CN114437500B - Polyether-ether-ketone composite powder for laser selective sintering and preparation method thereof - Google Patents
Polyether-ether-ketone composite powder for laser selective sintering and preparation method thereof Download PDFInfo
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Abstract
The invention discloses polyether-ether-ketone composite powder for laser selective sintering and a preparation method thereof, wherein the polyether-ether-ketone composite powder is prepared from the following components in parts by weight: 60-90 parts of polyether-ether-ketone powder, 5-20 parts of carbon, 0.3-20 parts of rare earth oxide, 0.1-2 parts of antioxidant and 0.2-3 parts of flow aid. According to the invention, by redesigning the proportion, the catalytic active elements and the like, the rare earth ions in the obtained polyether-ether-ketone composite powder are activated to generate high energy when the polyether-ether-ketone composite powder is irradiated by laser, so that the polyether-ether-ketone product can be sintered by laser under the condition of lower preheating temperature, and the problem of overhigh laser sintering preheating temperature of the existing polyether-ether-ketone powder is overcome; through tests, the tensile strength, tensile elongation, breaking impact strength and other strength performances of the polyether-ether-ketone product prepared by selective laser sintering all meet the strength requirements of the polyether-ether-ketone product, and the method has industrial feasibility.
Description
Technical Field
The invention relates to the technical field of preparation of selective laser sintering powder, in particular to polyether-ether-ketone composite powder for laser selective sintering and a preparation method thereof.
Background
Selective Laser Sintering (SLS) is a 3D printing technique that uses an infrared laser (e.g., CO 2 A laser and a fiber laser) as energy sources, and selectively sintering the laser beams under the control of a computer according to the layering section information during processing, and sintering the next layer after one layer is completed.
Polyether-ether-ketone (PEEK) belongs to a special polymer material, has good characteristics of high temperature resistance, chemical corrosion resistance, high mechanical strength, impact resistance, fatigue resistance and the like, can be used as a high-temperature-resistant structural material and an electrical insulation material, and is widely applied to the fields of aviation, medical appliances and industry because of high glass transition temperature (Tg=143 ℃) and melting point (Tm=343 ℃), and at present, when selective laser sintering of the polyether-ether-ketone is carried out, the polyether-ether-ketone needs to be preheated to about 310-340 ℃ in a storage bin and then sintered. However, the current selective laser sintering equipment on the market generally has the highest construction temperature of about 210 ℃ and cannot realize the sintering of the polyether-ether-ketone. Therefore, to realize the sintering of the polyether-ether-ketone, the equipment needs to be redesigned, and then higher requirements are put on the sealing performance of the equipment, the service life of the material and the like, so that the price of the equipment is very high, and the application of the polyether-ether-ketone in the field of selective laser sintering is limited.
Chinese patent CN105860431a discloses a polyether-ether-ketone-multiwall carbon nanotube conforming powder material for selective laser sintering technique and its preparation method, which is generally as follows: and modifying the polyether-ether-ketone by adopting an antioxidant, modifying the carbon nano tube by adopting a surfactant, and then mixing the modified polyether-ether-ketone and the carbon nano tube, drying and ball milling to obtain the modified polyether-ether-ketone. The technology overcomes the defects of poor ion regularity and low apparent density of the polyether-ether-ketone powder, and improves the mechanical property and the thermal property of the composite powder material couple under the condition of small dosage of the multi-wall carbon nano tube. However, the composite powder produced in this patent still needs to have a preheating temperature of 320 ℃ or higher (described in paragraph 0083 of the specification) when subjected to selective laser sintering, and the above-mentioned problems cannot be solved.
