CN1524977A - Artificial organs surface treatment method using sputtering technology - Google Patents
Artificial organs surface treatment method using sputtering technology Download PDFInfo
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- CN1524977A CN1524977A CNA031541720A CN03154172A CN1524977A CN 1524977 A CN1524977 A CN 1524977A CN A031541720 A CNA031541720 A CN A031541720A CN 03154172 A CN03154172 A CN 03154172A CN 1524977 A CN1524977 A CN 1524977A
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- titanium
- tantalum
- niobium
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- sputtering
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- 210000000056 organ Anatomy 0.000 title claims abstract description 58
- 238000004544 sputter deposition Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000005516 engineering process Methods 0.000 title claims description 17
- 238000004381 surface treatment Methods 0.000 title abstract 2
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 28
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 26
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000010955 niobium Substances 0.000 claims abstract description 23
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- RJSRQTFBFAJJIL-UHFFFAOYSA-N niobium titanium Chemical compound [Ti].[Nb] RJSRQTFBFAJJIL-UHFFFAOYSA-N 0.000 claims description 21
- VSSLEOGOUUKTNN-UHFFFAOYSA-N tantalum titanium Chemical compound [Ti].[Ta] VSSLEOGOUUKTNN-UHFFFAOYSA-N 0.000 claims description 21
- 239000001301 oxygen Substances 0.000 claims description 20
- 229910052760 oxygen Inorganic materials 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 18
- 238000007254 oxidation reaction Methods 0.000 claims description 17
- 239000010936 titanium Substances 0.000 claims description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 16
- 229910052719 titanium Inorganic materials 0.000 claims description 16
- 230000003647 oxidation Effects 0.000 claims description 15
- 229910001257 Nb alloy Inorganic materials 0.000 claims description 13
- 229910052786 argon Inorganic materials 0.000 claims description 11
- 239000000919 ceramic Substances 0.000 claims description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 11
- BFRGSJVXBIWTCF-UHFFFAOYSA-N niobium monoxide Chemical compound [Nb]=O BFRGSJVXBIWTCF-UHFFFAOYSA-N 0.000 claims description 9
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 8
- RAHKDDYJTIRXMG-UHFFFAOYSA-M [O-2].[O-2].[O-2].[O-2].[OH-].O.O.[Ti+4].[Ta+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[OH-].O.O.[Ti+4].[Ta+5] RAHKDDYJTIRXMG-UHFFFAOYSA-M 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000004408 titanium dioxide Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910001362 Ta alloys Inorganic materials 0.000 claims description 4
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 4
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 4
- 238000010301 surface-oxidation reaction Methods 0.000 claims description 2
- 239000013077 target material Substances 0.000 claims 4
- 239000008186 active pharmaceutical agent Substances 0.000 claims 1
- 238000004062 sedimentation Methods 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium(II) oxide Chemical compound [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 11
- 230000002429 anti-coagulating effect Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 40
- 239000008280 blood Substances 0.000 description 14
- 210000004369 blood Anatomy 0.000 description 14
- 239000000956 alloy Substances 0.000 description 12
- 229910045601 alloy Inorganic materials 0.000 description 11
- 210000003709 heart valve Anatomy 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 238000000151 deposition Methods 0.000 description 6
- 238000011160 research Methods 0.000 description 5
- 229910001275 Niobium-titanium Inorganic materials 0.000 description 4
- 210000000748 cardiovascular system Anatomy 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910010272 inorganic material Inorganic materials 0.000 description 3
- 239000011147 inorganic material Substances 0.000 description 3
- 238000010884 ion-beam technique Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000002526 effect on cardiovascular system Effects 0.000 description 2
- 239000007888 film coating Substances 0.000 description 2
- 238000009501 film coating Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 238000010849 ion bombardment Methods 0.000 description 2
- 210000005240 left ventricle Anatomy 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 235000005288 Annona lutescens Nutrition 0.000 description 1
- 244000030795 Annona lutescens Species 0.000 description 1
- 229910001020 Au alloy Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000002929 anti-fatigue Effects 0.000 description 1
- 230000010100 anticoagulation Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- Prostheses (AREA)
- Physical Vapour Deposition (AREA)
- Materials For Medical Uses (AREA)
Abstract
The invention provides a method for artificial organ surface treatment through sputtering technique, wherein tantalum, niobium doped titanium-oxygen surface modified layers are synthesized on the surfaces of artificial organs with complex shapes by means of sputtering method, the artificial organs processed by the method of the invention possesses substantially improved anticoagulant property and durability.
