CN101508821B - Polyetheretherketone composite material for tridimensional orienting headstock and method for producing the same - Google Patents
Polyetheretherketone composite material for tridimensional orienting headstock and method for producing the same Download PDFInfo
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- CN101508821B CN101508821B CN2009100216109A CN200910021610A CN101508821B CN 101508821 B CN101508821 B CN 101508821B CN 2009100216109 A CN2009100216109 A CN 2009100216109A CN 200910021610 A CN200910021610 A CN 200910021610A CN 101508821 B CN101508821 B CN 101508821B
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Abstract
The invention discloses a polyether ether ketone composite used for a solid positioning head frame and a preparation method thereof. The polyether ether ketone composite comprises the components with the weight percentage as follows: 35-52 percent of inorganic filling, 3-5 percent of modifier, 25-35 percent of matrix resin and 20-25 percent of reinforcing fiber. The reinforcing fiber is arranged in epoxy acetone solution to be soaked, subjected to gamma ray irradiation treatment and is dried subsequently; the polyether ether ketone is arranged in oxygen, hydrogen or argon plasma atmosphere to be irradiated for 30 minutes and then is subjected to banburying with the modifier and the inorganic filling in proportion as above; a product and chopped carbon fiber are added into a double-screw extruder to be extruded and granulated; plastic granules are dried, injected and pressurized at constant temperature and then are molded into the solid positioning head frame. In the invention, the proportion for producing the raw materials is lightened and the performance of the polyether ether ketone composite in CT/MRI working environment is improved.
Description
Technical field
The present invention relates to a kind of Neurological Surgery medicine equipment material, also relate to its preparation method.
Background technology
In neurosurgery, stereotactic system is being played the part of important role, and it plays significant effects for diagnosis, location, the treatment of intracranial lesion; And the headstock is the core component of whole stereotactic system, and it is most important for the whole process of the stability of whole orientation system and patient.In order to satisfy requirements such as intensity, rigidity, dimensional stability and sterilization, the most of metallic substance that adopts of the present domestic headstock.These metal headstocks in use, have had been found that following drawback, are badly in need of improving and improving:
1) weight reaches more than the 3kg, and the patient is after installing the headstock, like a hen on a hot girdle;
2) in CT (robot calculator layer radiography, Computed Tomography) scanning, metallic substance can block the CT image, causes metal artifacts, and diagnosis is caused disadvantageous effect.
And in MRI (Magnetic resonance imaging, Magnetic Resonance Image) scanning process, near the material interface of different susceptibility, magneticstrength has change, can produce magnetic susceptibility artifact in this case.Near ferromagnetic substance, often can see serious magnetic susceptibility artifact; In the MRI scanning process, magneticstrength and field direction constantly change on the other hand, might make the object in the magnetic field produce eddy current, and eddy current can make scan image produce serious deformation, causes scanning result inaccurate, and diagnosis is caused disadvantageous effect.
For fear of in CT, causing metal artifacts, in MRI, cause magnetic susceptibility artifact or producing the disadvantageous effect that eddy current causes scanning result, the existing metal headstock can not enter in the MRI magnetic field, headstock basic ring all is mounted in the bottom of patient's head in clinical, utilize the transition of installation column to be connected on the head, increased unnecessary connection, reduce setting accuracy, and increased the installation difficulty of the headstock, reduced the simplicity of clinical manipulation.
And cause the major cause of above drawback to be exactly:
1) metallic substance causes the headstock heavy than great;
2) the metallic substance electro permanent magnetic is strong, causes the pseudo-shadow of magnetic susceptibility artifact and eddy current.
Adopt metallic substance to make the above-mentioned drawback that the headstock causes in order to overcome, also the someone proposes to use polyether-ether-ketone composite material to make the headstock, but common carbon fiber reinforced polyetheretherketonecomposite composite material does not have enough rigidity and intensity to satisfy the central desired dimensional stability of CT, MRI scanning at present, particularly will guarantee that under the condition of high-temperature sterilization repeatedly the headstock is indeformable.In addition, because carbon fiber reinforced polyetheretherketonecomposite composite material still might produce magnetic susceptibility artifact to the influence in magnetic field, thereby reduce the precision of MRI.
Summary of the invention
In order to overcome prior art rigidity and undercapacity, still may to produce the deficiency of magnetic susceptibility artifact, the invention provides a kind of polyether-ether-ketone composite material that is used for tridimensional orienting headstock, alleviated and produced raw-material proportion, conductivity, susceptibility have been carried out modification, effectively reduced deformation.
The present invention also provides the preparation method who relates to this kind matrix material.
