CN109082569A - A kind of preparation method of nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material - Google Patents
A kind of preparation method of nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material Download PDFInfo
- Publication number
- CN109082569A CN109082569A CN201811069235.0A CN201811069235A CN109082569A CN 109082569 A CN109082569 A CN 109082569A CN 201811069235 A CN201811069235 A CN 201811069235A CN 109082569 A CN109082569 A CN 109082569A
- Authority
- CN
- China
- Prior art keywords
- magnesium
- composite material
- magnetic
- temperature
- radiography
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
-
- 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
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/02—Inorganic materials
- A61L31/022—Metals or alloys
-
- 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
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L31/18—Materials at least partially X-ray or laser opaque
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1073—Infiltration or casting under mechanical pressure, e.g. squeeze casting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/12—Making non-ferrous alloys by processing in a semi-solid state, e.g. holding the alloy in the solid-liquid phase
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/04—Alloys based on magnesium with zinc or cadmium as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0036—Matrix based on Al, Mg, Be or alloys thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Vascular Medicine (AREA)
- Surgery (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Life Sciences & Earth Sciences (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- Heart & Thoracic Surgery (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Materials For Medical Uses (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
Abstract
A kind of preparation method of nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material, is related to a kind of preparation method of magnesium-based composite material.The present invention is to solve the existing bio-medical magnesium-based composite material targeting technical problems that stationkeeping ability is poor, forming capacity is low.The present invention: one, nano-magnetic radiography particle combination is prepared；Two, ultrasonic coupling stirring Self-controlled processing, classification alternating temperature infiltration are hot-forming.The present invention is conducive to improve nanoscale silica hollow microspheres and Fe 3 O 4 magnetic particle interface activity by high-temperature machinery ball milling, ultrasonic coupling stirs Self-controlled processing, magnesium liquid can be reduced to be mingled with, improve structural homogenity, enhancing targeting stationkeeping ability, classification alternating temperature hot pressing can be further improved infiltration ability, it reduces casting flaw and refines crystal grain, under the action of ultrasonic coupling stirring Self-controlled processing and hot-forming classification alternating temperature infiltration, magnesium-based composite material obdurability can be made to be significantly improved.
Description
Technical field
The present invention relates to a kind of preparation methods of biological magnesium-based composite material.
Background technique
The curative effect to attract people's attention is achieved after the treatment of metallic support applying clinical, but easily leads to thrombosis, restenosis rate
Height, the problems such as causing vascular damaged.Magnesium base alloy is degradable, and has preferable vessel support power, efficiently reduces bracket
Restenosis, thus get the attention.But traditional magnesium base alloy cannot achieve to the efficient diagnosis of living tissue disease and
Real time monitoring, and intensity is low, plasticity is poor.
In view of the above problems, meso-porous nano biomaterial due to adjustable nanometer-size, high-specific surface area and
Kong Rong, chemical functional group abundant and good biocompatibility and degradability can be used as radiography particle and be easy to replace
It dissolves and ruptures in blood, and the gas microbubbles contrast agent that partial size is uncontrollable, be expected to diagnose in following mankind's major disease
It plays a significant role in treatment.Wherein mesoporous silicon oxide hollow nano-material has good biocompatibility and machinery steady
It is qualitative, and there is huge cavity nanostructure, high-specific surface area, macropore to hold, can produce strong echo under contrast mode
Signal can load guest molecule.Magnetic ferroferric oxide nanometer material has and commonly receives as a kind of special nano material
The fundamental characteristics of rice material, also has both special superparamagnetism and class enzymatic activity.
Summary of the invention
The present invention is to solve the targeting of existing bio-medical magnesium-based composite material, stationkeeping ability is poor, forming capacity is low
Technical problem, and a kind of nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material is provided
Preparation method.