Description
The application runs after fame and is called the dividing an application of No. 99117468.2 patent applications that " a kind of artificial organ surface modifying technology ", the applying date are on December 23rd, 1999.Be according to this original application the first time notification of examiner's opinion requirement carry out division, and according to the requirement of these examination reports, the applicant plans original application and is renamed as " a kind of artificial organ surface modifying method ".
Affiliated technical field
The present invention relates to inorganic material surface modification technology field, particularly the modification technology of artificial organs material.
Background technology
The biocompatibility of artificial organs and weather resistance are that artificial organs is used for clinical basic assurance, and especially important cardiovascular systems artificial organs such as artificial heart, heart valve prosthesis and left ventricle service pump have higher requirement to weather resistance and blood compatibility.With natural materials (pig, the OX-heart born of the same parents), artificial heart that macromolecular material is made and heart valve prosthesis are because weather resistance still can not satisfy above-mentioned requirements fully, see document 1 (moral is white forever-etc., numerous usefulness artificial organ present situation in the future, one artificial man's cap used in ancient times one, artificial organ, 1990,19 (3), 100-102 etc.), and with RESEARCH OF PYROCARBON, titanium alloy, inorganic materials such as cobalt-base alloy and stainless steel is that the heart valve prosthesis of main body also exists two aspect problems at present: the one, and blood compatibility is still good inadequately, and the 2nd, fatigue still may take place in the valve that such material is made behind implant into body, corrosion, wearing and tearing and brittle rupture.RESEARCH OF PYROCARBON with best blood compatibility has been represented the highest level that is used for clinical heart valve prosthesis based on mechanical prosthetic valve, but concerning clinical requirement, its blood compatibility still is not enough height, and its toughness only is 1/100 of metal.Studies show that for many years of this area, based on the cardiovascular system artificial organ surface of inorganic materials such as metal coated with the fabulous material of blood compatibility, comprehensively its metallic substance physical strength height, good endurance and the good advantage of covering material blood compatibility, thus the important trend that the development of the artificial organs of suitable application prospect material is arranged become.Document 2 (Mitamura.Y.etgl, Development of a Ceramic Valve, Journal of BiomaterialsApplications, 1989,4 (11), 33-55) discussed the technology with physical gas-phase deposite method overlay film titanium nitride on titanium heart valve prosthesis surface.At present, on cardiovascular system artificial organ, adopt method such as physical vapor deposition in the problem of existing soverlay technique such as heart valve materials surface deposition titanium nitride, diamond-film-like aspect having two: the one, the improvement degree of the blood compatibility of the material after overlay film is handled is limited, the 2nd, because the physical essence limitation of deposition method, film is lower with high base strength.Document 3 (China Patent No. ZL95111386.0) has provided the method for preparing titanium-oxygen/titanium nitride composite membrane with ion beam enhanced depositing method (IBED) on cardiovascular system artificial organ, this method can only realize planar, simple artificial cardiovascular organ overlay film, blade as heart valve prosthesis, can't be to complex-shaped, the artificial cardiovascular organ of curved surface is carried out uniform comprehensive overlay film, as the lobe frame surface of heart valve prosthesis, be only stable and the modification processing is all carried out on all surfaces that contact with blood of artificial organs, the reliable assurance that improves artificial organs performance and security.The result of document 4 shows that the IBED-titanium with characteristic of semiconductor-oxygen surface film material that obtains with the ion beam enhanced depositing method has the more excellent blood compatibility of RESEARCH OF PYROCARBON.(Huang Nan, Yang Ping etc., the research of ion beam enhanced depositing titanium oxide film and anticoagulation function thereof, hi-tech communication 1997,4,16-18).
The purpose of this invention is to provide and a kind ofly carry out artificial organs surface-treated method with sputtering technology, it can improve the blood compatibility and the mechanics of the complicated artificial organs in surfaces such as artificial heart, heart valve prosthesis and left ventricle service pump effectively
The present invention mixes metallic elements such as element or niobium, tantalum in the titanium oxide top layer on artificial organs surface, forms adulterated titanium-oxygen film, and to obtain to have the surface of excellent blood compatibility, its preparation can realize by following scheme:
(1) adopt the magnetron sputtering mode to prepare Doped with Titanium-oxygen film
This method was divided into for two steps
1, at first adopts the alloys target or the mosaic target of niobium-titanium or tantalum-titanium, utilize the film coating method of this high-speed low temperature of magnetron sputtering, at artificial organs surface deposition titanium-tantalum or titanium-niobium alloy film.The parameter of control alloy firm performance is: niobium atom content be 0.1%～20% or tantalum atom content be 0.1%～20% alloys target or mosaic target, sputtering voltage-100～-1000V, sputtering current 0.05～5 peace, substrate heating temperature 100～500 degree, sputtering time 0.1～2 hour, sputtering pressure 0.01～10 handkerchief, sample table bias voltage 0～-600 volt.
