CN108480622B - A kind of magnesium alloy spray printing slurry and preparation method thereof - Google Patents
A kind of magnesium alloy spray printing slurry and preparation method thereof Download PDFInfo
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- CN108480622B CN108480622B CN201810436573.7A CN201810436573A CN108480622B CN 108480622 B CN108480622 B CN 108480622B CN 201810436573 A CN201810436573 A CN 201810436573A CN 108480622 B CN108480622 B CN 108480622B
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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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
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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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- 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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- 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
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
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Abstract
A kind of magnesium alloy spray printing slurry and preparation method thereof, slurry by weight percentage, the magnesium alloy particles including 5-50wt%, the polydactyl acid particle and surplus auxiliary agent of quality accounting 10-40%；The auxiliary agent is made of solvent, consistency modifiers, activating agent and thixotropic agent；The magnesium alloy particles are AZ31 magnesium alloy, and partial size is 25-38 μm.Method is: weighing solvent, consistency modifiers and is mixed, it is sheared again with three-roller and thixotropic agent and activating agent is added, it weighs polylactic acid, nanometer hydroxyapatite, solvent and dispersing agent and mixes, weigh magnesium alloy particles and polydactyl acid particle and mixed with auxiliary agent.By adopting the above technical scheme, a little particle is played to the lubricating action of magnesium alloy bulky grain, improves the spray printing performance of slurry when slurry stress is slided by the way that the polydactyl acid particle of specified particle diameter is added.
Description
Technical field
The present invention relates to technical field of metal material preparation, are specifically magnesium alloy spray printing slurry and preparation method thereof.
Background technique
In recent years, magnesium and its alloy are increasingly becoming the research hotspot in degradable biomaterial field.With existing bone tissue work
Journey material is compared, and magnesium and its alloy have the advantage that there are good biocompatibility in (1) and human body, and magnesium can also promote bone to be cured
It closes, therefore magnesium has very big potentiality as bone graft in the reparation of oral cavity jaw defect；It (2) can degradable be in vivo magnesium
Ion is discharged after being absorbed by surrounding body tissues by human body fluid, and second operation is avoided, and mitigates burden of patients；(3) have and close
Suitable physical and mechanical property has with density similar in human body bone and elasticity modulus, is resistant to certain pressure, and be avoided that and answer
Power occlusion effect；(4) catabolite no cytotoxicity, magnesium are also thin without discovery to the no inhibiting effect of the growth of bone marrow cell
Cellular lysis phenomenon；(5) magnesium alloy resource is abundant, and price is low.Therefore, magnesium alloy can be used as effective medical embedded material and obtain
It uses.But due to magnesium alloy degradation in vivo excessive velocities, good supporting role cannot be played to bone tissue defect, it limits
Its application in biomedicine, industry generallyd use the magnesium alloy method compound with polylactic acid in recent years and optimized.?
In the technical solution reported at present, polylactic acid PLA organic coating directly such as is coated in Mg alloy surface, and has been reported that and utilizes electricity
Deposition method prepares magnesium hydroxide coating in Mg alloy surface, can improve the corrosion resistance of magnesium alloy to a certain extent,
But generally existing many problems, if porosity is excessively high, structure is not fine and close enough, and hydrolysate is reacted with magnesium alloy substrate generates hydrogen
The problems such as gas.
Polylactic acid (PLA) is a kind of polymer of biological degradability, its final catabolite is CO2And H2O, centre produce
Object lactic acid is also internal normal glucose, and therefore, polylactic acid will not generate adverse effect, machine to organism after degrading in vivo
It is gradually reduced during tool intensity degradation in vivo, stress can be made slowly to be transferred to fracture site, avoid stress force shelter reaction, together
When have preferable hot formability, be a kind of ideal interplantation material.However single polylactic acid exists absolutely as bone immobilizing material
It is lower to mechanical strength；Catabolite easily causes internal aseptic inflammation to react in acidity；Lack synosteosis ability, biology is living
Property is poor；There is penetrability to X-ray, be not easy to the disadvantages of observing of clinically developing.Therefore polylactic acid is modified to improve it
Correlated performance becomes research hotspot, and modified main purpose is to enhance its mechanical strength, control its degradation rate and neutralize drop
Solve the acidity of product.What the area research was the most active at present is exactly the modified lactic acid composite material of hydroxyapatite enhancing,
On the one hand it on the other hand can also delay the premature degradation speed of material with the initial mechanical intensity and rigidity of controlled material,
Keep its bioactivity more preferable.But since hydroxyapatite is difficult to dissolve and absorb, to office caused by after polylactic acid degradation in vivo
The neutralization of portion's acidic environment is to be improved.Magnesium has good biocompatibility and bioactivity, and its degradation process is in
Alkalinity, it is using this characteristic of magnesium, magnesium granules and polydactyl acid progress are compound, to neutralize the part after polylactic acid degradation
Acidic environment reduces the stimulation to tissue.
