CN110157149A - A kind of polyetherether ketone composition and preparation method thereof for selective laser sintering - Google Patents
A kind of polyetherether ketone composition and preparation method thereof for selective laser sintering Download PDFInfo
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- CN110157149A CN110157149A CN201910394430.9A CN201910394430A CN110157149A CN 110157149 A CN110157149 A CN 110157149A CN 201910394430 A CN201910394430 A CN 201910394430A CN 110157149 A CN110157149 A CN 110157149A
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- carbon fiber
- selective laser
- laser sintering
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- ether
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
Abstract
The polyetherether ketone composition and preparation method thereof that the invention discloses a kind of for selective laser sintering, belongs to field of compound material.This is used for the polyetherether ketone composition of selective laser sintering, in parts by weight, the carbon fiber including 80-95 parts of polyether-ether-ketone powders and 5-20 parts；The carbon fiber is the carbon fiber for removing sizing agent and impurity；The thermal decomposition temperature of the sizing agent and impurity is 350-500 DEG C.The polyetherether ketone composition has preferable SLS forming technology performance, the pre- thermal efficiency for showing as powder bed greatly improves, preheating temperature reduces, product intensity and modulus is significantly improved compared to more single resin product, can be widely used for the direct manufacture and small lot production of the terminal parts with complex structures in the fields such as aerospace, biology, machinery, military project.
Description
Technical field
The present invention relates to field of compound material, specifically a kind of polyetherether ketone composition for selective laser sintering and its
Preparation method.
Background technique
Selective laser sintering (Selective Laser Sintering, abbreviation SLS) is a kind of increases material manufacturing technology, with
Powdered metal, ceramics, macromolecule and its composite powder is raw material, is made with the high-power energy beam such as laser, electron beam
It for heat source, realizes that the selectivity of dusty material is melted under control of the computer, forms the shape of design after crystallisation by cooling, and by
Layer heap product is until form final products.Powder bed fusion sediment technique has many advantages, such as that shaping speed is fast, product intensity is high, especially
It is for crystallization and hypocrystalline high molecular material, the consistency of the product of selective laser sintering forming can reach 95% or more, by force
Degree can reach the level of its moulding substantially.
Currently, nylon based material is most commonly used material in SLS research, and including PA12, PA11, PA6 etc., SLS system
Part has preferable mechanical strength and craftsmanship, and preheating temperature has obtained extensive quotient generally between 160-180 DEG C at present
Industry application.But with the continuous extension of increases material manufacturing technology application range, the mechanical property of nylon based material, hot high temperature
Performance etc. is not able to satisfy the requirement of certain industries gradually, especially in aerospace field, polyether-ether-ketone (PEEK) material as a result,
SLS molding gradually researcher interest.
PEEK is a kind of hypocrystalline high molecular material, have very high mechanical property, heat resistance (fusing point be 330 DEG C extremely
385 DEG C), wearability and chemical corrosion resistance.In recent years, SLS of some scholars to polyether-ether-ketone (PEEK), polyether-ketone (PEK)
Technique and performance expand research, the experimental results showed that, the SLS product of polyether-ether-ketone has higher compared to nylon based material
Mechanical strength and heat resistance, but product intensity is still significantly lower than its moulding, and shapes the required higher (> of preheating temperature
320 DEG C), it is very high to requirements such as the heat resistances of equipment.
Summary of the invention
It is an object of the invention to overcome the above-mentioned prior art, a kind of polyethers for selective laser sintering is provided
Ether one compositions and preparation method thereof.
In order to achieve the above objectives, the present invention is achieved by the following scheme:
A kind of polyetherether ketone composition for selective laser sintering, in parts by weight, including 80-95 parts of polyethers
Ether ketone powder and 5-20 parts of carbon fiber；
The carbon fiber is the carbon fiber for removing sizing agent and impurity.
Further, the thermal decomposition temperature of the sizing agent and impurity is 350-500 DEG C.
Further, the partial size of polyether-ether-ketone powder is 20-100 μm.
Further, the partial size of polyether-ether-ketone powder is in normal distribution.
Further, the carbon fiber diameter is 7-10 μm.
Further, the carbon fiber length is 100-400 μm.
Further, the thermally treated removal sizing agent of the carbon fiber and impurity.
Further, the condition of the heat treatment is 350-500 DEG C, keeps the temperature 2-3h.
