CN117483162A

CN117483162A - Surface treatment equipment

Info

Publication number: CN117483162A
Application number: CN202311451338.4A
Authority: CN
Inventors: 胡浙平; 苗春光
Original assignee: Anhui Luohua Biotechnology Co ltd
Current assignee: Anhui Luohua Biotechnology Co ltd
Priority date: 2023-10-31
Filing date: 2023-10-31
Publication date: 2024-02-02

Abstract

The application discloses a surface treatment apparatus, the surface treatment apparatus includes: the device comprises a modifying treatment device (1), a strengthening modifying treatment device (2) and a conveying device (3), wherein the conveying device (3) is used for carrying a material to be subjected to surface treatment and sequentially passes through the modifying treatment device (1) and the strengthening modifying treatment device (2). The surface treatment equipment can carry out modification and strengthening modification treatment on the surface of the material, realizes automation of the whole process through the conveying device, and ensures the treatment effect of ultralow adsorption on the surface of the material.

Description

Surface treatment equipment

Technical Field

The present application relates to the field of material surface treatment, and more particularly to a surface treatment apparatus.

Background

The super-hydrophobic technology is a new technology for changing the surface property of a material, and the surface of the material treated by the technology has the important characteristics of adhesion resistance, water resistance, fog resistance, pollution prevention, self cleaning, current conduction prevention and the like, and has wider application prospect in the fields of scientific research, production, life and the like.

In the field of biology, the superhydrophobic technology can be applied to surface treatment of cell culture plates and the like. The cell culture container subjected to surface superhydrophobic treatment can realize cell suspension culture, and can also be used for suspension culture of adherent cells and semi-adherent cells, sphere culture of tumor cells and embryoid body formation experiments. The treatment process of the superhydrophobic surface often involves a plurality of condition parameters, the preparation process is complex, the treatment conditions are monitored at required time, and mass production is difficult to meet.

Therefore, providing a fully automated surface treatment apparatus is a technical problem that needs to be solved in the art.

Disclosure of Invention

In view of this, according to the present application, there is provided a surface treatment apparatus comprising: the device comprises a modifying treatment device, a strengthening modifying treatment device and a conveying device, wherein the conveying device is used for bearing a material to be subjected to surface treatment and sequentially passes through the modifying treatment device and the strengthening modifying treatment device.

Preferably, the modifying treatment apparatus includes an ion electrode for discharge-exciting a plasma, a vacuum device for maintaining a vacuum degree of the modifying treatment apparatus, and a gas supply device for supplying a plurality of working gases.

Preferably, the vacuum device includes a vacuum degree sensor installed inside the modification treatment device and a vacuum pump installed outside the modification treatment device.

Preferably, the air supply device includes: the gas source, with the air source communicate with each other and set up in the inboard gas inlet of modification processing apparatus and set up in the inboard gas sensor that is used for detecting gas of modification processing apparatus.

Preferably, the strengthening modification treatment device comprises a spraying device and a mixing device for uniformly coating the protein adsorption resistant substance.

Preferably, the spraying device comprises a solution source of an anti-protein adsorption substance and a nozzle, the nozzle is arranged in the strengthening modification treatment device, and the nozzle is connected with a pressurizing pump arranged outside the strengthening modification treatment device through the pipeline.

Preferably, the outlet of the pressurizing pump is provided with a pressure sensor for monitoring the output pressure of the pressurizing pump.

Preferably, the mixing device comprises a plurality of mixed flow fans and a plurality of concentration sensors for detecting the concentration of the droplets of the protein adsorption resistant substance solution in the strengthening modification treatment device.

Preferably, the strengthening modification treatment device comprises a soaking device for uniformly coating the protein adsorption resistant substance.

Preferably, the strengthening modification treatment device further comprises a drying device for drying the surface treatment material.

Preferably, the drying device includes a heating part and a temperature sensor.

Preferably, both ends of the modification treatment device and the strengthening modification treatment device are respectively provided with a cabin section airtight door which is switched between open and airtight.

The surface treatment equipment can carry out modification and strengthening modification treatment on the surface of the material, realizes automation of the whole process through the conveying device, and ensures the effect of material surface treatment.

Additional features and advantages of the present application will be set forth in the detailed description which follows.

Drawings

The accompanying drawings, which are included to provide a further understanding of the application, illustrate embodiments of the application and together with the description serve to explain the application. In the drawings:

FIG. 1 is a simplified flow chart of a method of modifying a surface of a material of the present application.