Printing techniques are the contactless, no pressure of one kind and the digital imaging technique for being not required to exposure mask, it can be design
Image information is printed on substrate by printer.The technology not only saves consumptive material, shortens printing time, can also be any
Patterning is carried out on substrate to scribe, and is not limited by stock shape and size, due to many advantages of the technology, so that spray printing
Technique obtains development at full speed in each field.For the composite material of magnesium alloy and polylactic acid PLA, if using Printing techniques into
Row printing speed, and solidified in the follow-up process using laser, the customization application in biomedicine may be implemented.Cause
This, the magnesium alloy spray printing slurry that research and development are suitable for Printing techniques has the popularization and use of Printing techniques and bio-medical material
Great meaning.
Summary of the invention
The purpose of the present invention is overcoming the shortcomings of the prior art, a magnesium alloy suitable for Printing techniques is provided
Spray printing slurry and preparation method thereof.
To achieve the above object, the technical scheme adopted by the invention is as follows: a kind of magnesium alloy spray printing slurry, is accounted for by quality
AZ31 magnesium alloy particles than 5-50%, polydactyl acid particle and surplus the auxiliary agent composition of quality accounting 10-40%.
AZ31 magnesium alloy particles therein, by weight percentage, by 95.83% Mg, 3.1% Al, 0.8% Zn,
0.15% Mn, 0.06% Si, 0.03% Cu, 0.02% Ni, 0.01% Fe composition.Particle size is 25-38 μm.
Polydactyl acid therein is nanometer hydroxyapatite (n-HA) enhancing polydactyl acid particle, modifying process
Are as follows: polylactic acid, nanometer hydroxyapatite, solvent and dispersing agent are mixed in a certain ratio, and carry out ultrasonic wave dispersion, is sufficiently stirred
It mixes, makes n-HA particle that equally distributed state be presented in PLA matrix and occur therewith compound；Then the solution prepared is adopted
It is centrifuged with supercentrifuge, washing drying then is carried out to it again, obtains composite powder.Wherein each substance percentage by weight
Than being made of the polylactic acid of 10-60%, the nanometer hydroxyapatite of 5-10%, the dispersing agent of 5-10% and balance solvent.Wherein
Polylactic acid be low molecule chain PLA, particle size range 10-100nm；Hydroxyapatite particle size range 0-40nm, Ca10(PO4)6(OH)2
>=99.5%；Solvent is one or both of dehydrated alcohol, polyethylene glycol, methylene chloride；Dispersing agent is calgon, carboxylic
One of Methyl cellulose acid sodium, gelatin or two kinds.
Auxiliary agent therein, by weight percentage, by the solvent of 15-55wt%, the consistency modifiers of 10-50%, 5-10%
Activating agent and surplus thixotropic agent composition.
The solvent is at least one of propylene glycol, ethyl acetate, butyl glycol ether, and main function is to dissolve other help
Agent provides carrier for other auxiliary agents.
The consistency modifiers are the one or two of polyethylene glycol, polypropylene glycol and methoxy poly (ethylene glycol), are mainly mentioned
High wettability and adjusting consistency.
The activating agent is one or both of succinic acid, adipic acid, glutaric acid, and effect is to guarantee enough work
Property, while oxide layer existing for magnesium alloy particles surface is effectively removed, good wetability is provided.
The thixotropic agent is one or both of hydrogen polyamide wax and rilanit special, main raising magnesium alloy pulp spraying
The thixotropic property of print process.
Wherein, auxiliary agent mass ratio first as described above weighs solvent, consistency modifiers, activating agent and thixotropic agent.First
It is stirred in beaker, then is sheared and be added by three-roller.Secondly mass ratio as described above weighs polylactic acid, nano-hydroxy
Apatite, solvent and dispersant simultaneously carry out ultrasonic wave dispersion, and acquired solution high speed centrifugation is changed after dry washing
Property composite powder.Then magnesium alloy powder and polydactyl acid particle is added in mass ratio as described above, first stirring by hand
To the degree of unobvious dry powder, then it is put in blender and is stirred under vacuum.Stirring technique parameter is as shown in the table.