A kind of preparation method of the polyetherether ketone composition for selective laser sintering, comprising the following steps:
1) component is weighed, 80-95 parts of polyether-ether-ketone powder and 5-20 parts of carbon fiber, the polyether-ether-ketone powder are weighed
Partial size be 20-100 μm；The carbon fiber diameter is 7-10 μm, and length is 100-400 μm；
2) carbon fiber is heat-treated, the heat treatment condition is 350-500 DEG C of temperature, soaking time 2-3 h；
3) by the carbon fiber powder after polyether-ether-ketone powder and heat treatment, it is stirred mixing, is obtained for selective laser
The polyetherether ketone composition of sintering.
Compared with prior art, the invention has the following advantages:
Polyetherether ketone composition and preparation method thereof for selective laser sintering of the invention, due to joined in removal
The carbon fiber for starching agent and impurity, in SLS forming process, sizing agent and impurity when avoiding heating on carbon fiber volatilize and make
The case where there are holes at sintered part；The polyetherether ketone composition has preferable SLS forming technology performance, shows as powder bed
The pre- thermal efficiency greatly improve, required preheating temperature reduces, and product intensity and modulus is obvious compared to more single polyether-ether-ketone product
Improve, can be widely used for the terminal parts with complex structures in the fields such as aerospace, biology, machinery, military project it is direct manufacture and
Small lot production.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, technical solution in the embodiment of the present invention
It is clearly and completely described, it is clear that the described embodiment is only a part of the embodiment of the present invention, rather than all
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art institute without making creative work
The every other embodiment obtained, should fall within the scope of the present invention.
It should be noted that the term " first ", " second " etc. in description and claims of this specification are to be used for
Similar object is distinguished, without being used to describe a particular order or precedence order.It should be understood that the data used in this way are suitable
It can be interchanged in the case of, so that the embodiment of the present invention described herein can be with the sequence other than in those of description
Implement.In addition, term " includes " and " having " and their any deformation, it is intended that cover it is non-exclusive include, for example,
The process, method, system, product or equipment for containing a series of steps or units those of are not necessarily limited to be clearly listed step
Or unit, but may include other steps being not clearly listed or intrinsic for these process, methods, product or equipment
Or unit.
Embodiment 1:
(1) according to following data precise each component: weighing the polyether-ether-ketone powder that 1.9kg partial size is 20-50 μm, adopt
Chopped carbon fiber is sieved with 60 mesh screens, the carbon fiber diameter after screening is 7-10 μm, and length is 300-400 μm, weighs screening
Carbon fiber 0.1kg afterwards；
(2) polyether-ether-ketone powder is placed in drying box and is sufficiently dried to remove moisture removal, temperature is 120 DEG C, time 3h, powder
Last thickness is no more than 50mm；By carbon fiber as in heat-treatment furnace, it is arranged 350 DEG C of temperature, keeps the temperature 2h, be cooled to room temperature taking-up；
(3) by the carbon fiber powder after sufficiently dry polyether-ether-ketone powder and heat treatment, be put into high-speed mixer into
Row is stirred, and mixing speed is 260 turns/min, and target material can be obtained in mixing time 2h.
Embodiment 2:
(1) according to following data precise each component: weighing the polyether-ether-ketone powder that 1.8kg partial size is 50-80 μm, adopt
Chopped carbon fiber is sieved with 60 mesh screens, the carbon fiber diameter after screening is 7-10 μm, and length is 250-400 μm, weighs screening
Carbon fiber 0.2kg afterwards；
(2) polyether-ether-ketone powder is placed in drying box and is sufficiently dried to remove moisture removal, temperature is 120 DEG C, time 3h, powder
Last thickness is no more than 50mm；By carbon fiber as in heat-treatment furnace, it is arranged 500 DEG C of temperature, keeps the temperature 2h, be cooled to room temperature taking-up；
(3) by the carbon fiber powder after sufficiently dry polyether-ether-ketone powder and heat treatment, be put into high-speed mixer into
Row is stirred, and mixing speed is 250 turns/min, and target material can be obtained in mixing time 3h.