FIG. 2 is a flow chart of a method of modifying a surface of a material of the present application.

FIG. 3 is a flow chart of a method of modifying a surface of a material according to one embodiment of the present application.

Fig. 4 is a schematic front view of a surface treatment apparatus according to a preferred embodiment of the present application.

Fig. 5 is a schematic side view of an inlet of a surface treatment apparatus according to a preferred embodiment of the present application.

FIG. 6 shows the ultra low adsorption effect of the cell culture plates or dishes of the examples and comparative examples of the present application.

FIG. 7 shows the ultra-low adsorption effect of the cell culture plates or dishes of the examples and comparative examples of the present application after 60d and 180d treatments.

FIG. 8 shows the cell suspension culture effect of the cell culture plates of the examples of the present application.

FIG. 9 shows the cell suspension culture effect of the cell culture plate of the comparative example of the present application.

Description of the numbering in the drawings: 1-a modification treatment device; 2-strengthening modification treatment device; 3-a conveyor belt; 4-ion electrode; 5-a vacuum sensor; 6-a vacuum pump; 7-a gas sensor; 8-nozzles; 9-a pipeline; 10-a booster pump; 11-a pressure sensor; 12-mixed flow fans; 13-a concentration sensor; 14-an electric heating tube; 15-a temperature sensor; 16-a closed door; 17-inlet; 18-outlet; 19-gas inlet; 20-a viewing window; 21-a touch display screen; 22-buttons and indicator lights; 23-alarm lamp; 24-feeding cabin section; 25-material trays.

Detailed Description

The technical solutions of the present application will be described in detail below with reference to the accompanying drawings in combination with embodiments.

1. Material surface modification method

In one aspect of the present application, a method for modifying a surface of a material is provided, comprising: s1, carrying out ultralow adsorption modification treatment on the surface of a material, wherein the material surface treatment method further comprises the following steps: s2, performing strengthening modification treatment on the surface subjected to the ultralow adsorption modification treatment.

Conventionally, the surface ultra-low adsorption modification method is to perform preliminary modification treatment on the surface of a material, so that the surface of the material has the characteristic of ultra-low adhesion in a short period, but the ultra-low adsorption surface has the problem of short maintenance time. Therefore, the application creatively provides a material surface modification method which carries out modification and strengthening modification treatment on the material surface so as to ensure that the material surface has the characteristic of ultralow adsorption for a long time and prevent the modified material from losing the characteristic of ultralow adsorption due to long-time unused.

In the technical scheme of the application, the surface of the material can be modified in a proper mode and is matched with the strengthening modification treatment in a proper mode.

According to a preferred embodiment of the present application, step S1 may include: s11, carrying out plasma cleaning on the surface of the material to be treated so as to open chemical bonds on the surface of the material. In this case, step S11 may be performed in a suitable manner to achieve the effect of cleaning the surface of the material and opening the surface chemical bonds. Specifically, the step S11 may include: plasma cleaning is performed on the surface of the material to be treated in a first gas atmosphere, preferably an inert gas (such as helium, neon, argon, helium, krypton, xenon and radon), preferably argon.

More specifically, according to an operational exemplary embodiment, the step S11 may include: placing the material to be treated into a plasma cleaning machine, vacuumizing to 10Pa, introducing argon with the flow of 200SCCM and the air pressure of 200Pa, and circulating for three times to fill the working cavity with argon; then, the air pressure is reduced to 50Pa, argon is continuously introduced, the air flow is 100SCCM, the air pressure is 100Pa, the discharge power is 500W, and the cleaning time is 10min, so that chemical bonds on the surface of the material are opened.

According to a preferred embodiment of the present application, step S1 may include: s12, carrying out material surface grafting treatment on the surface of the cleaned material. Step S12 may be performed in a suitable manner to achieve the surface grafting effect. Specifically, the step S12 may include: the material to be treated is subjected to plasma discharge cleaning under a second gas atmosphere, preferably the second gas is a fluorine-containing gas (such as trifluoromethane, difluoroethane, octafluorocyclobutane and carbon tetrafluoride), preferably the second gas is carbon tetrafluoride.

More specifically, according to one operational exemplary embodiment, the step S12 may include: introducing carbon tetrafluoride into the plasma cleaner for three times circularly, wherein the flow rate of the gas is 500SCCM, and the air pressure is 180Pa; then reducing the air pressure to 30Pa, continuously introducing carbon tetrafluoride, wherein the air flow is 240SCCM, the air pressure is 300Pa, the discharge power is 600W, and the pressure maintaining and cleaning time is 20min, so as to carry out grafting treatment on the surface of the material.

