CN101808459A - Low-temperature plasma treatment device used for modifying inner surface of tubular high polymer material support - Google Patents
Low-temperature plasma treatment device used for modifying inner surface of tubular high polymer material support Download PDFInfo
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- CN101808459A CN101808459A CN 201010125946 CN201010125946A CN101808459A CN 101808459 A CN101808459 A CN 101808459A CN 201010125946 CN201010125946 CN 201010125946 CN 201010125946 A CN201010125946 A CN 201010125946A CN 101808459 A CN101808459 A CN 101808459A
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- 238000009832 plasma treatment Methods 0.000 title abstract description 9
- 239000002861 polymer material Substances 0.000 title abstract 3
- 239000010453 quartz Substances 0.000 claims abstract description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000012545 processing Methods 0.000 claims description 23
- 238000012546 transfer Methods 0.000 claims description 17
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 20
- 210000002381 plasma Anatomy 0.000 abstract 2
- 230000008929 regeneration Effects 0.000 abstract 1
- 238000011069 regeneration method Methods 0.000 abstract 1
- 210000001519 tissue Anatomy 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 21
- 229920000642 polymer Polymers 0.000 description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- 230000004048 modification Effects 0.000 description 10
- 238000012986 modification Methods 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 229920001020 poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) Polymers 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 229920002521 macromolecule Polymers 0.000 description 5
- 239000002352 surface water Substances 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000001172 regenerating effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005685 electric field effect Effects 0.000 description 1
- -1 electronics Chemical class 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013138 pruning Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- Treatments Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a low-temperature plasma treatment device used for modifying the inner surface of a tubular high polymer material support, which comprises an electrode ring (7) and a quartz discharge tube (6). Both ends of the quartz discharge tube (6) are respectively connected with a rapid vacuum seal joint (3) and are fixed on rapid vacuum adapters (4) and (9) by locking nuts (5) and (8), wherein one end of the quartz discharge tube is connected with an air inlet by the vacuum adapters, and the other end thereof is connected to a tee joint by the vacuum adapters, and the other two ends of the tee joint are respectively a barometer connector and a mechanical pump connector. Long, thin and even plasmas can be generated by utilizing the treatment device; the plasmas are used for modifying the inner wall of the tubular high polymer material support to enable the inner surface of the support to be activated or to be inoculated with an active group without changing the properties of the support body; moreover, the work temperature is low, and therefore, heat damage can not be generated on materials. The device has wide application prospect in tissue engineering and regeneration medical field.
Description
Technical field
The present invention relates to a kind of apparatus for low-temperature plasma treatment to tubular high polymer stock support modifying inner surface.
Background technology
Plasma is a kind of molecule of ion, electronics, free radical, excitation state and ionized gas of atom of containing.What be usually used in Polymer Synthesizing, interfacial reaction is low temperature plasma, and its gas temperature is low, can be to the material production fire damage.When the plasma treatment material surface, electronics wherein, ion and active particle pass to the material surface molecule with self-energy, with material surface interactions, physicochemical change takes place on the surface, thereby make the material surface activation or insert active group and realize surface modification.With respect to chemical method and x ray irradiation x method, adopt lower temperature plasma technology be used for polymer modification have reaction temperature low, avoided solvent corrosion, convenient to material surface chemical constitution and character control, can not influence characteristics such as material body character, in macromolecule material surface modification, receive much attention.
Utilize existing low-temp plasma source, as inductively coupled plasma (ICP) and capacitance coupling plasma (CCP) etc., can produce the larger area homogeneous plasma, be applicable to and handle sheet layer material such as macromolecule membrane etc., or the outer surface of tubular high polymer support.Yet at regenerative medicine especially organizational engineering field, usually need the inner surface of small-caliber tubular polymeric stent is carried out the modification processing, therefore need to produce processing unit elongated, homogeneous plasma, make it when tubular high polymer stock support inner surface is carried out fine processing, do not change the character of its outer surface, and the effect repeatability can be guaranteed.
Summary of the invention
The purpose of this invention is to provide a kind of apparatus for low-temperature plasma treatment that tubular high polymer stock support inner surface is carried out modification of being used for.
Apparatus for low-temperature plasma treatment provided by the present invention comprises electrode retaining collar 7, discharge tube 6 and air inlet 1; Wherein, described quartz discharge tube 6 is set in the electrode retaining collar 7.
