CN106581782A - ALD technology-based energy saving method for producing oxidation layer on medical device - Google Patents

ALD technology-based energy saving method for producing oxidation layer on medical device Download PDF

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Publication number
CN106581782A
CN106581782A CN201611144058.9A CN201611144058A CN106581782A CN 106581782 A CN106581782 A CN 106581782A CN 201611144058 A CN201611144058 A CN 201611144058A CN 106581782 A CN106581782 A CN 106581782A
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ald
instruments
medical apparatus
oxide
drying
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徐福春
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Tianjin Fengmao Technology Co Ltd
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Tianjin Fengmao Technology Co Ltd
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/08—Materials for coatings
    • A61L31/082—Inorganic materials
    • A61L31/088—Other specific inorganic materials not covered by A61L31/084 or A61L31/086
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/08—Materials for coatings
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L31/16—Biologically active materials, e.g. therapeutic substances
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45555—Atomic layer deposition [ALD] applied in non-semiconductor technology
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
    • A61L2300/606—Coatings
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2420/00—Materials or methods for coatings medical devices
    • A61L2420/02—Methods for coating medical devices
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2420/00—Materials or methods for coatings medical devices
    • A61L2420/04—Coatings containing a composite material such as inorganic/organic, i.e. material comprising different phases
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2420/00—Materials or methods for coatings medical devices
    • A61L2420/08—Coatings comprising two or more layers

Abstract

An ALD technology-based energy saving method for producing an oxidation layer on a medical device concretely comprises the following steps: 1, cleaning and drying; 2, oxide selection; 3, gas introduction; 4, thickness selection; 5, solidification; and 5, antibacterial treatment. A gas phase is alternately introduced to a reactor through an atom layer deposition technology and undergoes a chemical reaction to form a film. An oxidation layer with the thickness of 100-200 nm is produced on the surface of an implantable alloy medical device, has very good stability and compactness, changes the adhesiveness, the biocompatibility and the blood compatibility, and avoids new medical problems caused by influences of shedding and cracking phenomena of a polymeric drug delivery layer of the implantable alloy medical device and non-degradable polymeric materials on functions of human bodies in in-vivo environment and in the expansion process of a scaffold.