Step S12 may also be performed in a suitable manner to achieve a stable surface grafting effect. Specifically, according to an operational exemplary embodiment, the step S12 may further include: after the plasma discharge cleaning, the pressure is kept unchanged under a third gas atmosphere, preferably, the third gas is an inert gas, and more preferably, the third gas is nitrogen. Preferably, the pressure is maintained in the third gas atmosphere for at least 10 minutes, preferably at least 20 minutes, more preferably at least 30 minutes, still more preferably 30 to 60 minutes, and still more preferably 30 to 40 minutes.

In the technical scheme of the application, the method is provided with reinforcing modification treatment measures besides the modification treatment by cleaning the surface of the material and opening the surface chemical bonds. Specifically, the step S2 may include: and placing the surface subjected to the ultralow adsorption modification treatment in the solution atmosphere of the protein adsorption resistant substance, so that the modified surface is uniformly coated with the protein adsorption resistant substance. The above-mentioned so-called "in atmosphere" can be achieved in a number of ways, in order to be able to achieve a uniform coating of the material surface, for example: the solution of the protein adsorption resistant substance can be sprayed on the surface subjected to the ultralow adsorption modification treatment; or directly soaking the surface subjected to the ultralow adsorption modification treatment in a solution of the protein adsorption resistant substance.

The conditions for the treatment of the 2-methacryloyloxyethyl phosphorylcholine polymer may be selected according to the desired prolonged use aging. Preferably, the treatment time may be 3h to 12h, preferably 5h to 12h, and more preferably 6h to 8h.

The protein adsorption resistant substance solution may be of a suitable type. For example, the protein adsorption resistant substance solution can be a 2-methacryloyloxyethyl phosphorylcholine polymer solution, and the concentration of the 2-methacryloyloxyethyl phosphorylcholine polymer is as follows: 0.05mol/L to 0.2mol/L, preferably 0.1mol/L to 0.15mol/L, and more preferably 0.125mol/L.

The 2-methacryloyloxyethyl phosphorylcholine polymer is polymerized by 2-methacryloyloxyethyl phosphorylcholine and a hydrophobic substance, and the hydrophobic substance may be n-butyl methacrylate or n-hexyl methacrylate. The hydrophobic substance in the present application is preferably n-hexyl methacrylate, and the polymer formed by free radical polymerization of 2-methacryloyloxyethyl phosphorylcholine and n-hexyl methacrylate has the characteristics of being hydrophilic at one end and hydrophobic at the other end.

Principle of binding protein adsorption-resistant substance to material surface: the modified material has opened chemical bond, grafted fluoride-containing functional group, formed C-F bond on the material surface to fluoride the material surface, so that the material surface has super-hydrophobic low adhesion characteristic, and the 2-methyl acryloyloxyethyl phosphorylcholine polymer is similar to phospholipid molecule on the cell membrane surface and has hydrophobic part combined with the hydrophobic part of the material surface to make the fluorinated surface hard to restore after the initial modification treatment, so as to maintain the super-low adhesion characteristic of the material surface.

In order to enable the protein adsorption resistant substance solution to be coated on the surface of the material more uniformly, in particular, after the polymer solution is processed at the constant temperature, the temperature is 60-80 ℃ and the time is 4-5 h.

2. Surface treatment equipment

As shown in fig. 4 and 5, the present application proposes a surface treatment apparatus including: a modifying device 1, a strengthening modifying device 2 and a conveying device 3, wherein the conveying device 3 is used for carrying a material to be subjected to surface treatment and sequentially passes through the modifying device 1 and the strengthening modifying device 2.

The transporting device 3 may transport the material to be processed into the cabins of the modifying device 1 and the reinforcing modifying device 2, and perform modifying and reinforcing modifying treatment on the surface of the material, and the transporting device may be a suitable type, for example, a drum type transporting device, a plate chain transporting device, a mesh belt transporting device, and a chain transporting device, and is preferably a belt type transporting device. The belt conveyor surface is more steady, and the transportation material is safer. In order to meet the internal sectional treatment requirements of the modification treatment device 1 and the strengthening modification treatment device 2, the transportation device is arranged in a sectional manner and can be divided into 1-5 sections, preferably 4 sections, which are respectively positioned at an inlet 17, the modification treatment device 1, the strengthening modification treatment device 2 and an outlet 18 of the surface treatment equipment.

