CN202096574U - Peritoneal dialysis catheterization guide wire/ tunnel guide with surface hard protecting membrane - Google Patents
Peritoneal dialysis catheterization guide wire/ tunnel guide with surface hard protecting membrane Download PDFInfo
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- CN202096574U CN202096574U CN2011201739991U CN201120173999U CN202096574U CN 202096574 U CN202096574 U CN 202096574U CN 2011201739991 U CN2011201739991 U CN 2011201739991U CN 201120173999 U CN201120173999 U CN 201120173999U CN 202096574 U CN202096574 U CN 202096574U
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- peritoneal dialysis
- tunnel guide
- surface hard
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Abstract
The utility model relates to the field of membrane preparation, in particular to a peritoneal dialysis catheterization guide wire/tunnel guide with a surface hard protecting membrane. The peritoneal dialysis catheterization guide wire/tunnel guide with the surface hard protecting membrane consists of a peritoneal dialysis catheterization guide wire/tunnel guide base and the surface hard protecting membrane, and the surface hard protecting membrane is a TiN single-layered protecting membrane or a Ti+TiN single-layered protecting membrane or a Ti+TiN multilayered protecting membrane, and accordingly wear resistance, high-temperature resistance, high-pressure disinfection, disinfectant corrosion resistance, anti-bacterium property and biocompatibility of the guiding wire/tunnel guide are improved. The peritoneal dialysis catheterization guide wire/tunnel guide effectively resolves the problem that local surfaces of the peritoneal dialysis catheterization guide wire/tunnel guide drop due to repeated high-temperature and high-pressure disinfection and disinfectant soaking, so that patients are infected and poisoned.
Description
Technical field
The present invention relates to the film preparation field, specifically is that a kind of peritoneal dialysis tube placing operation with surface hard protecting film is with seal wire/tunnel guide.
Background technology
Peritoneal dialysis has become the first-selected therapeutic scheme of uremic patient in China.Inserting of Dialysis tubing is a peritoneal dialysis first step of successful and a crucial step in the peritoneal dialysis tube placing operation.Successful Dialysis tubing is inserted the generation that can reduce the peritoneal dialysis catheters related complication.At present, seal wire that uses in the peritoneal dialysis tube placing operation and tunnel guide exist because of problems such as multiple high temp and autoclave sterilization and medicining liquid dipping generation casts.If getting into the abdominal cavity, cast will cause patient with operation to infect and poisoning.Therefore, the medical personnel who is engaged in peritoneal dialysis work presses for the seal wire and the serviceability and the stability of tunnel guide that improves in the tube placing operation, and this key problem that needs is solution seal wire and the high temperature resistant and high pressure of tunnel guide, anticorrosive and anti-microbial property.
Thin film technique is a kind of technology that plates the very thin film of one deck through physics or chemical method on object or material (matrix) surface.This technology does not change the structure and the performance of matrix material, but gives matrix many new, good physics and chemical properties, therefore is widely used in material and device surface modification.Titanium nitride membrane has been obtained extensive use at industrial circles such as machinery, plastics, weaving and microelectronics owing to have high rigidity, low-friction coefficient, good characteristics such as chemical inertness.In recent years, owing to finding that it has excellent biological compatibility and makes it attempted being applied to intravascular stent, esophageal stents appear, blade plate, intramedullary needle, root of the tooth, blood filter and the artificial heart pump etc. of medical circle.In addition, the oxidizing temperature of titanium nitride is 600 ℃, makes it under higher temperature, still can bring into play good effect.But the protection and the modification that titanium nitride membrane are used for medical guiding wire and tunnel guide also are not reported both at home and abroad.
Summary of the invention
To the weak point that exists in the prior art; The object of the present invention is to provide a kind ofly to have surface hard protecting film peritoneal dialysis tube placing operation with seal wire or tunnel guide, in order to improve the peritoneal dialysis tube placing operation with seal wire and tunnel guide wear-resisting, high temperature resistant and autoclave sterilization, the burn into of anti-the disinfectant is antibiotic and the purpose of biocompatibility.
