CN117442762A - Contamination-resistant plasma sterilization device, sterilization method and application - Google Patents
Contamination-resistant plasma sterilization device, sterilization method and application Download PDFInfo
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- CN117442762A CN117442762A CN202210840463.3A CN202210840463A CN117442762A CN 117442762 A CN117442762 A CN 117442762A CN 202210840463 A CN202210840463 A CN 202210840463A CN 117442762 A CN117442762 A CN 117442762A
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Classifications
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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
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
- A61L2/14—Plasma, i.e. ionised gases
-
- 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
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/26—Accessories or devices or components used for biocidal treatment
-
- 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
- A61L2202/00—Aspects relating to methods or apparatus for disinfecting or sterilising materials or objects
- A61L2202/20—Targets to be treated
- A61L2202/24—Medical instruments, e.g. endoscopes, catheters, sharps
Landscapes
- Health & Medical Sciences (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Apparatus For Disinfection Or Sterilisation (AREA)
Abstract
The invention provides an anti-contamination plasma sterilization device, a sterilization method and application, and belongs to the technical field of plasma sterilization. The sterilization apparatus includes: the inner wall of the sterilization chamber is provided with a heat-conducting graphite film; the heater is arranged outside the sterilizing chamber and is connected with the heat-conducting graphite film. According to the invention, the heat-conducting graphite film is arranged on the inner wall of the sterilization chamber, so that metals such as aluminum in the sterilization chamber can be prevented from being sputtered by high-speed moving particles in plasma in the sterilization process, and further, the metals are attached to the surface of an article to be sterilized to cause aluminum contamination, and hidden danger to human health and life safety is eliminated. The invention can realize a plurality of sterilization modes, and can select plasmas formed by different gases for sterilization according to different sterilization specifications.
Description
Technical Field
The invention belongs to the technical field of plasma sterilization, and particularly relates to an anti-contamination plasma sterilization device, a sterilization method and application.
Background
Common sterilization techniques in the prior art are autoclaving, ethylene oxide sterilization, radiation sterilization and plasma sterilization. For those delicate medical instruments which are afraid of moisture and heat, such as various endoscopes, medical optical fibers and the like, plasma sterilization is mainly adopted.
Plasma sterilization was studied starting in the 60 s of the 20 th century. In 1987, patent publication US4643876a disclosed for the first time the use of hydrogen peroxide vapor to generate a plasma for sterilizing articles. After several years, the us strong company developed a Starrad 100S commercial hydrogen peroxide plasma sterilizer and was approved by the FDA for marketing in 1997. In 2004, hydrogen peroxide plasma sterilization technique has entered china and is now widely used. The plasma sterilizer widely used at present is mostly a hydrogen peroxide plasma sterilizer, and the principle is based on US4643876A and series of patents.
Generally, the temperature in the sterilizing chamber needs to be maintained at 50-60 ℃ in the hydrogen peroxide plasma sterilizing period to achieve better sterilizing effect, and the water on the surface of the articles to be sterilized is fully evaporated and pumped away, so that the sterilizing chamber cavity of most of the commercial hydrogen peroxide plasma sterilizers is provided with a heater; the inner wall of a sterilizing chamber of a commercial hydrogen peroxide plasma sterilizer is mostly made of aluminum alloy materials, and the aluminum alloy has good heat conductivity, light weight and low price. However, during sterilization, the heater heats the sterilization chamber cavity so that high-speed charged particles in the plasma bombard the inner wall of the sterilization chamber cavity, sputtering out aluminum atoms on the surface of the cavity, and the free aluminum atoms can pass through the sterilization package and adhere to the surface of the sterilized medical instrument to form contamination to the medical instrument.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides an anti-contamination plasma sterilization device, a sterilization method and application, which solve the problems that the conventional plasma sterilization device can form aluminum contamination on articles to be sterilized and has hidden danger to human health and life safety.
The invention is realized by the following technical scheme:
in a first aspect of the present invention, there is provided an anti-contamination plasma sterilization apparatus comprising:
the inner wall of the sterilization chamber is provided with a heat-conducting graphite film;
the heater is arranged outside the sterilizing chamber and is connected with the heat-conducting graphite film.
The invention further improves that:
a through hole is formed in the lower portion of the side wall of the sterilization chamber, and the heat-conducting graphite film extends from the inner wall of the sterilization chamber to the outside of the through hole and is connected with the heater; preferably, the through hole has a sealing structure.
The invention further improves that:
the heat-conducting graphite film is selected from natural heat-conducting graphite flakes, artificial synthetic graphite films, nano composite graphite films, graphene films or coatings, and natural heat-conducting graphite flakes are preferred;
the thickness of the heat-conducting graphite film is 0.03-3mm, preferably 0.1-1.5mm.