2, then the synthetic alloy firm is carried out specific oxide treatment and can obtain tantalum or the adulterated titanium of niobium-oxygen film, can adopt following two kinds of technologies;
A, thermooxidizing, the artificial organs that is coated with titanium-tantalum or titanium-niobium alloy film is placed the vitreosil Glass tubing, be heated to certain temperature, feed oxygen with certain pressure simultaneously in quartz glass tube, at this moment alloy film has just obtained tantalum or the adulterated titanium of niobium-oxygen film through oxidation.The parameter of control film performance has: oxygen pressure 0.1～10 handkerchief, Heating temperature 400～900 degree, oxidization time (1 minute～2 hours), the composition niobium atom content of tantalum-titanium or niobium-titanium alloy thin films be 0.1%～20% or the tantalum atom percentage composition be 0.1%～20%.
B, plasma oxidation, the artificial organs that is coated with titanium-tantalum or titanium-tantalum or titanium-niobium alloy film is placed the vacuum chamber of plasma apparatus, charge into oxygen with certain pressure, utilize radio frequency or microwave discharge to produce oxygen plasma, at this moment artificial organs is immersed in the oxygen plasma atmosphere, the heating artificial organs, and on artificial organs, apply certain pulse voltage, utilize plasma oxidation process to obtain tantalum or the adulterated thin film of titanium oxide of niobium at the artificial organs surface oxidation.The parameter of control film performance is an oxygen pressure 10
-2～10 handkerchiefs, oxygen plasma volume density 10
8～10
13Centimetre
-3Heating temperature 100～600 degree, apply 0.2～3 kilovolt of pulse negative voltage amplitude, 1 minute～2 hours plasma oxidation time, 10～5000 hertz of pulse negative high voltage repetition rates, pulse width 20～500 μ s, the composition of titanium-tantalum or titanium-niobium alloy film: niobium atom content be 0.1%～20% or tantalum atom content be 0.1%～20%.
(2) adopt the radio-frequency sputtering mode to prepare Doped with Titanium-oxygen film
Adopt Niobium Pentxoxide-titanium dioxide or tantalum pentoxide-titanium dioxide ceramic as sputtering target, the molecule content of Niobium Pentxoxide in pottery be 0.1%～10% or the molecule content of tantalum pentoxide in pottery be 0.1%～10%.Feed the argon or the xenon of certain pressure in the radio-frequency (RF) sputtering equipment vacuum chamber, adopt RF-wise to form argon or xenon plasma body, utilize to sputter at the synthetic tantalum in artificial organs surface or the adulterated titanium of niobium-oxygen film.The parameter amount of control film performance: radio frequency power 200～3000W, air pressure 10
-2～10
1Handkerchief, 0.4～3 kilovolt of radio-frequency voltage, the sample Heating temperature is 100～600 degree, sputtering time 0.1～3 hour, the composition of Niobium Pentxoxide-titanium dioxide or tantalum pentoxide-titanium dioxide ceramic target be the molecule content of Niobium Pentxoxide in pottery be 0.1%～10% or tantalum pentoxide be 0.1%～10% at the molecule content of pottery.
The present invention compared with prior art, employing aforesaid method institute synthetic is mixed hydrogen, is mixed the titanium-oxygen film of tantalum or niobium, its advantage is: the adulterated titanium of institute's synthetic hydrogen, tantalum or niobium-oxygen film blood compatibility is fabulous, artificial organs to complicated shape, can realize the comprehensive modification of artificial organs, evenly reliable, can realize industrial applications, the blood compatibility of these doping oxide surface reforming layers significantly is better than internationally recognized Artificial heart valve mould material---the RESEARCH OF PYROCARBON of present clinical use, the modified layer easy control of components, and good reproducibility, the reliability height.In a word, adopt method of the present invention to handle the blood compatibility of the artificial organs that is obtained, antifatigue, anticorrosive and abrasion resistance properties are improved comprehensively.