To achieve these goals, technical scheme of the present invention is:
A kind of peritoneal dialysis tube placing operation with surface hard protecting film is with seal wire/tunnel guide; Have the peritoneal dialysis tube placing operation with seal wire/tunnel guide matrix and its surface hard protecting film, the surface hard protecting film is TiN monolayer protecting film, Ti+TiN monolayer protecting film or Ti+TiN multilayer proofing film.
The thickness of surface hard protecting film is 0.6～6.0 μ m.
Ti+TiN multilayer proofing film is the pure Ti phase of bottom, and the middle TiN of being mixes with Ti mutually mutually and TiN hands down, and the thickness direction gradient increases, and outermost layer is the gradient film of pure TiN phase; Or the multilayer film alternately arranged of one deck Ti film one deck TiN film, outermost layer is the TiN film.
The multilayer film that one deck Ti film one deck TiN film is alternately arranged, the Ti film is 0.3～2.5 with the thickness ratio of TiN film, outermost TiN film, thickness are 0.1～1.0 μ m.
The seal wire diameter is 1.0～2.5mm, length 30～80cm; Tunnel guide diameter 0.1～10mm, length 2～30cm.
Ti+TiN monolayer protecting film by TiN mutually with Ti mutually uniform mixing form.Wherein, TiN phase ratio is not less than 50% according to molar percentage.
Matrix material is selected from copper, copper alloy, titanium, titanium alloy or rustless steel.
The present invention adopts magnetron sputtering and arc ions plating to prepare the surface hard protecting film.
The principle mechanisms of magnetron sputtering of the present invention and arc ions plating is following:
Depositing TiN thin film can adopt magnetron sputtering and two kinds of technology of arc ion plating.The process that magnetron sputtering technique prepares the TiN film is: through discharge ar atmo is ionized into argon ion and electronics, the electronics under the effect in magnetic field and constraint has increased with the further collision of ar atmo and has produced more argon ion and secondary electron.Argon ion quickens bombardment Ti target under effect of electric field, sputter a large amount of Ti atoms and deposit film forming at substrate surface.If feed reacting gas N in the deposition process
2, then product TiN will be deposited on film forming on the substrate.If the N that feeds
2Content can not reach and make product be entirely TiN, with the mixed phase structure that forms Ti+TiN; Arc ion plating is a kind of of vacuum coating technology, and this technology makes the Ti ion high speed deposition that is evaporated on the substrate of band back bias voltage and form thin film through arc discharge and electric field action.If feed certain reaction gas N
2, then this gas will be reacted and form TiN by ionization and final and Ti ion.Titanium nitride is one of the most frequently used thin-film material of arc ion plating.
The present invention has following preferential and technique effect:
1. the invention solves the peritoneal dialysis tube placing operation with seal wire and tunnel guide can not satisfy the technical barrier that frequent high temperature, autoclave sterilization and medicining liquid dipping require, improved the peritoneal dialysis tube placing operation with seal wire and tunnel guide high temperature resistant with autoclave sterilization, anti-disinfectant solution burn into anti-microbial property and biocompatibility;
2. peritoneal dialysis tube placing operation of the present invention adopts the multilayer film of the increase of TiN phase gradient and one deck Ti film one deck TiN film with seal wire and tunnel guide; Not only help further to have improved protecting film high temperature resistant with autoclave sterilization, anti-disinfectant solution burn into anti-microbial property; Simultaneously also increase the adhesion of protecting film and seal wire and tunnel guide, and brought into play the outstanding biocompatibility characteristics of Ti film.
Description of drawings
Fig. 1 is the peritoneal dialysis of 1.2mm wherein one section schematic cross-section with seal wire for the diameter that embodiment 1 is coated with the TiN/Ti multilayer film;
Fig. 2 has wherein one section schematic cross-section of Ti+TiN gradient film for embodiment 2 seal wire surface depositions;
Fig. 3 has wherein one section schematic cross-section of TiN film for embodiment 3 tunnel guide surface depositions;
The diameter that Fig. 4 is coated with the TiN/Ti multilayer film for embodiment 1 is that the seal wire pattern is used in the peritoneal dialysis of 1.2mm;
Fig. 5 is embodiment 1 scanning electron microscopic observation corrosion back TiN/Ti multilayer film cross section pattern and N and Ti elemental line scan figure; Among the figure, N represents the nitrogen element, and T represents the Ti element.