The invention further improves that:
a commodity shelf is arranged in the sterilizing chamber;
the commodity shelf comprises a horizontal bracket, two ends of the horizontal bracket are respectively connected with a connecting piece, one end of each connecting piece is connected with the end part of the horizontal bracket, and the other end of each connecting piece extends upwards and outwards in an inclined mode along the end part of the horizontal bracket.
The commodity shelf is made of high-molecular polymer material, preferably at least one of polypropylene (PP), cycloolefin copolymer (COC) and cycloolefin polymer (COP). The shelf may be formed using conventional molding processes of the prior art, such as injection molding, compression molding, and the like.
The invention further improves that:
the bottom surface of the sterilization chamber is provided with a plasma coupling window, a plasma generating unit is fixed at the plasma coupling window, and the plasma generating unit is positioned below the plasma coupling window.
The invention further improves that:
the bottom of the sterilization chamber cavity is also provided with a vacuumizing system pipeline and a working gas pipeline respectively, and the vacuumizing system pipeline and the working gas pipeline are positioned at two sides of the plasma coupling window respectively;
and the pipeline of the vacuumizing system is connected with a vacuum pump.
The invention further improves that:
the top of the sterilizing chamber is provided with a hydrogen peroxide purifying system and a hydrogen peroxide injection system which are connected, and the hydrogen peroxide purifying system is communicated with the inside of the sterilizing chamber.
The invention further improves that:
the outer wall of the sterilization chamber is provided with a shell, and the shell is made of ABS, ultra-high molecular weight polyethylene, polyoxymethylene, nylon, polysulfone, polyether sulfone, polyphenylene sulfide, polyether ether ketone, polyimide, polytetrafluoroethylene, polyphenyl ether, reinforced polypropylene, reinforced nylon, reinforced polybutylene terephthalate and reinforced polyethylene terephthalate, preferably reinforced polypropylene, reinforced nylon, reinforced polybutylene terephthalate, reinforced polyethylene terephthalate, polyimide, polytetrafluoroethylene and blends thereof, preferably ABS and ultra-high molecular weight polyethylene.
In a second aspect of the invention, a plasma sterilization method is provided, and the contamination-resistant plasma sterilization device is adopted to sterilize and disinfect articles to be sterilized; preferably, the method comprises the steps of,
the sterilization method comprises the following steps:
the first sterilization method comprises the following steps: closing a working gas pipeline, opening a hydrogen peroxide injection system and a hydrogen peroxide purification system, introducing hydrogen peroxide into the cavity of the sterilization chamber, and sterilizing by adopting hydrogen peroxide plasma; or,
the second sterilization method is as follows: closing the hydrogen peroxide injection system and the hydrogen peroxide purification system, opening a working gas pipeline, introducing working gas into the cavity of the sterilization chamber, and sterilizing by adopting working gas plasmas.
The invention further improves that:
the working gas is selected from the group consisting of oxygen, nitrogen, helium, argon, chlorine, hydrogen, and mixtures thereof, preferably oxygen.
In a third aspect, the invention provides an application of the anti-contamination ion sterilization device in sterilization and disinfection.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the heat-conducting graphite film is arranged on the inner wall of the sterilization chamber, so that metals such as aluminum in the sterilization chamber can be prevented from being sputtered by high-speed moving particles in plasma in the sterilization process, and further, the metals are attached to the surface of an article to be sterilized to cause aluminum contamination, and hidden danger to human health and life safety is eliminated.
According to the invention, the inside of the sterilization chamber is respectively connected with the hydrogen peroxide injection system, the purification system and the working gas pipeline, so that a plurality of sterilization modes can be realized, and plasmas formed by different gases can be selected for sterilization according to different sterilization specifications.
Drawings
Fig. 1 is a schematic structural view of a contamination-preventive plasma sterilizing apparatus according to the present invention.
Wherein: 1. the hydrogen peroxide purifying device comprises a hydrogen peroxide injecting system, a heat conducting graphite film, 3, a shell, 4, a heater, 5, a vacuumizing system pipeline, 6, a vacuum pump, 7, a working gas pipeline, 8, a plasma generating unit, 9, a plasma coupling window, 10, a storage rack, 11 and a hydrogen peroxide purifying system.
