for sand blasting, the sand blasting distance is 10cm, the sand blasting pressure is 0.6MPa, the spraying time is 1min, and the coverage rate is more than 100%;
secondly, smoothing the concave surface of the mesh main body of the bone grafting bed device and the inner surface of the fixed wing by using a shot blasting process, wherein the shot blasting adopts glass shots with powder particle sizes between 220 meshes as abrasive materials, the sand blasting distance is 10cm, the sand blasting pressure is 0.8MPa, the injection time is 2min, and the coverage rate is more than 100%;
step three, the convex surface of the mesh main body of the bone grafting bed device and the outer surface of the fixed wing are frosted by utilizing a sand blasting process, and corundum sand with the powder particle size of 80 meshes and glass pill mixed abrasive with the powder particle size of 220 meshes are adopted for sand blasting, wherein the proportion of the corundum sand to the glass pills is 4:1, the sand blasting distance is 15cm, the sand blasting pressure is 3.0MPa, the spraying time is 1min, and the coverage rate is more than 100%;
step four, cleaning the bone grafting bed device obtained in the step three: under the assistance of an ultrasonic cleaner, acetone is used for cleaning for 3 times, absolute ethyl alcohol is used for cleaning for 3 times, the cleaning time is about 10 minutes each time, and nitrogen is used for drying after the cleaning is completed.
(a) The test strips are subjected to the same surface treatment, and the ultimate compressive strength of the zinc-cerium alloy test sample is 283.4MPa and the yield strength of the test strip is 202.8MPa, so that the ultimate tensile strength of the test strip is improved to a certain extent compared with that of the zinc-cerium alloy test sample without surface treatment.
Example 5:
the other parameters are the same as those in embodiment 2, and thus will not be described again. The difference is that the obtained bone grafting bed device is subjected to surface treatment. The method comprises the following steps: the obtained bone grafting bed device is subjected to surface treatment, and the steps are as follows:
firstly, carrying out primary surface treatment on the whole bone grafting bed device by utilizing a sand blasting process, wherein corundum sand with the powder particle size of 80 meshes is adopted as abrasive for sand blasting, the sand blasting distance is 15cm, the sand blasting pressure is 0.8MPa, the spraying time is 1.5min, and the coverage rate is more than 100%;
step two, carrying out smooth treatment on the inner surface of the bone grafting bed device by using a shot blasting process, wherein the shot blasting adopts glass shots with powder particle sizes between 180 meshes as abrasive materials, the sand blasting distance is 15cm, the sand blasting pressure is 0.8MPa, the spraying time is 3min, and the coverage rate is more than 100%;
step three, carrying out rough treatment on the outer surface of the bone grafting bed device by utilizing a sand blasting process, wherein corundum sand with the powder particle size of 24 meshes and glass pill mixed abrasive with the powder particle size of 180 meshes are adopted for sand blasting, and the proportion of the corundum sand to the glass pills is 4:1, the sand blasting distance is 10cm, the sand blasting pressure is 3.0MPa, the spraying time is 0.5min, and the coverage rate is more than 100%;
step four, cleaning the bone grafting bed device obtained in the step three: and (3) under the assistance of an ultrasonic cleaner, cleaning for 2 times by using acetone, cleaning for 4 times by using absolute ethyl alcohol, wherein the cleaning time is about 10 minutes each time, and drying by using nitrogen after cleaning.
(a) The ultimate tensile strength of the zinc-cerium alloy sample is 217.6MPa and the yield strength is 157.3MPa through mechanical property test, and the ultimate tensile strength of the zinc-cerium alloy sample is improved to a certain extent compared with that of the zinc-cerium alloy sample which is not subjected to surface treatment.
Comparative example 1:
the rest of the experimental conditions were identical to example 1, except that the cerium was present in a proportion of up to 0wt%.
(a) The antibacterial property of the zinc-cerium alloy is qualitatively and quantitatively tested, and the antibacterial ring of the zinc-cerium alloy is narrower and obviously smaller than that of the zinc metal by using a antibacterial ring test method (a halo method), wherein the test result is shown in figure 1; the antibacterial property of the zinc-cerium alloy is quantitatively tested, and the bacterial inhibition rate is less than 40 percent
(b) The ultimate tensile strength of the zinc-cerium alloy sample is 103.7MPa, the yield strength is 79.9MPa and the tensile deformation amount is 5.1 percent through mechanical property test.
