CN105949754A - Low-melting-point and low-crystallinity nylon 6 powder for SLS (Selective Laser Sintering) and preparation method of nylon 6 powder - Google Patents
Low-melting-point and low-crystallinity nylon 6 powder for SLS (Selective Laser Sintering) and preparation method of nylon 6 powder Download PDFInfo
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Abstract
The invention relates to the technical field of nylon materials for SLS (Selective Laser Sintering), in particular to low-melting-point and low-crystallinity nylon 6 powder for SLS and a preparation method of the nylon 6 powder. The nylon 6 powder is prepared from the following raw materials in parts by weight: 93-98 parts of nylon 6 granules, 7-2 parts of metal ion salt and 0.4-1 part of aids. The preparation method comprises steps as follows: step one, the nylon 6 granules and the metal ion salt powder are weighed in parts by weight, dried, mixed uniformly and extruded and granulated with a double-screw extruder, the rotating speed of screws is 150-170 r/min, and the temperature is controlled to be 200-250 DEG C; step two, the granules obtained in the step one are smashed and sieved, and powdery granules with diameter being 20-120 mu m are obtained; step three, the powdery granules obtained in the step two and the aids are uniformly mixed in proportion and sieved , and the nylon 6 powder with diameter being 20-120 mu m is obtained. The nylon 6 powder has lower melting point and lower crystallinity, and a product obtained through SLS has a good overall forming effect and high size precision.
Description
Technical field
The present invention relates to the nylon material technical field for SLS, be specifically related to a kind of low crystallization of the low melting point for SLS
Nylon 6 powder of degree and preparation method thereof.
Background technology
Selective laser sintering (Selective Laser Sintering is called for short SLS) is that development in recent years is the rapidest
One of rapid shaping technique, it is with pressed powder as raw material, uses laser successively to scan through the cross section of 3D solid
Become raw basin.SLS product is not limited by part shape complexity, can accurately fast restore design concept, quickly produce
The functional test part of new product, small lot batch manufacture complex parts etc., breach the restriction of traditional manufacturing technology.
In theory, the powder of any crystallization or those semi-crystalline materials can serve as SLS sintered material, scope of selecting material
It it is extensively one of SLS technique key factor of can be widely applied for each field.Nylon is a kind of crystalline polymer, its SLS system
Part all has more excellent performance at the aspect such as intensity, consistency, is a kind of macromolecule material being highly suitable for SLS technique
Material.Nylon-based resin material is a kind of semi-crystalline polymer, has good sintering character and relatively low melt viscosity, can be by
SLS straight forming consistency is higher, the preferable function part of mechanical property, becomes the SLS forming material being most widely used at present
One of material.
But being affected by SLS processing technique, the well suited Nylon type in SLS of energy is less at present, especially to melted
For temperature and the high nylon material (such as PA6, PA66 etc.) of degree of crystallinity, the high-melting-point of material can make in the SLS course of processing,
Material need to the highest at one at a temperature of be processed, and high temperature can make material oxidation the most serious.SLS processing mode is
By the most successively molding, and high-crystallinity can make material occur serious receipts in the course of processing due to crystallization
Contracting warping phenomenon, affects forming process and the global formation effect of product and the dimensional accuracy of SLS processing.
In order to improve the utilization rate of material and reduce the degree of oxidation of material in prior art, one is by improving SLS
The sealing of process equipment, reduces its oxygen content in the course of processing；Two is by adding antioxidant in a large number.But in reality
In process of manufacture, the interpolation of antioxidant is difficult to reach preferable effect first, and second antioxidant addition too may well
Influence whether the performance of product, and reduce the oxygen content in SLS equipment and especially current SLS equipment is proposed the highest wanting
Ask, particular for making product have the smooth of more preferable global formation stability and the SLS course of processing, often make
The SLS course of processing is had to be maintained at for a long time one higher at a temperature of.Therefore high-temperature nylon material is (such as PA6, PA66 at present
Deng) still can not well be applicable to SLS sintering.
Summary of the invention
In order to overcome shortcoming and defect present in prior art, it is an object of the invention to provide a kind of for SLS's
Nylon 6 powder of low melting point low-crystallinity, has relatively low fusing point and degree of crystallinity, so that can have one in the course of processing
Individual lower processing temperature so that it can preferably be applicable to selective laser sintering；And the reduction of degree of crystallinity so that
In scanning cross-section cooling procedure after laser scanning, keep good formed precision, receipts will not be produced because of rapid crystallization
Contracting inequality or scanning cross-section warping phenomenon, thus also make SLS processing product have good global formation dimensional accuracy.