Detailed Description
The invention is described in further detail below with reference to the attached drawing figures:
a first object of the present invention is to provide an anti-contamination plasma sterilization apparatus, as shown in fig. 1, comprising a sterilization chamber, wherein a heat conductive graphite film 2 is provided on an inner wall of the sterilization chamber, and a part of the heat conductive graphite film 2 extends to the outside of the sterilization chamber through a small hole on the sterilization chamber and is connected with a heater 4 outside the sterilization chamber, specifically, a through hole is provided at a lower part of a side wall of the sterilization chamber, and the heat conductive graphite film 2 extends from the inner wall of the sterilization chamber to the outside of the through hole and is connected with the heater 4; preferably, the through hole has a sealing structure.
The heater 4 heats the heat-conducting graphite film 2 extending out of the through hole of the side wall of the sterilization chamber, heat is transferred to the heat-conducting graphite film part of the inner wall of the sterilization chamber through the surface of the heat-conducting graphite film, and the heat-conducting graphite film of the inner wall of the sterilization chamber heats up and radiates heat into the sterilization chamber, so that the temperature in the sterilization chamber is increased, and finally, the temperature is maintained within the range of 50-60 ℃. The heater is positioned outside the sterilizing chamber and can measure and control the temperature in the sterilizing chamber.
The heater is mainly composed of a resistance wire, a circuit and a controller, wherein the resistance wire generates heat after being electrified and transmits the heat to the heat-conducting graphite film 2 in a contact mode. The controller regulates and controls the heat value generated by the resistance wire by regulating the current, so that the temperature of the heat-conducting graphite film can be regulated and controlled, and the temperature in the sterilization chamber 4 can be regulated and controlled. The power of the heater 4 is 0.1-10KW, preferably 0.5-5KW. The heater may be of a prior art product and is not described in detail herein.
The heat-conducting graphite film has high heat-conducting property, is easy to process, is used for heat dissipation management, heat dissipation of a power device in a limited area or auxiliary heat dissipation of the power device, and can be used for preparing lining materials of the inner wall of a cavity of a plasma sterilizer.
The heat-conducting graphite film, namely a high heat-conducting graphite plate (GTS) material, is a thin high heat-conducting material in the prior art. The heat-conducting graphite film has good reworkability, can be compounded or glued with other film materials such as PET and the like according to purposes, has elasticity, can be cut and punched into any shape, and can be bent for many times; the heat-conducting material is suitable for rapid heat conduction for converting a point heat source into a surface heat source, has high heat conducting property and is made of a highly oriented graphite polymer film. The heat-conducting graphite film can adopt various heat-conducting graphite films existing in the prior art, preferably at least one selected from natural heat-conducting graphite sheets, artificial synthetic graphite films, nano composite graphite films, graphene films or coatings, and preferably natural heat-conducting graphite sheets; the thickness is 0.03-3mm, preferably 0.1-1.5mm.
The device solves the problem of aluminum contamination in the prior art by arranging the heat-conducting graphite film 2 on the inner wall of the sterilization chamber, and the reason is as follows:
1. the graphite has excellent heat conduction performance, the heat resistance is 40% lower than that of aluminum and 20% lower than that of copper, and the heat conduction coefficient can reach 800-2500W/mK; the heat conductivity coefficient of the aluminum alloy 5052 commonly used for preparing the inner wall of a sterilization chamber of a plasma sterilization device is only 138W/mK, and the heat conductivity coefficients of other commonly used metals are all below 500W/mK; therefore, the heat conducting performance of the heat conducting graphite film is better than that of metal, and the constant temperature in the sterilizing chamber can be well maintained.
2. The metal bond energy of aluminum is about 321.7KJ/mol, while the metal bond energy of other common metals such as iron, chromium, nickel and copper is not more than 430KJ/mol. The carbon-carbon double bond energy in the graphite is about 611KJ/mol, so that compared with metals, the carbon-carbon double bond is more difficult to break by high-speed charged particles so as to splash carbon atoms; and one part of the sputtered carbon atoms can be combined with active oxygen in the plasma phase to generate carbon dioxide or carbon monoxide to be pumped away, and the other part of the sputtered carbon atoms reach the surface of the to-be-sterilized object, so that the to-be-sterilized object can not be damaged by human body.
As a preferred embodiment of the invention, a commodity shelf 10 is arranged in the sterilizing chamber, and at least one layer, preferably two layers, of commodity shelf 10 is arranged in the sterilizing chamber; the supporter 10 includes the horizontal bracket, and the both ends of horizontal bracket are connected with the connecting piece respectively, and the one end and the end connection of horizontal bracket of connecting piece, the other end upwards and outside slope extension along the tip of horizontal bracket, and the connecting piece can be fixed on the lateral wall in the sterilization room through the hot melt, also can be fixed through the joint with the lateral wall in sterilization room, specifically does: two opposite side walls in the sterilizing chamber are provided with clamping grooves, one end of the connecting piece, which is far away from the horizontal bracket, is provided with a buckle matched with the clamping grooves, and the buckle is matched with the clamping grooves, so that the shelf 10 is fixed in the sterilizing chamber.