The preparation of nano silica of the invention/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material
Method carries out according to the following steps:
One, nano silica/Fe 3 O 4 magnetic radiography particle combination is prepared: nano silica is hollow micro-
Ball and ferroferric oxide magnetic nano-particles carry out high energy ball milling under conditions of temperature is 250 DEG C~400 DEG C and mix, then into
Row hot pressing, cooled to room temperature obtain nano silica/Fe 3 O 4 magnetic radiography particle combination；
The mass ratio of the nanoscale silica hollow microspheres and ferroferric oxide magnetic nano-particles be 1:(1.8~
3)；
The Ball-milling Time of the high energy ball milling mixing is 0.5h~1.5h, and ball milling speed is 250r/min~400r/
min；
The temperature of the hot pressing is 250 DEG C~400 DEG C, pressure is 150MPa~250MPa, dwell time 3min；
Two, nano silica/Fe 3 O 4 magnetic radiography particle combination that step 1 obtains is heated to 150 DEG C
It~250 DEG C, is then added in the magnesium slurry of semisolid, is warming up to 680 DEG C~760 DEG C, the magnesium-based composite material for obtaining liquid is molten
Body, then temperature is 680 DEG C~760 DEG C, ultrasonic power is 600W~1800W and mechanical stirring rate be 500rpm~
The pure magnesium that temperature is 100 DEG C, the liquid after being adjusted is added under conditions of 1700rpm into the magnesium-based composite material melt of liquid
State magnesium alloy, then temperature is 680 DEG C~760 DEG C, ultrasonic power is 600W~1800W and mechanical stirring rate is 500rpm
Ultrasound 15min~30min is stirred under conditions of~1700rpm；Then heat to 780 DEG C, be subsequently placed at temperature be 550 DEG C~
It is hot-forming that classification alternating temperature infiltration is carried out in 650 DEG C of mold, obtains nano silica/Fe 3 O 4 magnetic radiography particle
Enhance biological magnesium-based composite material；
Nano silica/Fe 3 O 4 magnetic radiography particle combination in the liquid magnesium alloy adjusted
Quality is divided into 1%~15%；
The magnesium slurry of the semisolid is made of by mass fraction the Mg of 8% Zn, 4% Sr and 88%；
Tri- elements of Zn, Sr and Mg are formed by mass fraction in the liquid magnesium alloy adjusted are as follows: 2% Zn,
The Mg of 1% Sr and 97%；
It is as follows that the classification alternating temperature infiltrates hot-forming method: in temperature be 550 DEG C~650 DEG C and pressure is
Pressure maintaining 1min~2min carries out first order hot pressing under conditions of 300MPa~500MPa；Then temperature be 400 DEG C~550 DEG C and
Pressure maintaining 5min~8min progress second level hot pressing under conditions of pressure is 450MPa~700MPa, and the second level hot pressing
Temperature is less than the temperature of first order hot pressing.
The temperature of the magnesium slurry of the semisolid is 620 DEG C~640 DEG C.
The present invention is conducive to improve nanoscale silica hollow microspheres and Fe 3 O 4 magnetic by high-temperature machinery ball milling
Particle interface activity, ultrasonic coupling stir Self-controlled processing, it is possible to reduce magnesium liquid is mingled with, and improves structural homogenity, enhancing targeting
Stationkeeping ability, classification alternating temperature hot pressing can be further improved infiltration ability, reduce casting flaw and refine crystal grain, in ultrasonic coupling
It can make nano silica/Fe 3 O 4 magnetic under the action of the processing of stirring Self-controlled and classification alternating temperature infiltration are hot-forming
Radiography particulate reinforcement biology magnesium-based composite material obdurability is significantly improved.
A kind of a kind of Biological magnesium alloy of the Mg-Zn-Sr alloy as degradable angiocarpy bracket, intensity is low, moulding
Difference cannot be detected real-time intravascular stent situation by external device, joined silica/ferroso-ferric oxide radiography in the present invention
After particle, it can improve obdurability, and vitro detection may be implemented；Compared with high alloy content in the magnesium slurry of semisolid of the invention
Easily realize semisolid, reduction is mingled with, but alloying element is excessively high will lead to second mutually more, and degradation speed is too fast in alloy body, institute
After pure magnesium Dilute Alloy is then added, alloy corrosion resistance energy can be improved.
The specific purposes of present invention combination body implanting material and use environment select original from the thought of bionic principle
Material comprehensively considers the factors such as the influence of the ingredient and institutional framework of material to material mechanical performance and corrosion resistance, uses
Nano silica/Fe 3 O 4 magnetic radiography particle prepares biological magnesium-based composite material as reinforcement, fixed in addition to targeting
Position is convenient for medical diagnosis, also has the advantage that additive amount is few, performance increase rate is big, obtains the synchronous biology improved of obdurability
Magnesium-based composite material.
Beneficial effects of the present invention:
The first step is made by high-temperature machinery ball milling and hot pressing for nano silica/Fe 3 O 4 magnetic in the present invention
Shadow particle combination, this method nano silica/Fe 3 O 4 magnetic radiography grain obtained with higher interfacial activity
Sub- combination can significantly improve the combination degree with Biological magnesium alloy matrix；Second step ultrasonic coupling stirs Self-controlled processing,
Magnesium liquid can be reduced to be mingled with, improve structural homogenity, enhancing targeting stationkeeping ability, classification alternating temperature hot pressing can be further improved leaching
Infiltration ability reduces casting flaw and refines crystal grain, is hot pressed into ultrasonic coupling stirring Self-controlled processing and classification alternating temperature infiltration
It can make nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material obdurability under the action of type
Be significantly improved, tensile strength is reached for 380MPa or more, and yield strength reaches 350MPa or more, elongation percentage reach 9% with
On.