The surface treatment equipment realizes the whole-flow surface treatment of modification and strengthening modification, omits a complicated transfer flow, and avoids the condition of secondary pollution on the surface of the material in the transfer process.

The above-mentioned modifying treatment apparatus may perform vacuum plasma treatment on a material to be treated, and in particular, the modifying treatment apparatus 1 may include an ion electrode 4 for discharge-excited plasma, a vacuum apparatus for maintaining the vacuum degree of the modifying treatment apparatus 1, and a gas supply apparatus for supplying a plurality of working gases. The ion electrode 4 includes positive and negative electrodes, and can excite the gas charged into the interior of the modification treatment apparatus 1 to convert into plasma.

In order to optimize the vacuum degree of the modifying apparatus 1 and to optimize the modifying effect, the vacuum apparatus may include a vacuum degree sensor 5 mounted inside the modifying apparatus 1 and a vacuum pump 6 mounted outside the modifying apparatus 1.

To provide a plasma-exciting gas, in particular, the gas arrangement may comprise: the device comprises a gas source, a gas inlet which is communicated with the gas source and is arranged at the inner side of the modification treatment device 1, and a gas sensor 7 which is arranged at the inner side of the modification treatment device 1 and used for detecting gas. The gas source is arranged outside the surface treatment equipment and is communicated with the gas inlets 19 through pipelines, the number of the gas inlets 19 can be set according to the needs, for example, 3 gas inlets are arranged, gas required in the modification treatment process enters the modification treatment device 1 from different gas inlets respectively, the gas inlets are provided with automatic valves, and when the gas is introduced, the automatic valves are opened, and the gas enters the modification treatment device 1. The gas sensor 7 can monitor the gas concentration atmosphere in the reforming treatment device at any time. The vacuum degree of the modification treatment device 1 is reduced to make the distance between gas molecules and the movement distance of molecules or ions longer and longer, and when the ion electrode works, the gas molecules or ions collide with each other to form plasma. The plasma can open chemical bonds on the surface of the material to be treated, and combine with free radicals to form polar groups on the surface of the material. In order to observe the operation of the modification apparatus 1 during plasma discharge, an observation window 20 is provided outside the modification apparatus 1.

When the modification apparatus 1 is operated, electrons are present in a plasma state, and neutral atoms, molecules and radicals are in an activated state, and ionized atoms and molecules and unreacted atoms and molecules are present. Ions and free radicals excited by the discharge can physically and chemically react with organic pollutants and impurities on the surface of the material to be treated to form volatile substances, so that the aim of cleaning the surface of the material is fulfilled. The inert gas (argon) can etch the surface of the material in a plasma state to form reaction sites on the surface of the material, the fluorine-containing gas (carbon tetrafluoride) can form a hydrophobic film on the surface of the material in the plasma state, and finally, inert gas nitrogen is introduced to stabilize the surface treatment effect.

In order to achieve a uniform distribution of the polymer to be coated on the surface of the material, the reinforcing modification treatment device 2 may preferably include a spraying device and a mixing device for uniformly coating the protein adsorption resistant substance.

In order to fill the interior of the modification treatment apparatus with the polymer solution, the spraying apparatus may preferably include a solution source of an anti-protein adsorption substance, a plurality of nozzles 8 installed inside the reinforcement modification treatment apparatus 2, and the nozzles 8 are connected to a pressurizing pump 10 installed outside the reinforcement modification treatment apparatus 2 through the pipe 9. The nozzle 8 can enable the protein adsorption resistant substance solution to be subjected to pressure action, so that the polymer solution is atomized, the pressure pump 10 can be a variable-frequency pressure pump, and is connected with a protein adsorption resistant substance solution source arranged outside the surface treatment equipment, so that the protein adsorption resistant substance solution forms micron-sized (20-50 um) particle size spray, and uniform coating of the protein adsorption resistant substance solution on the surface of a material to be treated is ensured.

Preferably, the outlet of the booster pump 10 is provided with a pressure sensor 11 for monitoring the output pressure of the booster pump 10.