The material of supporter 10 is polymer material, and characteristics are: 1. the molecular structural formula only contains C, H, O element; 2. the heat distortion temperature is higher than 100 ℃;3. chemical corrosion resistance; 4. low moisture absorption and good dimensional stability; 5. the mechanical property is good. The material of the rack 10 is selected from polypropylene (PP), cyclic Olefin Copolymer (COC), cyclic Olefin Polymer (COP). The shelf is preferably a polymer material, more preferably at least one of polypropylene (PP), cyclic Olefin Copolymer (COC), cyclic Olefin Polymer (COP). The shelf may be formed using conventional molding processes of the prior art, such as injection molding, compression molding, and the like.
As a preferred embodiment of the invention, a plasma coupling window 9 is arranged on the bottom surface of the sterilizing chamber, a plasma generating unit 8 is fixed at the plasma coupling window 9, and the plasma generating unit 8 is positioned below the plasma coupling window 9.
As shown in fig. 1, a heat conducting graphite film is also arranged at the plasma coupling window 9, the plasma coupling window 9 is not required to be communicated with a sterilizing chamber, and plasma is generated by forming an alternating electromagnetic field in the sterilizing chamber without contact.
The plasma generating unit 8 is fixed at the bottom of the sterilization chamber, and the plasma generating unit 8 adopts the prior art products, which are not described herein.
As a preferred embodiment of the invention, the bottom of the sterilization chamber cavity is also provided with a vacuumizing system pipeline 5 and a working gas pipeline 7 respectively, the vacuumizing system pipeline 5 and the working gas pipeline 7 are respectively positioned at two sides of the plasma coupling window 9, and the vacuumizing system pipeline 5 is connected with a vacuum pump 6. In the sterilization process, the vacuum pump 6 is used for vacuumizing the sterilization chamber, so that the air concentration in the sterilization chamber is reduced, and the concentration of hydrogen peroxide or working gas is increased; and, the low vacuum environment facilitates diffusion of gaseous hydrogen peroxide or working gas and formation of plasma.
If necessary, working gas can be introduced into the sterilizing chamber through the working gas pipeline 7 to enable glow discharge to generate plasma so as to replace hydrogen peroxide for sterilization.
The working gas is introduced through the working gas pipeline 7, plasma is generated during glow discharge of the working gas, and the articles are sterilized by the following sterilization principle:
(1) The high-speed charged particles in the plasma can break down and etch the cell membranes of bacteria and viruses;
(2) Part of working gas, such as oxygen, can generate active groups in the process of forming plasma, and is extremely easy to be denatured by oxidation reaction with protein and nucleic acid substances in bacteria, mold, spores and viruses, so that various microorganisms die;
(3) During the formation of the plasma, partial ultraviolet light is generated, and the high-energy ultraviolet photons are absorbed by proteins in microorganisms or viruses, so that the molecules are denatured and deactivated.
The working gas is selected from the group consisting of oxygen, nitrogen, helium, argon, chlorine, hydrogen, and mixtures thereof, preferably oxygen.
As a preferred embodiment of the present invention, the top of the sterilization chamber is provided with a hydrogen peroxide purification system 11 and a hydrogen peroxide injection system 1 which are connected, and the hydrogen peroxide purification system 11 is communicated with the inside of the sterilization chamber. Hydrogen peroxide sequentially enters the sterilizing chamber through the hydrogen peroxide injection system 1 and the hydrogen peroxide purification system 11, and before plasma is generated, gaseous hydrogen peroxide is injected into the sterilizing chamber and is diffused, and the process has sterilizing effect, but has limited effect; after the injection of hydrogen peroxide for a certain period of time, plasma is generated by the plasma generating unit 8 for sterilization, which is the main sterilization process.
The hydrogen peroxide purification system 11 and the hydrogen peroxide injection system 1 are both fixed at the top of the sterilization chamber; the hydrogen peroxide injection system 1 comprises a cartridge feeding mechanism and a cartridge puncturing system; the hydrogen peroxide decontamination system 2 includes a decontamination cooling chamber and a diffusion heating chamber.
The hydrogen peroxide injection system 1 and the hydrogen peroxide purification system 11 are both prior art products, and are not described in detail herein.