Detailed description of the invention
Fig. 1 is that the classification alternating temperature infiltration in specific embodiment one in the hot pressing and step 2 of step 1 is hot-forming used
Device schematic diagram；
Fig. 2 is the signal that the classification alternating temperature in specific embodiment one in step 2 infiltrates hot-forming device used
Figure；
Fig. 3 is that nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based of one preparation of test is compound
The optical microstructure of material schemes；
Fig. 4 is that nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based of four preparation of test is compound
The optical microstructure of material schemes；
Fig. 5 is engineering stress-engineering strain curve graph；
Fig. 6 is engineering stress-engineering strain curve graph；
Fig. 7 is engineering stress-engineering strain curve graph.
Specific embodiment
Specific embodiment 1: present embodiment is that a kind of nano silica/Fe 3 O 4 magnetic radiography particle increases
The preparation method of Johnson & Johnson's object magnesium-based composite material, specifically carries out according to the following steps:
One, nano silica/Fe 3 O 4 magnetic radiography particle combination is prepared: nano silica is hollow micro-
Ball and ferroferric oxide magnetic nano-particles carry out high energy ball milling under conditions of temperature is 250 DEG C~400 DEG C and mix, then into
Row hot pressing, cooled to room temperature obtain nano silica/Fe 3 O 4 magnetic radiography particle combination；
The mass ratio of the nanoscale silica hollow microspheres and ferroferric oxide magnetic nano-particles be 1:(1.8~
3)；
The Ball-milling Time of the high energy ball milling mixing is 0.5h~1.5h, and ball milling speed is 250r/min~400r/
min；
The temperature of the hot pressing is 250 DEG C~400 DEG C, pressure is 150MPa~250MPa, dwell time 3min；
Two, nano silica/Fe 3 O 4 magnetic radiography particle combination that step 1 obtains is heated to 150 DEG C
It~250 DEG C, is then added in the magnesium slurry of semisolid, is warming up to 680 DEG C~760 DEG C, the magnesium-based composite material for obtaining liquid is molten
Body, then temperature is 680 DEG C~760 DEG C, ultrasonic power is 600W~1800W and mechanical stirring rate be 500rpm~
The pure magnesium that temperature is 100 DEG C, the liquid after being adjusted is added under conditions of 1700rpm into the magnesium-based composite material melt of liquid
State magnesium alloy, then temperature is 680 DEG C~760 DEG C, ultrasonic power is 600W~1800W and mechanical stirring rate is 500rpm
Ultrasound 15min~30min is stirred under conditions of~1700rpm；Then heat to 780 DEG C, be subsequently placed at temperature be 550 DEG C~
It is hot-forming that classification alternating temperature infiltration is carried out in 650 DEG C of mold, obtains nano silica/Fe 3 O 4 magnetic radiography particle
Enhance biological magnesium-based composite material；
Nano silica/Fe 3 O 4 magnetic radiography particle combination in the liquid magnesium alloy adjusted
Quality is divided into 1%~15%；
The magnesium slurry of the semisolid is made of by mass fraction the Mg of 8% Zn, 4% Sr and 88%；
Tri- elements of Zn, Sr and Mg are formed by mass fraction in the liquid magnesium alloy adjusted are as follows: 2% Zn,
The Mg of 1% Sr and 97%；
It is as follows that the classification alternating temperature infiltrates hot-forming method: in temperature be 550 DEG C~650 DEG C and pressure is
Pressure maintaining 1min~2min carries out first order hot pressing under conditions of 300MPa~500MPa；Then temperature be 400 DEG C~550 DEG C and
Pressure maintaining 5min~8min progress second level hot pressing under conditions of pressure is 450MPa~700MPa, and the second level hot pressing
Temperature is less than the temperature of first order hot pressing.