Chinese patent CN113429532a discloses the use of selective laser sintering of polyetheretherketone prepared from 1-butyl-3-methylimidazole bromide as starting material, and in this specification the paragraph 0040 indicates: sieving the obtained polyether-ether-ketone powder with 200 meshes, then carrying out on a selective laser sintering rapid forming machine, setting the scanning interval to be 0.1mm, the single-layer thickness to be 0.15mm, the scanning speed to be 1500mm/s, the preheating temperature to be 120-140 ℃, and the laser power to be 16W. However, through careful analysis of this patent document, it was found that this patent technology, compared with the conventional production of Polyetheretherketone (PEEK), only changed the solvent so that the reaction temperature was lower when PPEK was produced, did not change the melting point of PEEK, or enhanced the ability of PEEK to absorb laser energy, and therefore, according to the common knowledge, when selective laser sintering was employed, the preheating temperature of polyetheretherketone powder was required to be above its melting point, i.e., above 300 ℃, and the preheating temperature described by it was only 120-140 ℃, and the laser power was also 16W, and if described as true, it was supposed to be described as an advantage point, otherwise, against the common knowledge of the technician, there was a possibility that the technician would have difficulty in predicting that this patent technology could solve the problem that the preheating temperature of polyetheretherketone powder was too high when laser sintering was described.
Disclosure of Invention
The invention aims at: aiming at the problems, the invention provides polyether-ether-ketone composite powder for laser selective sintering and a preparation method thereof.
The technical scheme adopted by the invention is as follows: the polyether-ether-ketone composite powder for laser selective sintering is prepared from the following components in parts by weight: 60-90 parts of polyether-ether-ketone powder, 5-20 parts of carbon, 0.3-20 parts of rare earth oxide, 0.1-2 parts of antioxidant and 0.2-3 parts of flow aid.
Further, the rare earth oxide includes one or more of 15 kinds of lanthanide oxides, scandium oxide, and yttrium oxide, and may be selected according to specific needs. In the invention, the activated rare earth oxide generates high energy through laser energy irradiation, so that the preheating temperature of the polyether-ether-ketone can be quickly increased to an ideal value, the maximum construction temperature of sintering equipment is not required to be above 320 ℃, the existing sintering equipment with the maximum construction temperature of 210 ℃ is used for realizing the laser sintering of the polyether-ether-ketone, and the equipment cost and energy are saved.
Further, the antioxidant is a composite antioxidant consisting of a hindered phenol antioxidant and a phosphite antioxidant; the hindered phenol antioxidant is one or two of 1,3, 5-trimethyl-2, 4,6, -tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene and 2, 6-di-tert-butyl-4-methyl-phenol; the phosphite antioxidant is one or more of 2 '-ethylbis (4, 6-di-tert-butylphenyl) fluorophosphite and tetra (2, 4-di-tert-butylphenyl) -4,4' -biphenyl bisphosphite, and can be selected according to specific needs.
Further, the average particle size of the polyether-ether-ketone powder is 35-100 μm, and can be selected according to specific needs.
Further, the carbon is one or more of carbon black, nano graphene and carbon nano tube.
Preferably, the carbon is a carbon nanotube. The carbon nano tube has very wide light absorption spectrum and higher absorptivity, and can be used as a reinforcing body of a polyether-ether-ketone sintered part to improve the strength of the material.
Further, the flow aid is one or more of fumed silica, fumed alumina and nano titanium dioxide, and can be selected according to specific needs.
The invention also comprises a preparation method of the polyether-ether-ketone composite powder for laser selective sintering, which comprises the following steps:
A. weighing polyether-ether-ketone powder, carbon, an antioxidant and a flow aid according to a designed proportion, and then adding the mixture into ball milling equipment for uniform stirring and ball milling to obtain a mixture;
B. weighing the rare earth oxide with the designed amount, adding the rare earth oxide into the mixture, and continuing to uniformly stir and ball-mill;
C. sieving after stirring and ball milling, and drying at 70-100deg.C.
The invention also comprises a method for carrying out laser selective sintering by using the polyether-ether-ketone composite powder, wherein the prepared polyether-ether-ketone powder is subjected to laser sintering, the preheating temperature during sintering is lower than 210 ℃, the laser power is 40-60W, the scanning speed is 10-20m/s, and the sintering interval is 0.05-0.5mm.
