CN109912967A - A kind of nylon carbon fiber composite powder and preparation method thereof of the reduction material anisotropy for selective laser sintering - Google Patents
A kind of nylon carbon fiber composite powder and preparation method thereof of the reduction material anisotropy for selective laser sintering Download PDFInfo
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- CN109912967A CN109912967A CN201910051555.1A CN201910051555A CN109912967A CN 109912967 A CN109912967 A CN 109912967A CN 201910051555 A CN201910051555 A CN 201910051555A CN 109912967 A CN109912967 A CN 109912967A
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- carbon fiber
- nylon
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- selective laser
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Abstract
The invention belongs to selective laser sintering 3D printing field, it is related to being a kind of nylon carbon fiber composite powder and preparation method thereof for reducing material anisotropy for selective laser sintering；Including carbon fiber nucleus, the outer surface of the carbon fiber nucleus is coated with nylon layer, and the diameter of the carbon fiber nucleus is 5-20 μm, and the length of the carbon fiber nucleus is 40-120 μm, and the Average Particle Diameters of the composite powder are 40-90 μm；This material has the direction XYZ mechanics balancing performance with the product that SLS processes printing, and tensile strength of material, elasticity modulus are high, the characteristic haveing excellent performance；Carbon fiber vinylon composite powder particle prepared by the present invention, from microcosmic, each powder particle has carbon fiber to be wrapped by nylon, and two kinds of components are combined together, evenly dispersed, will not generate segregation phenomenon.
Description
Technical field
The invention belongs to selective laser sintering 3D printing field, especially a kind of reduction for selective laser sintering
Nylon carbon fiber composite powder of material anisotropy and preparation method thereof.
Background technique
Selective laser sintering (Selective Laser Sintering, abbreviation SLS) is with the fastest developing speed in recent years
One of rapid shaping technique, using solid powder as raw material, successively scanned through using section of the laser to 3D solid
At raw basin, manufacture is not limited by part shape complexity, accurately can quickly be restored design concept, quickly be produced newly
The functional test part of product, be widely applied in the fields such as automobile, ship, space flight and aviation, medicine and illumination.
In selective laser sintering (SLS) technology, due to using processing the mode of accumulation in layer, and print
When a certain layer, the material in the direction XY is to be sintered melt-forming simultaneously, and as a threedimensional model, from Z-direction
Molding, have successive.After first layer sinter molding, face powder rod spreads the second layer material, and then re-melting forms
The second layer.Therefore forming model can be much smaller than the side XY along the structural strength between layers of forming direction (namely Z axis)
To intensity.To which mechanical property of the SLS molded part on different three-dimensionals is different, anisotropy is showed.This
It is SLS printing disadvantage maximum compared with tradition stays processing.
In order to improve the mechanical property of SLS printing product, generally by way of adding filler in nylon material, such as carbon
Fiber, mineral fibres, glass microballoon etc. improve the performance of material in a certain respect by the filler of filling.
As patent CN102337021 by nylon powder add glass microballoon, improve printing product tensile strength and
Modulus.The method as described in patent CN 103951971A, CN105462244A.By in nylon resin add carbon fiber come
Improve the tensile strength of material.
But since two or more powder of different nature are relatively independent during patent CN 103951971A mechanical mixture
Different in the presence of, density, form is different, it is easy to generate composition cluster phenomenon, so as to cause in the part finally shaped at
It is unevenly distributed, so that the performance of part different location has bigger difference.
Patent CN105462244A is used carbon fiber powder, nylon pellet, and dispersing agent is added in the good solvent of nylon pellet,
Agitating and heating makes nylon and dispersant solvent in a solvent, and the poor solvent of nylon is then added into mixed solution, so that
Nylon is precipitated again.The evenly dispersed of nylon and carbon fiber is obtained with this.Opposite point of the nylon carbon fiber powder that the method obtains
It is scattered uniformly preferable, but on the one hand during nylon is precipitated again, since it is that spontaneous nucleation is precipitated, the Buddhist nun being finally precipitated
Dragon-carbon fiber particles pattern is irregular, and powder particle size distribution is too wide, has from several microns to several hundred microns；Afterwards
Phase filters out the powder that can be used for the molding particle size 40-70um of SLS less than 1/10th, causes very big waste；And this
Middle method is needed using a variety of chemical solvents, containing there are many chemical solvent, Wu Fajin in remaining solvent after final powder is precipitated
Row recycling uses.