Classification alternating temperature infiltration in the hot pressing and step 2 of step one in present embodiment one is hot-forming used
Device as shown in Figure 1, it is made of ultrasonic amplitude transformer 1, press ram 2, upper cushion block 3, lower cushion block 4 and furnace body 5；Ultrasound
The upper surface of amplitude transformer 1 and press ram 2 are fixed, and upper cushion block 3 is horizontally set in furnace body 5, the lower end surface of ultrasonic amplitude transformer 1
It is in close contact with the upper surface of upper cushion block 3, ultrasonic amplitude transformer 1 passes through the upper surface of furnace body 5, the side wall and furnace of ultrasonic amplitude transformer 1
The upper surface of body 5 seals and the upper surface of the side wall of ultrasonic amplitude transformer 1 and furnace body 5 is to be slidably connected, and lower cushion block 4 is fixed on furnace body
5 inner bottom surface, heating source 5-1 are fixed on the side wall of furnace body 5；The application method of the present apparatus is as follows: by 1 He of ultrasonic amplitude transformer
Upper cushion block 3 takes out from furnace body 5, and the material for being intended to processing is added in furnace body 5 (being the mold of step 2), then is being intended to add
It is horizontally arranged upper cushion block 3 on the material of work, is put into the upper end of ultrasonic amplitude transformer 1 and the lower end surface of ultrasonic amplitude transformer 1 and upper cushion block 3
Face is in close contact, and starting heating source 5-1 is heated, and applies pressure to ultrasonic amplitude transformer 1 by press ram 2, so that on
3 pairs of the cushion block materials to be processed carry out hot pressing, after first order hot pressing, close heating source 5-1, are then down to second to temperature
When grade hot pressing temperature, carry out second level hot pressing, ultrasonic amplitude transformer 1 can transmit in load to blank, the effect of upper cushion block 3 be
Apply classification alternating temperature infiltration hot pressing when transmit load, moved downwardly together with the material to be processed, the effect of lower cushion block 4 be
Apply the material to be processed of limitation when handing over the hot pressing of frequency ultrasonic coupling to move downward.
Device used in ultrasonic agitation in the step of present embodiment two is as shown in Fig. 2, it is by heating source 6, machinery
Blender 7, ultrasonic amplitude transformer 8 and furnace body 9 form；Heating source 6 is fixed on the side wall of furnace body 9, and mechanical agitator 7 and ultrasound become
Width bar 8 is each passed through the upper surface of furnace body 9 and seals with the upper surface of furnace body 9 and fixes；The application method of the present apparatus is as follows: being intended to
The magnesium alloy fused mass of processing is poured into furnace body 9, then be added preheating after solid pure magnesium, while start heating source 6, machinery stirs
Device 7 and ultrasonic amplitude transformer 8 are mixed, the mechanical stirring under ultrasonic vibration effect is carried out to magnesium alloy fused mass.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: nanometer described in step 1
The partial size of SiO 2 hollow microsphere is 40nm~100nm, and aperture is 15nm~35nm, and the porosity is 85%~100%.Other
It is same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: it is described in step 1
The partial size of ferroferric oxide magnetic nano-particles is 30nm~100nm.Other are the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: the nanometer
The mass ratio of SiO 2 hollow microsphere and ferroferric oxide magnetic nano-particles is 1:2.Other with specific embodiment one to
One of three is identical.
Specific embodiment 5: present embodiment is unlike specific embodiment four: obtaining step 1 in step 2
To nano silica/Fe 3 O 4 magnetic radiography particle combination be heated to 200 DEG C, be then added to the magnesium of semisolid
In slurry.Other are identical as specific embodiment four.
The present invention is verified with following tests:
Test one: this test is multiple for a kind of nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based
The preparation method of condensation material specifically carries out according to the following steps:
One, nano silica/Fe 3 O 4 magnetic radiography particle combination is prepared: nano silica is hollow micro-
Ball carries out high energy ball milling with ferroferric oxide magnetic nano-particles under conditions of temperature is 300 DEG C and mixes, and then carries out hot pressing,
Cooled to room temperature obtains nano silica/Fe 3 O 4 magnetic radiography particle combination；
The partial size of nanoscale silica hollow microspheres described in step 1 be 60nm~100nm, aperture be 20nm~
35nm, the porosity are 85%~100%；
The partial size of ferroferric oxide magnetic nano-particles described in step 1 is 60nm~100nm；
The mass ratio of the nanoscale silica hollow microspheres and ferroferric oxide magnetic nano-particles is 1:1.8；
The Ball-milling Time of the high energy ball milling mixing is 1.5h, ball milling speed 300r/min；
The temperature of the hot pressing is 300 DEG C, pressure 200MPa, dwell time 3min；
Two, nano silica/Fe 3 O 4 magnetic radiography particle combination that step 1 obtains is heated to 200
DEG C, it is then added in the magnesium slurry of semisolid, is warming up to 720 DEG C, the magnesium-based composite material melt of liquid is obtained, then in temperature