In summary, due to the adoption of the technical scheme, the beneficial effects of the invention are as follows: the invention redesigns proportioning, catalytic active elements and the like to obtain the polyether-ether-ketone composite powder, and the composite powder can activate rare earth ions in the composite powder to generate high energy when being irradiated by laser, so that the high-temperature melting of the polyether-ether-ketone is realized, and the polyether-ether-ketone product can be sintered by laser under the condition of lower preheating temperature, thereby overcoming the problem of overhigh laser sintering preheating temperature of the existing polyether-ether-ketone powder; through tests, the tensile strength, tensile elongation, breaking impact strength and other strength properties of the polyether-ether-ketone product prepared by selective laser sintering all meet the strength requirements of the polyether-ether-ketone product, so that the polyether-ether-ketone composite powder disclosed by the invention can be used in a selective laser sintering technology and has industrial applicability.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The mechanical myocardial infarction test criteria for the following examples and comparative examples are as follows:
tensile test criteria: GB/T1040.1-2018 determination of Plastic tensile Property
Impact strength test standard: GB/T1843-2008 "determination of impact Strength of Plastic cantilever beam
In order to embody the advantages of the polyether-ether-ketone conforming to the powder on laser sintering by the present invention, standard tensile and impact test bars were prepared by sintering the products of examples and comparative examples using a conventional laser sintering apparatus (maximum construction temperature 210 ℃) with a high temperature laser sintering apparatus (maximum construction temperature 350 ℃) as a spare apparatus.
Example 1
S1, weighing 1500g of polyether-ether-ketone, 360g of carbon nano tube, 20g of 2, 6-di-tert-butyl-4-methyl-phenol and 20g of fumed silica, and stirring and ball milling in a high-energy ball mill for 6h;
s2, weighing 100g of rare earth oxide Yb 2 O 3 Stirring and ball milling in a high-energy ball mill for 8 hours to obtain a mixture;
s3, passing the mixture through a 100-mesh screen, and drying the mixture in a vacuum drying oven at 80 ℃ for 4 hours;
s4, performing selective laser sintering, wherein equipment parameters are set as follows: the preheating temperature is 205 ℃, the laser power is 50W, the scanning speed is 15m/s, the sintering interval is 0.1mm, the thickness of a sintered layer is 0.1mm, the laser sintering is successful, and the tensile and impact test bars are obtained.
Example 2
S1, weighing 1500g of polyether-ether-ketone, 360g of nano graphene, 20g of 2, 6-di-tert-butyl-4-methyl-phenol and 20g of fumed silica, and stirring and ball milling in a high-energy ball mill for 6h;
s2, weighing 100g of rare earth oxide Yb 2 O 3 Continuing withStirring and ball milling for 8 hours in a high-energy ball mill to obtain a mixture;
s3, passing the mixture through a 100-mesh screen, and drying the mixture in a vacuum drying oven at 80 ℃ for 4 hours;
s4, performing selective laser sintering, wherein equipment parameters are set as follows: the preheating temperature is 205 ℃, the laser power is 50W, the scanning speed is 15m/s, the sintering interval is 0.1mm, the thickness of a sintered layer is 0.1mm, the laser sintering is successful, and the tensile and impact test bars are obtained.
Example 3
S1, weighing 1500g of polyether-ether-ketone powder, 360g of carbon nano tube, 20g of 2, 6-di-tert-butyl-4-methyl-phenol and 20g of fumed silica, and stirring and ball milling in a high-energy ball mill for 6h;
s2, weighing 100g of rare earth oxide La 2 O 3 Stirring and ball milling in a high-energy ball mill for 8 hours to obtain a mixture;
s3, passing the mixture through a 100-mesh screen, and drying the mixture in a vacuum drying oven at 80 ℃ for 4 hours;
s4, performing selective laser sintering, wherein equipment parameters are set as follows: the preheating temperature is 205 ℃, the laser power is 50W, the scanning speed is 15m/s, the sintering interval is 0.1mm, the thickness of a sintered layer is 0.1mm, the laser sintering is successful, and the tensile and impact test bars are obtained.