Another goal of the invention of the present invention is to provide nylon 6 powder of a kind of low melting point low-crystallinity for SLS
Preparation method, preparation method is easy, it is easy to manipulation, and production cost is low, and productivity is high, the fusing point of nylon 6 powder obtained and crystallization
Spend low, be highly suitable to be applied for SLS product.
The purpose of the present invention is achieved through the following technical solutions:
Nylon 6 powder of a kind of low melting point low-crystallinity for SLS, is made up of the raw material of following weight portion:
Nylon 6 pellet 93-98 part,
Metal cation salt 7-2 part,
Auxiliary agent 0.4-1 part.
Metal cation salt alleged by the present invention, refers at the compound melting or having under dissolved state metal ion,
The present invention, by metal ion and nylon molecules generation complex reaction, destroys the hydrogen bond structure of amido link, energy on nylon 6 strand
Enough crystallization temperatures effectively reducing nylon 6 and melt temperature.
Wherein, described metal cation salt is any one in CaCl2, CaSO4, NaCl, and cost of material is low, with the network of nylon 6
Close completely reacted, can effectively reduce crystallization temperature and the melt temperature of nylon 6.
NaCl's is the most hygroscopic, it is easy to operation.
Wherein, the particle diameter of described metal cation salt is less than 120 μm.Specific particle diameter is more preferable with nylon 6 mixed effect, favorably
In the degree of accuracy improving later stage product.The particle diameter of nylon 6 is 20-100 μm.
Wherein, described auxiliary agent is flow promortor, adds a small amount of flow promortor, is conducive to improving the degree of accuracy of product and whole
Body effect.
Wherein, described auxiliary agent is antioxidant, improves the antioxygenic property of nylon 6 powder.
Wherein, described auxiliary agent is flow promortor and the antioxidant additive package according to weight ratio 1:1, it is possible to improve simultaneously
The antioxygenic property of nylon 6 powder and mobility, improve the suitability in SLS technique of nylon 6 powder.
Concrete, in nylon 6 powder of 100 parts of weight portions, nylon 6 pellet is 93-with the mixed proportion of metal cation salt
98:7-2, auxiliary agent as the interpolation auxiliary agent in later stage, with nylon 6 pellet with the mixed powder particle of metal cation salt for metering base
Plinth, nylon 6 pellet of every 100 parts and metal cation salt compound add flow promortor and the antioxidant of 0.4-0.5 part.
Wherein, described flow promortor is aerosil.Be conducive to improving degree of accuracy and the whole structure of product.
Wherein, described antioxidant is antioxidant 9228 or antioxidant 1098.Improve the antioxygenic property of nylon 6 powder.
A kind of preparation method of nylon 6 powder of the low melting point low-crystallinity for SLS, including following preparation process:
Step one, weigh nylon 6 pellet and the dried mix homogeneously of metal ion salt powder by weight, utilize twin-screw extrusion
Machine extruding pelletization, screw speed is 150-170r/min, and temperature controls at 200-250 DEG C；
Step 2, pellet step one obtained pulverize and sieve, and obtain the powder particle that particle diameter is 20-120 μm；
Step 3, powder particle step 2 obtained mix in proportion with auxiliary agent, and sieving, to obtain particle diameter be 20-120 μm
Nylon 6 powder.
Wherein, the breaking method of described step 2 is deep cooling crush.By using low-temperature receiver and material to carry out heat exchange；Make thing
Material cools to brittle state；Material after embrittlement carries out shock many times by disintegrating mechanism in crushing chamber and finally becomes thin
Fine granularity, the fineness of materials after pulverizing can reach micron grade (600 ~ 2000 mesh).Low to the material properties affect of material, pulverize
Effective, efficiency is high.
Concrete, the technique of described deep cooling crush is:
A, prepared nylon pellet is immersed in liquid nitrogen, then with deep cooling crush machine, pellet is pulverized；
B, powder particle step A obtained cross 100 mesh vibrosieves, remove big diameter powders granule.
C, powder multi-stage classifier step B obtained sieve, by the powder particle classification below 20 μm out
I.e. can get nylon 6 powder.