Embodiment 3:
(1) according to following data precise each component: the polyether-ether-ketone powder that 1.8kg partial size is 70-100 μm is weighed,
Chopped carbon fiber is sieved using 100 mesh screens, the carbon fiber diameter after screening is 7-10 μm, and length is 150-200 μm, weighs sieve
Carbon fiber 0.2kg after point；
(2) polyether-ether-ketone powder being placed in drying box and is sufficiently dried to remove moisture removal, temperature is 120 DEG C, time 3-5h,
Powder thickness is no more than 50mm；By carbon fiber as in heat-treatment furnace, it is arranged 400 DEG C of temperature, keeps the temperature 3h, be cooled to room temperature and take
Out；
(3) by the carbon fiber powder after sufficiently dry polyether-ether-ketone powder and heat treatment, be put into high-speed mixer into
Row is stirred, and mixing speed is 260 turns/min, and target material can be obtained in mixing time 2h.
Embodiment 4:
(1) according to following data precise each component: the polyether-ether-ketone powder that 1.7kg partial size is 20-100 μm is weighed,
Chopped carbon fiber is sieved using 80 mesh screens, the carbon fiber diameter after screening is 7-10 μm, and length is 180-300 μm, weighs sieve
Carbon fiber 0.3kg after point；
(2) polyether-ether-ketone powder is placed in drying box and is sufficiently dried to remove moisture removal, temperature is 120 DEG C, time 3h, powder
Last thickness is no more than 50mm；By carbon fiber as in heat-treatment furnace, it is arranged 350 DEG C of temperature, keeps the temperature 2.5h, be cooled to room temperature and take
Out；
(3) by the carbon fiber powder after sufficiently dry polyether-ether-ketone powder and heat treatment, be put into high-speed mixer into
Row is stirred, and mixing speed is 260 turns/min, and target material can be obtained in mixing time 2h.
Embodiment 5:
(1) according to following data precise each component: the polyether-ether-ketone powder that 1.6kg partial size is 20-100 μm is weighed,
Chopped carbon fiber is sieved using 100 mesh screens, the carbon fiber diameter after screening is 7-10 μm, and length is 100-200 μm, weighs sieve
Carbon fiber 0.4kg after point；
(2) polyether-ether-ketone powder is placed in drying box and is sufficiently dried to remove moisture removal, temperature is 120 DEG C, time 4h, powder
Last thickness is no more than 50mm；By carbon fiber as in heat-treatment furnace, it is arranged 400 DEG C of temperature, keeps the temperature 3h, be cooled to room temperature taking-up；
(3) by the carbon fiber powder after sufficiently dry polyether-ether-ketone powder and heat treatment, be put into high-speed mixer into
Row is stirred, and mixing speed is 260 turns/min, and target material can be obtained in mixing time 2h.
It is multiple to polyether-ether-ketone powder and carbon fiber reinforced polyether-ether-ketone prepared by the present invention using selective laser formation system
It closes powder and has carried out SLS forming, the intensity and modulus such as table 1 of best forming technology and SLS drip molding under this condition, from table 1
As can be seen that preheating temperature is pre- compared to single polyether-ether-ketone using polyetherether ketone composition of the invention when SLS is formed
Hot temperature decreases, and product intensity and modulus are significantly improved compared to the product of more single polyether-ether-ketone.
Table 1 is using the material of PEEK and above-described embodiment as the mechanical property of the SLS drip molding of raw material
Toner in the present invention is polyether-ether-ketone powder, since in SLS technical process, powder diameter is needed one
In order to powdering and thermal sintering in a suitable range, experiment shows that the average grain diameter of SLS powder is usually no more than 100 μ
M, polyether-ether-ketone powder grain diameter used in the present invention is between 20-100 μm, and particle diameter distribution is in normal distribution, and shape is
Irregular particle.
Chopped carbon fiber diameter in the present invention is 7-10 μm, and preferred length is 100-400 μm.According to composite material strength
Theory, carbon fiber is longer, better to the reinforcing effect of basis material, but too long carbon fiber will cause and be difficult with toner
It is uniformly mixed, and the mobility of composite powder is lower, is unfavorable for powdering, is hardly formed more smooth powder bed, thus shadow
Ring the progress of selective laser sintering.
Chopped carbon fiber in the present invention needs before mixing with PEEK powder using high-temperature process, due to carbon
Fiber in process of production, in order to increase with the binding performance of thermosetting resin, reduce crude increase operability, can generally make
Use sizing agent.Since the fusing point of PEEK material is higher (330 DEG C of >), instantaneous temperature during selective laser sintering can be more
Height, so as to be pyrolyzed impurity or the sizing agent of carbon fiber surface, the gas that when pyrolysis generates can be taken away largely
Heat causes product to shape a large amount of holes, and consistency and intensity are poor.Currently preferred carbon fiber processing method is, by carbon
Fiber keeps the temperature 2-3h, as in 350-500 DEG C of heat-treatment furnace sufficiently to remove impurity and low molecule sizing agent.