It is as shown in the table, and 5min, mixing speed 10r/min are first stirred at 101KPa to magnesium alloy slurry；After standing 5min
It vacuumizes and reaches 0.1KPa, 10min is stirred under 35r/min revolving speed, keep standing 5min under vacuum；Finally under vacuum conditions
15min is stirred with 25r/min revolving speed, slurry preparation is completed.By adopting the above technical scheme, the invention has the following advantages that
(1) the present invention provides a kind of preparation method of the compound spray printing slurry of magnesium alloy, the system including first stage auxiliary agent
It is standby, the modification of second stage particles of polylactic acid and the preparation of phase III composite mortar, whole preparation process and subsequent spray printing
Technique is to carry out at normal temperature, at present prepare composite material of magnesium alloy when be higher temperature (usually all 300 DEG C with
On) under carry out, simple process, environmental protection and saving.Furthermore the particles of polylactic acid of the modified enhancing of nanometer hydroxyapatite is added, increases hydroxyl
Degree of scatter of the base apatite in polylactic acid, the material prepared by spray printing are also able to satisfy bio-medical requirement.
(2) there are magnesium alloy bulky grain and polydactyl acid small in the magnesium alloy spray printing slurry that the present invention is prepared
Grain, when slurry stress is slided, plays polydactyl acid little particle to the lubricating action of magnesium alloy bulky grain, improves slurry
Spray printing performance, uniform in spray printing time point diameter, consistent good, spray printing point is smooth full, and thixotropic property is excellent.Magnesium is closed by spray printing
Golden composite mortar carries out printing speed, then cured, and the customization application in biomedicine may be implemented.
Detailed description of the invention
Fig. 1 magnesium alloy particles stereoscan photograph；
Fig. 2 magnesium alloy particles particle size distribution figure；
1 spray printing point body formula micro-image (50 times) of Fig. 3 embodiment；
2 spray printing point body formula micro-image (50 times) of Fig. 4 embodiment；
3 spray printing point body formula micro-image (50 times) of Fig. 5 embodiment；
1 spray printing point 3D pattern photo of Fig. 6 embodiment；
2 spray printing point 3D pattern photo of Fig. 7 embodiment；
3 spray printing point 3D pattern photo of Fig. 8 embodiment；
Fig. 9 embodiment 1 shakes stress scans curve；
Figure 10 embodiment 2 shakes stress scans curve；
Figure 11 embodiment 3 shakes stress scans curve；
Figure 12 polydactyl acid little particle, which is added, changes magnesium alloy slurry spray printing performance principle；
Figure 13 preparation process figure.
Specific embodiment
Embodiment 1:
(1) preparation of auxiliary agent: solvent, consistency modifiers, activating agent and thixotroping are weighed respectively according to mass ratio 10: 7: 2: 1
Agent.Mixing is first passed through, then is sheared and is prepared with three-roller.
(2) polylactic acid modified: to weigh polylactic acid, nanometer hydroxyapatite, dispersing agent respectively according to mass ratio 3: 1: 1, stir
It mixes and mixes them thoroughly, the solution prepared is centrifuged using supercentrifuge, washing drying then is carried out to it again, is obtained
To composite powder.
(3) magnesium alloy particles (25-38 μm) and polydactyl acid particle (1-10 μm) preparation of magnesium alloy spray printing slurry: are taken
And auxiliary agent prepared by step (1), it is mixed according to mass ratio 1: 1: 1.Mechanical stirring is carried out first with spiral oscillator, then with super
Sound washer carries out sonic oscillation, stirs evenly, and slurry preparation is completed.
Embodiment 2:
(1) preparation of auxiliary agent: solvent, consistency modifiers, activating agent and thixotroping are weighed respectively according to mass ratio 10: 7: 2: 1
Agent.Mixing is first passed through, then is sheared and is prepared with three-roller.
(2) polylactic acid modified: to weigh polylactic acid, nanometer hydroxyapatite, dispersing agent respectively according to mass ratio 3: 1: 1, stir
It mixes and mixes them thoroughly, the solution prepared is centrifuged using supercentrifuge, washing drying then is carried out to it again, is obtained
To composite powder.
(3) magnesium alloy particles (25-38 μm) and polydactyl acid particle (1-10 μm) preparation of magnesium alloy spray printing slurry: are taken
And auxiliary agent prepared by step (1), it is mixed according to mass ratio 2: 1: 1.Mechanical stirring is carried out first with spiral oscillator, then with super
Sound washer carries out sonic oscillation, stirs evenly, and slurry preparation is completed.