In order to ensure uniform distribution of polymer solution particles in the modification treatment apparatus, the mixing apparatus may preferably include a plurality of mixed-flow fans 12 and a plurality of concentration sensors 13 for detecting the concentration of the protein adsorption-resistant substance solution in the reinforcing modification treatment apparatus 2, the mixed-flow fans 12 may be installed at appropriate positions, and preferably, the mixed-flow fans 12 are installed around the nozzles 8, and the concentration sensors may be disposed at appropriate positions, for example, may be arranged in a staggered manner in the modification treatment apparatus in order to accurately monitor the concentration of polymer particles in different positions of the reinforcing modification treatment apparatus. The concentration sensor 13 is used to monitor the concentration of atomized particles of the protein adsorption-resistant substance solution in the strengthening modification treatment apparatus 2.

When the strengthening modification treatment device works, the concentration sensor 13 is started, the atomization concentration of the polymer solution in the cabin is monitored in real time, the pressure sensor 11 monitors the output pressure of the pressurizing pump 10, the concentration sensors 13 transmit collected data to the control unit at the same time, the MCU timely calculates the average particle concentration value, and the control unit adjusts the output pressure of the pressurizing pump 10 in real time according to the value to control the particle size range of the atomized particles. Simultaneously, the rotating speed of the mixed flow fan is regulated, and the concentration uniformity of the particulate matters is controlled; so as to maintain the particle size range and uniformity of the atomization concentration of the particulate matter at the set values of the process requirements.

In order to achieve uniform distribution of the polymer to be coated on the surface of the material, the modification treatment device can comprise a soaking device for uniformly coating the protein adsorption resistant substance, and the material to be treated is soaked in the solution of the protein adsorption resistant substance, so that the surface of the material can be uniformly coated.

In order to uniformly coat the polymer solution on the surface of the material, specifically, the reinforcing modification treatment apparatus 2 further includes a drying apparatus for drying the surface-treated material. The drying device includes a heating part 14 and a temperature sensor 15. The temperature in the device can be raised to the required temperature, the treatment temperature in the cabin can be monitored at any time, and the heating part 14 can adjust the working state at any time. The heating portion 14 may be in a suitable form, and may be, for example, a heating wire, preferably an electric heating tube.

In order to ensure a closed environment in the cabin and to ensure the working environment required for the modification treatment and the strengthening modification treatment, specifically, both ends of the modification treatment device 1 and the strengthening modification treatment device 2 are respectively provided with cabin closed doors 16 which are switched between open and closed.

For convenience of setting the condition parameters in the modifying treatment apparatus 1 and the strengthening modifying treatment apparatus 2, the feeding compartment section 24 of the surface treatment apparatus is further provided with a control device, and the control device is a display screen 21 and a button 22 mounted outside the compartment. The display screen 21 may be a common display screen, preferably a touch display screen, and in use, various parameters are conveniently set. In order to monitor the internal operation of the device, an indicator light is also provided inside or beside the button 22, which indicates that this step of the process is being performed when the indicator light corresponding to a certain parameter is on.

In order to ensure the normal operation of the ultra-low adsorption treatment equipment in the use process, the ultra-low adsorption treatment equipment is also provided with an alarm lamp 23, and the alarm lamp 23 is started to remind workers when the equipment fails or the required substances and gases are insufficient in the operation process.

The method and procedure for surface modification of materials using the surface treatment apparatus of the present application are shown in the examples below.

1. Examples of methods for modifying surfaces of materials

Example 1

The embodiment provides a material surface modification method, which comprises the following steps:

A1. placing a cell culture plate or a cell culture dish made of polystyrene or PETG to be treated into an automatic ultralow adsorption treatment device, vacuumizing to about 10Pa, introducing argon, stopping air inflow at the flow of 200SCCM and the air pressure of 200Pa, circulating for three times, repeatedly introducing argon, discharging mixed gas through vacuumizing, and filling the plasma cleaner with argon.

A2. And (3) reducing the air pressure in the plasma cleaning machine to 50Pa, continuously introducing argon, enabling the flow to be 100SCCM, enabling the air pressure to be 100Pa, starting discharge (the discharge power is 500W) to clean for 10min, performing plasma cleaning on the surface of the cell culture plate or the culture dish in an argon atmosphere, removing surface pollutants, and opening surface chemical bonds.

A3. Introducing carbon tetrafluoride gas into the plasma cleaner at 500SCCM and air pressure of 180Pa, and repeating the steps for three times to graft the surface of the cell culture plate or culture dish in carbon tetrafluoride atmosphere to reach the surface modification effect of ultralow adsorption.