Description

The energy-saving method of oxide layer is prepared on the medical instrument based on ALD technique
Technical field
The present invention relates to energy-conserving and environment-protective technical fiel, specially one kind prepare oxidation on the medical instrument based on ALD technique The energy-saving method of layer.
Background technology
Medical apparatus and instruments refer to instrument, equipment, utensil, external diagnosis reagent and the calibration for being directly or indirectly used for human body The article of thing, material and other similar or correlations, including required computer software, wherein embedded type medical apparatus and instruments exist What is be employed in medical operating is gradually more and more, any by surgical operation, and apparatus enters human body or nature in whole or in part In tract；Stayed in the body after operation process terminates for a long time, or these instrument portions stay in the body at least more than 30 days, these Apparatus is considered as implantation instrument, with the sustainable development of China's implanted medical device industry, current country's implanted medical device Enterprise can substantially produce low side and part middle-end implanted medical device, and obtain in biocompatibility new material research field Certain progress.But product integral level is relatively low, and unification is serious.
Embedded type medical apparatus and instruments based on metal material are by the modified obtaining certain ductility, elasticity of surface With rigid characteristic, while and require have cell adhesion, histocompatibility and the blood compatibility of ceramic material etc. biological Can, existing embedded type medical apparatus and instruments easily occur the de- of macromolecule drug-loaded layer in vivo in the process of expansion of environment and support The phenomenon for falling and ftractureing, causes new medical care problem, and along with nondegradable macromolecular material has been used, to human body Technical ability will also result in certain impact.
The content of the invention
It is an object of the invention to provide a kind of energy-saving side for preparing oxide layer based on ALD technique on the medical instrument Method, with solve the of the prior art existing embedded type medical apparatus and instruments proposed in above-mentioned background technology in vivo environment and Easily occur the phenomenon for coming off and ftractureing of macromolecule drug-loaded layer in the process of expansion of frame, cause new medical care problem, and companion With nondegradable macromolecular material has been used, the problem of certain impact will also result in the technical ability of human body.
For achieving the above object, the present invention provides following technical scheme：One kind is prepared on the medical instrument based on ALD technique The energy-saving method of oxide layer, the energy-saving method concrete steps that should prepare oxide layer on the medical instrument based on ALD technique are such as Under：
S1：Cleaning-drying：The medical apparatus and instruments for needing to prepare oxide layer are picked out, the dust and oil of surface attachment is removed The pollutant such as dirt, are cleaned and drying process in being placed into specific medical apparatus and instruments cleaning sterilizing device；
S2：Oxide is selected：Suitable oxide is selected, wherein by aluminium oxide, silicon oxide, titanium oxide, stannum oxide and oxygen Change the common oxide storage such as zinc standby；
S3：It is passed through gas：The fixture of suitable dimension is selected, medical apparatus and instruments are placed into into ALD work after sterilization and drying In inner chamber, operating temperature in ALD deposition, carrier gas flux and nebulizer gas pressure are regulated, wherein operating temperature is set in 25-300 DEG C, carrier gas flux is set in 500-1000sccm, by ALD operating rooms evacuation, and is passed through noble gases and carries out cleaning operation；
The ALD such as volatile halogenide precursor compounds are passed through in ALD working cavities after setting each numerical value to steam Vapour, treats that compound steam is stably good and is passed through ozone again in ALD working cavities, and while measure oxygen with oxygen sensor Partial pressure, question response are passed through noble gases in terminating backward ALD working cavities, after purging cleaning is carried out to ALD operating rooms；
S4：Thickness is selected：According to S3 step repetitive operations, change the deposit thickness of medical apparatus surface with this；
S5：Curing operation：ALD operating temperatures in S3 steps are adjusted to appropriate scope, medical apparatus and instruments are taken out, 2-4h is placed under room temperature, is then placed in curing oven, addition helium is medium, and curing oven is heated up, and wherein temperature is set in 180-200 DEG C, 5-6h is processed at this temperature；
S6：Antimicrobial treatment：Medical apparatus and instruments in S5 steps are taken out into cooling, mass ratio is taken and is put into for 1%-10% titanate esters To in stirring container, lytic agent stirring is added, and mass ratio is sequentially added while lytic agent is added for 1%-10%'s Hydrochloric acid, water, silicon compound, mass ratio dispersant, the silver nitrate and mass ratio that mass ratio is 0.1%-1% for 0.1%-1% The zinc nitrate of 1%-4% is sufficiently stirred for, and antibiotic paint is obtained, the medical apparatus and instruments after cooling are placed into the antibacterial being stirred In coating solution, do up and down uniformly lift operation, carry out drying operation in being then placed into drying plant, wherein drying Dry temperature is set in 30-80 DEG C, and the medical apparatus and instruments after drying are positioned in calciner, forges at a temperature of 200-300 DEG C 20-50h is burnt, indoor temperature is naturally cooled to after taking-up, the Medical treatment device with antibacterial figure layer and oxide ceramics after taking-up, is obtained Tool.
Preferably, the probe voltage that oxygen sensor shows in step S3 is 900-950mV.
Preferably, the noble gases being passed through in step S3 are nitrogen, and are being passed through on the equipment used by nitrogen Choke valve is installed, wherein, the aperture opening ratio of choke valve is controlled in 30%-60%.
Preferably, embedded type medical apparatus and instruments of the medical apparatus and instruments for metal material.