Embodiment 3:
(1) preparation of auxiliary agent: solvent, consistency modifiers, activating agent and thixotroping are weighed respectively according to mass ratio 10: 7: 2: 1
Agent.Mixing is first passed through, then is sheared and is prepared with three-roller.
(2) polylactic acid modified: to weigh polylactic acid, nanometer hydroxyapatite, dispersing agent respectively according to mass ratio 3: 1: 1, stir
It mixes and mixes them thoroughly, the solution prepared is centrifuged using supercentrifuge, washing drying then is carried out to it again, is obtained
To composite powder.
(3) magnesium alloy particles (25-38 μm) and polydactyl acid particle (1-10 μm) preparation of magnesium alloy spray printing slurry: are taken
And auxiliary agent prepared by step (1), it is mixed according to mass ratio 3: 1: 1.Mechanical stirring is carried out first with spiral oscillator, then with super
Sound washer carries out sonic oscillation, stirs evenly, and slurry preparation is completed.
Embodiment 4
A kind of magnesium alloy spray printing slurry, by weight percentage, the AZ31 magnesium alloy particles including 5-50wt%, quality account for
Polydactyl acid particle and surplus auxiliary agent than 10-40%.In the present embodiment,
Each component is by weight percentage in the auxiliary agent: solvent 15-55wt%, consistency modifiers 10-50%, living
Property agent be 5-10wt% and surplus thixotropic agent；The solvent be propylene glycol, ethyl acetate, in butyl glycol ether at least
One kind for dissolving consistency modifiers, activating agent and thixotropic agent, and providing carrier；The consistency modifiers are polyethylene glycol, gather
At least one of propylene glycol and methoxy poly (ethylene glycol), for improving wetability and adjusting consistency；The activating agent is fourth two
At least one of acid, adipic acid, glutaric acid for guaranteeing enough activity, while being removed existing for magnesium alloy particles surface
Oxide layer provides good wetability；The thixotropic agent is one or both of polyamide wax and rilanit special, for mentioning
The thixotropic property of high magnesium alloy slurry jet printing process；The magnesium alloy particles are AZ31 magnesium alloy, and partial size is 25-38 μm；It is described
Polydactyl acid particle is that nanometer hydroxyapatite enhances modified compound powder, and partial size is 0-10 μm.
Embodiment 5
A kind of preparation method of magnesium alloy spray printing slurry, comprising the following steps:
S1. the solvent, consistency modifiers are weighed respectively by corresponding proportion and are mixed, then are added with three-roller shearing
Enter thixotropic agent and activating agent, 4~5 passages of grinding are uniformly non-discolouring to auxiliary agent, take out stand for standby use；
S2. polylactic acid, nanometer hydroxyapatite, solvent and the dispersing agent of corresponding proportion are weighed respectively and is mixed, and are sufficiently stirred
It mixes, and is dispersed using ultrasonic wave, duration of oscillation is no less than 30min, the solution prepared is centrifuged using supercentrifuge,
Then washing drying is carried out to it again, obtains polydactyl acid composite powder, wherein each substances in percentage by weight is 10-
60% polylactic acid, the nanometer hydroxyapatite of 5-10%, the dispersing agent of 5-10% and balance solvent, the solvent are anhydrous second
One or both of alcohol, polyethylene glycol, methylene chloride, for dissolving other compositions, the dispersing agent is calgon, carboxylic
One of Methyl cellulose acid sodium, gelatin or two kinds, for increasing degree of scatter of the hydroxyapatite in polylactic acid；
S3. magnesium alloy particles and polydactyl acid particle are weighed, are mixed with the auxiliary agent that S1 is obtained, the magnesium alloy spray is obtained
Printing paste material.