As a preferred embodiment of the invention, the outer wall of the sterilization chamber is provided with a shell 3, and the shell 3 is made of ABS (acrylonitrile-butadiene-styrene copolymer), ultra-high molecular weight polyethylene, polyoxymethylene, nylon, polysulfone, polyethersulfone, polyphenylene sulfide, polyether ether ketone, polyimide, polytetrafluoroethylene, polyphenylene oxide, reinforced polypropylene, reinforced nylon, reinforced polybutylene terephthalate, reinforced polyethylene terephthalate, preferably reinforced polypropylene, reinforced nylon, reinforced polybutylene terephthalate, reinforced polyethylene terephthalate, polyimide, polytetrafluoroethylene and blends thereof, preferably ABS and ultra-high molecular weight polyethylene. The molding method of the housing 3 employs a polymer molding process common in the art, such as injection molding, etc., including a common molding method and apparatus.
Typical settings of conditions and parameters for sterilization using the device of the invention are: the pressure in the room to be sterilized reaches 10 -6 When a specified value is within the range of 100Pa, 4-6mL of hydrogen peroxide with the concentration of 58% +/-2% or working gas with the concentration of 1-100sccm is introduced into the sterilizing chamber, the pressure of the sterilizing chamber is controlled to be a specified value within the range of 0.01-200Pa, the power of the plasma generating unit is usually set between 10W and 2000W, the temperature in the sterilizing chamber is controlled to be a set value between 25 ℃ and 60 ℃ in the sterilizing process, and the plasma treatment time is between 1 min and 60 min.
The second object of the invention is to provide a plasma sterilization method, which adopts the anti-contamination plasma sterilization device to sterilize and disinfect the articles to be sterilized.
The specific sterilization method is as follows:
when the sterilization requirement is very high, for example, the surgical instruments and the medical instruments are sterilized, the working gas connecting pipeline is closed, the hydrogen peroxide injection system and the hydrogen peroxide purification system are opened to introduce hydrogen peroxide into the sterilization chamber, and hydrogen peroxide plasma is adopted for sterilization;
when the sterilization requirement is not high, for example, common articles are sterilized, the hydrogen peroxide injection system and the hydrogen peroxide purification system are closed, the working gas pipeline is opened, working gas is introduced into the sterilization chamber, and working gas plasma is adopted for sterilization.
In the whole sterilization process, the vacuum pump 6 and the heater 4 are always in an on state, and the plasma generation unit 8 is only started in a stage of generating plasma.
The principle of sterilizing articles by using working gas plasma is as follows:
(1) The high-speed charged particles in the plasma can break down and etch the cell membranes of bacteria and viruses;
(2) Part of working gas, such as oxygen, can generate active groups in the process of forming plasma, and is extremely easy to be denatured by oxidation reaction with protein and nucleic acid substances in bacteria, mold, spores and viruses, so that various microorganisms die;
(3) During the formation of the plasma, partial ultraviolet light is generated, and the high-energy ultraviolet photons are absorbed by proteins in microorganisms or viruses, so that the molecules are denatured and deactivated.
The working gas is selected from the group consisting of oxygen, nitrogen, helium, argon, chlorine, hydrogen, and mixtures thereof, preferably oxygen.
A third object of the present invention is to provide a use of the above-mentioned anti-contamination ion sterilization apparatus for sterilization and disinfection.
The present invention is described in detail below with reference to specific embodiments, and it should be noted that the following embodiments are only for further description of the present invention and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adjustments of the present invention by those skilled in the art from the present disclosure are still within the scope of the present invention.
The heat-conducting graphite film, the rack material, the shell material and the like used in the embodiment of the invention are all commercial products.
Example 1
In the embodiment, the plasma sterilization device is adopted to sterilize the silicon wafer, wherein the heat conducting graphite film is a natural heat conducting graphite sheet (sold by the Mars company), the thickness is 0.5mm, the sterilization chamber is made of aluminum alloy 5052, the storage rack is made of polypropylene (the polypropylene raw material is sold by the China petrochemical and sea refining company, the model is H30S), and the sterilization chamber shell is made of ultra-high molecular weight polyethylene.
Closing a working gas pipeline, opening a hydrogen peroxide injection system and a hydrogen peroxide purification system, introducing hydrogen peroxide into a sterilization chamber, and sterilizing a silicon wafer by adopting hydrogen peroxide plasma, and specifically:
when the pressure in the sterilizing chamber reaches 0.01Pa, 6mL of hydrogen peroxide with the concentration of 58% is introduced into the sterilizing chamber, the pressure in the sterilizing chamber is controlled to be 80Pa, the power of the plasma generating unit is 500W, the temperature in the sterilizing chamber is controlled to be 50-55 ℃ in the sterilizing process, and the plasma treatment time is 8min.
