CN1539513A - Biologic coating material of carbon in use for medical inner embedded body and preparation method - Google Patents
Biologic coating material of carbon in use for medical inner embedded body and preparation method Download PDFInfo
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- CN1539513A CN1539513A CNA2003101119306A CN200310111930A CN1539513A CN 1539513 A CN1539513 A CN 1539513A CN A2003101119306 A CNA2003101119306 A CN A2003101119306A CN 200310111930 A CN200310111930 A CN 200310111930A CN 1539513 A CN1539513 A CN 1539513A
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000000576 coating method Methods 0.000 title claims abstract description 27
- 239000011248 coating agent Substances 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims description 11
- 239000000758 substrate Substances 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 5
- 239000000956 alloy Substances 0.000 claims abstract description 5
- 239000007943 implant Substances 0.000 claims description 13
- 230000000399 orthopedic effect Effects 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 11
- 210000000056 organ Anatomy 0.000 claims description 11
- 230000007704 transition Effects 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000011159 matrix material Substances 0.000 claims description 4
- 238000005452 bending Methods 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 150000001247 metal acetylides Chemical class 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 8
- 238000004544 sputter deposition Methods 0.000 abstract description 6
- 230000002429 anti-coagulating effect Effects 0.000 abstract 1
- 239000010409 thin film Substances 0.000 description 12
- 229910001069 Ti alloy Inorganic materials 0.000 description 9
- 239000010408 film Substances 0.000 description 9
- 210000004369 blood Anatomy 0.000 description 8
- 239000008280 blood Substances 0.000 description 8
- 230000006870 function Effects 0.000 description 7
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 6
- 210000003709 heart valve Anatomy 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 229910003460 diamond Inorganic materials 0.000 description 4
- 239000010432 diamond Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000010100 anticoagulation Effects 0.000 description 2
- 230000023555 blood coagulation Effects 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 102000002262 Thromboplastin Human genes 0.000 description 1
- 108010000499 Thromboplastin Proteins 0.000 description 1
- 208000007536 Thrombosis Diseases 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005842 biochemical reaction Methods 0.000 description 1
- 239000000560 biocompatible material Substances 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000003519 biomedical and dental material Substances 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000013642 negative control Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000013641 positive control Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
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- 230000001988 toxicity Effects 0.000 description 1
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- Prostheses (AREA)
Abstract
A biological carbon coating material for the medical body to be transplanted in human body features that a multi-arc magnetic-filter vacuum sputtering technology is used to deposit a layer of tetrohedral a mourphous carbon on the furace of medical metal or alloy substrate. Its advantages are high adhesion and bioactivity, and high anticoagulating performance.
Description
Technical field
The present invention relates to a kind of carbon element biological coating material that can be used for medical inner embedded body and preparation method thereof.
Background technology
Along with the raising of people's living standard and the progress of medical skill, interplantation artificial organ and orthopedic implant have been widely used in the clinical treatment, as artificial joint, artificial bone, Cardiac valve prosthesis, blood vessel stomach tube support etc.These implant great majority are made by titanium alloy (Ti6Al4V), high polymer or RESEARCH OF PYROCARBON etc., because the shortcoming of such material bio-compatible performance, when contacting with blood or body fluid, they will produce a series of biochemical reactions, cause platelet adhesion to form thrombosis, or cause biological respinses such as sensitization, toxicity, inflammation, produce some physiology negative interaction in vivo.Therefore, the surface modification of synthetic and the interplantation artificial organ or the orthopedic implant of biocompatible materials is one of key areas of bio-medical material research.We adopt multi sphere magnetic filtration vacuum sputtering ion technology to prepare tetrahedral carbon (ta-C) thin film, and the maximum characteristics of this thin film are sp in the film
3The content of key can be regulated with process conditions are different, and its character is similar to diamond thin or diamond like carbon film.Adopt this technology of preparing, sp
3The content of key can be controlled in the 20%-95% scope, and the blank between diamond thin and the diamond like carbon film has been filled up in the appearance of ta-C thin film.In thin film, has suitable sp
3During the content of key, this thin film has good blood compatibility and biocompatibility, therefore, prepare the fine carbon element biological coating of one deck thin film (ta-C thin film) at interplantation artificial organ and orthopedic implant surfaces, to satisfy required mechanical performance of interplantation artificial organ and orthopedic implant and bio-compatible performance simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of carbon element biological coating material that can be used for medical inner embedded body and preparation method thereof, this material can solve and improve the biocompatibility of interplantation artificial organ or orthopedic implant, satisfy physicochemical property and mechanical performance simultaneously, be applied to prepare the inner embedded body face coat.