In order to guarantee that plasma processing apparatus can form vacuum environment when working, described plasma processing apparatus also comprises two vacuum transfer tubes (being vacuum transfer tube A4 and B9), vacuum connection tube 2 and threeway 10; One end of described discharge tube 6 is sealedly and fixedly connected by the end of locking nut 5 and O-ring seal A13 and vacuum transfer tube A4; The other end of described discharge tube 6 is sealedly and fixedly connected with the end of vacuum transfer tube B9 by locking nut 8 and O-ring seal B13 '; The other end of described vacuum transfer tube A4 is connected to air inlet 1 by O-ring seal C3 and vacuum connection tube 2; The other end of described vacuum transfer tube B9 is tightly connected with an end of threeway 10 by O-ring seal D3 '.
Above-mentioned O-ring seal A, B, C, D are O-ring seal.
Described plasma processing apparatus also comprises following external equipment: external vacuum system gas supply system and 3 1) high-frequency high-voltage origin system, 2)).
Described high-frequency high-voltage origin system is electrically connected with electrode retaining collar 7; The operating frequency of described high-frequency high-voltage origin system can be 1-80KHZ.This high-frequency high-voltage origin system provides highfield to produce uniform glow discharge by connection electrode ring 7.
Described gas supply system is connected with air inlet 1, provides in order to produce the gas of plasma, as NH
3, N
2With Ar etc.
Described external vacuum system comprises barometer and mechanical pump; The barometer interface 11 of described barometer and threeway 10 is tightly connected, and the mechanical pump interface 12 of described mechanical pump and threeway 10 is tightly connected.
In the device of the present invention, described discharge tube 6 can be made by quartz or glass, and described electrode retaining collar 7 can be the annular metal by stainless steel, copper or aluminum; The internal diameter size of described electrode retaining collar 7 is identical with the outside dimension of quartz discharge tube 6.
The concrete size of described quartz discharge tube 6 is as follows: internal diameter is 3-20mm, and external diameter is 6-24mm, and length is 100-800mm.
Device of the present invention produces vacuum environment by external mechanical pump, and vacuum degree is shown that by external barometer reading its operational environment vacuum degree is 10-10
3Pa.
As shown from the above technical solution, plasma processing apparatus provided by the invention comes down to utilize the quartz tubular discharge cavity to form even, elongated plasma.When handling the tubular high polymer support, to put into quartz discharge tube behind the support cleaning-drying, air inlet is positioned at pending tubular bracket sample one end inboard, make internal stent be full of the gas that produces plasma, under the high voltage electric field effect, gas discharge produces plasma at internal stent, thereby realizes the modification of tubular high polymer support inner surface is handled.
Plasma processing apparatus provided by the present invention can produce elongated, uniform plasma.Utilizing this device that tubular high polymer stock support inwall is carried out modification handles, can make its inner surface activation or access active group and not change rack body character, and working temperature low (not can to the material production fire damage) has broad application prospects in organizational engineering, regenerative medicine field.
Description of drawings
Fig. 1 is the sectional elevation figure of plasma processing apparatus of the present invention.
Fig. 2 is the longitudinal section view of plasma processing apparatus of the present invention.
Embodiment
Below by specific embodiment device of the present invention is described, but the present invention is not limited thereto.
Embodiment 1, plasma processing apparatus
As shown in Figure 1, plasma processing apparatus disclosed by the invention comprises a cover electrode retaining collar 7 and a quartz discharge tube 6, and discharge tube 6 two ends are connected with vacuum transfer tube O-ring seal 13 respectively, are individually fixed in an end of vacuum transfer tube 4,9 by locking nut 5,8.Wherein, the other end of vacuum transfer tube 4 is connected in air inlet 1 by vacuum connection tube 2 under the sealing of O-ring seal 3; The other end of vacuum transfer tube 9 is connected to threeway 10 under the sealing of O-ring seal 3.The other two ends of threeway 10 are connected to barometer 11 and mechanical pump 12.
Described electrode retaining collar is the copper ring electrode, and is coaxial with quartz discharge tube, and internal diameter size is identical with the quartz discharge tube outside dimension.During actual fabrication, the internal diameter of discharge tube is by pending tubular bracket external diameter decision, and the wall thickness of quartz tube degree is 1.5mm.