Most importantly it uses diameter for 7-10 microns, and the carbon fiber that length is 10-50 microns, final nylon is with carbon fiber
When dimension is that nucleus is precipitated, obtained carbon fiber is that nylon is wrapped in the inside, when SLS molding, simultaneously due to carbon fiber
A framework bridge beam action cannot be played, therefore the addition of carbon fiber is limited to the mechanical property promotion of material.
And whether the mode of patent CN105462244A or patent CN 103951971A mechanical mixture diameter are 7-
10 microns, the mode for the carbon fiber that length is 201-350 microns.Due to powdering roller or powdering scraper each layer of powdering when
It waits, powdering roller or scraper are side-to-side movements along the X direction, and powder is also that the power pushed by one or so acts on, this
When material inside fiber can due to power effect and towards the direction XY.So that fiber can only form one in the direction XY
The effect of power strong mechanical performance is played in framework bridge beam action.And Z-direction is not due to having the enhancing structure of cross-layer and interlayer, the side Z
To the structural strength of only nylon resin itself, therefore the final reflected anisotropy ratio Buddhist nun of this carbon fibre composite
Imperial resin itself is more serious.This composite material is in SLS printing, often due to its more obvious anisotropy, and can not add
Work has the product of mechanics intensity requirement.Therefore it provides a kind of in all directions all with the material of excellent mechanical performances, reduction SLS
Anisotropy caused by processing method is necessary.
Summary of the invention
The purpose of the present invention is: overcome deficiency in the prior art, a kind of reduction for selective laser sintering is provided
The nylon carbon fiber composite powder of material anisotropy, this material have the direction XYZ mechanical property with the product that SLS processes printing
Can be balanced, tensile strength of material, elasticity modulus are high, the characteristic haveing excellent performance.SLS printing product is reduced since molding mode is led
The Coating combination of cause is weaker, so that printing product has the direction XY mechanical property more than the characteristic that Z-direction is had excellent performance；
Another object of the present invention is: providing a kind of nylon carbon fiber of reduction material anisotropy for selective laser sintering
The preparation method of composite powder, carbon fiber reinforced polyamide composite material powder particle obtained is advised with pattern through the invention
Whole, powder particle size is distributed the characteristics of concentrating.
In order to solve the above technical problems, The technical solution adopted by the invention is as follows:
A kind of nylon carbon fiber composite powder of the reduction material anisotropy for selective laser sintering, including carbon fiber
Nucleus is tieed up, the outer surface of the carbon fiber nucleus is coated with nylon layer, and the diameter of the carbon fiber nucleus is 5-20 μm, the carbon
The length of fiber nucleus is 40-120 μm, and the Average Particle Diameters of the composite powder are 40-90 μm.
A kind of preparation side of the nylon carbon fiber composite powder of the reduction material anisotropy for selective laser sintering
Method, the preparation method comprises the following steps:
(1) nylon pellet, carbon fiber and organic solvent are placed in sealing container, charge and discharge nitrogen, row is carried out to container
After the air in container, make the pressure that 0.2MPa is kept in container；
(2) material and solvent are heated, when temperature of charge is warming up to 160 DEG C, carries out insulated and stirred；
(3) after wait keep the temperature, cool down to material, be cooled to 100 DEG C of degree at a slow speed first；In this temperature-fall period,
Nylon can be precipitated by nucleus Step crystallization of carbon fiber；
(4) room temperature is cooled to rapidly to material, separation drying, institute is carried out to carbon fiber vinylon composite powder particle obtained
Obtained powder particle is target material；
(5) target material obtained in step (4) and a certain amount of flow promortor, antioxidant uniformly mix, gained powder
Sieving is the target material that can be used for selective laser sintering.