The distribution of the concentration of aluminum element on the surface of the silicon wafer after the hydrogen peroxide plasma sterilization and the non-sterilized silicon wafer with the depth was measured by using a secondary ion mass spectrum, and the measurement results are shown in table 1. As can be seen from Table 1, the distribution of aluminum on the surface of the silicon wafer was not very different between the sterilized and non-sterilized silicon wafer, indicating that there was no contamination of aluminum during the sterilization process in this example. And the display of the sterilization indicator card shows that the sterilization is available and the sterilization is qualified.
TABLE 1
Example 2
In the embodiment, the plasma sterilization device is adopted to sterilize the silicon wafer, wherein the heat conducting graphite film is a natural heat conducting graphite sheet (sold by the American star company), the thickness is 0.5mm, the sterilization chamber is made of aluminum alloy 5052, the storage rack is made of cycloolefin copolymer (sold by the Japanese Bao Jib company, the model is Topas 6017), and the sterilization chamber shell is made of ultra-high molecular weight polyethylene.
Closing the hydrogen peroxide injection system and the hydrogen peroxide purification system, opening a working gas pipeline, introducing oxygen into a sterilizing chamber, and sterilizing the silicon wafer by adopting oxygen plasma, and specifically:
when the pressure in the sterilizing chamber reaches 0.01Pa, 10sccm of working gas (oxygen) is introduced into the sterilizing chamber, the pressure in the sterilizing chamber is controlled to be 0.1Pa, the power of the plasma generating unit is 500W, the temperature in the sterilizing chamber is controlled to be 50-55 ℃ in the sterilizing process, and the plasma treatment time is 8min.
The distribution of the concentration of aluminum element on the surface of the silicon wafer after oxygen plasma sterilization and the non-sterilized silicon wafer with the depth was measured by using a secondary ion mass spectrum, and the measurement results are shown in table 2. As can be seen from Table 2, the distribution of aluminum on the surfaces of the sterilized and unsterilized silicon wafers almost coincides, indicating that there is no contamination of aluminum during the sterilization process of this example. And the display of the sterilization indicator card shows that the sterilization is available and the sterilization is qualified.
TABLE 2
Example 3
In the embodiment, the plasma sterilization device is adopted to sterilize the silicon wafer, wherein the heat-conducting graphite film is a synthetic graphite film (sold by the Margariti company), the thickness is 0.2mm, the sterilization chamber material is aluminum alloy 5052, the storage rack material is polypropylene (the polypropylene raw material is sold by the China petrochemical and sea refining company, the model is H30S), and the sterilization chamber shell material is ultra-high molecular weight polyethylene.
Closing a working gas pipeline, opening a hydrogen peroxide injection system and a hydrogen peroxide purification system, introducing hydrogen peroxide into a sterilization chamber, and sterilizing a silicon wafer by adopting hydrogen peroxide plasma, and specifically:
when the pressure in the sterilizing chamber reaches 0.01Pa, 6mL of hydrogen peroxide with the concentration of 58% is introduced into the sterilizing chamber, the pressure in the sterilizing chamber is controlled to be 80Pa, the power of the plasma generating unit is 500W, the temperature in the sterilizing chamber is controlled to be 50-55 ℃ in the sterilizing process, and the plasma treatment time is 8min.
The distribution of the concentration of aluminum element on the surface of the silicon wafer after the hydrogen peroxide plasma sterilization and the non-sterilized silicon wafer with the depth was measured by using a secondary ion mass spectrum, and the measurement results are shown in table 3. As can be seen from Table 3, the distribution of aluminum on the surface of the silicon wafer was not very different between the sterilized and non-sterilized silicon wafer, indicating that there was no contamination of aluminum during the sterilization process in this example. And the display of the sterilization indicator card shows that the sterilization is available and the sterilization is qualified.
TABLE 3 Table 3
Example 4
In the embodiment, the plasma sterilization device is adopted to sterilize the silicon wafer, wherein the heat-conducting graphite film is a nano composite graphite film (sold by Jiangsu Xianfeng nano material technology Co., ltd.) with the thickness of 0.1mm, the sterilization chamber material is aluminum alloy 5052, the commodity shelf material is cycloolefin copolymer (sold by Japanese Bao Jib Co., model number Topas 6017), and the sterilization chamber shell material is ultra-high molecular weight polyethylene.