The specific embodiment
The present invention adopts magnetron sputtering or electric arc ion-plating deposition device, selects high-purity Ti target and high-purity Ar and N2 as working gas, at seal wire and tunnel guide surface deposition TiN, TiN+Ti monolayer protecting film or TiN+Ti multilayer proofing film.Magnetic control sputtering device is intermediate frequency or rf magnetron sputtering device, and intermediate frequency that is equipped with or radio-frequency power supply power are 200～4000W.When depositing TiN or TiN+Ti monolayer protecting film, keeping vacuum indoor gas total pressure is 0.03～1.5Pa, Ar and N in control and the steady job gas
2Intrinsic standoff ratio 0～2.0.In the process of depositing Ti+TiN multilayer proofing film, keeping vacuum indoor gas total pressure is 0.03～2.0Pa, Ar and N in the dynamic adjustments working gas
2Intrinsic standoff ratio.When the sedimentation gradient film, select suitable working gas total pressure, only feed vacuum chamber Ar at first, feed N then
2And increase N gradually
2Dividing potential drop (reducing the Ar dividing potential drop).N
2It is 0.015～3.0Pa/ hour that dividing potential drop increases (reduction of Ar dividing potential drop) speed.Gradient through TiN phase in the rate of change control gradient film that changes two kinds of partial pressures; When the multilayer film of deposition one deck Ti film one deck TiN film, select suitable working gas total pressure, only feed vacuum chamber Ar15～180 second at first, turn off Ar afterwards and only feed N
215～240 seconds, and then turn off N
2Only fed Ar 15～180 seconds, and so hocketed.Can determine the thickness of monolayer Ti film and TiN film in the multilayer film through the time of controlling each feeding Ar and N2.
The deposition protecting film is before or/and in the process, to seal wire and tunnel guide heating, heating and temperature control is at 0～400 ℃.
Seal wire/tunnel guide to be coated cleaned 3～6 minutes through aura in vacuum chamber before adopting magnetron sputtering to prepare TiN, Ti+TiN monolayer protecting film or Ti+TiN multilayer proofing film; The interior Ar pressure of vacuum chamber was 0.3～3.0Pa when aura cleaned; Source current 0.5～2.0A, supply voltage 400～1000V; Source current is 2.0～6.0A in the preparation process, and Control of Voltage is at 300～450V.
Before arc ion plating prepares TiN, Ti+TiN monolayer protecting film or Ti+TiN multilayer proofing film, seal wire/tunnel guide to be coated in vacuum chamber through overbias be-600～-aura of 1000V cleans 3～6 minutes, arc light and cleaned 2～5 minutes.The interior Ar pressure of vacuum chamber was 1.0～4.0Pa when aura cleaned.The interior Ar pressure of vacuum chamber was 0.3～0.8Pa when arc light cleaned, and source current and voltage are respectively 55～75A and 16～22V; Source current is 45～65A in the preparation process, and Control of Voltage is at 16～22V.
Embodiment 1: adopt magnetic control sputtering device at seal wire surface deposition TiN/Ti multilayer film
Adopt plane fixed target magnetic control sputtering system.This system vacuum chamber is keep flat cylindrical, and the cylinder bottom surface is a door for vacuum chamber.Target is pure titanium (99.99%), after connect permanent magnet and water-cooling system, be positioned over vacuum chamber sidewall (face of cylinder).Selecting diameter is the copper wire of 50cm for 1.2mm length, after phosphoric acid,diluted cleaning, dehydrated alcohol ultrasonic cleaning, oven dry, hangs in the vacuum chamber of magnetic control sputtering device over against rectangle Ti target.Vacuum chamber is evacuated to 2 * 10
-3Behind the Pa, feed argon and keep the vacuum chamber gas pressure intensity at 2.0Pa.Power cathode connects target, and positive pole connects vacuum chamber housing and ground connection and device hanger bracket to be plated.Selecting the intermediate frequency power supply frequency is 20KHz, electric current 1.0A, and voltage 600V starts hanger bracket and makes the copper wire rotation, and the copper wire aura was cleaned 5 minutes.Pressure in vacuum tank is adjusted to 0.3Pa, then with Current Regulation to 3.5A, voltage 400V, depositing Ti film 3 minutes feeds nitrogen rapidly and turns off argon to pressure in vacuum tank 0.3Pa, depositing TiN film 3 minutes.And then feed argon rapidly and turn off nitrogen to pressure in vacuum tank 0.3Pa, depositing Ti film 3 minutes so repeats totally 13 circulations, and the last sedimentary TiN film time is 9 minutes.After the end, close target intermediate frequency power supply switch, turn off gas, continued evacuation (being that vacuum system works on) 1 hour.Close vacuum system, open vacuum chamber, copper wire behind the taking-up plated film.