Description of drawings
Description of drawings of the present invention is as follows:
Fig. 1 is the vacuum chamber synoptic diagram of the used rf magnetron sputtering platform of the present invention.
Fig. 2 is the used vitreosil pipe process furnace of the present invention.
The invention will be further described below in conjunction with accompanying drawing:
(1) adopt the magnetic controlled sputtering ion plating mode to prepare titania-doped film, this method was divided into for two steps, at first prepared titanium-niobium or titanium-tantalum alloy film.Utilize thermooxidizing or plasma oxidation process that alloy firm is carried out oxidation then, obtain the adulterated titanium of niobium or tantalum element-oxygen film, Fig. 2 is the used magnetron sputtering equipment synoptic diagram of the present invention, and embodiment is:
1, at first niobium-titanium or tantalum-titanium alloy target or mosaic target are contained on the target platform 6 of magnetron sputtering equipment, artificial organs 5 is placed on the sample table 6, and vacuum chamber is evacuated to 1 * 10
-4Handkerchief, heating artificial organs 5 is opened gas cylinder 8, feeds argon gas to vacuum chamber, argon pressure is 0.01～10 handkerchief, transfer lever 3 is allocated to direct supply 1, on target platform 4, adds certain negative high voltage, form argon plasma, under the negative voltage effect, argon ion bombardment titanium-niobium or titanium-tantalum target, generation titanium, niobium atom or titanium, tantalum atom are deposited on the artificial organs 5, form the au-alloy film.In order to improve film quality, in the deposition process, open grid bias power supply 7, on sample table 6, apply certain negative bias.Utilize the film coating method of this high-speed low temperature of magnetron sputtering, can obtain titanium-tantalum or titanium-niobium alloy film by four kinds of technologies shown in the table one.The parameter of control alloy firm performance is: niobium atom content be 0.1%～20% or tantalum atom content be 0.1%～20% alloys target or mosaic target, sputtering voltage-100～-1000V, sputtering current 0.05～5 peace, sample Heating temperature 100～500 degree, sputtering time 0.1～2 hour, sputtering pressure 0.01～10 handkerchief, sample table bias voltage 0～-600 volt.
Table one
| Embodiment | The atom content of tantalum or niobium in the target composition | Sputtering voltage (volt) | Sputtering current (peace) | Heating temperature (degree) | Sputtering time (hour) | Sputtering pressure (handkerchief) | Sample table bias voltage (volt) |
| One | 0.1％ | -300 | 0.05 | 100 | 1.5 | 0.05 | -200 |
| Two | 5％ | -600 | 1 | 300 | 0.8 | 1 | -300 |
| Three | 15％ | -1000 | 5 | 500 | 0.2 | 5 | -600 |
2, the synthetic alloy firm is carried out thermal oxidative treatment or plasma oxidation can obtain tantalum or the adulterated titanium of niobium-oxygen film, Fig. 3 is the used vitreosil pipe synoptic diagram of the present invention, and embodiment is respectively:
A, if adopt thermal oxidative treatment, embodiment is, the artificial organs 5 that is coated with titanium-niobium alloy film is placed vitreosil Glass tubing 9, opens vacuum system power supply 10, is evacuated to 1 * 10
-3Handkerchief is opened furnace power 11, and heating, vacuum quartz glass tube to 700 degree is opened inflation system 12, feeds the oxygen of 0.5 handkerchief in quartz glass tube 9, thermooxidizing 10 minutes, and at this moment alloy film has just obtained tantalum or the adulterated thin film of titanium oxide of niobium through oxidation.
B, if the using plasma oxidation, embodiment is, the artificial organs that is coated with titanium-tantalum or titanium-niobium alloy film is placed on the sample table of plasma source ion implantation device, is evacuated to 1 * 10
-4Handkerchief, charge into oxygen, open radio-frequency power supply or microwave power supply and produce oxygen plasma, at this moment artificial organs is immersed in the oxygen plasma atmosphere, the heating artificial organs, open the pulse power, on artificial organs, apply certain pulse negative voltage, utilize plasma oxidation process to obtain tantalum or the adulterated titanium deoxid film of niobium by three kinds of oxidizing procesies shown in the table five.The parameter of control film performance is oxygen pressure 0.01～10 handkerchief, oxygen plasma volume density 10
8～10
12Centimetre
-3, Heating temperature 100～600 degree, 0.2～3 kilovolt of pulse negative voltage amplitude, 1 minute～2 hours plasma oxidation time, 10～5000 hertz of pulse negative high voltage repetition rates, pulse width 20～500 μ s.Plasma oxidation also can adopt existing common equipment with microwave or radio frequency plasma body source.