Closing the hydrogen peroxide injection system and the hydrogen peroxide purification system, opening a working gas pipeline, introducing nitrogen into a sterilization chamber, and sterilizing the silicon wafer by adopting nitrogen plasma, and specifically:
when the pressure in the sterilizing chamber reaches 0.01Pa, introducing 20sccm working gas (nitrogen) into the sterilizing chamber, controlling the pressure in the sterilizing chamber to be 0.1Pa, controlling the power of the plasma generating unit to be 700W, controlling the temperature in the sterilizing chamber to be 50-55 ℃ in the sterilizing process, and controlling the plasma treatment time to be 6min.
The distribution of the concentration of aluminum element on the surface of the silicon wafer after nitrogen plasma sterilization and the non-sterilized silicon wafer with the depth was measured by using a secondary ion mass spectrum, and the measurement results are shown in table 4. As can be seen from Table 4, the distribution of aluminum on the surfaces of the sterilized and unsterilized silicon wafers almost coincides, indicating that there is no contamination of aluminum during the sterilization process of this example. And the display of the sterilization indicator card shows that the sterilization is available and the sterilization is qualified.
TABLE 4 Table 4
Example 5
In the embodiment, the plasma sterilization device is adopted to sterilize and disinfect a silicon wafer, wherein a graphene film (sold by Shenzhen Dilute conductive technology Co., ltd.) is selected as a heat conducting graphite film, the thickness is 0.05mm, an aluminum alloy 5052 is selected as a sterilization chamber material, polypropylene (sold by China petrochemical Zhenhai refining Co., model H30S) is selected as a storage rack material, and ultra-high molecular weight polyethylene is selected as a sterilization chamber shell material.
Closing a working gas pipeline, opening a hydrogen peroxide injection system and a hydrogen peroxide purification system, introducing hydrogen peroxide into a sterilization chamber, and sterilizing a silicon wafer by adopting hydrogen peroxide plasma, and specifically:
when the pressure in the sterilizing chamber reaches 0.01Pa, 6mL of hydrogen peroxide with the concentration of 58% is introduced into the sterilizing chamber, the pressure in the sterilizing chamber is controlled to be 0.1Pa, the power of the plasma generating unit is 700W, the temperature in the sterilizing chamber is controlled to be 50-55 ℃ in the sterilizing process, and the plasma treatment time is 6min.
The distribution of the concentration of aluminum element on the surface of the silicon wafer after the hydrogen peroxide plasma sterilization and the non-sterilized silicon wafer with the depth was measured by using a secondary ion mass spectrum, and the measurement results are shown in table 5. As can be seen from Table 5, the distribution of aluminum on the surface of the silicon wafer was not very different between the sterilized and non-sterilized silicon wafer, indicating that there was no contamination of aluminum during the sterilization process in this example. And the display of the sterilization indicator card shows that the sterilization is available and the sterilization is qualified.
TABLE 5
Comparative example
The silicon wafer was sterilized by a commercially available hydrogen peroxide plasma sterilizer of the old Kensil LK/KS150-A1 type (the material of the inner wall of the sterilization chamber is aluminum alloy 5052, specifically:
when the pressure in the sterilizing chamber reaches 0.01Pa, hydrogen peroxide with the same dosage as in the embodiment 1 is introduced into the sterilizing chamber, the pressure in the sterilizing chamber is controlled to be 80Pa, the power of the plasma generating unit is 500W, the temperature in the sterilizing chamber is controlled to be 50-55 ℃ in the sterilizing process, and the plasma treatment time is 8min.
The distribution of the concentration of aluminum element on the surface of the sterilized silicon wafer and the non-sterilized silicon wafer with the depth was measured by using a secondary ion mass spectrum, and the measurement results are shown in table 6. Compared with the silicon wafer which is not sterilized, the aluminum concentration on the surface of the silicon wafer after sterilization is obviously increased to 8.46 multiplied by 10 at the maximum 19 /cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The concentration profiles of the two aluminum products in Table 6 were respectively plotted and integrated with respect to depth and then subtracted to calculate that the contamination amount of the aluminum introduced during the sterilization of this comparative example was 7.9X10 12 /cm 2 . And the display of the sterilization indicator card shows that the sterilization is available and the sterilization is qualified.
TABLE 6
Comparative examples 1 to 5 and comparative examples, according to the present invention, aluminum impurities are hardly introduced during the sterilization process of the contamination prevention plasma sterilization apparatus, and the problem of aluminum contamination occurring in the prior art is solved.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "connected," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the description of the present invention, unless otherwise indicated, the terms "upper," "lower," "left," "right," "inner," "outer," and the like are used for convenience in describing the present invention and simplifying the description based on the orientation or positional relationship shown in the drawings, and do not denote or imply that the devices or elements in question must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention.