As shown in Figure 1; The surface of matrix 1 is coated with Ti film 21 and TiN film 22 successively; Ti film and TiN film cycle criterion are 13, and outermost Ti film n1 is identical with Ti film 21 thickness of other layers, and the thickness of outermost TiN film n2 is thicker than the TiN film of other layers; The gross thickness of surface hard protecting film is 1.4 μ m, has obvious periodic property stratiform characteristic.
Copper wire behind the plated film is cut a bit of preparation metallographic sample, as shown in Figure 4.Visible by figure, deposited film smooth surface and more even does not have significant difference on the length of whole silk.Ti+TiN multilayer film to being coated in the same experiment on the copper sheet prepares metallographic sample, corrodes then (to utilize the HF and the 9 volume HNO of 1 volume
3All the other are the corrosion of 90 volume distilled water solutions) and observe its cross section pattern, as shown in Figure 5.Can see that multilayer film thickness is 1.4 μ m, have obvious periodic property stratiform characteristic, bright place (TiN phase) is clear with interface, dark place (Ti mutually), and thickness is respectively 0.055 μ m and 0.045 μ m.The modulation period of deposited film, (single cycle period thickness) was about 0.1 μ m.Because the corrosion resistance of TiN phase is superior to the metal Ti phase, thereby when cross section handled with corrosive liquid, it is mutually perishable that Ti compares TiN, thus on cross section TiN cycle variation mutually is revealed with Ti mutually.The TiN of deposited film outermost end compares thick, and this is in order to make full use of the good characteristics of TiN phase corrosion resistance.N among Fig. 5 and Ti element are carried out line sweep.Can see that the scanning line of the Ti of cross section and N element is wavy, meet the peak value of the corresponding Ti line in dark place basically, and the peak value of the corresponding N line in bright place.
Adopting scarification to measure multilayer film and the base material adhesion of same process deposit on copper sheet is 24.9N; The plated film seal wire is through high temperature and high pressure steam sterilization (1.3KP
0, 120 ℃; P
0Be normal atmosphere) after 50 hours, the electron microscopic observation surface has no variation; The plated film seal wire soaked (concentration 500mg/L) 100 hours through chlorinated product, observed the surface under the Electronic Speculum and did not change.Seal wire is done 48 hours surfaces of antibacterial cultivation and is not found pathogenic bacterium behind autoclave sterilization; Seal wire is done 48 hours surfaces of antibacterial cultivation and is not found pathogenic bacterium after chlorinated product soaks.