For 720 DEG C, ultrasonic power be 1000W and mechanical stirring rate be 1200rpm under conditions of it is molten to the magnesium-based composite material of liquid
It is 100 DEG C of pure magnesium that temperature is added in body, the liquid magnesium alloy after being adjusted, then temperature is 720 DEG C, ultrasonic power is
1000W and mechanical stirring rate stir ultrasound 30min under conditions of being 1200rpm；780 DEG C are then heated to, temperature is subsequently placed at
Degree is hot-forming to carry out classification alternating temperature infiltration in 600 DEG C of mold, obtains nano silica/Fe 3 O 4 magnetic radiography
Particulate reinforcement biology magnesium-based composite material；
The semisolid magnesium slurry the preparation method is as follows: by magnesium alloy from room temperature to 760 DEG C, be then cooled to
620 DEG C, obtain the magnesium alloy fused mass of semisolid；
Nano silica/Fe 3 O 4 magnetic radiography particle combination in the liquid magnesium alloy adjusted
Quality is divided into 5%；
The magnesium slurry of the semisolid is made of by mass fraction the Mg of 8% Zn, 4% Sr and 88%；
Tri- elements of Zn, Sr and Mg are formed by mass fraction in the liquid magnesium alloy adjusted are as follows: 2% Zn,
The Mg of 1% Sr and 97%；
It is as follows that the classification alternating temperature infiltrates hot-forming method: in the item that temperature is 600 DEG C and pressure is 400MPa
Pressure maintaining 2min carries out first order hot pressing under part；Then under conditions of temperature is 400 DEG C and pressure is 550MPa pressure maintaining 6min into
The hot pressing of the row second level.
Test two: this test is comparative test, unlike test one in step 1: nano silica is hollow micro-
Ball and ferroferric oxide magnetic nano-particles carry out ball milling mixing at room temperature, then carry out hot pressing, cooled to room temperature obtains
To nano silica/Fe 3 O 4 magnetic radiography particle combination.It is other identical as test one.
Fig. 3 is that nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based of one preparation of test is compound
The optical microstructure of material, as shown, average grain size is about 40 μm, crystallite dimension is obviously refined, the distribution of the second phase
Uniformly, obdurability can be promoted to improve.
Nano silica-Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material is carried out at room temperature
Performance test obtains engineering stress-engineering strain curve as shown in figure 5, in figure ● indicates the nanometer titanium dioxide of two preparation of test
Silicon-Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material, ▼ indicates the nano-silica of one preparation of test in figure
SiClx-Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material tests the nanometer two of two preparations as shown in Figure 5
Silica-Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material is combined in the processing of step 1 room temperature mechanical ball milling
Tensile strength is 320MPa, yield strength 298MPa, elongation percentage 9.2% after body；The nano silica of one preparation of test/
The tensile strength of Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material is 374MPa, and yield strength is
349Mpa, elongation percentage 11.3%, hence it is evident that better than test two.
Test three: this test is unlike test one: the nanoscale silica hollow microspheres and ferroso-ferric oxide
The mass ratio of magnetic nano-particle is 1:3.It is other identical as test one.
Test four: this test is comparative test, unlike test three in step 1: nano silica is hollow micro-
Ball and ferroferric oxide magnetic nano-particles carry out ball milling mixing at room temperature, then carry out hot pressing, cooled to room temperature obtains
To nano silica/Fe 3 O 4 magnetic radiography particle combination.It is other identical as test three.
Fig. 4 is that nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based of four preparation of test is compound
The optical microstructure of material schemes, and as can be seen from the figure its crystallite dimension is big, and second hands down crystal boundary distribution, and plasticity is poor, intensity
It is low.
Nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material is carried out at room temperature
Performance test obtains engineering stress-engineering strain curve as shown in fig. 6, in figure ◆ indicates the nanometer titanium dioxide of four preparation of test
Silicon/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material, in figure ▲ indicate the nano-silicas of three preparation of test
SiClx/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material tests the nanometer two of four preparations as shown in Figure 6
Silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material is combined in the processing of step 1 room temperature mechanical ball milling
Tensile strength is 313MPa, yield strength 291MPa, elongation percentage 8.8% after body；More nanometer titanium dioxides of three preparation of test
Silicon/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material tensile strength is 361MPa, and yield strength is
346Mpa, elongation percentage 10.1%.
Test five: this test is unlike test one: by nanoscale silica hollow microspheres and four oxidations in step 1
Three ferromagnetism nanometer particles carry out high energy ball milling mixing under conditions of temperature is 400 DEG C, then carry out hot pressing, naturally cool to
Room temperature obtains nano silica/Fe 3 O 4 magnetic radiography particle combination.It is other identical as test one.