The technical solution adopted for the present invention to solve the technical problems is: comprise mineral filler, properties-correcting agent, matrix resin and fortifying fibre, the weight percent of its each composition is: inorganic filler content is 35～52%, modifier content is 3～5%, matrix resin content is 25～35%, and fortifying fibre accounts for 20%～25%; Wherein mineral filler was made up of glass fibre, mica, calcium carbonate superfine powder in 2: 1: 1 by weight percentage; Properties-correcting agent is titanic acid ester/aluminic acid ester or silane coupling agent; Matrix resin is a polyether-ether-ketone; Fortifying fibre is a chopped carbon fiber.This matrix material can not only improve headstock rigidity, and can reduce cost, and is a kind of very promising matrix material.
The material preparation step is as follows:
1) chopped carbon fiber being placed concentration is after 15～35% epoxy acetone solns soak into 24h, the carbon fiber of abundant infiltration is carried out gamma-ray irradiation handle in the dosage range of 1.17～1.33meV, and the carbon fiber oven dry after handling is handled;
2) polyether-ether-ketone is placed in oxygen, hydrogen or the argon plasma atmosphere and shone 30 minutes;
3) polyether-ether-ketone, properties-correcting agent, mineral filler are dropped into Banbury mixer according to the above ratio, banburying time 15～20min, 380 ℃ of banburying temperature, 350 ℃ of discharging material temperature, the material that banburying is good is the bulk material, can not have not plastifying powder or particulate material emit, if not plastifying powder or particulate material are arranged, then should empty material stock in the machine, add virgin material again and carry out this step;
4) product with the 3rd step joins in the twin screw extruder casing drum, and adds chopped carbon fiber from forcing machine fiber spout;
5) keep 380～400 ℃ of extruder barrel temperature, screw speed is 15～20r/min, and the cutting knife rotating speed is adjusted to particulate material length 3～4mm, carries out extruding pelletization;
6) pellet of moulding that adopted for the 5th step produced, is injected under 390 ℃ of barrel temperatures after 2 hours 160 ℃ of dryings, and injection pressure is 140MPa, 200 ℃ of die temperatures, and the constant temperature pressurize 90 seconds was the moulding tridimensional orienting headstock.
The invention has the beneficial effects as follows: owing to adopt the present invention reasonably to select the kind of matrix and reinforce, alleviated and produced raw-material proportion, and by filler conductivity, susceptibility are carried out modification, improve its performance in the CT/MRI Working environment, clinical experiment shows:
Adopt gamma-rays modified carbon fiber, gas ions modified polyetheretherketonefiber,, improve the polarity and the wetting ability on their surfaces well, improved the interface bond strength of various compositions, improved the intensity of matrix material by adding properties-correcting agent.
Add the effect that mineral filler is played carrying, reduced to be out of shape, and because thereby the adjustment of susceptibility is eliminated fully to magnetic field the headstock in the MRI environment influence can not produce magnetic susceptibility artifact, thereby obtain scan image more clearly, the accuracy of enhanced diagnosis greatly, and preparation technology is fairly simple, cost is lower.
The present invention is further described below in conjunction with embodiment.
Embodiment
Embodiment 1:
A kind of polyether-ether-ketone composite material that is used for tridimensional orienting headstock comprises that inorganic filler content is 1.2kg, and modifier content is 0.16kg, and matrix resin content is 0.8kg, and reinforced fiber content is 0.25kg; Mineral filler was made up of glass fibre, mica, calcium carbonate superfine powder in 2: 1: 1 by weight percentage, and properties-correcting agent is titanic acid ester; Matrix resin is a polyether-ether-ketone; Fortifying fibre is a chopped carbon fiber; Place the epoxy acetone soln to soak into 24h on carbon fiber, the back is carried out the gamma-ray irradiation processing to the carbon fiber of abundant infiltration at the dosage of 1.20meV, carbon fiber oven dry after handling is handled, adopt oxyanion precursor to handle polyether-ether-ketone about 30 minutes, with polyether-ether-ketone, titanic acid ester, mineral filler drops into Banbury mixer, banburying time 15min, 380 ℃ of banburying temperature, 350 ℃ of discharging material temperature join discharging in the twin screw extruder casing drum, and add chopped carbon fiber from forcing machine fiber spout, keep 380 ℃ of extruder barrel temperature, screw speed is 15r/min, and the cutting knife rotating speed is adjusted to particulate material length 3～4mm, carries out extruding pelletization; Mould pellet 160 ℃ of dryings 2 hours, 390 ℃ of barrel temperatures injections down, injection pressure is 140MPa, 200 ℃ of die temperatures, the constant temperature pressurize 90 seconds was the moulding tridimensional orienting headstock.