Embodiment 2: adopt arc ion plating apparatus at seal wire surface deposition Ti+TiN gradient film
Adopt homemade MIP-8-800 type arc ion plating apparatus.Selecting diameter is the titanium silk of 45cm for 1.5mm length, hangs on the vacuum chamber of arc ion plating apparatus through phosphoric acid,diluted cleanings, dehydrated alcohol ultrasonic cleaning, after drying over against the Ti target.In this device over against titanium silk 3 the Ti targets that are arranged above and below.Opening the sample heating system and temperature is set is 300 ℃.Vacuum chamber is evacuated to 3 * 10
-3Behind the Pa, feed argon and keep the vacuum chamber gas pressure intensity at 2.0Pa.Start hanger bracket and make the rotation of Ti silk.Add back bias voltage-800V (duty cycle adjustment is 5%) between target and metal Ti silk, the Ti silk is carried out aura cleaned 3 minutes; Afterwards, the strong 0.6Pa of adjustment argon flow amount to vacuum intraventricular pressure opens the Ti target power supply, and the control electric current is 70A (corresponding voltage is 21V), and the Ti silk was proceeded ion bom bardment 2 minutes.Being biased into-400V (duty cycle adjustment to 40%) between adjustment target and the Ti silk; Adjustment target source current is to 58A (corresponding voltage is 17.2V); Keeping the interior total pressure of vacuum chamber is 0.6Pa; Reduce argon flow amount gradually, feed nitrogen and increase its flow gradually, argon flow amount is 0 after 30 minutes.Continue deposition after 5 minutes, close grid bias power supply, close the target on and off switch, turn off gas, continued evacuation 1 hour.Close vacuum system, open vacuum chamber, take out plated film titanium silk.
Ti silk behind the plated film is cut a bit of preparation metallographic sample.Through scanning electron microscopic observation, the film on Ti silk surface is the multi-gradient film, and thickness is 2.6 μ m.This multilayer film increases along film thickness direction N constituent content gradually, and the Ti constituent content reduces gradually, and it is 1: 1 that there are 0.6 μ m zone, two element mol ratios on top layer.
As shown in Figure 2, Ti+TiN multilayer proofing film is the pure Ti phase 23 of bottom, and mix with Ti for TiN mutually mutually centre 24 and TiN hands down, and the thickness direction gradient increases, and outermost layer is the gradient film of pure TiN phase 25.
Adopting scarification to measure multilayer film and the base material adhesion of same process deposit on the titanium sheet is 36.3N; The plated film seal wire is through high temperature and high pressure steam sterilization (1.3KP
0, 120 ℃) and after 50 hours, the electron microscopic observation surface has no variation; The plated film seal wire soaked (concentration 500mg/L) 100 hours through chlorinated product, observed the surface under the Electronic Speculum and did not change.Seal wire is done 48 hours surfaces of antibacterial cultivation and is not found pathogenic bacterium behind autoclave sterilization; Seal wire is done 48 hours surfaces of antibacterial cultivation and is not found pathogenic bacterium after chlorinated product soaks.
Embodiment 3: adopt arc ion plating apparatus at tunnel guide surface deposition TiN film
Adopt homemade MIP-8-800 type arc ion plating apparatus.Select the 316L rustless steel tunnel guide of Ф 10 * 100mm, after phosphoric acid,diluted cleaning, dehydrated alcohol ultrasonic cleaning, oven dry, hang on the vacuum chamber of arc ion plating apparatus over against the Ti target.Select 2 Ti targets work that is arranged above and below in this device.Vacuum chamber is evacuated to 3 * 10
-3Behind the Pa, feed argon and keep the vacuum chamber gas pressure intensity at 2.0Pa.Start pivoted frame and make the tunnel guide rotation of suspension.Add back bias voltage-800V (duty cycle adjustment is 5%) between rustless steel tunnel guide and target, workpiece is carried out aura cleaned 3 minutes; Afterwards, the adjustment argon flow amount makes the vacuum chamber gas pressure intensity be adjusted into 0.6Pa.Open the titanium target power supply, the control electric current is 80A (voltage is 20V), and the rustless steel tunnel guide was proceeded ion bom bardment 2 minutes.Be biased into-350V (duty cycle adjustment to 40%) between adjustment rustless steel tunnel guide and target, adjustment target source current is to 60A (corresponding voltage is 18.2V), and the working time is 40 minutes.After the end, close grid bias power supply, close the target on and off switch, turn off gas, continued evacuation 1 hour.Close vacuum system, open vacuum chamber, take out the rustless steel tunnel guide.
Rustless steel tunnel guide behind the plated film is cut a bit of preparation metallographic sample.Through scanning electron microscopic observation, the film on rustless steel tunnel guide surface is the TiN film, and thickness is 2.2 μ m.Be 1: 1 along film thickness direction N and Ti element mol ratio.
As shown in Figure 3, the surface of matrix 1 is the TiN film 28 of monolayer.