Further, in described disintegrating process, the pulverizing temperature of pulverizing chamber controls between-120～-115 DEG C, regulation
Rotor clearance is 1.0～2mm, and engine speed is 3000-4000r/min, and feed rate controls at 5-10kg/kW.h.Pulverize
During control above-mentioned relevant parameter, it is ensured that pulverize obtain powder particle particle diameter distribution D50 between 40-60 μm, particle diameter exists
This scope can keep powder to have preferable mobility and bulk density, it is simple to SLS processing and the molding effect of SLS product.
General deep cooling crush is applied in terms of powdery paints: engine speed 6000～7500, rotor clearance 1. 5～4
Mm pulverizes temperature-80 DEG C, unit power treating capacity (feed rate) 2.7kg/kW.h, and the granule obtained is irregular flake powder
End.The present invention be directed to the goal of the invention of the present invention, the technique that the technique of deep cooling crush is obtained matters through numerous experiments
Parameter, the powder particle obtained is the rule particle that sphericity is high, and the powder diameter that different technical parameters obtains is distinguished such as following table
Shown in:
Traditional deep cooling crush technique is typically employed in paint field, because the granule that deep cooling crush technique obtains is irregular thin
Little granule, its specific surface area is big, and the absorption to coating has greatly improved.But the powder obtained by existing deep cooling crush
Grain can not be applicable to selective laser sintering (SLS) 3D and print field.Its main cause has these aspects:
1, the powder particle that presently used deep cooling crush obtains is less than normal, its granule-morphology often in irregular sheet-like particle, as
This is then in the SLS course of processing, and powder particle is too big due to its specific surface area, and the least meeting of granule makes powder be bonded at paving powder
On cylinder or scraper, it is impossible to the paving powder effect having had.
2, the powder particle that deep cooling crush obtains is due to adsorption, causes its mobility very poor, in the SLS course of processing
In, it is impossible to carry out spreading powder.Even if its mobility acquisition preferably paving powder effect can be improved by adding substantial amounts of flow promortor,
But to SLS technique, when flow promortor addition is the biggest when, can cause, in the SLS course of processing, working as laser scanning
The when of powder face, scanning edge can occur crimp, cannot continue so that print.Therefore flow promortor is added
Add and typically not can exceed that 1%.And to reach preferably to spread powder effect in the range of this flow promortor addition, deep cooling is prepared
Powder face granule and pattern require higher, and current deep cooling crush technique is unable to reach this requirement.
3, the principle of deep cooling crush is that the height utilizing material under ultralow temperature is brittle and make it pulverize by physical action,
Therefore, in crushing process, owing to producing stress induced molecular chain orientation institute during physical pulverization extremely, material is easier to crystallization,
So that the crystallization temperature of PA raises after deep cooling crush.
Following table is its crystalline temperature and the numerical tabular of fusing point before and after PA6 deep cooling crush.PA6 passes through as can be seen from the table
After deep cooling crush, its fusing point Tm improves about 3 DEG C, and its crystallization temperature improves nearly 20 DEG C.
| Tm | Tc | |
| PA6 deep cooling crush money | 223.8 | 167.9 |
| After PA6 pulverizes | 226.7 | 187.0 |
In the SLS course of processing, in order to keep 3D to print molding effect and the formed precision of product, it is required that SLS adds
Work product is maintained at a higher ambient temperature after the end of scan and (is expressed as working cylinder piston temperature in this temperature of SLS equipment
Degree and working cylinder cylinder wall temperature), this temperature is typically set in more than the crystallization temperature of material.Therefore to obtain more preferable product
Effect and preferably machinability and machined parameters and higher material reusability, the material for SLS technique the most all needs
There is lower crystallization temperature.Deep cooling crush then can improve the crystallization temperature of material itself.The present invention is by advance to PA material
Material carries out crystallization suppression, during deep cooling, can't improve because physical pulverization produces stress induced molecular chain orientation
Its crystallization temperature.
The beneficial effects of the present invention is: the nylon powder material of the present invention has relatively low fusing point and degree of crystallinity, thus
Make there is a lower processing temperature in the course of processing so that it can preferably be applicable to selective laser and burn
Knot；And the reduction of degree of crystallinity is so that in scanning cross-section cooling procedure after laser scanning, keep good formed precision,
Contraction inequality or scanning cross-section warping phenomenon will not be produced because of rapid crystallization, thus also make SLS processing product have good
Good global formation dimensional accuracy.