The foregoing technical solution is only one embodiment of the present invention, and various modifications and variations can be easily made by those skilled in the art based on the principles disclosed in the present invention, and are not limited to the technical solutions described in the foregoing specific examples of the present invention, therefore, the foregoing description is only preferred and not in any limiting sense.
Claims (11)
1. A contamination resistant plasma sterilization apparatus, the sterilization apparatus comprising:
the inner wall of the sterilization chamber is provided with a heat-conducting graphite film;
the heater is arranged outside the sterilizing chamber and is connected with the heat-conducting graphite film.
2. The contamination prevention plasma sterilization apparatus according to claim 1, wherein a through hole is provided at a lower portion of a side wall of the sterilization chamber, and the heat conductive graphite film extends from an inner wall of the sterilization chamber to an outside of the through hole and is connected to the heater; preferably, the through hole has a sealing structure.
3. The contamination prevention plasma sterilization apparatus according to claim 1 or 2, wherein the thermally conductive graphite film is selected from natural thermally conductive graphite sheets, synthetic graphite films, nanocomposite graphite films, graphene films or coatings, preferably natural thermally conductive graphite sheets;
the thickness of the heat-conducting graphite film is 0.03-3mm, preferably 0.1-1.5mm.
4. The contamination prevention plasma sterilization apparatus according to claim 1, wherein a shelf is provided inside the sterilization chamber; preferably, the method comprises the steps of,
the storage rack comprises a horizontal bracket, two ends of the horizontal bracket are respectively connected with a connecting piece, one end of each connecting piece is connected with the end part of the horizontal bracket, and the other end of each connecting piece extends upwards and outwards in an inclined mode along the end part of the horizontal bracket; and/or;
the rack is made of high polymer material, more preferably at least one of polypropylene, cycloolefin copolymer and cycloolefin polymer.
5. The contamination prevention plasma sterilization apparatus according to claim 1, wherein a plasma coupling window is provided on a bottom surface of the sterilization chamber, a plasma generating unit is fixed at the plasma coupling window, and the plasma generating unit is located below the plasma coupling window.
6. The contamination prevention plasma sterilization apparatus according to claim 5, wherein the bottom of the sterilization chamber cavity is further provided with a vacuum system pipe and a working gas pipe, respectively, and the vacuum system pipe and the working gas pipe are located at both sides of the plasma coupling window, respectively;
and the pipeline of the vacuumizing system is connected with a vacuum pump.
7. The contamination resistant plasma sterilization apparatus according to claim 1, wherein the sterilization chamber is provided at a top thereof with a hydrogen peroxide purification system and a hydrogen peroxide injection system connected thereto, the hydrogen peroxide purification system being in communication with an interior of the sterilization chamber.
8. The contamination prevention plasma sterilization apparatus according to claim 1, wherein a housing is provided on an outer wall of the sterilization chamber, and wherein the housing is made of a material selected from the group consisting of ABS, ultra-high molecular weight polyethylene, polyoxymethylene, nylon, polysulfone, polyethersulfone, polyphenylene sulfide, polyetheretherketone, polyimide, polytetrafluoroethylene, polyphenylene oxide, reinforced polypropylene, reinforced nylon, reinforced polybutylene terephthalate, reinforced polyethylene terephthalate, preferably reinforced polypropylene, reinforced nylon, reinforced polybutylene terephthalate, reinforced polyethylene terephthalate, polyimide, polytetrafluoroethylene, and blends thereof, preferably ABS and ultra-high molecular weight polyethylene.
9. A plasma sterilization method, characterized in that the contamination prevention plasma sterilization device according to any one of claims 1 to 8 is used for sterilizing and disinfecting an article to be sterilized; preferably, the method comprises the steps of,
the sterilization method comprises the following steps:
the first sterilization method comprises the following steps: closing a working gas pipeline, opening a hydrogen peroxide injection system and a hydrogen peroxide purification system, introducing hydrogen peroxide into the cavity of the sterilization chamber, and sterilizing by adopting hydrogen peroxide plasma; or,
the second sterilization method is as follows: closing the hydrogen peroxide injection system and the hydrogen peroxide purification system, opening a working gas pipeline, introducing working gas into the cavity of the sterilization chamber, and sterilizing by adopting working gas plasmas.
10. The plasma sterilization method according to claim 9, wherein the working gas is selected from the group consisting of oxygen, nitrogen, helium, argon, chlorine, hydrogen and mixtures thereof, preferably oxygen.
11. Use of an anti-fouling ion sterilization device according to any one of claims 1-8 for sterilization.
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