A4. The air pressure in the plasma cleaning machine is reduced to 30Pa, carbon tetrafluoride gas is continuously introduced until the air pressure is 300Pa, discharge (the discharge power is 600W) is started, the pressure is maintained and the cleaning is carried out for 20min, and further grafting treatment is carried out on the surface of a cell culture plate or a culture dish in the carbon tetrafluoride atmosphere.

A5. Stopping discharging, introducing nitrogen, maintaining the pressure for 40min, taking out, stabilizing the effect of ultralow adsorption modification on the surface of the cell culture plate or the culture dish, and preventing gases such as oxygen from contacting the surface of the cell culture plate or the culture dish after vacuum breaking, thereby reducing the surface grafting efficiency.

A6. And (3) putting the product into deionized water, ultrasonically cleaning for 15min, drying in an oven at 60 ℃, taking out, and cleaning the surface of a cell culture plate or a culture dish.

A7. Preparing a polymer solution, polymerizing 2-methacryloyloxyethyl phosphorylcholine (Shanghai microphone Biotechnology Co., ltd., 96%) and n-hexyl methacrylate (Shanghai microphone Biotechnology Co., ltd., 98%) to form a 2-methacryloyloxyethyl phosphorylcholine polymer, and adding the 2-methacryloyloxyethyl phosphorylcholine polymer into an ethanol solution (Shanghai microphone Biotechnology Co., ltd.) with a volume fraction of 75% to prepare a mixed solution with a concentration of 0.2mol/L.

A8. The product was placed in a polymer solution atmosphere for 12h.

A9. Placing in an incubator at 80 ℃ for 4 hours, taking out, and uniformly coating the surface of a cell culture plate or a culture dish with the polymer coating.

Example 2

The material surface modification method of example 1 was employed, wherein:

A5. the dwell time is 35min;

A7. the concentration of the polymer solution is 0.125mol/L;

A8. the treatment time of the polymer solution was 8.5h.

A9. The constant temperature treatment temperature is 70 ℃ and the time is 4.5h.

Example 3

The material surface modification method of example 1 was employed, wherein:

A5. the dwell time is 30min;

A7. the concentration of the polymer solution is 0.05mol/L;

A8. the treatment time of the polymer solution was 5h.

A9. The constant temperature treatment temperature is 60 ℃ and the time is 5 hours.

Example 4

The material surface modification method of example 1 was employed, wherein:

A5. the dwell time is 60min;

A7. the concentration of the polymer solution is 0.15mol/L;

A8. the treatment time of the polymer solution was 3 hours.

Example 5

The material surface modification method of example 1 was employed, wherein:

A5. the dwell time is 20min;

A7. the concentration of the polymer solution is 0.1mol/L;

A8. the treatment time of the polymer solution was 6 hours.

A9. The constant temperature treatment temperature is 70 ℃ and the time is 4 hours.

Example 6

The material surface modification method of example 1 was used, excluding A9.

Example 7

The material surface modification method of example 2 was used, excluding A9.

Example 8

The material surface modification method of example 5 was used, excluding A9.

Example 9

The material surface modification method of example 3 was used, excluding A7 and A8.

Example 10

The material surface modification method of example 4 was used, excluding A7 and A8.

Example 11

The material surface modification method of example 5 was used, excluding A7 and A8.

Comparative example 1

The material surface modification method of example 1 was used, wherein steps A7, A8 and A9 were not included.

Comparative example 2

The surface of the material is not modified and strengthened.

2. Test method

2.1 method for detecting ultra-low adsorption on surface of material

Ultra-low adsorption refers to the property of a solid surface that has ultra-hydrophobicity for droplets and low adsorptivity for cells and proteins.

The contact angle is the included angle theta between the tangent line of the gas-liquid interface and the solid-liquid interface, which is made at the intersection point of the gas phase, the liquid phase and the solid phase. The ability of a solid surface to be wetted by a liquid is known as wettability, and the contact angle θ is one of the key indicators used to evaluate the wettability of a solid surface. For a cell culture plate or dish, a higher contact angle indicates a stronger hydrophobicity and a lower adhesion of the protein or cell to the solid surface. The solid surface with contact angle greater than 150 deg. is an ultra-low adsorption surface.

The hydrophobicity of the material surface was measured using a contact angle measuring instrument (FCA 500P, shanghai Ai Feisai precision instruments limited) as follows:

1. the cell culture plate or the bottom plate of the culture dish after the surface treatment is individually cut off by a cutter.