Adopting scarification to measure monolayer TiN film and the base material adhesion of same process deposit on the 316L stainless steel substrates is 31.1N; The plated film tunnel guide is through high temperature and high pressure steam sterilization (1.3KP
0, 120 ℃) and after 50 hours, the electron microscopic observation surface has no variation; The plated film tunnel guide soaked (concentration 500mg/L) 100 hours through chlorinated product, observed the surface under the Electronic Speculum and did not change.Tunnel guide is done 48 hours surfaces of antibacterial cultivation and is not found pathogenic bacterium behind autoclave sterilization; Tunnel guide is done 48 hours surfaces of antibacterial cultivation and is not found pathogenic bacterium after chlorinated product soaks.
Claims (7)
1. the peritoneal dialysis tube placing operation with surface hard protecting film is with seal wire/tunnel guide; It is characterized in that; Have the peritoneal dialysis tube placing operation with seal wire/tunnel guide matrix and its surface hard protecting film, the surface hard protecting film is TiN monolayer protecting film, Ti+TiN monolayer protecting film or Ti+TiN multilayer proofing film.
By the described peritoneal dialysis tube placing operation of claim 1 with surface hard protecting film with seal wire/tunnel guide, it is characterized in that the thickness of surface hard protecting film is 0.6～6.0 μ m.
By the described peritoneal dialysis tube placing operation of claim 1 with surface hard protecting film with seal wire/tunnel guide; It is characterized in that; Ti+TiN multilayer proofing film is the pure Ti phase of bottom, and the middle TiN of being mixes with Ti mutually mutually and TiN hands down, and the thickness direction gradient increases, and outermost layer is the gradient film of pure TiN phase; Or the multilayer film alternately arranged of one deck Ti film one deck TiN film, outermost layer is the TiN film.
By the described peritoneal dialysis tube placing operation of claim 3 with surface hard protecting film with seal wire/tunnel guide; It is characterized in that, the multilayer film that one deck Ti film one deck TiN film is alternately arranged, the Ti film is 0.3～2.5 with the thickness ratio of TiN film; Outermost TiN film, thickness are 0.1～1.0 μ m.
By the described peritoneal dialysis tube placing operation of claim 1 with surface hard protecting film with seal wire/tunnel guide, it is characterized in that the seal wire diameter is 1.0～2.5mm, length 30～80cm; Tunnel guide diameter 0.1～10mm, length 2～30cm.
By the described peritoneal dialysis tube placing operation of claim 1 with surface hard protecting film with seal wire/tunnel guide; It is characterized in that; Ti+TiN monolayer protecting film by TiN mutually with Ti mutually uniform mixing form, wherein, TiN phase ratio is not less than 50% according to molar percentage.
By the described peritoneal dialysis tube placing operation of claim 1 with surface hard protecting film with seal wire/tunnel guide, it is characterized in that matrix material is selected from copper, copper alloy, titanium, titanium alloy or rustless steel.
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|---|---|---|---|
| CN2011201739991U CN202096574U (en) | 2011-05-27 | 2011-05-27 | Peritoneal dialysis catheterization guide wire/ tunnel guide with surface hard protecting membrane |
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|---|---|---|---|
| CN2011201739991U CN202096574U (en) | 2011-05-27 | 2011-05-27 | Peritoneal dialysis catheterization guide wire/ tunnel guide with surface hard protecting membrane |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109105987A (en) * | 2018-09-26 | 2019-01-01 | 波司登羽绒服装有限公司 | The method for preventing down jackets suture from boring suede |
| CN111012581A (en) * | 2019-12-17 | 2020-04-17 | 苏州涂冠镀膜科技有限公司 | Medical ear hook and preparation method thereof |
-
2011
- 2011-05-27 CN CN2011201739991U patent/CN202096574U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109105987A (en) * | 2018-09-26 | 2019-01-01 | 波司登羽绒服装有限公司 | The method for preventing down jackets suture from boring suede |
| CN111012581A (en) * | 2019-12-17 | 2020-04-17 | 苏州涂冠镀膜科技有限公司 | Medical ear hook and preparation method thereof |
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