In the step S3, it when magnesium alloy particles, polydactyl acid particle being mixed with auxiliary agent, is vibrated first with spiral
Device carries out mechanical stirring, then carries out sonic oscillation with ultrasonic cleaning machine, stirs evenly, and slurry preparation is completed.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of magnesium alloy spray printing slurry, which is characterized in that by weight percentage, the AZ31 magnesium alloy including 5-50wt%
Grain, the polydactyl acid particle and surplus auxiliary agent of quality accounting 10-40%,
Polydactyl acid therein is nanometer hydroxyapatite (n-HA) enhancing polydactyl acid particle, modifying process are as follows: will
Polylactic acid, nanometer hydroxyapatite, solvent and dispersing agent are mixed in a certain ratio, and carry out ultrasonic wave dispersion, are sufficiently stirred, are made
Equally distributed state is presented in PLA matrix and occurs therewith compound for n-HA particle；Then by the solution prepared using high
Fast centrifuge is centrifuged, and is then carried out washing drying to it again, is obtained composite powder, wherein each substances in percentage by weight,
It is made of the polylactic acid of 10-60%, the nanometer hydroxyapatite of 5-10%, the dispersing agent of 5-10% and balance solvent, it is therein
Polylactic acid is low molecule chain PLA, particle size range 10-100nm；Hydroxyapatite particle size range 0-40nm, Ca10(PO4)6(OH)2≥
99.5%；Solvent is one or both of dehydrated alcohol, polyethylene glycol, methylene chloride；Dispersing agent is calgon, carboxylic first
One of base Carboxymethylcellulose sodium, gelatin or two kinds.
2. a kind of magnesium alloy spray printing slurry according to claim 1, which is characterized in that each component is by weight in the auxiliary agent
Percentages: solvent 15-55wt%, consistency modifiers 10-50%, the thixotroping of activating agent 5-10wt% and surplus
Agent.
3. a kind of magnesium alloy spray printing slurry according to claim 2, which is characterized in that the solvent is propylene glycol, acetic acid
At least one of ethyl ester, butyl glycol ether for dissolving consistency modifiers, activating agent and thixotropic agent, and provide carrier.
4. a kind of magnesium alloy spray printing slurry according to claim 2, which is characterized in that the consistency modifiers are poly- second two
At least one of alcohol, polypropylene glycol and methoxy poly (ethylene glycol), for improving wetability and adjusting consistency.
5. a kind of magnesium alloy spray printing slurry according to claim 2, which is characterized in that the activating agent be succinic acid, oneself
At least one of diacid, glutaric acid for guaranteeing enough activity, while removing the existing oxidation in magnesium alloy particles surface
Layer, provides good wetability.
6. a kind of magnesium alloy spray printing slurry according to claim 2, which is characterized in that the thixotropic agent be polyamide wax and
One or both of rilanit special, for improving the thixotropic property of magnesium alloy slurry jet printing process.
7. a kind of magnesium alloy spray printing slurry according to claim 1 or 2, which is characterized in that the magnesium alloy particles are
AZ31 magnesium alloy, partial size are 25-38 μm；The polydactyl acid particle is that nanometer hydroxyapatite enhances modified compound powder,
Partial size is 0-10 μm.
8. a kind of preparation method of magnesium alloy spray printing slurry, feature described in any one of claim 2-7 claim
It is, comprising the following steps:
S1. the solvent in the auxiliary agent, consistency modifiers are weighed respectively by corresponding proportion and are mixed, then are sheared with three-roller
Thixotropic agent and activating agent is added, 4~5 passages of grinding are uniformly non-discolouring to auxiliary agent, take out stand for standby use；
S2. polylactic acid, nanometer hydroxyapatite, solvent and the dispersing agent of corresponding proportion are weighed respectively and is mixed, and are sufficiently stirred, and
Dispersed using ultrasonic wave, duration of oscillation is no less than 30min, the solution prepared is centrifuged using supercentrifuge, then
Washing drying is carried out to it again, obtains polydactyl acid composite powder, wherein each substances in percentage by weight is 10-60%'s
Polylactic acid, the nanometer hydroxyapatite of 5-10%, the dispersing agent of 5-10% and balance solvent, the solvent are dehydrated alcohol, gather
One or both of ethylene glycol, methylene chloride, for dissolving other compositions, the dispersing agent is calgon, carboxymethyl
One of Carboxymethylcellulose sodium, gelatin or two kinds, for increasing degree of scatter of the hydroxyapatite in polylactic acid；
S3. magnesium alloy particles and polydactyl acid particle are weighed, are mixed with the auxiliary agent that S1 is obtained, the magnesium alloy spray printing slurry is obtained
Material.
9. a kind of preparation method of magnesium alloy spray printing slurry according to claim 8, which is characterized in that by magnesium in step S3
When alloying pellet, polydactyl acid particle are mixed with auxiliary agent, mechanical stirring is carried out first with spiral oscillator, it is then clear with ultrasound
It washes device and carries out sonic oscillation, stir evenly, slurry preparation is completed.
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