Further, in the step (1) nylon pellet select nylon 12, nylon 11, nylon 1212, in nylon 1010
It is one or more of.
Further, organic solvent is alcohols solvent in the step (1), and the alcohols solvent selects methanol, ethyl alcohol, second
One or more of glycol.
Further, the mass fraction of carbon fiber is 10%-30% in the step (1).
Further, the diameter of carbon fiber is 5-20 μm in the step (1), and the length of carbon fiber is 40-120 μm.
Further, the time of insulated and stirred is 2h in the step (2).
Further, the speed to cool down at a slow speed in the step (3) is 0.7 DEG C/min.
Further, the speed to cool down rapidly in the step (4) is 3 DEG C/min.
Further, the mass fraction of flow promortor is 0.1%-1%, the mass fraction of antioxidant in the step (5)
For 0.1%-2%.
It is using the beneficial effect of technical solution of the present invention:
1, the finally obtained carbon fiber nylon powder particle of the present invention, nylon are coated on outside carbon fiber, and regular appearance is in
It is spherical.Particle size distribution concentrates particle size between 40-90um.
2, the pattern of powder particle is round, and closer to spherical-like morphology, then the mobility of powder is better, is more conducive to SLS
Processing.
3 and carbon fiber vinylon composite powder particle prepared by the present invention, from microcosmic, each powder particle has carbon fiber
Dimension is wrapped by nylon, and two kinds of components are combined together, evenly dispersed, will not generate segregation phenomenon.Finally with material system in this
Standby SLS molded part performance stable equilibrium.It is evenly distributed simultaneously by the carbon fiber direction that nylon resin wraps up, final SLS molding
Also the moon is balanced for the performance of product all directions, stablizes.
4, present invention process is easy to operate, and in process, by controlling rate of temperature fall, mixing speed is final to control
The size and pattern of the powder particle of preparation.
5, present invention process is simple, and cost is very low.Organic solvent in preparation process may be repeated use, will not
It pollutes or wastes.
Detailed description of the invention
Fig. 1 is the pattern comparison diagram of the material for preparing under 100 power microscopes in comparative example 2.
Fig. 2 is the pattern comparison diagram of the material for preparing under 100 power microscopes in embodiment 2.
Fig. 3 is the pattern comparison diagram of the material for preparing under 400 power microscopes in embodiment 2.
Specific embodiment
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Embodiment 1
1,9KgPA12 particle, 1kg carbon fiber and 100L ethyl alcohol are added in sealing container, to carrying out charge and discharge in container
Nitrogen 3 times, pressure in sealed container reaches 0.2MPa.
2, heat temperature raising, when its temperature reaches 160 DEG C, insulated and stirred 2 hours then are carried out to material.Then it is dropped
Temperature；100 DEG C are cooled to 0.7 DEG C/min first, is then quickly down to room temperature by 3 DEG C/min.
3, the obtained powder particle of step 2 is subjected to separation drying, particle is separated, obtained powder particle
As target product.
4, the powder particle and antioxidant obtained step 3, flow promortor are mixed according to 1:0.001:0.001 proportions
It closes, screening obtains a kind of selective laser sintering nylon-solid glass micro-bead composite powder material.
5, step 4 powder is formed in SLS equipment, preparation technology parameter are as follows: laser power 40W, scanning speed
4000mm/s, sweep span 0.3, sintered layer thickness 0.12mm；Gained SLS product is tested for the property by iso standard, is as a result seen
Table 1.
Embodiment 2
1,8KgPA12 particle, 2kg carbon fiber and 100L ethyl alcohol are added in sealing container, to carrying out charge and discharge in container
Nitrogen 3 times, pressure in sealed container reaches 0.2MPa.