Finally, it should be noted that: the above examples are only specific embodiments of the present invention, and are not intended to limit the scope of the present invention, but it should be understood by those skilled in the art that the present invention is not limited thereto, and that the present invention is described in detail with reference to the foregoing examples: any person skilled in the art may modify or easily conceive of the technical solution described in the foregoing embodiments, or perform equivalent substitution of some of the technical features, while remaining within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention, and are intended to be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope.
Claims (3)
1. The preparation method of the degradable zinc-cerium alloy bone grafting bed device for the back of the vertebral body is characterized in that the degradable zinc-cerium alloy bone grafting bed device comprises a net-shaped main body structure and fixing wings on two sides of the net-shaped main body, the degradable zinc-cerium alloy bone grafting bed device is formed by melting degradable zinc-cerium alloy powder through a laser powder bed, and the zinc-cerium alloy powder comprises 1-3 wt% of cerium and 97-99 wt% of zinc;
the preparation method of the degradable zinc-cerium alloy bone grafting bed device for the rear of the vertebral body comprises the following steps:
step one, constructing a three-dimensional bone grafting bed model through 3D modeling;
step two, mixing zinc-cerium powder by a high-energy ball milling process to obtain degradable zinc-cerium alloy powder;
step three, a sintering process is selected through laser, and a degradable cerium-zinc alloy bone grafting bed device is printed and sintered according to the built three-dimensional bone grafting bed model;
in the second step, the degradable zinc-cerium alloy powder is prepared by: weighing 1-3 parts of cerium powder and 97-99 parts of zinc powder in parts by weight, taking stainless steel grinding balls as grinding bodies, uniformly mixing in an argon atmosphere through a planetary ball mill, wherein the ball milling speed is 150rpm, and the ball milling time is 2-3 hours, wherein each continuous ball milling is set to be 30 minutes for rest 15 minutes, then the high-energy ball mill is reversed for 30 minutes, and after the ball milling is completed, taking out zinc-cerium alloy powder in a vacuum glove box after the ball milling tank body is completely cooled, so as to obtain degradable zinc-cerium alloy powder; the ball-to-material ratio between the stainless steel grinding ball and the zinc-cerium premixed powder is 10:1, a step of;
the surface treatment steps of the degradable zinc-cerium alloy bone grafting bed device are as follows:
firstly, carrying out primary surface treatment on the whole bone grafting bed device by utilizing a sand blasting process, wherein corundum sand with the powder particle size of 80 meshes is adopted as abrasive for sand blasting, the sand blasting distance is 10cm, the sand blasting pressure is 0.6-0.8 MPa, the spraying time is 1-1.5 min, and the coverage rate is more than 100%;
secondly, smoothing the concave surface of the mesh main body of the bone grafting bed device and the inner surface of the fixed wing by using a shot blasting process, wherein the shot blasting adopts glass shots with powder particle size of 180-220 meshes as abrasive materials, the sand blasting distance is 10-15 cm, the sand blasting pressure is 0.5-0.8 MPa, the spraying time is 2-3 min, and the coverage rate is more than 100%;
step three, the convex surface of the mesh main body of the bone grafting bed device and the outer surface of the fixed wing are frosted by utilizing a sand blasting process, corundum sand with the powder particle size of 24-80 meshes and glass pill mixed abrasive with the powder particle size of 180-220 meshes are adopted for sand blasting, wherein the proportion of the corundum sand to the glass pills is 4:1, the sand blasting distance is 10-15 cm, the sand blasting pressure is 3.0MPa, the spraying time is 0.5-1 min, and the coverage rate is more than 100%;
step four, cleaning the bone grafting bed device obtained in the step three: under the assistance of an ultrasonic cleaner, acetone is used for cleaning 2-3 times, absolute ethyl alcohol is used for cleaning 3-4 times, each cleaning time is about 10min, and nitrogen is used for drying after cleaning is completed.
2. The method for preparing the degradable zinc-cerium alloy bone grafting bed device according to claim 1, wherein the particle size of the zinc powder is 17-45 μm, and the purity is 99.9%; the particle size of the cerium powder is 1-5 mu m, and the purity is 99.9%; the purity of the argon gas was 99.999%.
3. The method for preparing the degradable zinc-cerium alloy bone grafting bed device according to claim 1, wherein the laser selection sintering process comprises the following steps: the zinc-cerium alloy powder is paved in a laser powder bed melting and forming system, and is printed and sintered into a degradable cerium/zinc alloy bone grafting bed device layer by layer according to the built three-dimensional model, wherein an alternate scanning strategy is adopted, namely, the scanning direction is rotated by 90 degrees compared with the previous layer; the laser scanning power is 45-55W, the scanning speed is 270-320 mm/s, and the thickness of single-layer powder is 40-60 mu m.
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