Example 4
S1, weighing 1500g of polyether-ether-ketone, 360g of nano graphene, 20g of 2, 6-di-tert-butyl-4-methyl-phenol and 20g of fumed silica, and stirring and ball milling in a high-energy ball mill for 6h;
s2, weighing 100g of rare earth oxide La 2 O 3 Stirring and ball milling in a high-energy ball mill for 8 hours to obtain a mixture;
s3, passing the mixture through a 100-mesh screen, and drying the mixture in a vacuum drying oven at 80 ℃ for 4 hours;
s4, performing selective laser sintering, wherein equipment parameters are set as follows: the preheating temperature is 205 ℃, the laser power is 50W, the scanning speed is 15m/s, the sintering interval is 0.1mm, the thickness of a sintered layer is 0.1mm, the laser sintering is successful, and the tensile and impact test bars are obtained.
Example 5
S1, weighing 1500g of polyether-ether-ketone, 360g of carbon nano tube, 20g of 2, 6-di-tert-butyl-4-methyl-phenol and 20g of fumed silica, and stirring and ball milling in a high-energy ball mill for 6h;
s2, weighing 100g of rare earth oxide Y 2 O 3 Stirring and ball milling in a high-energy ball mill for 8 hours to obtain a mixture;
s3, passing the mixture through a 100-mesh screen, and drying the mixture in a vacuum drying oven at 80 ℃ for 4 hours;
s4, performing selective laser sintering, wherein equipment parameters are set as follows: the preheating temperature is 205 ℃, the laser power is 50W, the scanning speed is 15m/s, the sintering interval is 0.1mm, the thickness of a sintered layer is 0.1mm, the laser sintering is successful, and the tensile and impact test bars are obtained.
Example 6
S1, weighing 1500g of polyether-ether-ketone, 360g of carbon black, 20g of 2, 6-di-tert-butyl-4-methyl-phenol and 20g of fumed silica, and stirring and ball milling in a high-energy ball mill for 6h;
s2, weighing 100g of rare earth oxide Yb 2 O 3 Stirring and ball milling in a high-energy ball mill for 8 hours to obtain a mixture;
s3, passing the mixture through a 100-mesh screen, and drying the mixture in a vacuum drying oven at 80 ℃ for 4 hours;
s4, performing selective laser sintering, wherein equipment parameters are set as follows: the preheating temperature is 205 ℃, the laser power is 50W, the scanning speed is 15m/s, the sintering interval is 0.1mm, the thickness of a sintered layer is 0.1mm, the laser sintering is successful, and the tensile and impact test bars are obtained.
Comparative example 1
Comparative example 1 is the same as example 1 except that no rare earth oxide was added. When laser sintering is carried out, the laser sintering is unsuccessful under the condition of preheating at 205 ℃, and the preheating temperature is too low, so that the replacement equipment, namely high-temperature laser sintering equipment, is adopted to carry out sintering at 330 ℃, the laser power is 50W, the scanning speed is 15m/s, the sintering interval is 0.1mm, the thickness of a sintered layer is 0.1mm, and the laser sintering is successful, so that the tensile and impact test sample bar is obtained.
Comparative example 2
Comparative example 2 is the same as example 1 except that no carbon component was added. Under the condition of preheating at 205 ℃, laser sintering is unsuccessful, and therefore, a replacement device, namely a high-temperature laser sintering device, is adopted to sinter at 330 ℃, the laser power is 50W, the scanning speed is 15m/s, the sintering interval is 0.1mm, the thickness of a sintered layer is 0.1mm, and the laser sintering is successful, so that a tensile and impact test spline is obtained.