2, heat temperature raising, when its temperature reaches 160 DEG C, insulated and stirred 2 hours then are carried out to material.Then it is dropped
Temperature；100 DEG C are cooled to 0.7 DEG C/min first, is then quickly down to room temperature by 3 DEG C/min.
3, the obtained powder particle of step 2 is subjected to separation drying, particle is separated, obtained powder particle
As target product.
4, the powder particle and antioxidant obtained step 3, flow promortor are mixed according to 1:0.005:0.005 proportions
It closes, screening obtains a kind of selective laser sintering nylon-solid glass micro-bead composite powder material.
5, step 4 powder is formed in SLS equipment, preparation technology parameter are as follows: laser power 40W, scanning speed
4000mm/s, sweep span 0.3, sintered layer thickness 0.12mm；Gained SLS product is tested for the property by iso standard, is as a result seen
Table 1, micrograph is shown in Fig. 2 and Fig. 3.
Embodiment 3
1,7KgPA12 particle, 3kg carbon fiber and 100L ethyl alcohol are added in sealing container, to carrying out charge and discharge in container
Nitrogen 3 times, pressure in sealed container reaches 0.2MPa.
2, heat temperature raising, when its temperature reaches 160 DEG C, insulated and stirred 2 hours then are carried out to material.Then it is dropped
Temperature；100 DEG C are cooled to 0.7 DEG C/min first, is then quickly down to room temperature by 3 DEG C/min.
3, the obtained powder particle of step 2 is subjected to separation drying, particle is separated, obtained powder particle
As target product.
4, the powder particle and antioxidant obtained step 3, flow promortor are mixed according to 1:0.01:0.02 proportions,
Screening, obtains a kind of selective laser sintering nylon-solid glass micro-bead composite powder material.
5, step 4 powder is formed in SLS equipment, preparation technology parameter are as follows: laser power 40W, scanning speed
4000mm/s, sweep span 0.3, sintered layer thickness 0.12mm；Gained SLS product is tested for the property by iso standard, is as a result seen
Table 1.
Comparative example 1
1,10KgPA12 particle and 100L ethyl alcohol are added in sealing container, are carried out charge and discharge nitrogen 3 times in container, it is close
Envelope container inner pressure reaches 0.2MPa.
2, heat temperature raising, when its temperature reaches 160 DEG C, insulated and stirred 2 hours then are carried out to material.Then it is dropped
Temperature；100 DEG C are cooled to 0.7 DEG C/min first, is then quickly down to room temperature by 3 DEG C/min.
3, the obtained powder particle of step 2 is subjected to separation drying, particle is separated, obtained powder particle with
Antioxidant, flow promortor are mixed according to 1:0.05:0.05 proportions, and screening obtains a kind of selective laser sintering nylon
Dusty material.
4, step 3 powder is formed in SLS equipment, preparation technology parameter are as follows: laser power 40W, scanning speed
4000mm/s, sweep span 0.3, sintered layer thickness 0.12mm；Gained SLS product is tested for the property by iso standard, is as a result seen
Table 1.
Comparative example 2
Mechanical mixture 1h in vertical stirrer is added in PA12 powder prepared by 9kg comparative example one, 1kg carbon fiber together
Obtain the nylon 12- glass microballoon dusty material of solid glass micro-bead enhancing.It is formed in SLS equipment, preparation technology parameter
Are as follows: laser power 40W, scanning speed 4000mm/s, sweep span 0.15, sintered layer thickness 0.12mm；Gained SLS product is pressed
Iso standard is tested for the property, and the results are shown in Table 1, and micrograph is by Fig. 1.
Table 1: the mechanical property of material SLS printing product
Flow promortor in the present invention can use polypropylene plastics flow increasing using the common flow promortor in this field
Agent, polycarbonate plastic flow increasing agent, polyester flow increasing agent, Hips Plastics flow increasing agent etc..
Antioxidant in the present invention can use Phosphorus antioxidant, phenols using the common plastics antioxidant in this field
Antioxidant or natural inhibitor etc..