Compared with prior art, the invention has the beneficial effects as follows：One kind that the invention is provided is based on ALD technique in Medical treatment device The energy-saving method of oxide layer is prepared on tool, by technique for atomic layer deposition, gas phase is alternately passed through reactor disease in deposition Medical apparatus and instruments surface on there is chemical reaction forming a kind of method of thin film, the method has excellent large area uniform Property, the control of accurate simple film thickness just simply can control to aoxidize layer film thickness by controlling the number of times of circular response, And depositing temperature is relatively low, the change of flow affects little to deposition effect, can be on the surface of embedded type alloy medical apparatus and instruments The oxide layer of prepared 100-200nm thickness, with good stability and compactness, changes the viscous of original embedded type medical apparatus and instruments Attached property, biocompatibility and blood compatibility, it is to avoid embedded type medical apparatus and instruments are in vivo in the process of expansion of environment and support There is the phenomenon for coming off and ftractureing of macromolecule drug-loaded layer, and nondegradable macromolecular material, the technical ability of human body can also be made Into impact cause new medical care problem.
Description of the drawings
Fig. 1 is present invention process flow chart.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.It is based on Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made Embodiment, belongs to the scope of protection of the invention.
Embodiment 1
A kind of method for preparing oxide layer based on ALD technique on vertebra inner fixer,
Vertebra inner fixer is taken out, the pollutant such as the dust and greasy dirt of surface attachment is removed, is placed into medical apparatus and instruments clear In wash disinfection device, opening electric rotating machine and cleaning sprayer carries out rotary-cleaning operation to vertebra inner fixer, is put after cleaning again High temperature drying and disinfecting action are carried out in putting drying unit, dried vertebra inner fixer is taken out into standby；
Suitable aluminium oxide and silicon oxide is selected to stay with standby；
Put in the operation inner chamber of ALD using the fixture gripping vertebra inner fixer after dry disinfection, while ALD is sunk The operating temperature of product device is adjusted to 100 DEG C, and carrier gas flux is adjusted to 500sccm, by ALD operating rooms evacuation, and is passed through Noble gases carry out cleaning operation, clean 3 times come in the state of ensureing that ALD working cavities are in cleaning, it is to avoid pollutant effect The operation of oxide layer is prepared to vertebra inner fixer；
To ALD deposition device after the good numerical value of operating and setting, the ALD forerunners such as volatile halogenide are passed through in working cavities Body compound steam, treats that compound steam is stably good and is passed through ozone again in ALD working cavities, and while use oxygen detection Device measures oxygen partial pressure, and question response is passed through inert nitrogen gas in terminating backward ALD working cavities, and then again ALD is worked Room carries out purging cleaning, is an ALD deposition cycle job to this, can repeatedly operate, change vertebra with this The probe voltage that the deposit thickness on inner fixer surface, wherein oxygen sensor show is 900mV, and is made nitrogen is passed through Choke valve is installed on equipment, wherein, the aperture opening ratio of choke valve is controlled 30%, for reducing exhaust efficiency, is conducive to First reacting gas residual fraction is indoor in the reaction of ALD deposition device；
Operate through multiple ALD deposition, the vertebra inner fixer of appropriate deposition thickness is obtained, ALD operating temperatures are carried out Adjust to appropriate scope, vertebra inner fixer is taken out, under room temperature, place 2h, increase oxide and sink on vertebra inner fixer Long-pending efficiency, then puts into the vertebra inner fixer for having cooled down in curing oven, and addition helium is medium, by curing oven liter Temperature, temperature are set in 180 DEG C, at this temperature cured 5h, improve sticky limit of the oxide on vertebra inner fixer；
Vertebra inner fixer after cured is taken out into cooling, is taken mass ratio and stirring container is put into for 1% titanate esters In, lytic agent stirring is added, and hydrochloric acid, water, silication that mass ratio is 1% are sequentially added while lytic agent is added and closed Thing, mass ratio are that the zinc nitrate of 0.1% dispersant, the silver nitrate that mass ratio is 0.1% and mass ratio 1% is fully stirred Mix, be obtained antibiotic paint, it is this antibiotic paint good stability, good biocompatibility, nontoxic, pollution-free and repeatedly long-acting can make With the vertebra inner fixer after cooling is placed in the antibiotic paint solution being stirred, uniformly lifting up and down is done Operation, carries out drying operation in being then placed into drying plant, wherein drying temperature is set in 60 DEG C, by the vertebra after drying Holder is positioned in calciner, calcines 20h, naturally cool to indoor temperature, after taking-up after taking-up at a temperature of 200 DEG C Obtain the vertebra inner fixer with antibacterial figure layer and oxide ceramics.
Embodiment 2
A kind of method for preparing oxide layer based on ALD technique on embedded type alloy medical apparatus and instruments,
Similar to Example 1, difference can be to adjust operating temperature in ALD deposition device, carrier gas flux and carrier gas pressure Power, wherein operating temperature are set in 25-300 DEG C, and carrier gas flux is set in 500-1000sccm, are passed through the choke valve of noble gases Aperture opening ratio can increase to 50%, the probe voltage that oxygen sensor shows is 920mV, and the curing oven in curing operation Temperature may be set in 200 DEG C, the time of solidification can bring up to 6h, during antimicrobial treatment, titanate esters, hydrochloric acid, nitre Sour silver and zinc nitrate mass ratio may be adjusted to 5%, 0.5%, 0.5% and 2.5% with this；
When embedded type alloy medical apparatus and instruments are prepared with oxidation layer operation, different from vertebra inner fixer oxidation operation , after can embedded type alloy medical apparatus and instruments be carried out with the circulation A LD deposition operation of 100-200 time, and circulation A LD deposition Need heat treatment to be carried out to embedded type alloy medical apparatus and instruments, be placed in heater, adjust temperature to 650 DEG C, heat treatment Time can be controlled in 10-15h, the oxidation of 100-200nm thickness can be obtained on the surface of embedded type alloy medical apparatus and instruments Layer, with good stability and compactness, changes adhesiveness, biocompatibility and the blood phase of original embedded type medical apparatus and instruments Capacitive, it is to avoid embedded type medical apparatus and instruments occur in the process of expansion of environment and support in vivo macromolecule drug-loaded layer come off and The phenomenon of cracking, and nondegradable macromolecular material, the impact that will also result in the technical ability of human body cause new medical care problem.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with Understanding can carry out various changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention And modification, the scope of the present invention be defined by the appended.