The main external equipment of device of the present invention comprises a high-frequency high-voltage origin system, a gas supply system and a vacuum environment system.Described high-frequency and high-voltage power supply provides highfield by the connection electrode ring, and during actual fabrication, selected frequency is the high-frequency and high-voltage power supply of 1-80KHz, and maximum output voltage is 30KV; Described gas supply system is connected with device by air inlet, provide in order to produce the gas of plasma, during actual treatment, can select the multiple gases that produce plasma discharge such as mist of inert gas, ammonia, air or above-mentioned gas as required; Described vacuum environment system is by the mechanical pump generation vacuum environment of bleeding, and vacuum degree shows that by the barometer reading actual working environment vacuum degree is 10-10
3Pa.
The workflow of the present invention when handling the macromolecule article is summarized as follows:
1, cleans pending tubular high polymer support;
2, dry support;
3, tubular high polymer support 14 is placed quartz discharge tube, and quartz discharge tube is connected with vacuum transfer tube 4,9 with O-ring seal 13 with locking nut 5,8 respectively;
4, confirm each junction sealing of device, open mechanical pump, will install internal gas pressure and be evacuated to base vacuum;
5, open intake valve, feed, reach preset value until barometer display unit internal gas pressure in order to produce the gas of plasma;
6, energized produces plasma discharge in the quartz discharge tube, the tubular bracket inner surface is handled.Processing time is set as requested.
After processing finished, powered-down and mechanical pump were opened vent valve, when treating to press in the device with the atmospheric pressure balance, took out support, and work finishes.
Utilize ammonia as plasma generation gas, the plasma processing apparatus by embodiment 1 is that 3mm, length are that 10cm, pipe thickness are that poly butyric-capronate macromolecular material tubular bracket inner surface of 0.5mm is handled to internal diameter.
The preparation internal diameter is that 3mm, length are that 10cm, pipe thickness are the macromolecular material tubular bracket of 0.5mm, and concrete grammar is as follows:
With poly butyric-capronate (PHBHHx is available from the anti-medical Group Co.,Ltd in Shandong, Shandong) material is that 15% concentration is mixed with chloroform by quality-volume ratio, and 60 ℃ of abundant backflow 4h make it to dissolve fully.Utilize the described solution of 30ml to prepare tubular bracket by electrostatic spinning technique, sampling system is selected syringe needle for use No. 16, voltage 20kV, and receiving range 25cm, receiving system are the stainless steel bar of rotatable diameter 3mm, rotary speed 300rpm.After preparation finishes, receiving system integral body is placed the air-dry 24h of fume hood, chloroform is volatilized fully, then stainless steel bar is extracted out from type support, pruning the support two ends with double-edged razor blade is 10cm to length, and obtaining internal diameter is that 3mm, length are that 10cm, pipe thickness are the PHBHHx macromolecule tubulose support of 0.5mm.Utilize deionized water to embathe support three times, each 1h, then will prop up be placed in the drier stand-by.
Tubular bracket is carried out modification:
Dried PHBHHx macromolecule tubulose support is connected to the plasma processing apparatus of embodiment 1, wherein, described quartz discharge bore is 4mm, gas in order to the generation plasma is ammonia, and operating air pressure is 50Pa, and operating frequency is 50KHz, discharge voltage is 2kV, processing time is respectively 30s, 60s, 120s.
Before and after handling, use contact angle measurement (Model JY-82 purchases in Chengde testing machine Co., Ltd) to measure the water contact angle value of tubular bracket inner surface and outer surface respectively.In the detected materials surface, on the protractor of measuring instrument, read the value of contact angle with the accurate deionized water that drips 10 μ l of micro-liquid getting device.Measure the contact angle value of inside and outside surperficial 6 the diverse location points of tubular bracket respectively, total data is represented with x ± s, uses SPSS10.0 statistical software (available from SPSS Inc.), check the analysis bank differences with t, p<0.05 is variant, and there is significant difference p<0.01, down together.
The result is as shown in table 1, as can be seen from Table 1, utilize ammonia as plasma generation gas, device by embodiment 1 is that 3mm, length are that 10cm, pipe thickness are after the PHBHHx tubular bracket of 0.5mm carries out inner surface treatment to internal diameter, support inner surface water contact angle reduces, amplitude increases with handling time lengthening, behind the processing 30s significant difference is arranged promptly, does not have difference and handle front and back support outer surface water contact angle.
Tubular high polymer support surfaces externally and internally water contact angle changed (* p<0.01) before and after table 1 ammonia plasma treatment was handled
Utilize nitrogen as plasma generation gas, the device by embodiment 1 is that 8mm, length are that 10cm, pipe thickness are that the PHBHHx macromolecular material tubular bracket of 1mm carries out inner surface treatment to internal diameter.
Basic implementation process is with embodiment 2, and difference is: in the preparation PHBHHx tubular bracket process, the liquor capacity of employing is 150ml, and receiving system is the stainless steel bar of rotatable diameter 8mm.The macromolecular material tubular bracket is being carried out in the surface-treated process, and the quartz discharge bore of employing is 10mm, is nitrogen in order to the gas that produces plasma.
Before and after handling, measure the water contact angle value of tubular bracket inner surface and outer surface respectively, the result is as shown in table 2, as can be seen from Table 2, utilize nitrogen as plasma generation gas by device disclosed by the invention to internal diameter for 8mm, length for 10cm, pipe thickness for after the PHBHHx macromolecular material tubular bracket of 1mm carries out inner surface treatment, support inner surface water contact angle reduces, amplitude increases with handling time lengthening, after handling 30s significant change is arranged promptly, handle 120s after-poppet inner surface water contact angle and promptly can not detect.There is not difference and handle front and back support outer surface water contact angle.
Tubular high polymer support surfaces externally and internally water contact angle changes (* p<0.01) before and after table 2 nitrogen plasma treatment
Claims (9)
1. plasma processing apparatus, it is characterized in that: described plasma processing apparatus comprises electrode retaining collar (7), discharge tube (6) and air inlet (1); Wherein, described discharge tube (6) is set in the electrode retaining collar (7).
2. device according to claim 1 is characterized in that: described plasma processing apparatus also comprises vacuum transfer tube A (4), vacuum transfer tube B (9), vacuum connection tube (2) and threeway (10); One end of described discharge tube (6) is sealedly and fixedly connected by the end of locking nut (5) and O-ring seal A (13) and vacuum transfer tube A (4); The other end of described discharge tube (6) is sealedly and fixedly connected by the end of locking nut (8) and O-ring seal B (13 ') and vacuum transfer tube B (9); The other end of described vacuum transfer tube A (4) is connected to air inlet (1) by O-ring seal C (3) and vacuum connection tube (2); The other end of described vacuum transfer tube B (9) is tightly connected with an end of threeway (10) by O-ring seal D (3 ').
3. device according to claim 2 is characterized in that: described plasma processing apparatus also comprises high-frequency high-voltage origin system, gas supply system and external vacuum system.
4. device according to claim 3 is characterized in that: described high-frequency high-voltage origin system is electrically connected with electrode retaining collar (7); The operating frequency of described high-frequency high-voltage origin system is 1-80KHZ.
5. according to claim 3 or 4 described devices, it is characterized in that: described gas supply system is connected with air inlet (1).
6. according to arbitrary described device among the claim 3-5, it is characterized in that: described external vacuum system comprises barometer and mechanical pump; The barometer interface (11) of described barometer and threeway (10) is tightly connected, and the mechanical pump interface (12) of described mechanical pump and threeway (10) is tightly connected.
7. according to arbitrary described device among the claim 1-6, it is characterized in that: described discharge tube (6) is made by quartz or glass, and described electrode retaining collar (7) is the annular metal of stainless steel, copper or aluminum; The internal diameter size of described electrode retaining collar (7) is identical with the outside dimension of discharge tube (6).
8. according to arbitrary described device among the claim 1-7, it is characterized in that: described quartz discharge tube (6) internal diameter is 3-20mm, and external diameter is 6-24mm, and length is 100-800mm.
9. according to arbitrary described device among the claim 1-8, it is characterized in that: the vacuum work condition of described plasma processing apparatus is produced by the mechanical pump in the described external vacuum system, and the vacuum degree under the described vacuum work condition is 10-103Pa.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108342896A (en) * | 2018-02-13 | 2018-07-31 | 南通大学 | Tubing surfaces externally and internally plasma processing apparatus and its application method |
CN109049659A (en) * | 2018-06-28 | 2018-12-21 | 苏州大学 | The method of plasma processing of tubular medical inner surface |
CN109769335A (en) * | 2019-03-06 | 2019-05-17 | 大连理工大学 | A kind of long scale plasma generating device of radio frequency micro discharge and method |
CN111565912A (en) * | 2017-11-07 | 2020-08-21 | 爱尔兰国立大学都柏林大学学院 | Surface preparation |
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Cited By (6)
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CN111565912A (en) * | 2017-11-07 | 2020-08-21 | 爱尔兰国立大学都柏林大学学院 | Surface preparation |
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