Comparative example 3 (rare earth oxide excess)
Comparative example 3 is the same as example 1 except that Yb 2 O 3 The amount of (2) added was 800g. Preheating at 205 ℃, and then carrying out laser sintering, wherein the sintering parameters are as follows: the laser power was 50W, the scanning speed was 15m/s, the sintering pitch was 0.1mm, and the sintered layer thickness was 0.1mm, to obtain a tensile and impact sample bar.
Comparative example 4
Comparative example 4 is the same as example 1 except that the carbon component and the rare earth oxide are not added. Under the condition of preheating at 205 ℃, laser sintering is unsuccessful, and the problem of too low preheating temperature exists, therefore, replacement equipment, namely high-temperature laser sintering equipment, is adopted to sinter at 330 ℃, the laser power is 50W, the scanning speed is 15m/s, the sintering interval is 0.1mm, the thickness of a sintered layer is 0.1mm, and the laser sintering is successful, so that a tensile and impact test spline is obtained.
Tensile and impact test bars prepared in examples 1 to 6 and comparative examples 1 to 5 were subjected to tensile and impact tests, and the test results are shown in Table 1:
TABLE 1 results of tensile and impact tests for examples 1-6 and comparative examples 1-5 samples
From table 1:
as can be obtained by comparative examples 1 (carbon nanotubes), 2 (nano graphene) and 6 (carbon black), the tensile strength, tensile elongation and breaking impact strength of the sintered product were highest when the carbon nanotubes were used, thereby indicating that the carbon nanotubes selected from the components had the best performance and the reinforcing effect of the carbon nanotubes was the best.
As can be obtained by comparing example 2 with example 4, yb is obtained 2 O 3 Replaced by La 2 O 3 At the same time, the tensile strength and tensile elongation of example 2 were slightly higher than those of example 4, and the impact strength was comparable, thus indicating Yb 2 O 3 Has a slightly better reinforcing effect than La 2 O 3。
As can be obtained by comparing examples 1 and 3, yb was obtained 2 O 3 Replaced by La 2 O 3 When the tensile strength, tensile elongation and impact strength of example 3 were slightly lower than those of example 1, yb was demonstrated 2 O 3 The reinforcing effect in the sintered part is slightly better than La 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the At the same time, as can be obtained from example 5, when the rare earth oxide is Y 2 O 3 When the tensile strength, tensile elongation and impact strength were slightly lower than those of example 1, yb was demonstrated 2 O 3 The reinforcing and toughening effects of the steel are slightly better.
As can be seen from the results of comparative example 1, the polyether-ether-ketone composite powder, without the addition of rare earth oxide, was laser sintered at a preheating temperature of 330℃and, at the same time, the prepared samples had lower tensile strength, tensile elongation and impact strength than those of example 1 and comparative example 4, indicating that the addition of carbon alone would destroy the strength of the material.
As can be seen from the result of comparative example 2, the polyether-ether-ketone composite powder cannot be laser sintered at the preheating temperature of 205 ℃ and can be laser sintered only at the preheating temperature of 330 ℃ without adding the carbon component, and the prepared sample has a tensile strength and an impact strength which are both greater than those of example 4, which indicates that the rare earth oxide has a certain reinforcing effect.
As can be seen from the results of comparative example 3, when the rare earth oxide is excessive, the tensile strength, tensile elongation and impact strength at break are greatly reduced, indicating that the rare earth oxide is excessive and that over-sintering occurs during sintering, thereby affecting the strength properties of the article.