Claims (4)

1. a kind of energy-saving method for preparing oxide layer based on ALD technique on the medical instrument, it is characterised in that：Should be based on ALD Technology prepares the energy-saving method of oxide layer on the medical instrument and comprises the following steps that：
S1：Cleaning-drying：The medical apparatus and instruments for needing to prepare oxide layer are picked out, the dust and greasy dirt for removing surface attachment is dirty Dye thing, is cleaned and drying process in being placed into specific medical apparatus and instruments cleaning sterilizing device；
S2：Oxide is selected：Suitable oxide is selected, wherein by aluminium oxide, silicon oxide, titanium oxide, stannum oxide and Zinc Oxide Common oxide storage is standby；
S3：It is passed through gas：The fixture of suitable dimension is selected, medical apparatus and instruments are placed into into ALD working cavities after sterilization and drying In, operating temperature in ALD deposition, carrier gas flux and nebulizer gas pressure are regulated, wherein operating temperature is set in 25-300 DEG C, carries Throughput is set in 500-1000sccm, by ALD operating rooms evacuation, and is passed through noble gases and carries out cleaning operation；
Volatile halogenide ALD precursor compound steam, waiting are passed through after setting each numerical value in ALD working cavities Compound steam stable is well passed through ozone again in ALD working cavities, and while measure oxygen partial pressure with oxygen sensor, treats Reaction is passed through noble gases in terminating backward ALD working cavities, after purging cleaning is carried out to ALD operating rooms；
S4：Thickness is selected：According to S3 step repetitive operations, change the deposit thickness of medical apparatus surface with this；
S5：Curing operation：ALD operating temperatures in S3 steps are adjusted to appropriate scope, medical apparatus and instruments are taken out, room temperature Lower placement 2-4h, is then placed in curing oven, and addition helium is medium, and curing oven is heated up, and wherein temperature is set in 180- 200 DEG C, 5-6h is processed at this temperature；
S6：Antimicrobial treatment：Medical apparatus and instruments in S5 steps are taken out into cooling, mass ratio is taken and is put into for 1%-10% titanate esters and stir Mix in container, add lytic agent stirring, and add lytic agent while sequentially add mass ratio be 1%-10% hydrochloric acid, Water, silicon compound, mass ratio dispersant, the silver nitrate and mass ratio 1%- that mass ratio is 0.1%-1% for 0.1%-1% 4% zinc nitrate is sufficiently stirred for, and antibiotic paint is obtained, the medical apparatus and instruments after cooling are placed into the antibiotic paint being stirred In solution, do up and down uniformly lift operation, carry out drying operation in being then placed into drying plant, wherein drying temperature Degree is set in 30-80 DEG C, and the medical apparatus and instruments after drying are positioned in calciner, 20- is calcined at a temperature of 200-300 DEG C 50h, naturally cools to indoor temperature after taking-up, the medical apparatus and instruments with antibacterial figure layer and oxide ceramics are obtained after taking-up.
2. a kind of energy-saving method for preparing oxide layer based on ALD technique on the medical instrument according to claim 1, its It is characterised by：The probe voltage that oxygen sensor shows in step S3 is 900-950mV.
3. a kind of energy-saving method for preparing oxide layer based on ALD technique on the medical instrument according to claim 1, its It is characterised by：The noble gases being passed through in step S3 are nitrogen, and are provided with being passed through on the equipment used by nitrogen Choke valve, wherein, the aperture opening ratio of choke valve is controlled in 30%-60%.
4. a kind of energy-saving method for preparing oxide layer based on ALD technique on the medical instrument according to claim 1, its It is characterised by：Embedded type medical apparatus and instruments of the medical apparatus and instruments for metal material.
CN201611144058.9A 2016-12-13 2016-12-13 ALD technology-based energy saving method for producing oxidation layer on medical device Pending CN106581782A (en)

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Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101864562A (en) * 2010-07-07 2010-10-20 南京大学 Method for preparing oxide surface on metal medical appliance by Atomic Layer Deposition (ALD) technology
CN104194424A (en) * 2014-09-19 2014-12-10 沈阳沃鑫源商贸有限公司 Preparation method of antimicrobial coating for metal of medical equipment
WO2015107476A1 (en) * 2014-01-15 2015-07-23 Instytut Fizyki Pan Method for production of antimicrobial coating in low temperatures, and metallic material, natural or artificial, coated with metal oxide nanolayers of disinfecting action and neutral to mucous membranes

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101864562A (en) * 2010-07-07 2010-10-20 南京大学 Method for preparing oxide surface on metal medical appliance by Atomic Layer Deposition (ALD) technology
WO2015107476A1 (en) * 2014-01-15 2015-07-23 Instytut Fizyki Pan Method for production of antimicrobial coating in low temperatures, and metallic material, natural or artificial, coated with metal oxide nanolayers of disinfecting action and neutral to mucous membranes
CN104194424A (en) * 2014-09-19 2014-12-10 沈阳沃鑫源商贸有限公司 Preparation method of antimicrobial coating for metal of medical equipment

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