The artificial organ of making at present widely used titanium and metal alloy thereof and the characteristics of orthopedic implant biocompatibility difference, we adopt multi sphere magnetic to filter the vacuum sputtering ion technology, on the metal or alloy matrix of interplantation artificial organ or orthopedic implant, be coated with layer of metal carbide transition zone, be coated with one deck on the surface and contain sp
3/ (sp
3+ sp
2) the carbon element biological coating, the carbon element biological coating is sp
3/ (sp
3+ sp
2) tetrahedral carbon films (the tetrohedral amourphous carbon of content between 20%-95%, be abbreviated as ta-C), thereby form strong adhesion and have " titanium alloy/titanium carbide transition zone/ta-C biological coating " function gradient film of good anticoagulation function, make it in the requirement that reaches clinical use aspect biocompatibility and the comprehensive mechanical property.Thickness of thin layer is the 300-800 nanometer, metal carbides transition region thickness 5-20 nanometer.The carbon element biological coating material that can be used for medical inner embedded body comprises at capital equipment that the solenoid coil of plasma sputter source, 90 ° of bendings filters in the equipment of magnetic field, workpiece biasing negative bias voltage and carries out sputter that the base vacuum degree is 4.0 * 10
-2Pa-1.0 * 10
-3Pa (handkerchief), operating air pressure are 5-15Pa (handkerchief), and magnet exciting coil magnetic field is 30-80mT (milli tesla), and underlayer temperature is 27-300 ℃, substrate bias V
b+ 100V～-2000V is adjustable continuously, and shielding power supply is direct current or pulse voltage 1.3-2.2kV, and sputter gas is high-purity argon gas, nitrogen or ammonia.
When back of the body end vacuum is higher than 4.0 * 10
-2Pa-1.0 * 10
-3During Pa, feed argon as sputter gas, the voltage that adds high pressure makes argon ionization, and argon ion sputter graphite target under electric field action produces carbon ion, also can produce carbon neutral atom and macroscopical carbon particle simultaneously.The effect of magnetic filter is that carbon neutral atom and macroscopical carbon particle that sputter produces are filtered out, the C of 100% ionization almost
+Ion is guided to and is formed carbon film on the substrate.Save the energy that incides the carbon ion on the substrate by the adjustable size that changes substrate bias, preparation sp
3/ sp
2The carbon film material that ratio is different.
The orthopedic implant of various artificial organs, fixed support, interplantation and the medical equipment of Titanium, titanium alloy preparation.As the various interplantation artificial organs or the orthopedic implant of titanium alloy (Ti6Al4V) preparation, such as artificial joint, artificial bone, Cardiac valve prosthesis and support, orthopedic implant support etc.Its architectural feature is for as shown in Figure 1, forms strong adhesion and has " titanium alloy/titanium carbide is layer/ta-C biological coating excessively " function gradient structure of good anticoagulation function.
The device sketch map that multi sphere magnetic filters vacuum sputtering ion deposition technology as shown in Figure 2, the ion source structure sketch is as shown in Figure 3.The ion source negative electrode is high-purity, highdensity graphite plectane, and anode is a wire netting; Filter the solenoid coil generation of magnetic field, change the size that the coil current scalable is filtered magnetic field by bending; Between anode and substrate, substrate bias is set, incides the energy of the carbon ion on the substrate by the adjustable size joint of regulating bias voltage.And the energy of carbon ion is to influence sp in the carbon film
3/ sp
2The technological parameter of the most critical of ratio and character
Description of drawings
Fig. 1 is " Titanium or alloy substrate/titanium carbide transition zone/ta-C biological coating " function gradient film structural representation.
Fig. 2 is that single arc magnetic filters vacuum sputtering ion deposition technique device sketch map.
Fig. 3 is a plasma sputter source structure sketch map.
Among Fig. 1, on on-plane surface metal or alloy matrix 3, inject by carbon ion, form the titanium carbide transition zone 2 of thickness 5-20 nanometer, the atom percentage concentration of titanium reduces gradually up to 0 in the transition zone, and the atom percentage concentration of carbon increases up to 100% gradually by 0, and forming thickness at last is the biological coating thin film 1 of 300-800 nanometer.
Among Fig. 2,11 is air intake, and 12 is the plasma sputter source, and 13 for filtering field coil, and 14 is metal works (sample) platform, and 15 is the vacuum pump interface, 16 workpiece negative bias power supplys, and 17 ion source high voltage power supplies, 18 is vacuum reaction chamber.