Test six: this test is comparative test, in step 1 that nano silica is hollow micro- unlike test three
Ball carries out high energy ball milling with ferroferric oxide magnetic nano-particles under conditions of temperature is 400 DEG C and mixes, and then carries out hot pressing,
Cooled to room temperature obtains nano silica/Fe 3 O 4 magnetic radiography particle combination.Others test three-phase
Together.
Test seven: this test is comparative test, unlike test two in step 1: nano silica is hollow micro-
Ball and ferroferric oxide magnetic nano-particles room temperature mechanical ball milling, obtain nano silica/Fe 3 O 4 magnetic radiography grain
Sub- combination.Others test two is identical.
Nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material is carried out at room temperature
Performance test obtains engineering stress-engineering strain curve as shown in fig. 7, in figure ▲ indicates the nanometer titanium dioxides of five preparation of test
Silicon/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material, ■ indicates the nano-silicas of six preparation of test in figure
SiClx/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material, in figure ◆ indicate the nanometers two of seven preparation of test
Silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material tests the nanometer of five preparations as shown in Figure 7
Silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material tensile strength is 397Mpa, and surrender is strong
Degree is 354Mpa, elongation percentage 13.8%；Nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement of six preparation of test
The tensile strength of biological magnesium-based composite material is 355MPa, yield strength 310MPa, elongation percentage 13.1%.Seven preparation of test
Nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material tensile strength be 245MPa,
Yield strength is 169MPa, elongation percentage 6.2%.
Claims (6)
1. a kind of nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material preparation method,
It is characterized in that nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material preparation method is
It carries out according to the following steps:
One, prepare nano silica/Fe 3 O 4 magnetic radiography particle combination: by nanoscale silica hollow microspheres with
Ferroferric oxide magnetic nano-particles carry out high energy ball milling mixing under conditions of temperature is 250 DEG C~400 DEG C, then carry out heat
Pressure, cooled to room temperature obtain nano silica/Fe 3 O 4 magnetic radiography particle combination；
The mass ratio of the nanoscale silica hollow microspheres and ferroferric oxide magnetic nano-particles is 1:(1.8~3)；
The Ball-milling Time of the high energy ball milling mixing is 0.5h~1.5h, and ball milling speed is 250r/min~400r/min；
The temperature of the hot pressing is 250 DEG C~400 DEG C, pressure is 150MPa~250MPa, dwell time 3min；
Two, by nano silica/Fe 3 O 4 magnetic radiography particle combination that step 1 obtains be heated to 150 DEG C~
It 250 DEG C, is then added in the magnesium slurry of semisolid, is warming up to 680 DEG C~760 DEG C, obtains the magnesium-based composite material melt of liquid,
Then temperature is 680 DEG C~760 DEG C, ultrasonic power is 600W~1800W and mechanical stirring rate is 500rpm~1700rpm
Under conditions of temperature is added into the magnesium-based composite material melt of liquid is 100 DEG C of pure magnesium, the liquid magnesium after being adjusted closes
Gold, then temperature is 680 DEG C~760 DEG C, ultrasonic power is 600W~1800W and mechanical stirring rate be 500rpm~
Ultrasound 15min~30min is stirred under conditions of 1700rpm；780 DEG C are then heated to, being subsequently placed at temperature is 550 DEG C~650
DEG C mold in carry out classification alternating temperature infiltration hot-forming, obtain nano silica/Fe 3 O 4 magnetic radiography particle and increase
Johnson & Johnson's object magnesium-based composite material；
Nano silica/Fe 3 O 4 magnetic radiography particle combination quality in the liquid magnesium alloy adjusted
It is divided into 1%~15%；
The magnesium slurry of the semisolid is made of by mass fraction the Mg of 8% Zn, 4% Sr and 88%；
Zn, Sr and Mg tri- elements are formed by mass fraction in the liquid magnesium alloy adjusted are as follows: 2% Zn, 1%
The Mg of Sr and 97%；
It is as follows that the classification alternating temperature infiltrates hot-forming method: temperature be 550 DEG C~650 DEG C and pressure be 300MPa~
Pressure maintaining 1min~2min carries out first order hot pressing under conditions of 500MPa；Then be 400 DEG C~550 DEG C in temperature is with pressure
Pressure maintaining 5min~8min carries out second level hot pressing under conditions of 450MPa~700MPa, and the temperature of the second level hot pressing is small
In the temperature of first order hot pressing.
2. a kind of nano silica according to claim 1/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based
The preparation method of composite material, it is characterised in that the partial size of nanoscale silica hollow microspheres described in step 1 be 40nm~
100nm, aperture are 15nm~35nm, and the porosity is 85%~100%.