The polyetherether ketone composition has preferable SLS forming technology performance, shows as the pre- thermal efficiency of powder bed substantially
It improving, experimental result is shown, in powder bed warm-up phase, when powder bed preheating temperature is set as 300 DEG C, polyether-ether-ketone combination
There was only the 1/4 of single polyether-ether-ketone powder preheating time the time required to object, required preheating temperature reduces, product intensity and modulus phase
Relatively simple polyether-ether-ketone product significantly improves, and can be widely used for the terminal in the fields such as aerospace, biology, machinery, military project
The directly manufacture and small lot production of parts with complex structures.
The above content is merely illustrative of the invention's technical idea, and this does not limit the scope of protection of the present invention, all to press
According to technical idea proposed by the present invention, any changes made on the basis of the technical scheme each falls within claims of the present invention
Protection scope within.
Claims (9)
1. a kind of polyetherether ketone composition for selective laser sintering, which is characterized in that in parts by weight, including 80-
The carbon fiber of 95 parts of polyether-ether-ketone powder and 5-20 part；
The carbon fiber is the carbon fiber for removing sizing agent and impurity.
2. the polyetherether ketone composition according to claim 1 for selective laser sintering, which is characterized in that the starching
The thermal decomposition temperature of agent and impurity is 350-500 DEG C.
3. the polyetherether ketone composition according to claim 1 for selective laser sintering, which is characterized in that polyether-ether-ketone
The partial size of powder is 20-100 μm.
4. the polyetherether ketone composition according to claim 3 for selective laser sintering, which is characterized in that polyether-ether-ketone
The partial size of powder is in normal distribution.
5. the polyetherether ketone composition according to claim 1 for selective laser sintering, which is characterized in that the carbon fiber
Tieing up diameter is 7-10 μm.
6. the polyetherether ketone composition according to claim 5 for selective laser sintering, which is characterized in that the carbon fiber
Tieing up length is 100-400 μm.
7. the polyetherether ketone composition according to claim 1 for selective laser sintering, which is characterized in that the carbon fiber
Tie up thermally treated removal sizing agent and impurity.
8. the polyetherether ketone composition according to claim 7 for selective laser sintering, which is characterized in that at the heat
The condition of reason is 350-500 DEG C, keeps the temperature 2-3h.
9. a kind of preparation side of the polyetherether ketone composition according to claim 1-8 for selective laser sintering
Method, which comprises the following steps:
1) component is weighed, 80-95 parts of polyether-ether-ketone powder and 5-20 parts of carbon fiber, the grain of the polyether-ether-ketone powder are weighed
Diameter is 20-100 μm；The carbon fiber diameter is 7-10 μm, and length is 100-400 μm；
2) carbon fiber is heat-treated, the heat treatment condition is 350-500 DEG C of temperature, soaking time 2-3h；
3) by the carbon fiber powder after polyether-ether-ketone powder and heat treatment, it is stirred mixing, is obtained for selective laser sintering
Polyetherether ketone composition.
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2019
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|---|---|---|---|---|
| US20180142070A1 (en) * | 2015-04-08 | 2018-05-24 | Arevo, Inc. | Method to manufacture polymer composite materials with nano-fillers for use in additive manufacturing to improve material properties |
| CN104774425A (en) * | 2015-04-27 | 2015-07-15 | 苏州中亚芯能新材料科技有限公司 | Fiber-reinforced polyetheretherketone composite material and preparation method thereof |
| CN105985632A (en) * | 2015-10-28 | 2016-10-05 | 合肥学院 | Powder material for selective laser sintering and preparation method thereof |
| CN105860431A (en) * | 2016-04-13 | 2016-08-17 | 汪艳 | Polyether ether ketone/multi-walled carbon nanotube composite powder material used for selective laser sintering technology, and preparation method thereof |
| CN107353644A (en) * | 2017-07-27 | 2017-11-17 | 广州新诚生物科技有限公司 | A kind of 3D printing material and preparation method thereof |
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Application publication date: 20190823 |