Table two
| Embodiment | The oxygen pressure handkerchief | Oxygen plasma volume density centimetre -3 | The Heating temperature degree | Pulse negative voltage volt | Time hour | The repetition rate hertz | Pulse width μ s |
| One | 0.01 | 10 8 | 200 | -0.2 | 2 | 10 | 500 |
| Two | 1 | 10 9 | 400 | -1 | 0.5 | 500 | 100 |
| Three | 10 | 10 12 | 600 | -3 | 0.05 | 5000 | 20 |
(2) adopt Niobium Pentxoxide-titanium dioxide or tantalum pentoxide-titanium dioxide ceramic target, utilize the radio-frequency sputtering mode to prepare niobium or tantalum Doped with Titanium-oxygen film, embodiment is:
At first Niobium Pentxoxide-titanium dioxide or tantalum pentoxide-titanium dioxide ceramic target are placed on the target platform 4 of magnetron sputtering equipment, artificial organs 5 is placed on the sample table 6, is evacuated to 1 * 10
-4Handkerchief, heating artificial organs 7, open gas cylinder 8, feed argon gas, argon pressure is 0.01～10 handkerchief, transfer lever 3 is allocated to radio-frequency power supply 2, on target platform 4, add certain voltage, form argon plasma, argon ion bombardment Niobium Pentxoxide-titanium dioxide or tantalum pentoxide-titanium dioxide ceramic target, generation titanium, niobium, Sauerstoffatom or titanium, tantalum, Sauerstoffatom are deposited on the artificial organs 5, synthetic tantalum or the adulterated titanium of niobium-oxygen film.In order to improve film quality, in the deposition process, open grid bias power supply 7, on sample table 6, apply certain negative bias.Can sputter at the synthetic tantalum in artificial organs surface or the adulterated titanium of niobium-oxygen film by three kinds of technology utilizations shown in the table six.The parameter of the energy of control film performance is: radio frequency power 200～3000W, air pressure 10
-2～10
9Handkerchief, 0.4～3 kilovolt of radio-frequency voltage, sample Heating temperature are 100～600 degree, sputtering time 0.1～3 hour.
Table three
| Embodiment | Tantalum pentoxide or Niobium Pentxoxide molecule content in the target | Heating temperature (degree) | Radio frequency power (watt) | Gaseous tension (handkerchief) | Radio-frequency voltage (volt) | Sputtering time (hour) | Sample table bias voltage (volt) |
| One | 0.1％ | 200 | 200 | 5 | 400 | 2 | 0 |
| Two | 2.5％ | 400 | 800 | 05 | 800 | 1 | -300 |
| Three | 8％ | 600 | 2500 | 0.01 | 2500 | 0.5 | -500 |
Claims (5)
1, a kind ofly carries out artificial organs surface-treated method with sputtering technology, it is characterized in that: the target material of employing is: titanium-niobium alloy target or titanium-tantalum alloy target or titanium-niobium mosaic target or titanium-tantalum mosaic target, perhaps Niobium Pentxoxide-titanium dioxide ceramic target or tantalum pentoxide-titanium dioxide ceramic target, utilize argon plasma to make the artificial organs surface of target material sputtering sedimentation on the sample table, sputtering pressure is 0.01～10 handkerchief.
2, according to claim 1ly carry out artificial organs surface-treated method with sputtering technology, it is characterized in that, described target material is titanium-niobium alloy target or titanium-tantalum alloy target or titanium-niobium mosaic target or titanium-tantalum mosaic target, on target, apply volts DS, target is carried out magnetically controlled DC sputtering, sputtering voltage-100～-1000V, sputtering current 0.05～5 peace, sample table bias voltage 0～-600 volt, sample Heating temperature 100～500 degree, sputtering time 0.1～2 hour obtains titanium-niobium or titanium-tantalum alloy on the artificial organs surface, and the composition tantalum of titanium-tantalum or titanium-niobium alloy film or the atom content of niobium are 0.1%～20%; Carry out oxide treatment then.