Among Fig. 3,21 is the copper electrode plate, and 22 is high purity graphite negative electrode target, and 23 is plastics king dead ring, and 24 is plastics king fixed jacket, and 25 is the metal anode net, 26 blowholes, and 27 is the ion source power supply lead wire.
The specific embodiment
Embodiment 1: biological coating preparation technology and performance
At base vacuum is 5.0 * 10
-2Pa when the reacting gas ar pressure is that 7Pa, sputtering voltage are that 1.4kV, solenoidal field are 40 milli teslas and workpiece temperatures when being room temperature, regulates workpiece bias V
bFor+20V～-prepared one group of biological coating thin film during 120V.Determined sp in the coating by means such as x-ray photoelectron spectroscopy, Raman spectrum, ellipse polarisation spectrum and electronic field emission
3Content and surface work function, the result as shown in Table 1:
Table one: workpiece negative bias voltage (V
b) with the biological coating thin film in sp
3Percentage composition (sp
3/ (sp
3+ sp
2)) relation
| V b(volt) | +20 | ?0 | -10 | -20 | -50 | -60 | -80 | -100 | -120 |
| sp 3(％) | 30±8 | ?54±5 | ?85±3 | ?91±3 | ?89±5 | ?60±5 | ?50±8 | ?41±8 | ?32±10 |
| Work function (volt) | 0.035 | ?0.038 | ?0.021 | ?0.017 | ?0.020 | ?0.018 | ?0.028 | ?0.031 | ?0.033 |
Embodiment 2: the control experiment of blood compatibility performance
Embodiment 1 described one group of sample carried out platelet is centrifugal sticks experiment, microsphere post method, partial prothrombinase active appraisal experiment (KPTT, PT, TT, dynamically blood coagulation) research.And make negative control with U.S. PolyMedica company a heatable brick bed blood coagulation biomaterial " Merlon Polyurethane (Phrono flex) " that produce, that clinical practice is best, compare experiment with the poorest glass as positive control.The result shows: the ta-C thin film for preparing under different negative substrate bias conditions, its sp
3Content difference, blood compatibility are also different.Sp
3Content is high more, and blood compatibility is good more.The ta-C thin film for preparing under-20 volts of negative bias voltages, its blood compatibility are better than the standard sample (Phrono flex) of the clinical use of the U.S..
Embodiment 3: the preparation technology of biological coating Cardiac valve prosthesis
Through Chemical cleaning, the vacuum reaction chamber of packing into is when base vacuum is 5.0 * 10 with the cardiac valve of titanium alloy (Ti6Al4V) preparation
-2During Pa, when the feeding argon makes reative cell air pressure be 7Pa, at first on workpiece, apply a 2.0kV negative bias voltage, carry out surface of the work and cleaned 5 minutes; Secondly, the high pressure that applies 1.4kV between ion source negative electrode and anode is kept the workpiece negative bias voltage of 2.0kV to produce carbon ion, and is under the situation of 40 milli teslas in the overanxious magnetic field of solenoid, carries out C
+Ion implantation 30 clocks form the titanium carbide transition zone; At last, peace reduces workpiece negative bias voltage behind-20V gradually according to certain speed, keeps this process conditions, prepares certain thickness biological coating time (as～500 nanometers).Confirm on the titanium alloy artificial cardiac valve, to have formed multiple structure (Ti/TiCx/ta-C) by the composition depth analysis with " matrix titanium alloy/titanium carbide transition zone/ta-C biological coating ", by Mechanics Performance Testing and blood compatibility analysis, its adhesive force of coatings, hardness, anti-wear performance, fineness and blood compatibility etc. all can satisfy interplantation artificial organ or the required requirement of orthopedic implant.
Claims (4)
1, a kind of carbon element biological coating material that can be used for medical inner embedded body is characterized in that being coated with layer of metal carbide transition zone on the metal or alloy matrix of interplantation artificial organ or orthopedic implant, is coated with one deck on the surface and contains sp
3/ (sp
3+ sp
2) the carbon element biological coating.
2, a kind of as the said carbon element biological coating material that can be used for medical inner embedded body of claim 1, it is characterized in that the carbon element biological coating is sp
3/ (sp
3+ sp
2) tetrahedral carbon films of content between 30%-90%, film thickness is the 300-800 nanometer.