The present invention another advantage is that: preparation method is simple, it is easy to operation.
Accompanying drawing explanation
Fig. 1 is the contrast of the profiled member that the nylon 6 material that the present invention prepares utilizes SLS processing to prepare with pure nylon 6 material
Figure.
Detailed description of the invention
For the ease of the understanding of those skilled in the art, below in conjunction with embodiment, the present invention is further illustrated, real
The content that the mode of executing is mentioned not limitation of the invention.
Embodiment 1
A kind of preparation method of nylon 6 powder of the low melting point low-crystallinity for SLS, including following preparation process:
Step one, weigh 98 weight portion nylon 6 pellets and the 2 weight portion dried mix homogeneously of CaCl2 powder, utilize twin screw to squeeze
Going out machine extruding pelletization, screw speed is 150r/min, and temperature controls at 200 DEG C；
Step 2, pellet step one obtained pulverize and sieve, and obtain the powder particle that particle diameter is 20 μm；
Step 3, powder particle step 2 obtained and aerosil, antioxidant 9228 are by weight 1:0.003:
0.003 mix homogeneously, sieves and obtains nylon 6 powder that particle diameter is 20 μm.
Embodiment 2
A kind of preparation method of nylon 6 powder of the low melting point low-crystallinity for SLS, including following preparation process:
Step one, weigh 96 weight portion nylon 6 pellets and the 4 weight portion dried mix homogeneously of CaSO4 powder, utilize twin screw to squeeze
Going out machine extruding pelletization, screw speed is 160r/min, and temperature controls at 220 DEG C；
Step 2, pellet step one obtained pulverize and sieve, and obtain the powder particle that particle diameter is 60 μm；
Step 3, powder particle step 2 obtained and aerosil, antioxidant 1098 are by weight 1:0.004:
0.004 mix homogeneously, sieves and obtains nylon 6 powder that particle diameter is 60 μm.
Embodiment 3
A kind of preparation method of nylon 6 powder of the low melting point low-crystallinity for SLS, including following preparation process:
Step one, weigh 94 weight portion nylon 6 pellets and the 6 weight portion dried mix homogeneously of CaCl2 powder, utilize twin screw to squeeze
Going out machine extruding pelletization, screw speed is 170r/min, and temperature controls at 250 DEG C；
Step 2, pellet step one obtained pulverize and sieve, and obtain the powder particle that particle diameter is 80 μm；
Step 3, powder particle step 2 obtained and aerosil, antioxidant 9228 are by weight 1:0.005:
0.005 mix homogeneously, sieves and obtains nylon 6 powder that particle diameter is 80 μm.
Embodiment 4
A kind of preparation method of nylon 6 powder of the low melting point low-crystallinity for SLS, including following preparation process:
Step one, weigh 97 weight portion nylon 6 pellets and the 3 weight portion dried mix homogeneously of CaCl2 powder, utilize twin screw to squeeze
Going out machine extruding pelletization, screw speed is 160r/min, and temperature controls at 240 DEG C；
Step 2, pellet step one obtained pulverize and sieve, and obtain the powder particle that particle diameter is 120 μm；
Step 3, powder particle step 2 obtained and aerosil, antioxidant 1098 are by weight 1:0.005:
0.005 mix homogeneously, sieves and obtains nylon 6 powder that particle diameter is 120 μm.
Comparative example 1
A kind of preparation method of nylon 6 powder, including following preparation process:
Step one, weigh 92 weight portion nylon 6 pellets and the 8 weight portion dried mix homogeneously of CaCl2 powder, utilize twin screw to squeeze
Going out machine extruding pelletization, screw speed is 160r/min, and temperature controls at 240 DEG C；
Step 2, pellet step one obtained pulverize and sieve, and obtain the powder particle that particle diameter is 100 μm；
Step 3, powder particle step 2 obtained and aerosil, antioxidant 1098 are by weight 1:0.005:
0.005 mix homogeneously, sieves and obtains nylon 6 powder that particle diameter is 100 μm.
Comparative example 2
By embodiment 1-5 and comparative example 1 preparation-obtained nylon 6 powder and the fusing point of pure nylon 6, that crystallization temperature is carried out is right
Ratio.