2. The well bottom plate sample was placed on a contact angle measuring instrument, 2 microliters of deionized water was sucked up, randomly dropped on the measurement surface, and contact angle measurement was performed using the optical imaging principle.

3. Randomly selecting 5 points on the surface to be measured, measuring the contact angle, and taking an average value.

2.2 method for testing cell culture vessel treated by surface modification method of Material

In the application, liver cancer cells are selected as test objects, and a 6-pore plate treated by a material surface modification method is taken as an example, wherein the inoculation density is 1-10 ³ Individual cells/well, placed at 37℃in 5% CO ₂ Is cultured in a cell culture box, and the cell states are observed under a mirror after 24 hours and 48 hours of inoculation respectively.

3. Experimental results

3.1 evaluation of the Effect of ultra-Low adsorption on the Material surface

The ultra-low adsorption effect of the cell culture plates or petri dishes of examples 1-11 and comparative examples 1 and 2 was tested by contact angle measurement as shown in FIG. 6. As can be seen from FIG. 6, the liquid contact angles of the surfaces of the cell culture plates or the cell culture dishes of examples 1 to 5 (the surfaces of the materials were subjected to the modification and strengthening modification treatment) and examples 6 to 8 (the surfaces of the materials were not subjected to the constant temperature treatment after the immersion in the 2-methacryloyloxyethyl phosphorylcholine solution) were each greater than 150℃and the liquid contact angles of the surfaces of the cell culture plates or the cell culture dishes of examples 9 to 11 (the surfaces of the materials were subjected to the constant temperature treatment only and the surfaces of the materials were not subjected to the strengthening modification treatment) were about 150℃and the liquid contact angles of the surfaces of the cell culture plates or the cell culture dishes of examples 1 to 11 and comparative example 1 were far greater than the surfaces of the cell culture plates or the cell culture dishes of comparative example 2 (the surfaces were not subjected to the surface modification and strengthening modification treatment). Therefore, the surface of the cell culture plate or the culture dish subjected to the modification treatment has an excellent ultralow adsorption effect, and the cell culture plate or the culture dish subjected to the material surface modification method has a relatively good ultralow adsorption effect.

3.2 evaluation of the Effect of maintaining ultra Low adsorption on the Material surface for a long time

FIG. 7 shows the ultra-low adsorption effect of examples 1-11 and comparative examples 1 and 2 of the present application after 1d, 60d and 180d of treatment. As can be seen from fig. 7, with the extension of the standing time, the cell culture plates or dishes of examples 6 to 8 (without constant temperature treatment after immersing in the 2-methacryloyloxyethyl phosphorylcholine solution) had a liquid contact angle of less than 150 ° after 60d treatment and a liquid contact angle of less than 120 ° after 180d treatment; examples 9-11 (with only constant temperature treatment, without 2-methacryloyloxyethyl phosphorylcholine solution immersion) cell culture plates or dishes had liquid contact angles decayed to around 120 ° after 60d treatment and to below 100 ° after 180d treatment; the liquid contact angle of the surface of the cell culture plate or the culture dish of comparative example 1 (without strengthening modification treatment) was remarkably reduced, the liquid contact angle was attenuated to about 110 ° after treatment for 60d, the contact angle was not remarkably different from the contact angle of the surface of the cell culture plate or the culture dish of comparative example 2 (without surface modification treatment) after treatment for 180d, the contact angle was already attenuated to less than 90 °, and the liquid contact angle of the cell culture plate or the culture dish of examples 1 to 5 (with material surface modification and strengthening modification treatment) was still greater than 150 ° after treatment for 180 d. Therefore, the time for maintaining the ultralow adsorption characteristic of the surface of the modified material can be prolonged by soaking the 2-methacryloyloxyethyl phosphorylcholine solution and then performing constant temperature treatment, so that the cell culture plate or the culture dish prepared by the material surface modification method has a good ultralow adsorption effect after being treated for a period of time.

3.3 evaluation of the Effect of culturing suspension cells in an ultra Low adsorption cell culture vessel

FIG. 8 shows cell morphology of liver cancer cells cultured in cell culture plates treated by the material surface modification method of example 1 for 0h,24h and 48h, and FIG. 9 shows cell morphology of liver cancer cells cultured in cell culture plates not treated by the material surface modification method of comparative example 2 for 0h,24h and 48 h. As can be seen from FIG. 8, after the inoculation of liver cancer cells, the cells were aggregated into spheres after 24h and 48h culture, and were not grown by adherence, whereas the liver cancer cells cultured in comparative example 2 in FIG. 9 were grown by adherence after 24h culture, and a large number of cells were adhered after 48h culture. Therefore, the cell culture vessel prepared by the material surface modification method has good ultralow adsorption characteristic.