3. a kind of nano silica according to claim 1/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based
The preparation method of composite material, it is characterised in that the partial size of ferroferric oxide magnetic nano-particles described in step 1 is 30nm
~100nm.
4. a kind of nano silica according to claim 1/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based
The preparation method of composite material, it is characterised in that the nanoscale silica hollow microspheres and ferroferric oxide magnetic nano grain
The mass ratio of son is 1:2.
5. a kind of nano silica according to claim 1/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based
The preparation method of composite material, it is characterised in that the nano silica for obtaining step 1 in step 2/ferroso-ferric oxide magnetic
Property radiography particle combination be heated to 200 DEG C, be then added to semisolid magnesium slurry in.
6. a kind of nano silica according to claim 1/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based
The preparation method of composite material, it is characterised in that semisolid described in step 2 magnesium slurry the preparation method is as follows: magnesium is closed
Then gold is cooled to 620 DEG C from room temperature to 760 DEG C, obtain the magnesium alloy fused mass of semisolid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811069235.0A CN109082569B (en) | 2018-09-13 | 2018-09-13 | Preparation method of nano silicon dioxide/ferroferric oxide magnetic contrast particle enhanced biological magnesium-based composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811069235.0A CN109082569B (en) | 2018-09-13 | 2018-09-13 | Preparation method of nano silicon dioxide/ferroferric oxide magnetic contrast particle enhanced biological magnesium-based composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109082569A true CN109082569A (en) | 2018-12-25 |
| CN109082569B CN109082569B (en) | 2020-04-21 |
Family
ID=64841657
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811069235.0A Active CN109082569B (en) | 2018-09-13 | 2018-09-13 | Preparation method of nano silicon dioxide/ferroferric oxide magnetic contrast particle enhanced biological magnesium-based composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109082569B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112045195A (en) * | 2020-08-10 | 2020-12-08 | 广州有研粉体材料科技有限公司 | Metal powder for 3D printing and metal powder surface nano-modification method |
| CN113385677A (en) * | 2021-06-04 | 2021-09-14 | 孙晓华 | Stirring ball-milling pretreatment method for titanium powder particles of vacuum sintering porous titanium coating |
| CN117731845A (en) * | 2023-12-05 | 2024-03-22 | 材慧新材料(上海)有限公司 | Magnesium-based composite implant, preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0365365A1 (en) * | 1988-10-21 | 1990-04-25 | Honda Giken Kogyo Kabushiki Kaisha | Silicon carbide-reinforced light alloy composite material |
| CN101182614A (en) * | 2007-12-21 | 2008-05-21 | 南京信息工程大学 | Magnesium-base porous compound material and method of producing the same |
| CN102206782A (en) * | 2011-04-14 | 2011-10-05 | 太原理工大学 | Degradable Mg-Zn-Y-Ca intravascular stent material and preparation method thereof |
| CN102220529A (en) * | 2011-02-23 | 2011-10-19 | 郑州大学 | Mg-Zn-Y-Nd alloy for novel biodegradable vascular stents and preparation method thereof |
| US20120059455A1 (en) * | 2010-09-07 | 2012-03-08 | Boston Scientific Seimed, Inc. | Bioerodible Magnesium Alloy Containing Endoprostheses |
| CN105886876A (en) * | 2016-06-22 | 2016-08-24 | 陆志强 | High-heat-resistance titanium-magnesium alloy material and preparation method thereof |
-
2018
- 2018-09-13 CN CN201811069235.0A patent/CN109082569B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0365365A1 (en) * | 1988-10-21 | 1990-04-25 | Honda Giken Kogyo Kabushiki Kaisha | Silicon carbide-reinforced light alloy composite material |
| CN101182614A (en) * | 2007-12-21 | 2008-05-21 | 南京信息工程大学 | Magnesium-base porous compound material and method of producing the same |
| US20120059455A1 (en) * | 2010-09-07 | 2012-03-08 | Boston Scientific Seimed, Inc. | Bioerodible Magnesium Alloy Containing Endoprostheses |
| CN102220529A (en) * | 2011-02-23 | 2011-10-19 | 郑州大学 | Mg-Zn-Y-Nd alloy for novel biodegradable vascular stents and preparation method thereof |
| CN102206782A (en) * | 2011-04-14 | 2011-10-05 | 太原理工大学 | Degradable Mg-Zn-Y-Ca intravascular stent material and preparation method thereof |