As can be seen from the results of comparative example 4, the polyether-ether-ketone composite powder required laser sintering at a preheating temperature of 330℃and, although the tensile strength, tensile elongation and impact strength were slightly higher than those of example 1, the difference was small. This demonstrates that example 1 reduces the preheat temperature for laser sintering of the polyetheretherketone composite powder after addition of the carbon component and rare earth oxide.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (7)
1. The polyether-ether-ketone composite powder for laser selective sintering is characterized by comprising the following components in parts by weight: 60-90 parts of polyether-ether-ketone powder, 5-20 parts of carbon, 0.3-20 parts of rare earth oxide, 0.1-2 parts of antioxidant and 0.2-3 parts of flow aid; the rare earth oxide comprises one or more of 15 lanthanide oxides, scandium oxides and yttrium oxides, and the carbon is one or more of carbon black, nano graphene and carbon nano tube.
2. The polyether ether ketone composite powder for laser selective sintering according to claim 1, wherein the antioxidant is a composite antioxidant composed of a hindered phenol type antioxidant and a phosphite type antioxidant; the hindered phenol antioxidant is one or two of 1,3, 5-trimethyl-2, 4,6, -tri (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene and 2, 6-di-tert-butyl-4-methyl-phenol; the phosphite antioxidant is one or more of 2 '-ethylbis (4, 6-di-tert-butylphenyl) fluorophosphite and tetra (2, 4-di-tert-butylphenyl) -4,4' -biphenyl bisphosphite.
3. The polyetheretherketone composite powder for laser selective sintering according to claim 1, wherein the polyetheretherketone powder has an average particle size of 35-100 μm.
4. The polyether ether ketone composite powder for laser selective sintering according to claim 1, wherein the carbon is carbon nanotube.
5. The polyether-ether-ketone composite powder for laser selective sintering according to claim 1, wherein the flow aid is one or more of fumed silica, fumed aluminum oxide and nano titanium dioxide.
6. The method for preparing the polyether-ether-ketone composite powder for laser selective sintering according to any one of claims 1 to 5, comprising the following steps:
A. weighing polyether-ether-ketone powder, carbon, an antioxidant and a flow aid according to a designed proportion, and then adding the mixture into ball milling equipment for uniform stirring and ball milling to obtain a mixture;
B. weighing the rare earth oxide with the designed amount, adding the rare earth oxide into the mixture, and continuing to uniformly stir and ball-mill;
C. sieving after stirring and ball milling, and drying at 70-100deg.C.
7. A method for carrying out laser selective sintering by using polyether-ether-ketone composite powder is characterized in that the polyether-ether-ketone composite powder prepared by the method in claim 6 is adopted for carrying out laser sintering, the preheating temperature during sintering is lower than 210 ℃, the laser power is 40-60W, the scanning speed is 10-20m/s, and the sintering interval is 0.05-0.5mm.
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| CN103709737A (en) * | 2013-12-05 | 2014-04-09 | 吴江中瑞机电科技有限公司 | High-molecular composite powder material for SLS and preparation method therefor |
| CN104650582A (en) * | 2014-09-30 | 2015-05-27 | 青岛科技大学 | Poly(imino ether ketone) material rapidly formed based on selective laser sintering |
| 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 |
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| FR3058918B1 (en) * | 2016-11-18 | 2021-01-01 | Arkema France | COMPOSITION OF MAGNETIC SINTERABLE POWDER AND THREE-DIMENSIONAL OBJECTS MANUFACTURED BY SINTERING SUCH COMPOSITION |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709737A (en) * | 2013-12-05 | 2014-04-09 | 吴江中瑞机电科技有限公司 | High-molecular composite powder material for SLS and preparation method therefor |
| CN104650582A (en) * | 2014-09-30 | 2015-05-27 | 青岛科技大学 | Poly(imino ether ketone) material rapidly formed based on selective laser sintering |
| 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 |
Non-Patent Citations (1)
| Title |
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| 表面活性剂PAA对羟基磷灰石微粒分散性的调控及机理研究;刘海;林栎阳;孙青竹;蒋海兵;;化学研究与应用(03);全文 * |
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