3, a kind of as the said carbon element biological coating material that can be used for medical inner embedded body of claim 1, it is characterized in that metal carbides transition region thickness 5-20 nanometer.
4, a kind of carbon element biological coating preparation methods that can be used for medical inner embedded body as claimed in claim 1, it is characterized in that comprising at capital equipment that the solenoid coil of unique plasma sputter source, 90 ° of bendings filters in the equipment of magnetic field, workpiece bias voltage carries out sputter, the base vacuum degree is 4.0 * 10
-2Pa-1.0 * 10
-3Pa, operating air pressure are 5-15Pa, and magnet exciting coil magnetic field is 30-80mT, and underlayer temperature is 27-300 ℃, selected substrate bias V
b, can+100V～-2000V is adjustable continuously, shielding power supply is direct current or pulse voltage 1.3-2.2kV, sputter gas is high-purity argon gas, nitrogen or ammonia.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101119306A CN100502955C (en) | 2003-10-29 | 2003-10-29 | Carbon biological coating material for medical implant and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101119306A CN100502955C (en) | 2003-10-29 | 2003-10-29 | Carbon biological coating material for medical implant and its preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1539513A true CN1539513A (en) | 2004-10-27 |
| CN100502955C CN100502955C (en) | 2009-06-24 |
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768720A (en) * | 2010-03-31 | 2010-07-07 | 西安交通大学 | Method for preparing amorphous carbon coating on surface of medical stainless steel knife saw |
| CN102442632A (en) * | 2011-12-09 | 2012-05-09 | 中山大学 | Micro-nano multi-scale patterned anticoagulation composite biological material and method for preparing same |
| CN103046001A (en) * | 2013-01-21 | 2013-04-17 | 浙江大学 | Amorphous carbon complex coating and preparation method thereof |
| CN103708708A (en) * | 2012-09-28 | 2014-04-09 | Hoya株式会社 | Moulding die, manufacturing method thereof, and method for manufacturing optical glass element |
| CN105200383A (en) * | 2015-10-27 | 2015-12-30 | 中国科学院兰州化学物理研究所 | Apparatus for preparing superhard super-smooth tetrahedral carbon film through magnetron sputtering and method |
| CN105441872A (en) * | 2015-04-03 | 2016-03-30 | 中奥汇成科技股份有限公司 | Amorphous carbon composite coating and preparation method and application thereof |
-
2003
- 2003-10-29 CN CNB2003101119306A patent/CN100502955C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768720A (en) * | 2010-03-31 | 2010-07-07 | 西安交通大学 | Method for preparing amorphous carbon coating on surface of medical stainless steel knife saw |
| CN102442632A (en) * | 2011-12-09 | 2012-05-09 | 中山大学 | Micro-nano multi-scale patterned anticoagulation composite biological material and method for preparing same |
| CN102442632B (en) * | 2011-12-09 | 2014-10-01 | 中山大学 | Micro-nano multi-scale patterned anticoagulation composite biological material and method for preparing same |
| CN103708708A (en) * | 2012-09-28 | 2014-04-09 | Hoya株式会社 | Moulding die, manufacturing method thereof, and method for manufacturing optical glass element |
| CN103708708B (en) * | 2012-09-28 | 2017-03-29 | Hoya株式会社 | The manufacture method of compression molding die and its manufacture method and glass optical component |
| CN103046001A (en) * | 2013-01-21 | 2013-04-17 | 浙江大学 | Amorphous carbon complex coating and preparation method thereof |
| CN103046001B (en) * | 2013-01-21 | 2015-07-08 | 浙江大学 | Amorphous carbon complex coating and preparation method thereof |
| CN105441872A (en) * | 2015-04-03 | 2016-03-30 | 中奥汇成科技股份有限公司 | Amorphous carbon composite coating and preparation method and application thereof |
| CN105441872B (en) * | 2015-04-03 | 2018-03-13 | 中奥汇成科技股份有限公司 | A kind of amorphous carbon composite coating and its preparation method and application |
| CN105200383A (en) * | 2015-10-27 | 2015-12-30 | 中国科学院兰州化学物理研究所 | Apparatus for preparing superhard super-smooth tetrahedral carbon film through magnetron sputtering and method |
| CN105200383B (en) * | 2015-10-27 | 2019-03-01 | 中国科学院兰州化学物理研究所 | A kind of magnetron sputtering prepares the apparatus and method of superhard ultra-smooth tetrahedral carbon films |
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| Publication number | Publication date |
|---|---|
| CN100502955C (en) | 2009-06-24 |
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