| CN105886876A (en) * | 2016-06-22 | 2016-08-24 | 陆志强 | High-heat-resistance titanium-magnesium alloy material and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| BINGCHENG GE等: "Unique strengthening mechanisms of ultrahigh pressure Mg alloys", 《BIOACTIVE MATERIALS 》 * |
| SHAN-SHAN ZHOU等: "Effects of volume ratio on the microstructure and mechanical properties of particle reinforced magnesium matrix composite", 《MATERIALS AND DESIGN》 * |
| 李江波等: "Mg-Zn-Sr生物医用材料在模拟体液中的腐蚀性能研究", 《试验研究》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112045195A (en) * | 2020-08-10 | 2020-12-08 | 广州有研粉体材料科技有限公司 | Metal powder for 3D printing and metal powder surface nano-modification method |
| CN113385677A (en) * | 2021-06-04 | 2021-09-14 | 孙晓华 | Stirring ball-milling pretreatment method for titanium powder particles of vacuum sintering porous titanium coating |
| CN113385677B (en) * | 2021-06-04 | 2023-10-31 | 孙晓华 | Titanium powder particle stirring ball milling pretreatment method for vacuum sintering porous titanium coating |
| CN117731845A (en) * | 2023-12-05 | 2024-03-22 | 材慧新材料(上海)有限公司 | Magnesium-based composite implant, preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109082569B (en) | 2020-04-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109082569A (en) | A kind of preparation method of nano silica/Fe 3 O 4 magnetic radiography particulate reinforcement biology magnesium-based composite material | |
| Kwon et al. | Large‐scale synthesis and medical applications of uniform‐sized metal oxide nanoparticles | |
| Dheyab et al. | Synthesis and coating methods of biocompatible iron oxide/gold nanoparticle and nanocomposite for biomedical applications | |
| Laurent et al. | Iron oxide based MR contrast agents: from chemistry to cell labeling | |
| Jiang et al. | Preparation and biomedical applications of gold-coated magnetic nanocomposites | |
| Nuzhina et al. | Preclinical evaluation and clinical translation of magnetite-based nanomedicines | |
| CN105997944B (en) | A kind of hot, nano-medicament carrier of photo-thermal effect and preparation method thereof with magnetic | |
| Liu et al. | Polydopamine doped reduced graphene oxide/mesoporous silica nanosheets for chemo-photothermal and enhanced photothermal therapy | |
| Teng et al. | A magnetic droplet vaporization approach using perfluorohexane-encapsulated magnetic mesoporous particles for ultrasound imaging and tumor ablation | |
| Chen et al. | Multitheragnostic multi‐GNRs crystal‐seeded magnetic nanoseaurchin for enhanced in vivo mesenchymal‐stem‐cell homing, multimodal imaging, and stroke therapy | |
| CN106086559B (en) | A kind of long-periodic structure mutually enhances Mg-RE-Ni magnesium alloy semi-solid state blanks and preparation method thereof | |
| Han et al. | Glucose-functionalized Au nanoprisms for optoacoustic imaging and near-infrared photothermal therapy | |
| CN104894419B (en) | A kind of coated magnesium oxide Graphene strengthens the method for magnesium base composite material | |
| CN109453398B (en) | Mesoporous polydopamine-encapsulated liquid fluorocarbon ultrasonic contrast agent and preparation method thereof | |
| CN109500396A (en) | A kind of biological kirsite and preparation method thereof of transgranular-intergranular composite strengthening | |
| You et al. | Specific recognition and photothermal release of circulating tumor cells using near-infrared light-responsive 2D MXene nanosheets@ hydrogel membranes | |
| Zhang et al. | Engineered Fe 3 O 4-based nanomaterials for diagnosis and therapy of cancer | |
| CN113456837A (en) | MXene @ BSA nano diagnosis and treatment agent with controllable size and preparation and application thereof | |
| CN108904800A (en) | Upper conversion nano hybrid systems, preparation method and application based on Technique of Nano Pd Heteroepitaxy | |
| Wang et al. | An efficient strategy to synthesize a multifunctional ferroferric oxide core@ dye/SiO 2@ Au shell nanocomposite and its targeted tumor theranostics | |
| CN106929704B (en) | A kind of preparation method of the biological magnesium-based composite material of nano titanium carbide particle enhancing | |
| WO2013002532A2 (en) | Oxygen atom-dispersed metal-based composite material and method for manufacturing same | |
| CN102172411B (en) | Nano complex particles with targeted MR (magnetic resonance) development and photothermal therapy performance and preparation method thereof | |
| CN106310259B (en) | A kind of multifunctional nanocomposites and its preparation method and application | |
| Lei et al. | Enhanced magnetothermal effect of high porous bioglass for both bone repair and antitumor therapy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |