CN102698352A - Preparation method of trachea developing ring for minimally invasive treatment - Google Patents
Preparation method of trachea developing ring for minimally invasive treatment Download PDFInfo
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- CN102698352A CN102698352A CN2012102123420A CN201210212342A CN102698352A CN 102698352 A CN102698352 A CN 102698352A CN 2012102123420 A CN2012102123420 A CN 2012102123420A CN 201210212342 A CN201210212342 A CN 201210212342A CN 102698352 A CN102698352 A CN 102698352A
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Abstract
The invention relates to a preparation method of a trachea developing ring for cardiovascular minimally invasive treatment. The developing ring is used for depositing a tantalum or tungsten film which is impermeable for X rays on the surface of medical stainless steel by adopting a physical vapor deposition technology. According to the developing ring, the specific position of a cardiovascular minimally invasive treatment trachea can be displayed in an interventional treatment process, a doctor can perform interventional operation conveniently, and the operation accuracy is increased.
Description
Technical field
The invention belongs to medical instruments field, be specifically related to the method for preparing of minimally-invasive treatment with the development ring of conduit.
Background technology
Since the nineties, the minimally-invasive treatment technology was used in the therapeutic treatment field, particularly aspect cardiovascular disease therapies, interventional minimally-invasive treatment had become treatment cardiovascular diseases's first-selected Therapeutic Method.So-called interventional minimally-invasive treatment refers under the help by X ray and medical imaging technique, and the otch in patient body a part is again through using the intervention equipment to reach the operative treatment that carries out behind the lesions position.Must set up intervention apparatus by conduit in the operation of cardiovascular interventional therapy arrives focus enforcement apparatus placement or uses apparatus to carry out surgical action.How to judge whether that intervention apparatus arrives accurately that desired position is the precondition of performing the operation and carrying out smoothly in patient's focus or the art, so cardiovascular interventional therapy conduit must demonstrate conduit definite position in vivo under the help with becket that X ray do not penetrate or sheet.Treat employed delivery sheath, foley's tube, microtubular, electrophysiologicalcatheter catheters such as congenital structural heart disease, coronary heart disease, arrhythmia, aneurysm, vascular dissection and all need have the development ring (like Fig. 1) that X ray does not penetrate at the front end of conduit.
As everyone knows, determine by its density that density greatly then development property is good, otherwise development property is poor if having the master metal of X ray tightness.In all metals, descending osmium (22.57 g/cm that are followed successively by of density
3), iridium (22.42 g/cm
3), platinum (21.35g/cm
3), tungsten (19.3 g/cm
3), the gold (18.88 g/cm
3), tantalum (16.65 g/cm
3).At present, the used development ring of cardiovascular diseases's interventional therapy conduit is platinoiridita (PTIR10) alloy.Platinum is rare precious metal, its price very expensive up to 340 yuan/gram, and because of the ring that develops is the thickness annulus of (0.02mm) as thin as a wafer, the processing difficulty is big, cost is high.Therefore, seeking a kind of platinumiridio of can replacing develops and has encircled into urgent problem.
Tantalum has the X ray tightness because of its density is high, and excellent biological compatibility, physical and chemical performance make and aspect medical apparatus and instruments, obtain more applications, and low price makes it can substitute platinumiridio fully.Yet tantalum has as lively as a cricket chemical property, under normal pressure, with oxygen very strong affinity is arranged, and form tantalum pentoxide in the course of processing easily, so the difficulty of processing of tantalum light-wall pipe is big, and cost is high.Therefore, in the production and processing that is fit to such as the surface deposition thickness of stainless-steel thin-wall pipe, the simple metal tantalum film of dense structure can be good at solving the tantalum light-wall pipe, and can better reduce production costs.The performance of utilizing surface treatment technology of material to improve material is fundamental method of material science; The eighties in last century; The physical vapor deposition (PVD) technology is developed rapidly, is applied at aspects such as tool and mould, semiconductor device, optics and auto parts and components.Well solved the light-wall pipe difficult processing at stainless steel tube or other alloy pipe surface deposition tantalum metal films, cost is high, can satisfy the visible requirement under X ray that conduit develops and encircles simultaneously again.
Summary of the invention
In order to solve the expensive problem of platinumiridio development ring, the present invention provides following technical scheme:
The present invention utilizes physical gas phase deposition technology to have observability simple metal tantalum or W film under the X ray in deposition on the stainless steel thin-wall ring, and its thickness is 5-10 μ m.The purity requirement of desired tantalum or tungsten target is more than 99.9%.
The cardiovascular minimally-invasive treatment is with the method for preparing of the development ring of conduit, comprises with annulus through pre-polish(ing) tantalum, tungsten or tantalum-tungsten alloy thin film deposition process, deposition back polishing process.
Below 2 kinds of methods can realize the preparation of tantalum or W film:
1, multi-arc ion coating tantalum or W film
To polish, the stainless steel ring that cleans the back dehydration is inserted on the pivoted frame of vacuum chamber of multi-arc ion coating stove, is evacuated to 1 * 10
-3Pa, heating-up temperature is set to 400 ℃.Open grid bias power supply and make voltage reach 800V, feed Ar gas and make surface of the work form glow discharge, clean and the activation surface of the work.After 10 minutes, be evacuated to 3 * 10
-2Pa opens the arc source, bias voltage 800V, target current 80A, 2 minutes time.Then, feed the vacuum that Ar gas makes and maintain 6-8 * 10
-1Pa, arc current 60-70A, bias voltage 100-300V, sedimentation time 60-100 minute (can adjust according to technology) taken out workpiece after being cooled to 150 ℃ at last.
2, magnetron sputtering tantalum or W film
To polish, the stainless steel ring that cleans the back dehydration is inserted on the pivoted frame of vacuum chamber of magnetron sputtering stove, is evacuated to 1 * 10
-3Pa, heating-up temperature is set to 400 ℃.Open grid bias power supply and make voltage reach 800V, feed Ar gas and make surface of the work form glow discharge, clean and the activation surface of the work.Adopt the superimposed pulses DC voltage, bias voltage 200V, dutycycle 50%, sputtering current 20A feeds Ar gas, and vacuum is 3-4 * 10
-1Pa, takes out workpiece behind the intact postcooling to 150 of plated film ℃ at the 150-180 minute plated film time (can adjust according to technology).
Annulus adopts implanted medical device with rustless steel or other ferroalloy materials.
The present invention has following beneficial effect:
1, with low cost, the development ring of tantalum or W film is with respect to the development circumpolar tool price advantage of present platinumiridio.Simultaneously, also keep good development effect.2, adopt this method for preparing, plated film is even, can effectively avoid the formation of oxide, and development effect is good.
Description of drawings
The conduit that Fig. 1 band develops and encircles.
The development effect comparison diagram of Fig. 2 rustless steel tantalum coating ring and platinumiridio ring.
The specific embodiment
Embodiment 1:
The multi-arc ion coating tantalum: with after the stainless steel ring oil removing of well cutting the ultrasonic waves for cleaning that alkaline cleaning fluid is housed 10 minutes, ultrasonic 1 minute then at clear water, deionized water for ultrasonic 1 minute, at last with dehydrated alcohol dehydration, dry for standby.Cleaned stainless steel ring is hung in the stove on the pivoted frame, and the distance of stainless steel ring and tantalum target remains on 100-170mm, has closed fire door.Vacuum chamber is evacuated to vacuum to being lower than 6Pa, opens the high valve of vacuum, heater is heated to 400 ℃ with the vacuum chamber temperature, 60 minutes heat tracing time, pumping high vacuum to 1 * 10
-3Pa.Open grid bias power supply, bias voltage transfers to 800V in the stove, opens gas flowmeter and in vacuum chamber, feeds argon, make the stainless steel ring surface form after the glow discharge air pressure remain on 3.0-4.0Pa carry out Ar Hong, 10 minutes time; Then, vacuum in the stove is evacuated to 1 * 10
-3Pa, regulating Ar throughput to vacuum is 3-4 * 10
-2Pa opens 2 titanium targets, target current 50A carry out titanium Hong, the time is 2 minutes, titanium Hong after, bias voltage is reduced to 400V, opens 4 titanium targets, target current 50A, after 2 minutes in feeding Ar gas to the stove vacuum be 6-8 * 10
-1Pa, bias voltage is reduced to 100V, target current 50A, 100 minutes plated film time.Plated film finishes to open fire door behind the postcooling to 150 ℃ and takes out workpiece.Finished product is installed in Minimally Invasive Surgery with on the conduit, the experiment of developing.The result shows that the development ring of this programme preparation has outstanding development effect (as shown in Figure 2).
Embodiment 2:
The magnetron sputtering tantalum: with after the stainless steel ring oil removing of well cutting the ultrasonic waves for cleaning that alkaline cleaning fluid is housed 10 minutes, ultrasonic 1 minute then at clear water, deionized water for ultrasonic 1 minute, at last with dehydrated alcohol dehydration, dry for standby.Cleaned stainless steel ring is hung in the stove on the pivoted frame, and the distance of stainless steel ring and tantalum target remains on 100-170mm, has closed fire door.Vacuum chamber is evacuated to vacuum to being lower than 6Pa, opens the high valve of vacuum, heater is heated to 400 ℃ with the vacuum chamber temperature, and 60 minutes heat tracing time, pumping high vacuum is to 1X10
-3Pa.Open grid bias power supply, bias voltage transfers to 800V in the stove, open gas flowmeter and in vacuum chamber, feed argon, the stainless steel ring that makes surface form after the glow discharge air pressure remain on 3.0-4.0Pa carry out Ar Hong, 10 minutes time; Ar reduces to 200V with bias voltage after finishing, dutycycle 50%, and sputtering current 20A feeds argon and makes vacuum reach 3-4 * 10
-1Pa, sputtering time 150 minutes.Plated film finishes to open fire door behind the postcooling to 150 ℃ and takes out workpiece.Finished product is installed in Minimally Invasive Surgery with on the conduit, the experiment of developing.The result shows that the development ring of this programme preparation has outstanding development effect.
Embodiment 3:
Multi-arc ion coating tungsten: with after the stainless steel ring oil removing of well cutting the ultrasonic waves for cleaning that alkaline cleaning fluid is housed 10 minutes, ultrasonic 1 minute then at clear water, deionized water for ultrasonic 1 minute, at last with dehydrated alcohol dehydration, dry for standby.Cleaned stainless steel ring is hung in the stove on the pivoted frame, and the distance of stainless steel ring and tungsten target remains on 100-170mm, has closed fire door.Vacuum chamber is evacuated to vacuum to being lower than 6Pa, opens the high valve of vacuum, heater is heated to 400 ℃ with the vacuum chamber temperature, 60 minutes heat tracing time, pumping high vacuum to 1 * 10
-3Pa.Open grid bias power supply, bias voltage transfers to 800V in the stove, opens gas flowmeter and in vacuum chamber, feeds argon, make the stainless steel ring surface form after the glow discharge air pressure remain on 3.0-4.0Pa carry out Ar Hong, 10 minutes time; Then, vacuum in the stove is evacuated to 1 * 10
-3Pa, regulating Ar throughput to vacuum is 3-4 * 10
-2Pa opens 2 titanium targets, target current 50A carry out titanium Hong, the time is 2 minutes, titanium Hong after, bias voltage is reduced to 400V, opens 6 titanium targets, target current 50A, after 2 minutes in feeding Ar gas to the stove vacuum be 6-8 * 10
-1Pa, bias voltage is reduced to 100V, target current 50A, 60 minutes plated film time.Plated film finishes to open fire door behind the postcooling to 150 ℃ and takes out workpiece.Finished product is installed in Minimally Invasive Surgery with on the conduit, the experiment of developing.The result shows that the development ring of this programme preparation has outstanding development effect.
Embodiment 4:
Magnetron sputtering tungsten: with after the stainless steel ring oil removing of well cutting the ultrasonic waves for cleaning that alkaline cleaning fluid is housed 10 minutes, ultrasonic 1 minute then at clear water, deionized water for ultrasonic 1 minute, at last with dehydrated alcohol dehydration, dry for standby.Cleaned stainless steel ring is hung in the stove on the pivoted frame, and the distance of stainless steel ring and tungsten target remains on 100-170mm, has closed fire door.Vacuum chamber is evacuated to vacuum to being lower than 6Pa, opens the high valve of vacuum, heater is heated to 400 ℃ with the vacuum chamber temperature, 60 minutes heat tracing time, pumping high vacuum to 1 * 10
-3Pa.Open grid bias power supply, bias voltage transfers to 800V in the stove, open gas flowmeter and in vacuum chamber, feed argon, the stainless steel ring that makes surface form after the glow discharge air pressure remain on 3.0-4.0Pa carry out Ar Hong, 10 minutes time; Ar reduces to 200V with bias voltage after finishing, dutycycle 60%, and sputtering current 30A feeds argon and makes vacuum reach 3-4 * 10
-1Pa, sputtering time 120 minutes.Plated film finishes to open fire door behind the postcooling to 150 ℃ and takes out workpiece.Finished product is installed in Minimally Invasive Surgery with on the conduit, the experiment of developing.The result shows that the development ring of this programme preparation has outstanding development effect.
Claims (4)
1. minimally-invasive treatment is with the method for preparing of the development ring of conduit, and this method comprises annulus through pre-polish(ing), tantalum, tungsten or tantalum-tungsten alloy thin film deposition process, deposition back polishing process.
2. method for preparing as claimed in claim 1 is characterized in that said thin film deposition process takes following scheme: will polish, the stainless steel ring that cleans the back dehydration is inserted on the pivoted frame of vacuum chamber of multi-arc ion coating stove, is evacuated to 1 * 10
-3Pa, heating-up temperature is set to 400 ℃; Open grid bias power supply and make voltage reach 800V, feed Ar gas and make surface of the work form glow discharge, clean and the activation surface of the work; After 10 minutes, be evacuated to 3 * 10
-2Pa opens the arc source, bias voltage 800V, target current 80A, 2 minutes time; Then, feed the vacuum that Ar gas makes and maintain 6-8 * 10
-1Pa, arc current 60-70A, bias voltage 100-300V sedimentation time 60-100 minute, takes out workpiece after being cooled to 150 ℃ at last.
3. method for preparing as claimed in claim 1 is characterized in that said thin film deposition process is: will polish, the stainless steel ring that cleans the back dehydration is inserted on the pivoted frame of vacuum chamber of magnetron sputtering stove, is evacuated to 1 * 10-3Pa, and heating-up temperature is set to 400 ℃; Open grid bias power supply and make voltage reach 800V, feed Ar gas and make surface of the work form glow discharge, clean and the activation surface of the work; Adopt the superimposed pulses DC voltage, bias voltage 200V, dutycycle 50%, sputtering current 20A feeds Ar gas, and vacuum is 3-4 * 10-1Pa, 150-180 minute plated film time, takes out workpiece behind the intact postcooling to 150 of plated film ℃.
4. method for preparing as claimed in claim 1 is characterized in that annulus adopts implanted medical device with rustless steel or other ferroalloy materials.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104046942A (en) * | 2013-03-12 | 2014-09-17 | 中国兵器工业第五九研究所 | Metal tantalum coating preparation method |
| CN111926289A (en) * | 2020-08-19 | 2020-11-13 | 重庆文理学院 | Preparation method of tantalum coating |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5724989A (en) * | 1995-06-20 | 1998-03-10 | The Microspring Company, Inc. | Radiopaque medical devices |
| WO2002055120A2 (en) * | 2001-01-12 | 2002-07-18 | Impra, Inc. A Subsidiary Of C.R. Bard, Inc. | Encapsulated radiopaque markers |
| CN200966659Y (en) * | 2006-06-07 | 2007-10-31 | 北京乐普医疗器械有限公司 | Wedge-shaped frame of bifurcation blood vessels |
| CN101230445A (en) * | 2008-02-25 | 2008-07-30 | 哈尔滨工业大学 | Method for improving developobility of TiNi alloy bracket under X-ray |
-
2012
- 2012-06-26 CN CN2012102123420A patent/CN102698352A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5724989A (en) * | 1995-06-20 | 1998-03-10 | The Microspring Company, Inc. | Radiopaque medical devices |
| WO2002055120A2 (en) * | 2001-01-12 | 2002-07-18 | Impra, Inc. A Subsidiary Of C.R. Bard, Inc. | Encapsulated radiopaque markers |
| CN200966659Y (en) * | 2006-06-07 | 2007-10-31 | 北京乐普医疗器械有限公司 | Wedge-shaped frame of bifurcation blood vessels |
| CN101230445A (en) * | 2008-02-25 | 2008-07-30 | 哈尔滨工业大学 | Method for improving developobility of TiNi alloy bracket under X-ray |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104046942A (en) * | 2013-03-12 | 2014-09-17 | 中国兵器工业第五九研究所 | Metal tantalum coating preparation method |
| CN104046942B (en) * | 2013-03-12 | 2016-09-14 | 中国兵器工业第五九研究所 | A kind of preparation method of metal tantalum coating |
| CN111926289A (en) * | 2020-08-19 | 2020-11-13 | 重庆文理学院 | Preparation method of tantalum coating |
| CN111926289B (en) * | 2020-08-19 | 2022-10-21 | 重庆文理学院 | Preparation method of tantalum coating |
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Application publication date: 20121003 |