Tc and Tm is respectively peak crystallization temperature and melting peak temperature；△ H is crystalline fusion enthalpy；X is degree of crystallinity, and its computing formula is(the melting enthalpy of the material that embodiment 1-5 and comparative example 1 prepare under wherein △ H is experiment condition；
△H0For the pure PA6 melting enthalpy when 100% crystallization, its numerical value is 240J/g；W is the mass fraction of PA6), concrete data are shown in
Following table:
By above-mentioned data it can be seen that crystallinity X/% represents the degree of crystallinity of material, material crystalline degree is the lowest, and material is at SLS
Deformation in the course of processing is less, and dimensional accuracy is higher, and its product stress is relatively low.See that in accompanying drawing 1, A product is pure nylon 6
The product that obtained by SLS technique of material, B product is the product that nylon 6 pellet of the present invention is obtained by SLS technique, and contrast can
To find out, product deformation prepared by nylon 6 powder of the present invention is little.Melt temperature Tm/ DEG C is related in the material SLS course of processing
Processing sintering temperature, SLS processing temperature is the lowest more good.Represent lower to equipment requirements, the lowest to equipment damage.Degree of crystallinity
Being the lowest more good, material formed precision in the SLS course of processing is the highest.
Above-described embodiment is the present invention preferably implementation, and in addition, the present invention can realize with alternate manner,
Without departing from obvious replacement any on the premise of present inventive concept all within protection scope of the present invention.
Claims (10)
1. nylon 6 powder for the low melting point low-crystallinity of SLS, it is characterised in that: by the raw material group of following weight portion
Become:
Nylon 6 pellet 93-98 part,
Metal cation salt 7-2 part,
Auxiliary agent 0.4-1 part.
Nylon 6 powder of a kind of low melting point low-crystallinity for SLS the most according to claim 1, it is characterised in that: institute
Stating metal cation salt is any one in CaCl2, CaSO4, NaCl.
Nylon 6 powder of a kind of low melting point low-crystallinity for SLS the most according to claim 1, it is characterised in that: institute
State the particle diameter of metal cation salt less than 120 μm.
Nylon 6 powder of a kind of low melting point low-crystallinity for SLS the most according to claim 1, it is characterised in that: institute
Stating auxiliary agent is flow promortor or antioxidant.
Nylon 6 powder of a kind of low melting point low-crystallinity for SLS the most according to claim 1, it is characterised in that: institute
Stating auxiliary agent is flow promortor and the antioxidant additive package according to weight ratio 1:1.
6., according to nylon 6 powder of a kind of low melting point low-crystallinity for SLS described in claim 4 or 5, its feature exists
In: described flow promortor is aerosil.
7., according to nylon 6 powder of a kind of low melting point low-crystallinity for SLS described in claim 4 or 5, its feature exists
In: described antioxidant is antioxidant 9228 or antioxidant 1098.
8. the preparation method of a kind of low melting point low-crystallinity for SLS described in any one of claim 1 to 7, its feature exists
In: include following preparation process:
Step one, weigh nylon 6 pellet and the dried mix homogeneously of metal ion salt powder by weight, utilize twin-screw extrusion
Machine extruding pelletization, screw speed is 150-170r/min, and temperature controls at 200-250 DEG C；
Step 2, the pellet that step one extruding pelletization obtains is pulverized and sieved, obtain the powder particle that particle diameter is 20-120 μm；
Step 3, powder particle step 2 obtained mix in proportion with auxiliary agent, and sieving, to obtain particle diameter be 20-120 μm
Nylon 6 powder of a kind of low melting point low-crystallinity for SLS.
The preparation method of a kind of low melting point low-crystallinity for SLS the most according to claim 8, it is characterised in that: institute
The breaking method stating step 2 is deep cooling crush, and the flouring technology of described deep cooling crush is:
A, the pellet obtained by extruding pelletization are immersed in liquid nitrogen, then pulverize pellet with deep cooling crush machine；Control
The broken powder particle particle diameter obtained of powder process is distributed between 40-60 μm；
B, powder particle step A obtained cross 100 mesh vibrosieves, remove big diameter powders granule；
C, powder multi-stage classifier step B obtained sieve, and by the powder particle classification of less than 20 microns are out
Available nylon 6 powder.
The preparation method of a kind of low melting point low-crystallinity for SLS the most according to claim 8, it is characterised in that: institute
The pulverizing temperature stating pulverizing chamber in disintegrating process controls between-120～-115 DEG C, regulation rotor clearance be 1.0～
2mm, engine speed is 3000-4000r/min, and feed rate controls at 5-10kg/kW.h.
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