Embodiment 2:
A kind of polyether-ether-ketone composite material that is used for tridimensional orienting headstock comprises that inorganic filler content is 2kg, and modifier content is 0.16kg, and matrix resin content is 1.25kg, and reinforced fiber content is 0.25kg; Mineral filler was made up of glass fibre, mica, calcium carbonate superfine powder in 2: 1: 1 by weight percentage, and properties-correcting agent is silane coupling agent; Matrix resin is a polyether-ether-ketone; Fortifying fibre is a chopped carbon fiber; Place the epoxy acetone soln to soak into 24h on carbon fiber, the back is carried out the gamma-ray irradiation processing to the carbon fiber of abundant infiltration at the dosage of 1.20meV, carbon fiber oven dry after handling is handled, adopt oxyanion precursor to handle polyether-ether-ketone about 30 minutes, with polyether-ether-ketone, silane coupling agent, mineral filler drops into Banbury mixer, banburying time 20min, 380 ℃ of banburying temperature, 350 ℃ of discharging material temperature join discharging in the twin screw extruder casing drum, and add chopped carbon fiber from forcing machine fiber spout, keep 380 ℃ of extruder barrel temperature, screw speed is 20r/min, and the cutting knife rotating speed is adjusted to particulate material length 3～4mm, carries out extruding pelletization; Mould pellet 160 ℃ of dryings 2 hours, 390 ℃ of barrel temperatures injections down, injection pressure is 140MPa, 200 ℃ of die temperatures, the constant temperature pressurize 90 seconds was the moulding tridimensional orienting headstock.
Claims (1)
1. a preparation method who is used for the polyether-ether-ketone composite material of tridimensional orienting headstock is characterized in that comprising the steps:
(a) prepare starting material by following weight percent: inorganic filler content is 35～52%, and modifier content is 3～5%, and matrix resin content is 25～35%, and fortifying fibre accounts for 20%～25%; Wherein mineral filler was made up of glass fibre, mica, calcium carbonate superfine powder in 2: 1: 1 by weight percentage; Properties-correcting agent is titanic acid ester/aluminic acid ester or silane coupling agent; Matrix resin is a polyether-ether-ketone; Fortifying fibre is a chopped carbon fiber;
(b) chopped carbon fiber being placed concentration is after 15～35% epoxy acetone solns soak into 24h, the carbon fiber of abundant infiltration is carried out gamma-ray irradiation handle in the dosage range of 1.17～1.33meV, and the carbon fiber oven dry after handling is handled;
(c) polyether-ether-ketone is placed in oxygen, hydrogen or the argon plasma atmosphere and shone 30 minutes;
(d) polyether-ether-ketone, properties-correcting agent, mineral filler are dropped into Banbury mixer according to the above ratio, banburying time 15～20min, 380 ℃ of banburying temperature, 350 ℃ of discharging material temperature, the material that banburying is good is the bulk material, can not have not plastifying powder or particulate material emit, if not plastifying powder or particulate material are arranged, then should empty material stock in the machine, add virgin material again and carry out this step; Described properties-correcting agent is titanic acid ester, aluminic acid ester or silane coupling agent; Described mineral filler was made up of glass fibre, mica, calcium carbonate superfine powder in 2: 1: 1 by weight percentage;
(e) product with step (c) joins in the twin screw extruder casing drum, and adds the chopped carbon fiber that step (a) processing obtains from forcing machine fiber spout;
(f) keep 380～400 ℃ of extruder barrel temperature, screw speed is 15～20r/min, and the cutting knife rotating speed is adjusted to particulate material length 3～4mm, carries out extruding pelletization;
(g) pellet of moulding that adopts step (e) to produce, is injected under 390 ℃ of barrel temperatures after 2 hours 160 ℃ of dryings, and injection pressure is 140MPa, 200 ℃ of die temperatures, and the constant temperature pressurize 90 seconds was the moulding tridimensional orienting headstock.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100216109A CN101508821B (en) | 2009-03-18 | 2009-03-18 | Polyetheretherketone composite material for tridimensional orienting headstock and method for producing the same |
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| CN2009100216109A CN101508821B (en) | 2009-03-18 | 2009-03-18 | Polyetheretherketone composite material for tridimensional orienting headstock and method for producing the same |
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| CN101508821B true CN101508821B (en) | 2011-01-19 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102775726B (en) * | 2012-08-29 | 2014-06-04 | 吉林大学 | Polyether-ether-ketone composite material containing gadolinium oxide and preparation method of composite material |
| CN102851781A (en) * | 2012-09-29 | 2013-01-02 | 马海燕 | Large-diameter polyether-ether-ketone monofilament and production method thereof |
| US10526468B2 (en) | 2015-05-21 | 2020-01-07 | Solvay Specialty Polymers Usa, Llc | Poly(aryletherketone) compositions |
| CN105219018A (en) * | 2015-10-12 | 2016-01-06 | 上海利物盛企业集团有限公司 | A kind of preparation method of modified carbon fiber reinforced polyether ether ketone matrix material |
| CN105504670A (en) * | 2015-12-30 | 2016-04-20 | 中国科学院长春应用化学研究所 | Polyether-ether-ketone composite material |
| CN111499955A (en) * | 2020-06-01 | 2020-08-07 | 南方医科大学第三附属医院（广东省骨科研究院） | Stretcher suitable for radiation environment |
| CN113214526B (en) * | 2021-06-29 | 2022-11-11 | 中国人民解放军空军军医大学 | Surface amination 3D printing polyether-ether-ketone implant and preparation method thereof |
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