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.It is all in essence of the invention
Within mind and principle, any modification, equivalent substitution, improvement and etc. done be should all be included in the protection scope of the present invention.This
The technical scope of item invention is not limited to the contents of the specification, it is necessary to its technology is determined according to scope of the claims
Property range.
Claims (10)
1. a kind of nylon carbon fiber composite powder of the reduction material anisotropy for selective laser sintering, feature exist
In: including carbon fiber nucleus, the outer surface of the carbon fiber nucleus is coated with nylon layer, and the diameter of the carbon fiber nucleus is 5-
20 μm, the length of the carbon fiber nucleus is 40-120 μm, and the Average Particle Diameters of the composite powder are 40-90 μm.
2. a kind of preparation method of the nylon carbon fiber composite powder of the reduction material anisotropy for selective laser sintering,
It is characterized by: the preparation method comprises the following steps:
(1) nylon pellet, carbon fiber and organic solvent are placed in sealing container, charge and discharge nitrogen is carried out to container, exclude to hold
After air in device, make the pressure that 0.2MPa is kept in container；
(2) material and solvent are heated, when temperature of charge is warming up to 160 DEG C, carries out insulated and stirred；
(3) after wait keep the temperature, cool down to material, be cooled to 100 DEG C of degree at a slow speed first；In this temperature-fall period, nylon
It can be precipitated by nucleus Step crystallization of carbon fiber；
(4) room temperature is cooled to rapidly to material, separation drying is carried out to carbon fiber vinylon composite powder particle obtained, it is acquired
Powder particle be target material；
(5) target material obtained in step (4) and a certain amount of flow promortor, antioxidant uniformly mix, the sieving of gained powder
It as can be used for the target material of selective laser sintering.
3. a kind of nylon carbon fiber of reduction material anisotropy for selective laser sintering according to claim 2
The preparation method of composite powder, it is characterised in that: nylon pellet selects nylon 12, nylon 11, nylon in the step (1)
1212, one or more of nylon 1010.
4. a kind of nylon carbon fiber of reduction material anisotropy for selective laser sintering according to claim 2
The preparation method of composite powder, it is characterised in that: organic solvent is alcohols solvent in the step (1), the alcohols solvent choosing
With methanol, ethyl alcohol, one or more of ethylene glycol.
5. a kind of nylon carbon fiber of reduction material anisotropy for selective laser sintering according to claim 2
The preparation method of composite powder, it is characterised in that: the mass fraction of carbon fiber is 10%-30% in the step (1).
6. a kind of nylon carbon fiber of reduction material anisotropy for selective laser sintering according to claim 2
The preparation method of composite powder, it is characterised in that: the diameter of carbon fiber is 5-20 μm in the step (1), the length of carbon fiber
It is 40-120 μm.
7. a kind of nylon carbon fiber of reduction material anisotropy for selective laser sintering according to claim 2
The preparation method of composite powder, it is characterised in that: the time of insulated and stirred is 2h in the step (2).
8. a kind of nylon carbon fiber of reduction material anisotropy for selective laser sintering according to claim 2
The preparation method of composite powder, it is characterised in that: the speed to cool down at a slow speed in the step (3) is 0.7 DEG C/min.
9. a kind of nylon carbon fiber of reduction material anisotropy for selective laser sintering according to claim 2
The preparation method of composite powder, it is characterised in that: the speed to cool down rapidly in the step (4) is 3 DEG C/min.
10. a kind of nylon carbon fiber of reduction material anisotropy for selective laser sintering according to claim 2
Tie up the preparation method of composite powder, it is characterised in that: the mass fraction of flow promortor is 0.1%-1%, antioxygen in the step (5)
The mass fraction of agent is 0.1%-2%.
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Cited By (1)
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|---|---|---|---|---|
| CN112453401A (en) * | 2020-12-04 | 2021-03-09 | 西安交通大学 | Method for reducing anisotropy of rare earth molybdenum alloy material |
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