3, according to claim 2ly carry out artificial organs surface-treated method with sputtering technology, it is characterized in that: described oxide treatment is: the artificial organs that is coated with titanium-tantalum or titanium-niobium alloy film after the sputter is placed the silica tube process furnace, utilize thermal oxidation technology to obtain tantalum or the adulterated titanium of niobium-oxygen film at workman's organ surface, the parameter of control film performance has: oxygen pressure 0.1～10 handkerchief, Heating temperature is crossed 400～900 degree, oxidization time 1 minute～2 hours.
4, according to claim 2ly carry out artificial organs surface-treated method with sputtering technology, it is characterized in that: described oxide treatment is: the artificial organs that is coated with titanium-tantalum or titanium-niobium alloy film after the sputter is placed in the plasma device, obtain tantalum or the adulterated titanium of niobium-oxygen film with plasma oxidation process at the artificial organs surface oxidation, oxygen pressure 0.01～10 handkerchief, oxygen plasma volume density 10
8～10
13Centimetre
-3Heating temperature 100～600 degree, apply pulse voltage amplitude-0.2～-3 kilovolt, 1 minute plasma oxidation time kind～2 hour, 10～5000 hertz of pulse negative voltage repetition rates, pulse width 20～500 μ s, the composition niobium of titanium-tantalum or titanium-niobium alloy film or the atom content of tantalum are 0.1%～20%.
5, artificial organ surface modifying technology according to claim 1, it is characterized in that: described target material is Niobium Pentxoxide-titanium dioxide ceramic target or tantalum pentoxide-titanium dioxide ceramic target, the molecule content of Niobium Pentxoxide or tantalum pentoxide is 0.1%～10% in the ceramic target, on target, apply radio-frequency voltage, target is carried out rf magnetron sputtering, radio frequency power 200～3000W, 0.4～3 kilovolt of radio-frequency voltage, sample Heating temperature 100～600 degree, sputtering time 0.1～3 hour.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03154172 CN1274870C (en) | 1999-12-23 | 1999-12-23 | Artificial organs surface treatment method using sputtering technology |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03154172 CN1274870C (en) | 1999-12-23 | 1999-12-23 | Artificial organs surface treatment method using sputtering technology |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB991174682A Division CN1158403C (en) | 1999-12-23 | 1999-12-23 | Process for modifying surface of artificial organ |
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| CN1524977A true CN1524977A (en) | 2004-09-01 |
| CN1274870C CN1274870C (en) | 2006-09-13 |
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|---|---|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1316058C (en) * | 2005-03-24 | 2007-05-16 | 上海交通大学 | Method for modifying surface of polymer microffow chip by sputtering TiO2 |
| CN102000702A (en) * | 2010-12-21 | 2011-04-06 | 重庆大学 | Processing technology of high-purity tantalum sputtering target material |
| CN102127737A (en) * | 2011-02-25 | 2011-07-20 | 陕西科技大学 | Method for preparing anti-oxidation Nb coating on surface of carbon material |
| CN105821386A (en) * | 2015-10-07 | 2016-08-03 | 重庆工业职业技术学院 | Preparation method for artificial heart valve leaflet coating material with anticoagulation function |
| CN112522674A (en) * | 2021-02-18 | 2021-03-19 | 中南大学湘雅医院 | Titanium alloy surface composite coating and preparation method thereof |
-
1999
- 1999-12-23 CN CN 03154172 patent/CN1274870C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1316058C (en) * | 2005-03-24 | 2007-05-16 | 上海交通大学 | Method for modifying surface of polymer microffow chip by sputtering TiO2 |
| CN102000702A (en) * | 2010-12-21 | 2011-04-06 | 重庆大学 | Processing technology of high-purity tantalum sputtering target material |
| CN102000702B (en) * | 2010-12-21 | 2012-09-26 | 重庆大学 | Processing technology of high-purity tantalum sputtering target material |
| CN102127737A (en) * | 2011-02-25 | 2011-07-20 | 陕西科技大学 | Method for preparing anti-oxidation Nb coating on surface of carbon material |
| CN105821386A (en) * | 2015-10-07 | 2016-08-03 | 重庆工业职业技术学院 | Preparation method for artificial heart valve leaflet coating material with anticoagulation function |
| CN105821386B (en) * | 2015-10-07 | 2018-06-08 | 重庆工业职业技术学院 | The preparation method of heart valve prosthesis leaflet coating material with anticoagulant functions |
| CN112522674A (en) * | 2021-02-18 | 2021-03-19 | 中南大学湘雅医院 | Titanium alloy surface composite coating and preparation method thereof |
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