In summary, by carrying out plasma modification treatment on the surface of the material and uniformly coating 2-methacryloyloxyethyl phosphorylcholine polymer on the modified surface of the material, the ultra-low adsorption characteristic of the surface of the material is obtained, and meanwhile, the time for maintaining the ultra-low adsorption characteristic of the surface of the material is prolonged.

The ultra-low adsorption surface treatment equipment provided by the application can be used for finishing material surface modification treatment (modification and strengthening modification treatment), realizing full-flow automatic production, and saving complex and difficult-to-control process flows and transfer flows; and through the arrangement of a series of sensors, the condition parameter precision and automation of the material surface modification treatment method are realized.

Materials that the ultra-low adsorption treatment apparatus and material surface modification methods of the present application may be suitable for include, but are not limited to, polymeric organic materials and glasses, such as: polystyrene, PETG, glass, etc., are not limited by the shape of the article being treated, and may be, for example, cell culture plates, cell culture dishes, cell culture flasks, gun tips, and pipettes.

When the modified material is a glass surface, the evaporated silicone oil is added in the carbon tetrafluoride grafting treatment step.

The preferred embodiments of the present application have been described in detail above, but the present application is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solutions of the present application within the scope of the technical concept of the present application, and all the simple modifications belong to the protection scope of the present application.

In addition, the specific features described in the foregoing embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described in detail.

Moreover, any combination of the various embodiments of the present application may be made without departing from the spirit of the present application, which should also be considered as the disclosure of the present invention.

Claims

1. A surface treatment apparatus, characterized in that the surface treatment apparatus comprises:

the surface treatment device comprises a modification treatment device (1), a strengthening modification treatment device (2) and a conveying device (3), wherein the conveying device (3) is used for carrying a material to be subjected to surface treatment and sequentially passes through the modification treatment device (1) and the strengthening modification treatment device (2).

2. The surface treatment apparatus according to claim 1, wherein the modifying treatment device (1) comprises an ion electrode (4) for discharge-excited plasma, a vacuum device for maintaining the vacuum degree of the modifying treatment device (1), and a gas supply device for supplying a plurality of working gases.

3. The surface treatment apparatus according to claim 2, characterized in that the vacuum device comprises a vacuum degree sensor (5) mounted inside the modifying treatment device (1) and a vacuum pump (6) mounted outside the modifying treatment device (1).

4. A surface treatment apparatus according to claim 2, wherein the air supply means comprises: the gas source, the gas inlet which is communicated with the gas source and is arranged at the inner side of the modification treatment device (1) and the gas sensor (7) which is arranged at the inner side of the modification treatment device (1) and used for detecting gas.

5. The surface treatment apparatus according to claim 1, wherein the strengthening modification treatment device (2) comprises a spraying device and a mixing device for uniformly coating the protein adsorption resistant substance.

6. The surface treatment apparatus according to claim 5, wherein the spraying device comprises a solution source of an anti-protein adsorption substance, a plurality of nozzles (8) installed inside the strengthening modification treatment device (2), and the nozzles (8) are connected with a pressurizing pump (10) installed outside the strengthening modification treatment device (2) through the pipeline (9).

7. A surface treatment apparatus according to claim 6, characterized in that the outlet of the pressurizing pump (10) is provided with a pressure sensor (11) for monitoring the output pressure of the pressurizing pump (10).

8. The surface treatment apparatus according to claim 5, wherein the mixing device comprises a plurality of mixed-flow fans (12) and a plurality of concentration sensors (13) for detecting the concentration of the droplets of the protein adsorption-resistant substance solution inside the strengthening modification treatment device (2).

9. Surface treatment apparatus according to claim 1, characterized in that the strengthening modification treatment means (2) comprises soaking means for a uniform coating of the protein adsorption resistant substance.

10. The surface treatment apparatus according to claim 5, wherein the strengthening modification treatment device (2) further comprises a drying device for drying the surface treatment material.

11. Surface treatment apparatus according to claim 10, characterized in that the drying means comprise a heating section (14) and a temperature sensor (15).

12. Surface treatment device according to claim 1, characterized in that both ends of the modifying treatment means (1) and the strengthening modifying treatment means (2) are provided with compartment closing doors (16) switching between open and closed, respectively.